Illinois River (Peoria Area)

Pecatonica River Total Maximum Daily Load and Load Reduction Strategies

Stage 2 Report

1021 North Grand Avenue East P.O. Box 19276 Springfield, Illinois 62794-9276

Report Prepared by:

Tetra Tech 413 Wacouta Street, Suite 435 Saint Paul, MN 55101 and Tetra Tech EMI 1 South Wacker Drive Chicago, IL 60606

October 2, 2015

Pecatonica River Stage 2 Report October 2, 2015

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Contents

1. Introduction .................................................................................................................................... 1

2. Data Collection and Monitoring .................................................................................................... 3 2.1 Monitoring Locations ................................................................................................................... 3 2.2 Approach ...................................................................................................................................... 6

2.2.1 Surface Water ..................................................................................................................... 6 2.2.2 Groundwater ....................................................................................................................... 7

2.3 Deviations from Monitoring Plan ................................................................................................. 7

3. Data Results ................................................................................................................................... 7

4. Ammonia Source Assessment ................................................................................................... 10

5. Conclusions and Recommendations for Stage 3 ..................................................................... 11

Appendix A. Quality Assurance Project Plan......................................................................................... 12

Appendix B. Lab Reports ......................................................................................................................... 13


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Figures

Figure 1-1. Watershed locations ................................................................................................................... 2 Figure 2-1. Winneshiek Creek sampling sites............................................................................................... 4 Figure 2-2. Spring Branch sampling sites ..................................................................................................... 5

Tables

Table 2-1. Monitoring site locations ............................................................................................................. 3 Table 2-2. Monitoring sites and dates of data collection .............................................................................. 6 Table 3-1. Sample Results from Winneshiek Creek ..................................................................................... 8 Table 3-2. Sample Results from Spring Branch ........................................................................................... 8 Table 3-3. Field Measurements from Winneshiek Creek ............................................................................. 9 Table 3-4. Field Measurements from Spring Branch .................................................................................... 9 Table 3-5. Field Observations from Spring Branch .................................................................................... 10


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1. Introduction

This report documents the monitoring and assessment completed for Stage 2 of the Pecatonica River

watershed total maximum daily load (TMDL) and load reduction strategies (LRS) study. The monitoring

included field data collection and laboratory assessment of water quality parameters in the Winneshiek

Creek watershed and Spring Branch watershed (Figure 1-1). Stage 2 monitoring, along with the existing

monitoring data presented and assessed in the Stage 1 report, will support the development of TMDLs

and LRSs in the Pecatonica River watershed.


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Figure 1-1. Watershed locations


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2. Data Collection and Monitoring

2.1 Monitoring Locations

Surface samples were collected from one site in the Winneshiek Creek watershed (Figure 2-1) and three

sites in the Spring Branch watershed (Figure 2-2). Monitoring was completed in accordance with the

Quality Assurance Project Plan (QAPP) “Water Quality Sampling for Total Maximum Daily Loads for

Pecatonica River Watershed, Winneshiek Creek and Spring Branch” (Appendix A). Locations of all

monitoring sites were measured with a handheld GPS device with sub-meter accuracy (Table 2-1).

Tetra Tech made an in-field adjustment to the location of sampling point SB-01 during the December

2014 sampling event. Upon arriving to the site, Tetra Tech determined that there were no accessible roads

within approximately 1 mile of the location chosen for SB-01 in the approved QAPP. Tetra Tech’s field

team consulted with project management, and selected a new location for SB-01 that was closer to an

accessible road, while remaining downstream of most observable discharges to Spring Branch. The

updated location of SB-01 was collected with a sub-meter accuracy handheld GPS device, which was

used in subsequent sampling events to ensure consistency in sampling locations. See Figure 2-2 and Table

2-1 for a depiction of the updated location of SB-01.

Table 2-1. Monitoring site locations

Water Body

IEPA Station Code

Sampling Site

Latitude* Longitude* Description

Winneshiek Creek

(PWL-01)

PWL-01

WC-01 42.306203 -89.514405

Approximately 215 feet upstream of Fawver Road and 1.3 river miles upstream of confluence with Pecatonica River

Spring Branch (PWNC)

PWNC-01 SB-01 42.242854 -89.795896 Approximately 2,500 feet upstream from the confluence with Yellow Creek

PWNC-03 SB-02 42.238077 -89.828829

375 feet upstream of Spring Branch split on the southern tributary (split occurs approximately 930 feet along the creek upstream from the bridge crossing at IL-73)

PWNCA-

01 SB-03 42.238921 -89.829000

240 feet upstream of Spring Branch split on the northern tributary (split occurs approximately 930 feet along the creek upstream from the bridge crossing at IL-73)

PWNC-02 SB-04 42.242022 -89.803758 At the edge of Spring Branch on the downstream side of the Loran Road Bridge

*Latitude and longitude are reported using North American Datum of 1983 (NAD83)


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Figure 2-1. Winneshiek Creek sampling sites


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Figure 2-2. Spring Branch sampling sites


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2.2 Approach

At the sampling site on Winneshiek Creek, field measurements were made for the following water quality

parameters: temperature, dissolved oxygen (DO), pH, and conductivity (Table 2-2). Flow information

including depth, velocity, and stream geometry were also measured. Water samples were collected for

laboratory analysis for concentrations of total phosphorus (TP) and total suspended solids (TSS).

At each sampling site along Spring Branch, field measurements were made for the following water

quality parameters: temperature, DO, pH, and conductivity. Flow information including depth, velocity,

and stream geometry was also measured. Water samples were collected for laboratory analysis for

concentrations of total Kjeldahl nitrogen (TKN), total ammonia (T-ammonia), and total nitrite (NO2) plus

nitrate (NO3). Only the sample collected at the most downstream sampling location (SB-01) was analyzed

for total phosphorus. Field samples were collected in the streams between 0 and 1 foot below the water

surface. Water samples were preserved with sulfuric acid when appropriate, stored on ice, and delivered

to the laboratory, STAT, for filtration and analysis.

Table 2-2. Monitoring sites and dates of data collection

DO – Dissolved oxygen T-ammonia – Total ammonia TP – Total phosphorus NO2 + NO3 – nitrite plus nitrate-nitrogen TSS – Total suspended solids TKN – Total Kjeldahl nitrogen

2.2.1 Surface Water

Stream sampling procedures occurred at the center of the stream and followed SOP No. 009, Section 2.1,

“Surface Water Sampling by Submerging Sample Container” (see Appendix A). Stream samples were

collected from 0 and 1 foot below the water surface. A composite sample was collected of water from the

left bank, right bank, and center of the stream.

Stream measurement procedures were conducted in a standardized fashion. Velocity measurements were

taken at multiple points along the cross-section of the stream, at a depth of 0.6 multiplied by total depth.

Stream geometry measurements were collected at all significant geometric features, and were measured

using the water surface as a reference elevation. The samples and measurements were collected on

December 11, 2014; March 24, 2015; and April 17, 2015.

In Spring Branch, channel substrate, percent cloud cover, percent shading, and coarse streamside

vegetative summary were observed at the surface to help evaluate the streambed material composition.

Stream shading observations were recorded at each specific sampling location, and general observations

on stream shading were made while traveling between sampling locations. Percent shading was

determined through field observations, and confirmed by taking a photo of the stream and estimating the

amount of shade on the water.

Water Body (Segment)

Sampling Site

Matrix Field Parameters Laboratory Parameter

Monitoring Dates

Winneshiek Creek (PWL-01)

WC-01 Water Temperature, DO, pH, conductivity,

flow TP, TSS

12/11/2014, 3/24/2015, 4/17/2015


SB-01 SB-02 SB-03

Water Temperature, pH, conductivity, DO,

flow

TKN, T-ammonia, Total NO2 + NO3, TP (TP at SB-01 only)

12/11/2014, 3/24/2015, 4/17/2015


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2.2.2 Groundwater

Tetra Tech attempted to collect a groundwater sample from sampling location SB-04 within the Spring

Branch watershed during two sampling events. During the first sampling event (December 11, 2014),

Tetra Tech attempted to install a temporary piezometer at sampling location SB-04. Specifically, Tetra

Tech used a hand auger to create a boring to a depth of approximately 3 feet below ground surface (bgs).

This boring was located adjacent to Spring Branch, and reached a depth of approximately 2 feet below the

water surface of Spring Branch. Tetra Tech installed a 1-inch diameter PVC piezometer, screened at the

bottom foot (2–3 feet bgs), and installed sand around the boring to promote flow and filtration of

groundwater. After completing this installation, Tetra Tech attempted to allow water to collect in the

piezometer, but this process was hindered by slow recharge rates. Tetra Tech attempted to allow the

piezometer to recharge with groundwater for approximately one hour, with no significant accumulation of

water. Tetra Tech utilized a hand auger to create an additional boring adjacent to the temporary

piezometer to observe the soil profile. This boring was completed to a depth of approximately 5 feet bgs.

Tetra Tech encountered topsoil from approximately 0 – 2 feet bgs, and a dense clay layer from 2 – 5 feet

bgs. Due to the slow piezometer recharge rate and observation of clay to 5 feet bgs, this groundwater

sampling attempt was abandoned.

During the second sampling event (March 24, 2015), Tetra Tech again attempted to install a temporary

piezometer at sampling location SB-04. On this occasion, Tetra Tech used a 2-inch diameter steel

piezometer screen, a total of 3.5 feet in length and screened along the entire length. Tetra Tech installed

this piezometer screen to a depth of approximately 3 feet bgs at a location immediately adjacent to Spring

Branch. Tetra Tech attempted to allow the piezometer to recharge with groundwater, allowing

approximately 1.25 hours of recharge time with no accumulation of groundwater. Due to this slow

recharge rate, this groundwater sampling attempt was abandoned.

During the third sampling event (April 17, 2015), Tetra Tech did not observe any seeps or springs in the

Spring Branch watershed. Tetra Tech did not attempt to install a temporary piezometer during the third

sampling event, due to the slow recharge rates and preponderance of clay observed in the subsurface

during previous sampling events.

2.3 Deviations from Monitoring Plan

See Section 2.2 for a discussion of deviation from the approved monitoring plan due to difficulty

collecting groundwater samples. The location of sample SB-01 was also adjusted in the field based on

field conditions. Specifically, the location for SB-01 depicted in the monitoring plan was not reasonably

accessible (over 1 mile from any parking location). The location of SB-01 was adjusted as needed, and

the new location for SB-01 was determined.

3. Data Results

All samples collected for laboratory analysis were analyzed by STAT Analysis of Chicago, Illinois.

Analytical results were provided in Level II data packages, consisting of a basic laboratory report and an

electronic data deliverable (EDD) format spreadsheet. Tetra Tech performed Level II data validation of

all analytical results. The data validation report is provided in Appendix B.

Surface water samples collected at sampling location WC-01 in the Winneshiek Creek watershed were

analyzed for total suspended solids and total phosphorus. The results of these analyses are presented

below in Table 3-1.


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Table 3-1. Sample Results from Winneshiek Creek

Sample Number Date Collected

Total Suspended Solids (mg/L)

Phosphorus (mg/L)

WC-01 12/11/2014 < 7.5 K 0.10

WC-01-FD 12/11/2014 < 7.5 K NA

WC-01 3/24/2015 10 0.17

WC-01 4/17/2015 < 7.5 K 0.41

WC-01-FD 4/17/2015 < 7.5 K NA Notes: FD “FD” appended to Sample Number indicates that the specified sample is a field duplicate sample K The reported result is greater than the actual concentration of the analyte in the sample. The

reported result is the minimum practical quantitation limit of the analysis NA Not analyzed

All sample results may be used, as qualified, for any purposes.

Surface water samples were collected at sampling locations SB-01, SB-02, and SB-03 in the Spring

Branch watershed. Samples collected at SB-02 and SB-03 were analyzed for total ammonia, nitrate-

nitrite, and TKN. Samples collected at SB-01 were analyzed for total ammonia, nitrate-nitrite, TKN, and

total phosphorus. The results of these analyses are presented below in Table 3-2.

Table 3-2. Sample Results from Spring Branch

Sample Number Date Collected

Nitrogen, Ammonia (mg/L)

Nitrogen, Nitrate-Nitrite (mg/L)

Total Kjedlahl Nitrogen (mg/L)

Phosphorus (mg/L)

SB-01 12/11/2014 0.12 11 < 1.0 K,S 0.16

SB-01-FD 12/11/2014 0.10 10 < 1.0 K,S 0.63

SB-02 12/11/2014 0.071 9.5 < 1.0 K,S NA

SB-03 12/11/2014 0.10 14 < 1.0 K,S NA

SB-01 3/24/2015 0.15 11 < 1.0 K,S 0.12

SB-02 3/24/2015 0.17 9.6 1.0 S NA

SB-03 3/24/2015 0.26 12 < 1.0 K,S NA

SB-01 4/17/2015 0.25 9.3 < 1.0 K,S 0.078

SB-01-FD 4/17/2015 0.14 9.2 < 1.0 K,S 0.19

SB-02 4/17/2015 0.21 8.7 < 1.0 K,S NA

SB-03 4/17/2015 0.25 13 < 1.0 K,S NA Notes: FD “FD” appended to sample number indicates that the specified sample is a field duplicate sample. K The reported result is greater than the actual concentration of the analyte in the sample. The

reported result is the minimum practical quantitation limit of the analysis. NA Sample not analyzed for specified analytical parameter.

S The reported result was generated by a laboratory other than the one that reported the result. The reporting laboratory assures the validity of the reported result and its corresponding qualifiers.

All sample results may be used, as qualified, for any purposes.


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Tetra Tech also performed field monitoring in accordance with the approved monitoring plan. At each

sampling location, Tetra Tech used a Horiba U-10 Water Quality Checker to collect water quality data

including temperature, conductivity, dissolved oxygen, and pH. The flow rates at each surface water

sampling location in Winneshiek Creek and Spring Branch were calculated using flow velocities and

stream geometry measured in the field. Specifically, each stream cross section was broken down into

relevant geometrical areas based on the locations at which flow velocity was measured with a Flowwatch

flow velocity meter. The flow rates were then calculated using Riemann sums by multiplying the cross

sectional area of each geometrical area by the flow velocity measured in that area. The results of these

flow calculations and the field measurements discussed above are presented in Table 3-3 and Table 3-4.

Table 3-3. Field Measurements from Winneshiek Creek

Sample Number

Date Collected

Temperature (oC)

Conductivity (ms/cm)

Dissolved Oxygen (mg/L)

pH Flow Rate (ft3/s)

WC-01 12/11/2014 2.17 0.407 15.97 8.07 10.01

WC-01 3/24/2015 2.34 0.443 27.64 7.55 4.50

WC-01 4/17/2015 9.43 0.519 11.64 8.02 10.15

Table 3-4. Field Measurements from Spring Branch

Sample Number

Date Collected

Temperature (oC)

Conductivity (ms/cm)

Dissolved Oxygen (mg/L)

pH Flow Rate (ft3/s)

SB-01 12/11/2014 2.53 0.416 17.37 8.25 2.28

SB-02 12/11/2014 2.79 0.41 17.4 8.25 1.01

SB-03 12/11/2014 3.32 0.458 17.63 8.38 0.66

SB-01 3/24/2015 6.18 0.494 22.08 8.1 4.63

SB-02 3/24/2015 4.15 0.446 26.37 8.03 2.54

SB-03 3/24/2015 6.63 0.54 25.6 8.25 2.06

SB-01 4/17/2015 11.69 0.531 16.18 8.44 2.32

SB-02 4/17/2015 9.23 0.494 14.8 8.35 1.08

SB-03 4/17/2015 10.56 0.564 17.32 8.59 1.18

In addition to water quality measurements, field observations were recorded for the Spring Branch

watershed. These observations included percent cloud cover, percent shading, general vegetation, and

channel substrate. Vegetation identification efforts were limited by the timing of the sampling events

outside of the growing season. Where possible, Tetra Tech recorded observations both for the exact

sampling location, and for the general vicinity of the sampling location. The results of these field

observations are presented in Table 3-5.


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Table 3-5. Field Observations from Spring Branch

Sample Number

Date & Time Collected

Cloud Cover

Shading Vegetation Substrate

SB-01 12/11/2014 13:56

0% 100% at SB-01 40% throughout Spring Branch near SB-01

Hay, fescue, unidentified shrubs, unidentified trees unidentified grasses

Fine silt, some organic matter

SB-02 12/11/2014 11:28


Goldenrod (Solidago spp); fescue/ unidentified grasses, maple trees

Fine silt with decomposing organic matter, with fine gravel beneath

SB-03 12/11/2014 12:15


Hay, fescue, unidentified grasses

Fine gravel in riffles with fine silt and clay throughout

SB-01 3/24/2015 13:33

10% 10% at SB-01

Fescue, shrubs, unidentified trees, unidentified grasses

Silty-sand mixture. Significant bank erosion

SB-02 3/24/2015 11:30


Goldenrod (Solidago spp), fescue, maple trees, unidentified grasses

Silt with medium sized gravel. Bank erosion significant

SB-03 3/24/2015 11:58


Fescue, goldenrod (Solidago spp), unidentified grasses

Gravel, silt, gray clay. Bank erosion significant

SB-01 4/17/2015 11:15

30% 5% at SB-01 Unidentified grasses, fescue, unidentified trees

Silt with trace fine gravel. Bank erosion significant

SB-02 4/17/2015 09:58


Goldenrod (Solidago spp), fescue, maple trees

Silt with fine gravel. Bank erosion significant

SB-03 4/17/2015 10:20


Grass, fescue Clay, coarse gravel, silt. Bank erosion significant

4. Ammonia Source Assessment

Tetra Tech performed field reconnaissance in an attempt to determine potential sources of ammonia in the

Spring Branch watershed. This reconnaissance was performed through general observations during each

sampling event, with a focus on the ammonia source assessment during the March 2015 sampling event.


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The primary potential source of ammonia observed during field reconnaissance was the agricultural fields

that dominate land use in the watershed. During the December 2014 field event, Tetra Tech observed

manure being spread in an agricultural field located near sampling locations SB-02 and SB-03. Tetra Tech

did not observe any notable evidence of cattle use or access to Spring Branch. Tetra Tech did observe

apparent livestock farming operations in the watershed. The waste management practices of these

facilities are not known, but these operations could act as ammonia sources if waste is not controlled

appropriately. Tetra Tech also observed drain tiles from agricultural fields draining into Spring Branch

between sampling locations SB-02 and SB-01, including one drain tile located in the immediate vicinity

of SB-04.

5. Conclusions and Recommendations for Stage 3

Additional data collection was recommended in the Pecatonica River Total Maximum Daily Load

(TMDL) and Load Reduction Strategy (LRS) Stage 1 report. The additional data were necessary to

confirm impairments in Winneshiek Creek and Spring Branch and to support TMDLs and LRSs.

Winneshiek Creek

Winneshiek Creek is listed as impaired for sedimentation/siltation, total suspended solids, and

phosphorus. Monitoring data collected during 2014 and 2015 as part of this Stage 2 study show

concentrations of total suspended solids well below the water quality target of 40 mg/L. Sampling took

place during high and mid-range flow conditions in the creek. The data indicate that there is not a

sedimentation/siltation or total suspended solids impairment.

Phosphorus in the creek was found to be higher than the water quality target (0.156 mg/L), and therefore

phosphorus impairment has been verified and a LRS should be developed.

Recommendations:

Consider delisting this stream for sedimentation/siltation and total suspended solids; no TSS LRS

should be included in the Stage 3 report.

Include a total phosphorus LRS in the Stage 3 report.

Spring Branch

Spring Branch is listed as impaired for total ammonia and total phosphorus. Data collected during 2014

and 2015 as part of this Stage 2 study show concentrations of total ammonia well below the acute water

quality standard and TMDL endpoint of 15 mg/L. A source assessment conducted in the field and through

the use of aerial photos also did not identify any significant or continuous potential sources of ammonia in

the watershed. The data indicate that there is not an ammonia impairment, however there is likely

insufficient data to support delisting at this time. The samples were not collected during the critical

condition for ammonia in a stream, which would typically occur during low flow, hot summer months.

Phosphorus in the stream was found to be higher than the water quality target, and therefore phosphorus

impairment has been verified and a LRS should be developed.

Recommendations:

Consider collecting additional samples during critical conditions (low flow, warm temperatures)

to support delisting this stream for total ammonia; no total ammonia TMDL should be included in

the Stage 3 report.

Include a total phosphorus LRS in the Stage 3 report.


Appendix A. Quality Assurance Project Plan

WATER QUALITY SAMPLING FOR TOTAL MAXIMUN DAILY LOADS FOR PECATONICAWATERSHED,

WINNESHIEK CREEK AND SPRING BRANCH

QUALITY ASSURANCE PROJECT PLANDocument Control Number 408, Revision 0

(valid through December 2015)

Prepared for

ILLINOIS ENVIRONMENTAL PROTECTION AGENCYBUREAU OF WATER

1021 North Grand Avenue EastSpringfield, Illinois 62794-9276

Contract FWN 13304

Date Prepared : December 1, 2014Prepared By : Tetra Tech, Inc.Tetra Tech Project Manager : Andrea PlevanTelephone No. : (612) 354-2224IEPA Work Assignment Manager : Abel HaileTelephone No. : (217) 782-9143

Water Quality Sampling Quality Assurance Project Plan QAPP 408, Revision 0for TMDLs for Pecatonica Watershed, Winneshiek Creek and Spring Branch Date: December 1, 2014

Page ii of vii

Stage 2 – Water Quality Sampling

CONTENTSSection Page

TITLE AND APPROVAL SHEET ...............................................................................................................I

ACRONYMS AND ABBREVIATIONS .................................................................................................... V

DISTRIBUTION LIST ............................................................................................................................. VII

INTRODUCTION ........................................................................................................................................ 1

1.0 PROJECT MANAGEMENT........................................................................................................... 1

1.1 PROJECT/TASK ORGANIZATION................................................................................. 3

1.2 PROBLEM DEFINITION AND BACKGROUND ........................................................... 5

1.3 PROJECT/TASK DESCRIPTION ..................................................................................... 5

1.4 DATA QUALITY OBJECTIVES AND CRITERIA FOR MEASUREMENT DATA... 11

1.4.1 Data Quality Objectives....................................................................................... 11

1.4.2 Measurement Quality Objectives......................................................................... 11

1.4.2.1 Sensitivity ............................................................................................ 13

1.4.2.2 Accuracy.............................................................................................. 16

1.4.2.3 Precision .............................................................................................. 17

1.4.2.4 Completeness....................................................................................... 18

1.4.2.5 Representativeness .............................................................................. 18

1.4.2.6 Comparability ...................................................................................... 19

1.5 SPECIAL TRAINING CERTIFICATION AND REQUIREMENTS ............................. 19

1.6 DOCUMENTATION AND RECORDS .......................................................................... 19

1.6.1 Field Operation Records ...................................................................................... 20

1.6.2 Laboratory Records.............................................................................................. 22

1.6.3 Data Handling Records........................................................................................ 22

2.0 DATA GENERATION AND ACQUISITION ............................................................................. 23

2.1 SAMPLING PROCESS DESIGN .................................................................................... 23

2.2 SAMPLING METHODS REQUIREMENTS.................................................................. 24

2.3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS ....................................... 27

2.3.1 Field Logbooks .................................................................................................... 27

2.3.2 Field Sampling Records....................................................................................... 28

2.3.3 Sample Labels...................................................................................................... 28

2.3.4 Sample Designation ............................................................................................. 29

2.3.5 Chain-of-Custody Record .................................................................................... 29

2.3.6 Sample Packaging................................................................................................ 32

2.4 ANALYTICAL METHODS REQUIREMENTS............................................................. 32

2.5 QUALITY CONTROL REQUIREMENTS ..................................................................... 33

2.5.1 Field Quality Control Requirements.................................................................... 33

2.5.2 Laboratory Quality Control Requirements .......................................................... 34

2.5.2.1 Laboratory Control Samples................................................................ 34

2.5.2.2 Matrix Spike and Matrix Spike Duplicates ......................................... 34

2.5.3 Laboratory Quality Control Procedures............................................................... 35


Page iii of vii


CONTENTS

Section Page

2.6 INSTRUMENT AND EQUIPMENT TESTING, INSPECTION, AND MAINTENANCEREQUIREMENTS............................................................................................................ 35

2.6.1 General Requirements.......................................................................................... 35

2.6.2 Field Equipment and Instruments ........................................................................ 36

2.6.3 Laboratory Instruments........................................................................................ 36

2.7 INSTRUMENT CALIBRATION AND FREQUENCY .................................................. 36

2.7.1 Calibration of Field Instruments .......................................................................... 37

2.7.2 Calibration of Laboratory Equipment.................................................................. 38

2.8 REQUIREMENTS FOR INSPECTION AND ACCEPTANCE OF SUPPLIES ANDCONSUMABLES............................................................................................................. 39

2.9 NON-DIRECT MEASUREMENTS ................................................................................ 40

2.10 DATA MANAGEMENT ................................................................................................. 40

3.0 ASSESSMENT AND OVERSIGHT............................................................................................. 42

3.1 ASSESSMENT AND RESPONSE ACTIONS ................................................................ 42

3.1.1 Field Assessments................................................................................................ 42

3.1.2 Laboratory Assessments ...................................................................................... 42

3.1.3 Field Corrective Action Procedures..................................................................... 43

3.1.4 Laboratory Corrective Action Procedures ........................................................... 43

3.2 REPORTS TO MANAGEMENT..................................................................................... 44

4.0 DATA VALIDATION AND USABILITY................................................................................... 45

4.1 DATA REVIEW, Verification, and validation................................................................. 45

4.2 Verification AND ValidATION METHODS................................................................... 45

4.2.1 Data Validation Responsibilities.......................................................................... 46

4.2.2 Data Validation Procedures ................................................................................. 46

4.3 RECONCILIATION WITH DATA QUALITY OBJECTIVES ...................................... 46

REFERENCES ........................................................................................................................................... 48

Attachment

A STAT QUALITY ASSURANCE MANUAL AND SOPs

B INSTRUMENT INSTRUCTION MANUALS AND SOPs


Page iv of vii


TABLES

Table Page

1 KEY PROJECT PERSONNEL AND RESPONSIBILITIES.......................................................... 3

2 KEY PROJECT PERSONNEL CONTACT INFORMATION....................................................... 4

3 SUMMARY OF WATER QUALITY SAMPLING REQUIREMENTS........................................ 7

4 SAMPLING SITE DESCRIPTIONS .............................................................................................. 8

5 PROJECT DATA QUALITY OBJECTIVES ............................................................................... 12

6 SUMMARY OF MMCs, MMOs, MDLs AND RLs ..................................................................... 15

7 PERSONNEL QUALIFICATIONS .............................................................................................. 21

8 REQUIRED SAMPLE VOLUMES, ANALYTICAL METHODS, CONTAINERS,PRESERVATION TECHNIQUES, AND HOLDING TIMES..................................................... 26

9 FIELD QUALITY CONTROL SAMPLES................................................................................... 33

FIGURES

Figure Page

1 WATERSHED LOCATIONS ......................................................................................................... 2

2 TEAM ORGANIZATIONAL CHART........................................................................................... 4

3 WINNESHIEK SAMPLING SITES ............................................................................................... 9

4 SPRING BRANCH SAMPLING SITES....................................................................................... 10

5 EXAMPLE SAMPLE LABEL ...................................................................................................... 29

6 EXAMPLE CHAIN-OF-CUSTODY FORM ................................................................................ 31


Page v of vii


ACRONYMS AND ABBREVIATIONS

BMP Best management practiceBOW Bureau of Water

CFR Code of Federal RegulationsCWA Clean Water Act

DO Dissolved oxygenDQO Data quality objective

GIS Geographic Information SystemGPS Global positioning system

IEPA Illinois Environmental Protection Agency

LCS Laboratory control sampleLCSD Laboratory control sample duplicate

MDL Method detection limitmg/L Milligrams per LitermL Milliliter

MMC Minimum Measurement CriteriaMMO Minimum Measurement ObjectiveMS Matrix spikeMSD Matrix spike duplicate

NH3 AmmoniaNO2 NitriteNO3 NitrateNWIS National Water Information System

PM Project manager

QA Quality assuranceQAPP Quality assurance project planQC Quality controlQCO Quality control officer

RL Reporting limitRPD Relative percent difference

SOP Standard operating procedureSM Standard methodSQL Sample quantitation limitSTART Superfund Technical Assessment and Response TeamSTAT STAT Analytical Corporation

T-ammonia Total ammoniaTDS Total dissolved solidsTetra Tech Tetra Tech Inc.


Page vi of vii


TKN Total Kjeldahl nitrogenTMDL Total maximum daily loadTP Total phosphorusTS Total solidsTSS Total suspended solids

USDA U.S. Department of AgricultureUSEPA U.S. Environmental Protection AgencyUSGS U.S. Geological Survey

WAM Work assignment manager

WQ Water quality


Page vii of vii


DISTRIBUTION LIST

Illinois Environnemental Protection Agency

Name: Abel HaileTitle: Illinois Environmental Protection Agency Bureau of Water

Work Assignment Manager

Name: Michelle RouseyTitle: Illinois Environmental Protection Agency Bureau of Water

Quality Assurance Officer

Tetra Tech, Inc.

Name: Andrea PlevanTitle: Tetra Tech, Inc., Project Manager

Name: John O’DonnellTitle: Tetra Tech, Inc., Quality Assurance Officer

Name: John Dirgo, Ph.D.Title: Tetra Tech, Inc., Quality Control Officer

Name: Adam PetercaTitle: Tetra Tech, Inc., Field Team Leader

STAT Analysis Corporation

Name: Jason KornfeindTitle: STAT Analysis Corporation Project Manager

Name: Tom BauerTitle: STAT Analysis Corporation Laboratory Manager – Quality Assurance Officer

Water Quality Sampling Quality Assurance Project Plan for QAPP 408, Revision 0TMDLs for Pecatonica Watershed, Winneshiek Creek and Spring Branch Date: December 1, 2014

Page 1 of 48


INTRODUCTION

This quality assurance project plan (QAPP) has been prepared for the Illinois Environmental Protection

Agency (IEPA) for surface water quality data collection in Pecatonica watershed, including the

Winneshiek Creek and Spring Branch (see Figure 1). This QAPP was prepared by Tetra Tech, Inc. (Tetra

Tech), along with laboratory subcontractor STAT Analysis Corporation (STAT). STAT’s laboratory

capabilities for all project analytical requirements were evaluated on the basis of its quality management

system documentation (summarized in Attachment A), its geographic presence within Illinois, and its past

performance on similar and related projects.

Data will be collected to support the development of a total maximum daily load (TMDL) report for the

watershed and target water bodies identified therein (see Figure 1). This document describes the quality

control (QC) and quality assurance (QA) procedures to be used to ensure that the data generated during

field activities are accurate, complete, and representative of actual field conditions. All personnel working

on the project are required to read and comply with the procedures defined in this document to ensure the

quality and usability of the data. Field data collection and analysis will be conducted under the

responsibility of Tetra Tech.

This QAPP presents the project data quality objectives (DQO) developed through the U.S. Environmental

Protection Agency’s (USEPA) seven-step DQO process (USEPA 2006) and covers all 24 QAPP elements

required by QA/R-5 (USEPA 2001). Specifically, Section 1.0 discusses project management, Section 2.0

explains data generation and acquisition, Section 3.0 describes assessment and oversight actions, and

Section 4.0 discusses data validation and usability. Attachment A provides STAT’s specific analytical

methods and the QA manual. Attachment B includes standard operating procedures (SOP) that will be

followed during sample collection and instrument instruction manuals for field equipment.

1.0 PROJECT MANAGEMENT

This section discusses the project/task organization, the problem definition and background, the

project/task description, DQOs and criteria for measurement data, special training certification and

requirements, and documentation and records.


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FIGURE 1WATERSHED LOCATIONS


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1.1 PROJECT/TASK ORGANIZATION

Table 1 below summarizes the names, titles, and responsibilities of the multidisciplinary team of

technically qualified professionals who will staff this project. This team includes staff from the IEPA,

Tetra Tech, and STAT. Table 2 provides contact information for the team. Figure 2 presents a team

organizational chart and identifies project roles.

TABLE 1KEY PROJECT PERSONNEL AND RESPONSIBILITIES

Name Title and ResponsibilitiesIEPAAbel Haile BOW Work Assignment Manager (WAM) – The IEPA WAM will monitor

Tetra Tech’s performance and provide direction to the Tetra Tech projectmanager.

Michelle Rousey QA Officer – The IEPA QA officer will review and approve the QAPPdeveloped in support of this data collection effort, support the IEPA WAM in theassessment of contractor performance and in the development of technicaldirection, and participate in any audits conducted during the course of this datacollection effort. No audits are currently planned or scheduled for this project.

Tetra TechAndrea Plevan Project Manager (PM) – The project manager will coordinate project activities,

staffing, and budgets, and maintain responsibility for project QA. She willcoordinate with IEPA, oversee all field activities, and coordinate with the TetraTech sampling team leader and STAT project manager. She will also providewritten and verbal progress reports to the IEPA WAM.

John O’Donnell QA Officer – The QA Officer will assist the Project Manager in the oversight ofQAPP development, and will review and approve the final plan. Also responsiblefor consulting with the PM with respect to QA requirements and implementation,and for assisting with oversight of any significant corrective action investigationor implementation.

John Dirgo QC Officer – The QC Officer is responsible for implementing the QAPP withthe field and laboratory technical teams. The QC Officer will monitor QCactivities to determine conformance with the QAPP and review the QAPP forcompleteness and consistency. He will also be responsible for performing orverifying data validation and assessment processes.

Adam Peterca Field Team Leader – The sampling field team leader will be responsible forretrieving samples from each watershed and delivering them to the STATlaboratory and will oversee sampling activities.

Cordell Renner Field Sampling Technician – The assigned field sampling technician will assistwith collection of samples, temporary chilling and storing of sample containersprior to submittal for analysis, and coordination with the analytical laboratory.

STATJason Kornfeind Project Manager – The QA officer and project manager will oversee STAT

laboratory analytical activities. He will also coordinate data review, validation,and auditing requirements, and will review all work products for technical qualityand consistency.

Tom Bauer QA Officer/Laboratory Manager - The QA officer will ensure that the QA/QCprocedures described in this QAPP are implemented for STAT sample analysesand STAT laboratory report preparation.


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TABLE 2KEY PROJECT PERSONNEL CONTACT INFORMATION

Name Title Organization EmailPhone

Number

Abel Haile Work Assignment Manager IEPA [email protected] 217-782-3362

Michelle Rousey Quality Assurance Officer IEPA [email protected] 217-785-3944

Andrea Plevan Project Manager Tetra Tech [email protected] 612-354-2224

John O’Donnell Quality Assurance Officer Tetra Tech john.o'[email protected] 703-385-6000

John Dirgo Quality Control Officer Tetra Tech [email protected] 312-201-7765

Adam Peterca Field Team Leader Tetra Tech [email protected] 312- 201-7768

Cordell Renner Field Sampling Technician Tetra Tech [email protected] 312-201-7759

Jason KornfeindProject Manager

STATAnalysis [email protected] 312-733-0551

Tom BauerQuality Assurance

Officer/Laboratory ManagerSTAT

Analysis [email protected] 312-733-0551

FIGURE 2TEAM ORGANIZATIONAL CHART


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1.2 PROBLEM DEFINITION AND BACKGROUND

Section 303(d) of the Clean Water Act (CWA) and USEPA’s Water Quality Planning and Management

Regulations (Title 40 of the Code of Federal Regulations [CFR] Part 130) require states to identify water

bodies that do not meet water quality standards and to determine TMDLs for pollutants causing the

impairment. A TMDL is the total amount of pollutant load that a water body can receive and still meet the

water quality standards. It is the sum of the individual waste load allocations for point sources, load

allocations for nonpoint sources, and natural background loads with a margin of safety.

Under Section 303(d) of the CWA, IEPA has identified two segments within the Pecatonica watershed

identified in Section 1.1 as being impaired:

Winneshiek Creek (PWL-01)


Figure 1 shows the locations of these listed segments in the watersheds. The segments have been placed

on the 303(d) list, which includes water bodies that are not meeting the State of Illinois water quality

standards.

IEPA has adopted the following three-stage approach for TMDL development:

Stage 1 – Watershed characterization, data analysis, and methodology selection

Stage 2 – Water quality sampling to fill data gaps identified during Stage 1

Stage 3 – Development of model, TMDL scenarios, and implementation plan

Tetra Tech has completed the Stage 1 report, for all of the segments, which has been reviewed by IEPA

(Tetra Tech 2014). Based on the Stage 1 report, IEPA has determined that additional data collection is

needed. IEPA has contracted Tetra Tech to conduct Stage 2 water quality sampling to support TMDL

development for the listed segments. This plan was developed to address the Stage 2 water quality

sampling.

1.3 PROJECT/TASK DESCRIPTION

The goal of the project is to collect water quality data at specific locations within each impaired segment

of the watershed for the purposes of TMDL development. The project includes the following tasks:


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1. Prepare a QAPP for the data collection activities.

2. Conduct field sampling at the sampling sites including water quality and laboratory analysis.

3. Conduct a field investigation in the Spring Branch watershed for possible ammonia sources.

4. Submit three interim reports that discuss progress, problems encountered, and preliminary

findings. The first interim report will include the initial sampling plan and map(s) of monitoring

locations. The second interim report will include the resulting data and the third will be the final

report with all this information.

5. Submit the data collected for Stage 2 (in either ACCESS or EXCEL format) and a final report

which discusses data collection and/or monitoring process, data gaps and the reason therefore

should any exist, summarization of the data and the results of the collection/monitoring effort.

Table 3 summarizes the sampling requirements for the listed segments, including parameters to be

measured, sampling frequency, and timeframe. Table 4 lists the latitude and longitude of each sampling

site and provides a brief description of each site. Upon locating the sampling sites with a hand-held

Global Positioning System (GPS), Tetra Tech will evaluate the sampling site to confirm it is the best

location to collect the required samples. Conditions that may require sampling site relocation may

include:

If a discharge point for runoff into the stream is noted downstream of the proposed sampling site,

the sampling site may be relocated downstream of the discharge point.

The stream is inaccessible at the proposed sampling site.

If changes to the sampling sites locations are implemented in the field, the new sampling site locations

will be chosen in the same stream segment as the proposed sampling site noted in Figures 3 and 4. Each

final sampling site will be verified with a hand-held GPS and recorded in the field notes.

Sampling will be conducted in October – December 2014 or March 2015 depending on weather

conditions. The sampling events are to occur during varied flow conditions, yet spaced as close together

as possible. Figures 3 and 4 show the locations of sampling sites at each watershed.

The final data collection report, including the electronic water quality database, will be submitted to IEPA

for review 45 days after the final analytical data have been received.


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TABLE 3SUMMARY OF WATER QUALITY SAMPLING REQUIREMENTS

Notes:

DO Dissolved oxygenNO2 + NO3 Nitrite plus nitrate-nitrogenT-ammonia Total ammoniaTKN Total Kjeldahl nitrogenTP Total phosphorusTSS Total suspended solids

WatershedWaterBody

ImpairmentCause(s) of

ConcernSegment

SamplingSite

MatrixField

ParametersLaboratoryParameter

SamplingFrequency

No. ofLocations

Dates

Pecatonica

WinneshiekCreek

TSS andphosphorus

PWL-01 WC01 Water

Temperature,DO, pH,

conductivity,flow (depth,velocity, and

streamgeometry)

TP, TSS 3 X 1Varying flow conditions

November – December 2014or March – April 2015

SpringBranch

Totalammonia

andphosphorus

PWNC

SB01SB02SB03SB04

Water

Temperature,pH,

conductivity,DO, flow(depth,

velocity andstream

geometry)

TKN, T-ammonia,

Total NO2 +NO3, TP

(downstreamonly)

3 X 3Varying flow conditions


GroundwaterTemperature,

DOT-ammonia,NO2 + NO3

3 X 1Varying flow conditions



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TABLE 4SAMPLING SITE DESCRIPTIONS

Watershed Water Body SegmentSampling

SiteCounty Latitude† Longitude† Description

Pecatonica

WinneshiekCreek

PWL-01 WC01 Stephenson 42.306203 -89.514405

Approximately 215 feetupstream of Fawver Road and1.3 river miles upstream ofconfluence with PecatonicaRiver

Spring Branch PWNC

SB01 Stephenson 42.247254 -89.789886400 feet upstream from theconfluence with Yellow Creek

SB02 Stephenson 42.238077 -89.828829

375 feet upstream of SpringBranch split on the southerntributary (split occursapproximately 930 feet alongthe creek upstream from thebridge crossing at IL-73)

SB03 Stephenson 42.238921 -89.829000

240 feet upstream of SpringBranch split on the northerntributary (split occursapproximately 930 feet alongthe creek upstream from thebridge crossing at IL-73)

SB04 Stephenson 42.242022 -89.803758At the edge of Spring Branchon the downstream side of theLoran Road Bridge

†Latitude and longitude are reported using North American Datum of 1983 (NAD83)


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Stage 2 – Water Quality Sampling November 2014

FIGURE 3WINNESHIEK SAMPLING SITES


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FIGURE 4SPRING BRANCH SAMPLING SITES


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1.4 DATA QUALITY OBJECTIVES AND CRITERIA FOR MEASUREMENT DATA

This section describes the DQOs and measurement quality objectives (such as precision and accuracy) for

data that will be collected.

1.4.1 Data Quality Objectives

DQOs are qualitative and quantitative statements developed through a seven-step process based on

USEPA’s guidance for planning data collection projects (2006). Table 5 summarizes the project-specific

DQOs. The seven steps are as follows:

Step 1. State the Problem. Concisely describe the problem to be studied.

Step 2. Identify the Goals of the Study. Identify what questions the study will attempt to answerand what actions may result.

Step 3. Identify Information Inputs. Identify information that needs to be obtained andmeasurements that need to be taken to make decisions and resolve key study questions.

Step 4. Define the Study Boundaries. Specify the time periods and spatial area to which thestudy results will apply.

Step 5. Develop the Analytical Approach. The purpose of this step is to define specificparameters of interest, specify action levels for these parameters, integrate this information withoutputs from previous DQO steps, and describe a logical basis for choosing appropriate actionsbased on study results.

Step 6. Specify Performance or Acceptance Criteria. Identify the performance or acceptancecriteria that the collected data will need to achieve to minimize the possibility of either makingerroneous conclusions or incorrect decisions.

Step 7. Develop the Plan for Collecting Data. Evaluate information from the previous steps andgenerate alternative data collection designs.

Table 5 summarizes the DQOs for the project.

1.4.2 Measurement Quality Objectives

The overall QA objective for this water quality sampling effort is to implement procedures for field

sampling, chain of custody, laboratory analysis, and data reporting to produce well-documented data of

known quality.


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TABLE 5PROJECT DATA QUALITY OBJECTIVES

STEP 1 STEP 2 STEP 3 STEP 4 STEP 5 STEP 6 STEP 7State the Problem Identify the Goals of

the StudyIdentify

Information InputsDefine StudyBoundaries

Develop theAnalyticalApproach

Specify Performanceor Acceptance

Criteria

Develop the Plan forCollecting Data

Two segmentswithin thePecatonicawatershed inIllinois have beenidentified byIEPA as beingimpaired and havebeen placed onthe 303(d) list.

Supplementaldata must becollected tocomplete TMDLdevelopment.

This data collectionwill inform estimatesof pollutant loads frompoint sources andnonpoint sources in thestudy area.

Based on the Stage 2sampling results, IEPAwill prepare animplementation planthat uses BMPs toreduce the existingpollutant loads andachieve the TMDLgoals, eventuallybringing the waterbody in compliancewith water qualitystandards.

Numeric andnarrative waterquality standards toestablish analyticalgoals for the Stage 2sampling, waterquality targetsdescribed in Stage 1report

Hydrologic andwater quality data

Known pointsources andnonpoint sourcesfrom watershed areaactivities/operations

National or localweather serviceforecasts to predictprecipitation eventsand variable flowconditions

The spatial boundaryof the study isdefined by thefollowing waterbodies: Winneshiek

Creek Spring Branch

The temporalboundary of thestudy is Octoberthrough December2014 and March2015

Sampling sites wereselected based onStage 1 results forthe watershed.

Samples will becollected undervariable flowconditions from twosegments in thePecatonicawatershed primarilyto fill data gapsidentified duringStage 1.

The sampling design isnot statistically based;therefore, there are nospecific decision errorsthat apply to projectresults.

Measurements will beperformed by qualifiedfield personnel and afully accreditedanalytical laboratory.

The analyticallaboratory will employmethods which aresuitably sensitive tocharacterize conditionsrelative to prevailingWQ standards and WQtargets described inStage 1, and for whichit retains currentaccreditation and validprocedures.

Sampling in eachwater body will bedirected. Thesampling sites wereselected based ondata gaps identifiedduring Stage 1 andinclude stations thatalready exist on thewater bodies.

Field staff willendeavor to capturemultiple flowconditions throughcoordination withthe laboratory andforecastinginformationavailable from thenational or localforecasts

Specific samplingprotocols arepresented inSection 2.2.

Notes:BMP Best management practiceIEPA Illinois Environmental Protection AgencyTMDL Total maximum daily loadWQ Water Quality

Water Quality Sampling Quality Assurance Project Plan forTMDLs for Pecatonica Watershed, Winneshiek Creek and Spring Branch

QAPP 408, Revision 0Date: December 1, 2014

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Stage 2 Water Quality Sampling

Other sections of this QAPP describe specific procedures for sampling, chain-of-custody documentation,

laboratory instrument calibration, laboratory analysis, data reporting, internal QC, audits, preventive

maintenance of field equipment, and corrective action. The purpose of this section is to address the level

of QC effort and the specific QA objectives for the data quality indicators of sensitivity, accuracy,

precision, completeness, representativeness, and comparability. Specific measurement quality objectives

for precision and accuracy of the analytical methods to be used are included in the laboratory SOPs for

those methods.

If analytical data fail to meet the QA objectives described in this section, Tetra Tech will explain in

writing why the data failed to meet the objectives (for example, matrix interferences caused by a high

concentration of one analyte would require dilution of the sample and an increase in the reporting limit)

and will describe the limitations and usefulness of the data. The following corrective actions may be taken

for data that do not meet QA objectives: (1) verifying that the analytical measurement system was in

control; (2) thoroughly checking all calculations; (3) assuming a sufficient quantity of sample is available,

reanalyzing the affected samples if authorized by IEPA; and (4) reporting data with appropriate qualifiers.

Corrective actions are discussed in Section 3.1.

1.4.2.1 Sensitivity

The QA objective for sensitivity is expressed in the form of the method detection limit (MDL) or

quantitation limit for the analytical method selected. Analyte MDLs shall be determined by the USEPA

method given in the Code of Federal Regulations (CFR), Volume 40, Part 136, Appendix B. The MDL is

defined as “the minimum concentration of a substance that can be measured and reported with 99%

confidence that the analyte concentration is greater than zero and is determined from analysis of a sample

in a given matrix containing the analyte.” Since the MDL procedure is based upon precision obtained for

a standard greater than the MDL, it also is a measure of method sensitivity at concentrations near the

MDL.

Quantitation limits, however, reflect the influences of the sample matrix on method sensitivity and are

typically higher than detection limits. Quantitation limits indicate the amount of material needed to

produce an instrument response that can be routinely identified and reliably quantified.



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STAT’s quantitation limits are listed in the SOPs in Attachment A. STAT will provide results to the

sensitivity of the MDL with appropriate data qualifiers. The reporting limits (RLs) are the level to which

data are reported administratively for a specific test method and/or sample. The laboratory maintains RLs

higher than MDLs. The RL is considered the same as sample quantitation limit (SQL). Table 6

summarizes MMCs, MMOs, MDLs and RLs for various parameters. MMC are State of Illinois water

quality standards for general use waters where applicable. Where no MMC can be identified, the water

samples will be analyzed to the lowest concentration readily achievable by the STAT laboratory. The

MMO will be set at approximately one-fifth of the minimum measurement criteria shown to ensure that

analytes will be measured with reasonable accuracy at the MMC concentrations, and measured to

reasonable levels below the MMC.



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TABLE 6SUMMARY OF MMC, MMO, AND MDLs AND RLs

Parameter Method Matrix MMC MMO MDL RLMS/MSDAccuracy

MS/MSDPrecision

LCSAccuracy

LCS Completeness

T-ammonia SM 4500-NH3 C-1997 Water 15.0 mg/L NA 0.025 mg/L 0.05 mg/L 75-125% <20% 80-120% 90%

Total NO2 +NO3

SM 4500NO3 F-2000 Water No Standard NA 0.035 mg/L 0.2 mg/L 75-125% <20% 80-120% 90%

TKN EPA 351.2 v2.0 1993 Water No Standard NA 0.3 mg/L 1.0 mg/L 75-125% <20% 80-120% 90%

TSS SM 2540 D-1997 Water No Standard NA 3.82 mg/L 7.5 mg/L NA NA 80-120% 90%

Phosphorus –Total

SM 4500P B,E-1999 Water 0.05 mg/L NA 0.01 mg/L 0.01 mg/L 75-125% <20% 80-120% 90%

TemperatureHoriba U-10

Instruction Manual*;SOP 061* and 11-2*

Water NA 1º C NA NA NA NA NA NA

DOHoriba U-10

Instruction Manual*Water NA

0.1mg/L

NA NA NA NA NA NA

pHHoriba U-10


Water NA 0.1 pH NA NA NA NA NA NA

ConductivityHoriba U-10


Water NA0.1

mS/cmNA NA NA NA NA NA

Flow Flowwatch Manual* Water NA0.1m/s

NA NA NA NA NA NA

Notes:

º C Degree CelsiusDO Dissolved oxygenEPA Environmental Protection AgencyLCS Laboratory control sampleMDL Method detection limitm/s Meters per secondmg/L Milligram per litermS/cm Micro Siemens per centimeterMMC Minimum Measurement Criteria (State of Illinois

General Water Use Quality Standard)MMO Minimum measurement objectiveMS/MSD Matrix spike/matrix spike dublicate

NA Not applicableNH3 AmmoniaNO2 NitriteNO3 NitrateRL Reporting limitSOP Standard operating procedureSM Standard MethodT-ammonia Total ammoniaTKN Total Kjeldahl nitrogenTSS Total suspended solids* Presented in Appendix B



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1.4.2.2 Accuracy

Accuracy is the degree of agreement between an analytical measurement and a reference accepted as a

true value. The accuracy of a measurement system is affected by errors introduced through the sampling

process by field contamination, sample preservation, and sample handling. Other factors that may affect

accuracy are sample matrix, sample preparation, and analytical techniques. Sampling bias will be assessed

based on the results of the analysis of field duplicates, and on correlation of field data to laboratory

analytical results. Field duplicates are two samples collected from the same location and submitted blind

to the laboratory to identify the same analyte detection. The analytical laboratory will analyze laboratory

blanks and laboratory control samples (LCS) to evaluate laboratory accuracy in accordance with STAT’s

QA manual. Laboratory blanks are aliquots of laboratory reagent water processed with samples through

the entire analytical process to demonstrate that no target analytes are introduced in the measurement

system. LCSs are aliquots of laboratory water that have been spiked with known concentrations of target

analytes, and processed with environmental samples to assess potential bias of the measurement system.

These QC samples will be analyzed in each analytical batch or one set per analytical batch, whichever is

more frequent. The results of the spiked samples are used to calculate the percent recovery for evaluating

accuracy using the following formula:

Percent Recovery = [(S - C) / T] *100 (Equation 1)

where

S = Measured spiked sample concentration

C = Sample concentration

T = True or actual concentration of the spike

Data may be evaluated for accuracy using, in order of priority, LCSs and LCS duplicates (LCSD) and

matrix spike/matrix spike duplicates (MS/MSD). Failures of LCS, or LCSDs to meet QC criteria may

invalidate data, while MS/MSD results should be used with caution in assessing overall analytical bias

and precision.

Samples will be collected in sufficient quantity so that the laboratory has enough volume to accommodate

MS/MSD and laboratory duplicates in addition to an aliquot reserved for actual sample analysis. The

designated laboratory QC sample will include sufficient volume so that one reanalysis may be performed



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if necessary. The sample chosen for laboratory QC sample collection shall be randomly selected for the

initial sampling event and rotated from one sampling location to the next for subsequent sampling events.

1.4.2.3 Precision

Precision is the degree of mutual agreement between individual measurements of the same property under

prescribed similar conditions. Data precision is affected by field sampling precision and laboratory

analytical precision. It is evaluated by collecting and analyzing field duplicates at a frequency of

10 percent or at least once per event. Field duplicates are used to assess precision for the entire sample

collection and measurement systems. Laboratory precision is evaluated by analyzing laboratory duplicates

or MS/MSDs as appropriate for the reference method. A laboratory duplicate would be analyzed if called

for in the laboratory’s SOP. A laboratory duplicate might also be used to evaluate precision for an

analysis that does not use or require MS/MSD samples. Laboratory duplicates or MS/MSD pairs are

usually prepared and analyzed at a rate of one per analytical batch. The results of the duplicate analysis

are used to calculate the relative percent difference (RPD) for evaluating precision using the following

formula:

RPD = [(A – B) / (A + B)/2] *100 (Equation 2)

where

A = Original sample concentration

B = Duplicate sample concentration

Four factors may impair the precision of duplicate data: matrix interference, laboratory imprecision,

sample heterogeneity, and the nature of the RPD calculation when applied to low native-sample

concentrations. Constituents present in the field sample may interfere with accurate quantification of the

target analyte. Laboratory imprecision is a result of inconsistency in preparing and analyzing the samples.

Heterogeneity in sediment samples is inherent because of the varied composition of natural materials and

the subsequent difficulty in collecting homogeneous samples. The relatively small sample sizes used in

inorganic analyses increases the potential for heterogeneity. Because the RPD calculation compares the

absolute difference of the values to the mean, if nondetect results are treated as zeros and only one of the

samples yields a nondetect result, the calculation would always yield an inflated 200 percent RPD result.

Even with the reporting of estimated results below the sample quantitation limit, low-level sample results

may indicate high RPDs and thus poor precision. Precision results require close examination when low-



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level sample concentrations are being assessed. Data are generally not qualified strictly on the basis of

duplicate sample precision; rather, a determination must be made as to whether an apparent precision

deficit is due to matrix interference, heterogeneity, or field or laboratory imprecision.

1.4.2.4 Completeness

Completeness is defined as an assessment of the amount of valid analytical data obtained from a

measurement system compared with the amount of analytical data needed to achieve a particular level of

confidence. The percent completeness is calculated by dividing the number of valid sample results by the

total number of samples planned, and multiplying the result by 100 percent. Completeness will be

reported as the percentage of all measurements judged valid. The following equation will be used to

determine completeness:

%C = (V/T) * 100% (Equation 3)

where

%C = Percent completeness

V = Number of measurements judged valid

T = Total number of measurements planned

For this project, the QA objective for degree of completeness for both field and laboratory data is

90 percent. If completeness is less than the target of 90 percent, Tetra Tech will evaluate the data to

determine whether (1) there are enough data to complete the TMDLs or (2) additional data collection is

necessary.

1.4.2.5 Representativeness

Representativeness expresses the degree to which sample data accurately and precisely represent the

characteristics of a population, parameter variations at a sampling point, or an environmental condition

that they are intended to represent. Representativeness of data will be ensured using established field and

laboratory procedures and their consistent application. To aid in the evaluation of the representativeness

of the sample data, field and laboratory blank samples will be evaluated for the presence of contaminants,

and all data will be compared with available historical results and with results for similar samples

collected during the study. Data deemed non-representative through comparison with existing data will be

used only if accompanied by appropriate data qualifiers and limits of uncertainty.



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1.4.2.6 Comparability

Comparability expresses the confidence with which one data set can be compared with another.

Comparability will be maximized by using standard analytical methods and standardized, documented

sampling techniques. Tetra Tech will document all sampling locations, conditions, and field sampling

methods. All results will be reported in standard units or, for field parameters, as defined in the method.

All laboratory calibrations will be performed using standards traceable to the National Institute for

Standards and Technology, IEPA-approved sources, or another certified reference standard source.

1.5 SPECIAL TRAINING CERTIFICATION AND REQUIREMENTS

Tetra Tech employs professionals who have been educated and trained in all aspects of water quality

sampling, and maintains comprehensive training programs to ensure that staff are up-to-date in proper

techniques for collecting representative samples from aquatic environments. As shown in Table 7, Tetra

Tech personnel are experienced at sampling a wide variety of media, including surface water and

sediment. In addition, Tetra Tech is not aware of any certifications or requirements necessary to complete

this sampling project.

Prior to the first sampling event, the Tetra Tech project manager and sampling personnel will review the

field procedures outlined in the QAPP, including the SOPs, and health and safety concerns. The Tetra

Tech project manager will ensure that any additional sampling personnel will have similar qualifications

and will review the QAPP and field procedures before their first sampling event.

1.6 DOCUMENTATION AND RECORDS

This section discusses the procedures for maintaining field operation, laboratory, and data handling

records. All records will be stored in a specific project folder on Tetra Tech’s internal drive. The drive is

password protected with only Tetra Tech personnel having access. Tetra Tech maintains project

documents and records for a minimum of 10 years. Hard copies of documents such as field log books will

be scanned and stored on Tetra Tech’s password protected internal drive. After electronic distribution to

IEPA and the field team, the final approved QAPP with signatures and dates will be stored on Tetra

Tech’s internal drive in the project specific folder.



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1.6.1 Field Operation Records

Overall field operations will be documented. The documentation will consist of the following: sample

collection records, chain-of-custody records, QC sample records, records of general field procedures, and

corrective action reports. Documentation during sampling is essential to ensure proper sample

identification. Standard sample custody procedures will be used to maintain and document sample

integrity during collection, transportation, storage, and analysis. Field personnel will use permanently

bound field logbooks (See SOP 024) with sequentially numbered pages to maintain field records. The

front cover of the logbook will list the contract name and number, the project number, the site name,

names of subcontractors, the client, and name of the project manager. The following information will be

recorded in the field logbook:

Name and affiliation of all personnel present

Weather conditions during the field activity

Log and summary of daily activities and significant events

References to other field logbooks or forms that contain specific information

Discussions of problems encountered and their resolution

Discussions of deviations from the QAPP or other governing documents

Description of all photographs taken



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TABLE 7PERSONNEL QUALIFICATIONS

Employee Years ofExperience

SPECIFIC TRAINING AND QUALIFICATIONS

Andrea Plevan 14 Ms. Plevan has 14 years of experience in water qualityinvestigations, aquatic ecology, total maximum daily load studies,lake and watershed management plans, and monitoring plans. Shehas overseen monitoring and data collection for a variety of lake,stream, and watershed water quality investigations.

John O’Donnell 32 Mr. O’Donnell is an analytical chemist by training with over 20years of laboratory and field sampling and analysis experience, andover 12 years of direct quality assurance management. He is amember of Tetra Tech’s Quality Council and is responsible for thepreparation of quality system descriptions (quality managementplans [QMPs]); oversight, development and implementation ofprogram and project-specific QA Guidance (QAPPs); developmentof standard operating procedures; participating in quality reviewprocesses including document and data reviews; and for overseeingcorrective action investigations, identification of remedies, andverification of corrective action effectiveness.

John Dirgo 35 Dr. Dirgo has 35 years of experience in air compliance andregulatory support, source and ambient air sampling, air pollutioncontrol, hazardous waste site investigations, risk assessment, andcompliance evaluations. He is currently a member of Tetra Tech’scorporate quality management team. He regularly conducts QAaudits of program activities; provides corrective actionrecommendations for work that does not fully meet programstandards; and provides corporate resources to assist in resolvingQA issues.

Adam Peterca 5 Mr. Peterca has over 5 years of experience in the environmental field as anecological engineer. He has experience sampling a variety ofenvironmental media, including designing habitat and biota assessments.In addition, Mr. Peterca has experience with habitat restoration design,including hydrologic and hydraulic modeling. Mr. Peterca is a projectmanager for EPA’s Superfund Technical Assessment and Response Team(START), and also has experience conducting environmental assessmentsand wetland delineations.

Cordell Renner 1 Mr. Renner has over 1 year of applied experience as an environmentalscientist. He has experience sampling a variety of environmental media.Mr. Renner has assisted in investigation activities at several contaminatedsites. Mr. Renner has also conducted numerous groundwater, soil, surfacewater, and waste water sampling events.



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1.6.2 Laboratory Records

The following documentation will be required from STAT:

Transmittal letter

Case narratives, which will describe all QC nonconformances encountered during analysis ofsamples, in addition to any corrective actions taken, including

Sample results

Laboratory chronicle

Summary QC results, including but not limited to the following:

– Method blanks– Spike blanks– Matrix spike/matrix spike duplicate

Chain-of-custody forms pertaining to each sample delivery group or sample batch analyzed

List of data qualifiers and abbreviations

The project manager, in cooperation with the QA officer, will define site-specific requirements for data

reporting. The laboratory QA officer is responsible for ensuring that all laboratory data reporting

requirements in the QAPP are met.

1.6.3 Data Handling Records

Records documenting the protocols used in data reduction, verification, and validation will be maintained

primarily by the project manager but also possibly by the QA officer. Data reduction protocols address

operations such as converting raw data into reportable quantities and units, use of significant figures,

recording of extreme values, and blank corrections. Data verification ensures the accuracy of data

transcription and calculations, if necessary, through the manual checking of a set of computer

calculations. Data validation ensures that QC criteria are met.

STAT will submit analytical data reports to Tetra Tech. Each data report will contain a case narrative that

briefly describes the number of samples, the analyses, and any noteworthy analytical difficulties or

QA/QC issues associated with the submitted samples. The data report will also include signed chain-of-

custody forms, cooler receipt forms, analytical data, a QC package, and raw data.



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2.0 DATA GENERATION AND ACQUISITION

This section describes the collection and analysis of the samples as well as the processes employed to

ensure the quality of the data. Section 2.1 summarizes the sampling process design. Section 2.2 describes

sampling methods requirements. Section 2.3 includes information on sample handling and custody.

Section 2.4 discusses analytical methods requirements. Section 2.5 discusses QC requirements. Sections

2.6 and 2.7 discuss the instrument and equipment testing, inspection, and maintenance, and instrument

calibration and frequency, respectively. Section 2.8 discusses requirements for inspection and acceptance

of supplies and consumables. Section 2.9 describes non-direct measurements. Section 2.10 discusses data

management.

2.1 SAMPLING PROCESS DESIGN

Based on the data gaps identified in the Stage 1 reports, samples will be collected from two segments

within the watersheds as shown in Figure 1. Figures 3 and 4 show the specific sampling sites along each

segment. Table 3 in Section 1.3 provides a complete summary of the sampling design for this project,

including the matrices, field and laboratory parameters, sampling frequency, and sampling dates for each

location.

At the sampling site on Winneshiek Creek, field measurements will be made for the following water

quality parameters: temperature, dissolved oxygen (DO), pH, and conductivity. Flow information

including depth, velocity, and stream geometry will also be measured. Water samples will be collected for

laboratory analysis for concentrations of total phosphorus (TP) and total suspended solids (TSS).

At each sampling site along Spring Branch, field measurements will be made for the following water

quality parameters: temperature, DO, pH, and conductivity. Flow information including depth, velocity,

and stream geometry will also be measured. Water samples will be collected for laboratory analysis for

concentrations of total Kjeldahl nitrogen (TKN), total ammonia (T-ammonia), Total nitrite (NO2)/nitrate

(NO3). TP will be collected at the most downstream site only. Field measurements will be collected in the

streams between 0 and 1 foot below the water surface. Water samples will be delivered to the laboratory,

STAT, for filtration and analysis.



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A groundwater grab sample will be collected from a shallow well at one location along Spring Branch. If

a shallow well is not found, alternate field methods to obtain shallow groundwater samples (e.g., seeps,

springs, mini-piezometer) will be investigated. Assuming a shallow well is not found in the area, a seep or

spring will be sampled. If a seep or spring is not found in the field, groundwater grab samples will be

collected from a mini-piezometer installed at sample point SB-04 in Figure 4. The groundwater sample

will be analyzed for t- ammonia and nitrite plus nitrate, and field measurements will be made for

temperature and DO. Groundwater sampling will follow SOP No. 010 “Groundwater Sampling” (see

Attachment B).

Stream sampling procedures will occur at the center of the stream and will follow SOP No. 009, Section

2.1, “Surface Water Sampling by Submerging Sample Container” (see Attachment B). Stream samples

will be collected from 0 and 1 foot below the water surface. A composite sample will be collected of

water from the left bank, right bank, and center of the stream. The samples and measurements will be

collected between November and December of 2014 or between March and April of 2015 at varying

flows, although spaced as close as possible together. If a high flow event does not occur during this time

period, sampling may be conducted in March of 2015 to collect high flow conditions.

In Spring Branch, channel substrate, percent cloud cover, percent shading, and coarse streamside

vegetative summary will be observed at the surface to help evaluate the streambed material composition.

If the site conditions (such as accessibility) permit, the stream shading data collection will extend between

the upper and lower monitoring sites. Percent shading will be determined by taking a photo of the stream

and estimating the amount of shade that falls on the water.

2.2 SAMPLING METHODS REQUIREMENTS

For each sampling method, Tetra Tech will follow procedures outlined in the SOPs included in

Attachment B. The sampling methods and SOPs include the following:

Surface water sampling (see SOP No. 009, Section 2.1, for surficial stream sampling)

Groundwater sampling (SOP No. 010)



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Tetra Tech will use a Horiba U-10 Water Quality Checker or similar device to measure the remaining

field parameters. The Horiba U-10 Water Quality Checker instruction manual is included in Attachment

B and includes procedures (see SOP 061) for measuring pH, conductivity, DO, turbidity, and temperature

(see Section 2 of the instruction manual).

Tetra Tech will use a Flowatch® flow measurement instrument or similar device to measure water

velocity at each of the sampling locations. The instruction manual is included in Attachment B and

includes procedures for measuring water velocity. Discharge will be computed by multiplying the water

velocity in each segment by its corresponding cross-sectional area. The cross-sectional area will be

calculated as the sum of all the segmental areas across the width of the stream at various individual water

depths. Table 8 summarizes the sample volume, preservation technique, and holding time requirements

for each laboratory analytical parameter.



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TABLE 8REQUIRED SAMPLE VOLUMES, ANALYTICAL METHODS, CONTAINERS,

PRESERVATION TECHNIQUES, AND HOLDING TIMES

Parameter Analytical MethodInstrumentation-

Equipment

Volumeand

Container

PreservationTechnique

HoldingTimea

Laboratory

T-ammonia SM 4500-NH3 C-1997Selective ion

probe

1-L plasticbottle

Chill to ≤6ºC, pH2 with H2SO4

28 days

Total NO2 +NO3

SM 4500NO3 F-2000 Spectrophotometer1-L plastic

bottleChill to ≤6ºC, pH2 with

H2SO428 daysb

TKN EPA 351.2 v2.0 1993 Spectrophotometer1-L plastic

bottleChill to ≤6ºC, pH<2

with H2SO428 days

TSS SM 2540 D-1997Gravimetric-

analytical balance1-L plastic

bottleChill to <6ºC 7 days

Phosphorus– Total

SM 4500P B,E-1999 Spectrophotometer1-L plastic

bottleChill to ≤6ºC, pH<2

with H2SO428 days

Field

TemperatureHoriba U-10


Horiba U-10Plasticbottle

NA NA

DOHoriba U-10

Instruction Manual*Horiba U-10

Plasticbottle

NA NA

pHHoriba U-10



NA NA

ConductivityHoriba U-10



NA NA

Flow Flowwatch Manual* Flowwatch NA NA NA

Notes:

H2SO4 Sulfuric acidL LiterNH3 AmmoniaNO2 NitriteNO3 NitrateT-ammonia Total ammonia

TKN Total Kjeldahl nitrogenTP Total phosphorusTSS Total suspended solidsEPA Environmental Protection Agency

SM Standard Method

* Presented in Appendix B

a Holding time is measured from the time of sample collection to the time of sample preparation, extraction, or analysis.

b Samples to be analyzed for NO2 and NO3 only must be chilled to < 6ºC and analyzed within 48 hours; however, for thecombined analysis of NO2 + NO3, samples may be acidified, chilled, and analyzed within 28 days. Similarly, if samplesare to be analyzed for orthophosphate, they must be chilled to <6ºC and filtered within 15 minutes before analyzed andanalyzed within 48 hours; however, samples to be analyzed for TP may be acidified, chilled, and analyzed within 28days.



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2.3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS

Each sample collected by Tetra Tech will be traceable from the point of collection through analysis and

final disposition to ensure sample integrity. The team will use standard procedures to identify, track,

monitor, and maintain the chain of custody for all samples. These procedures are discussed below.

2.3.1 Field Logbooks

Daily field activities will be documented through journal entries in a bound field logbook dedicated to the

project. The logbook will be water-resistant, and all entries will be made in indelible ink. The logbook

will contain all pertinent information about sampling activities, site conditions, field methods used,

general observations, and other pertinent technical information. Examples of typical logbook entries

include the following:

Personnel present

Daily temperature and other climatic conditions including cloud cover

Field measurements, activities, and observations

Referenced sampling site descriptions (in relation to a stationary landmark) and map

Media sampled

Sample collection methods and equipment

Dates and times of sample collection

Types of sample containers used

Sample identification and cross-referencing

Sample types and preservatives used

Analytical parameters

Sampling personnel, distribution, and transporters

Instrument calibration procedures and frequency, and calibration records

The sampling team leader or designee will be responsible for maintaining all field records. Each logbook

page will be numbered, dated, and signed by the person making the entry. Corrections to the logbook will

be made by using a single strike mark through the entry to be corrected, then recording and initialing the

correct entry. For corrections made at a later date, the date of the correction will be noted.



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Color digital photographs will be taken during the sampling activities. The name of the photographer,

date, time, site location, photograph orientation, and photograph description will be entered in the

logbook as photographs are taken.

Data collection sheets will be used to record all information pertaining to field measurements.

Information on these sheets will include sample identification, location (including latitude and longitude),

sampler, weather conditions, sample matrix, and the measured value for each parameter. Personnel

conducting sample measurements will be responsible for completing the data collection sheets. The

sampling team leader will review the sheets in the field to verify completion and accuracy.

2.3.2 Field Sampling Records

Logbooks, data collection sheets, and chain-of-custody forms will contain all information pertaining to

sample collection. Information recorded will include sample identification, location (including latitude

and longitude), sampling depth, date, time, sampler, and sample matrix. Ultimate responsibility for

maintaining and recording information belongs to the sampling team leader. All paperwork will be

completed using indelible ink.

2.3.3 Sample Labels

A sample label will be affixed to each sample container sent to the laboratory. This identification label

will be completed with the following information in indelible ink:

Water body (for example, “WC” for Winneshiek Creek)

Sample designation (see Section 2.3.4)

Date and time of sample collection

Preservative used

Sample collector’s initials

Analysis required

An example of a blank sample label is shown in Figure 5.



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FIGURE 5EXAMPLE SAMPLE LABEL

2.3.4 Sample Designation

A sample numbering scheme has been developed to allow each sample to be uniquely identified and to

provide a means of tracking the sample from collection through analysis. The numbering scheme

indicates the sampling site, sample type (W = water), collection date, sample number, and depth (if

applicable). For example, the first water sample collected from Winneshiek Creek would be designated

WC01-W-082714-1(0-12). The unique sample number will be entered on sample labels, chain-of-custody

forms, and other records documenting sampling activities.

QC samples will be designated as follows: field duplicates will be designated by “FD” after the sample

type designation (“W”), respectively.

2.3.5 Chain-of-Custody Record

Standard sample chain-of-custody procedures will be used to maintain and document sample integrity

during collection, transportation, storage, and analysis. Sample chain-of-custody documents must be

written in indelible ink. Where necessary, the documents will be corrected by drawing one line through

the incorrect entry, entering the correct information, and initialing and dating the correction. A sample is

considered to be in custody if one of the following statements applies:

It is in a person’s physical possession or view.

It is in a secure area with restricted access.

It is placed in a container and secured with an official custody seal so that the sample cannot bereached without breaking the seal.



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Samples and documentation must be maintained in the custody of authorized personnel or under

documented control in a secure area. The sampling team leader is responsible for proper sample handling

and documentation, so that the possession and handling of individual samples can be traced from the time

of collection to laboratory receipt. STAT’s QA officer is responsible for establishing a control system that

will allow sample possession to be traced from laboratory receipt to final disposition. Chain-of-custody

procedures provide an accurate written record that traces the possession of individual samples from the

time of collection in the field until they are accepted at the laboratory. The chain-of-custody record will

also be used to document the samples collected and the analyses requested. Figure 6 shows an example of

a blank chain-of custody form. Information to be recorded on the chain-of-custody record includes the

following:

Project name and number

Name and signature of sampler

Destination of samples

Technical contact and telephone number

Sample identification number

Sampling location

Date and time of collection

Sample matrix

Number and type of containers filled

Analysis or analyses requested

Preservatives used

Signatures of individuals involved in custody transfer (including date and time of transfer)

Relevant remarks related to sample analysis (such as samples selected for MS/MSD analysis)

Unused lines on the chain-of-custody record will be crossed out and initialed. Field personnel will sign

chain-of-custody records initiated in the field, place the record in a plastic bag, and tape it to the inside of

the lid of the shipping container used for sample transport. The field personnel will retain and file copies

of the chain-of-custody record before delivering samples to the lab. Multiple coolers may be sent in one

shipment to the laboratory. Each cooler will contain a separate chain-of-custody record of the samples.



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FIGURE 6

EXAMPLE CHAIN-OF-CUSTODY FORM



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2.3.6 Sample Packaging

After being appropriately containerized and labeled, samples should be packaged using the procedures

summarized below.

1. Place the sample in a resealable plastic bag.

2. Place the bagged sample in a cooler, and pack the cooler to prevent breakage.

3. Prevent breakage of bottles during shipment by either wrapping the sample containers in bubblewrap or lining the cooler with a noncombustible material such as vermiculite.

4. Add a sufficient quantity of ice to the cooler to cool samples to < 6 °C. Ice should be double-bagged in resealable plastic bags to prevent the melted ice from leaking out. As anoption, a temperature blank (a sample bottle filled with distilled water) can be included inthe cooler.

5. Seal the completed chain-of-custody forms in a plastic bag and tape the plastic bag to the insideof the cooler lid.

6. Tape any instructions for returning the cooler to the inside of the lid.

7. Close the lid of the cooler and tape it shut by wrapping strapping tape around both ends and thehinges of the cooler at least once. Tape shut any drain plugs on the cooler.

8. Transport samples to the laboratory for analysis.

Tetra Tech field personnel will deliver the samples to STAT’s Chicago laboratory following each

sampling event. Sample disposal will occur only on the order of the laboratory project manager, in

consultation with Tetra Tech and IEPA or when it is certain that the information is no longer required or

the samples have deteriorated.

2.4 ANALYTICAL METHODS REQUIREMENTS

STAT will conduct all analyses of water samples collected. STAT will analyze water samples for TKN,

T-ammonia , NO2 + NO3, TSS, and TP using methods specified in Table 8. Analytical methods are

included in STAT’s QA manual and the SOPs in Attachment A. In all cases, appropriate methods of

sample preparation, cleanup, and analyses are based on specific analytical parameters of interest, sample

matrices, and required quantitation limits. The requested standard turnaround time for sample results is

seven days.



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2.5 QUALITY CONTROL REQUIREMENTS

The main functions of any sampling and analysis program are to obtain accurate and representative

environmental samples and to provide defensible analytical data. A program to evaluate field and

laboratory data was developed to achieve these goals. The quality of the field data will be assessed

through the collection and analysis of field QC samples on a regularly scheduled basis. Laboratory QC

samples will also be analyzed in accordance with the laboratory’s QA requirements and referenced

analytical method protocols to ensure that laboratory procedures and analyses are conducted properly.

The following subsections discuss the types of QC samples to be collected and analyzed for this project

and their role in ensuring acceptable project data. Specifically, the following subsections discuss field QC

requirements, laboratory QC requirements, and laboratory QC procedures. QC procedures are not limited

to those discussed in this section. Field and laboratory personnel, in accordance with specific method

protocols, may implement additional procedures.

2.5.1 Field Quality Control Requirements

Field QC samples are used to evaluate the validity of the field sampling effort. They are collected for

laboratory analysis to check sampling and analytical precision, accuracy, and representativeness. Table 9

summarizes the types and frequency of collection for field QC samples.

TABLE 9FIELD QUALITY CONTROL SAMPLES

Sample Type Frequency of AnalysisField duplicate 1 every other sampling eventa

Matrix spike/matrix spike duplicate 1 every other sampling eventb

Note:a A sampling event is defined as a round of sampling conducted at each sampling location. Table 4 lists

sampling locations.b Matrix spike / matrix spike duplicate are not applicable to TSS.

Field duplicate samples are independent samples collected as close as possible, in space and time, to the

original investigative sample. Field duplicate samples can measure the influence of sampling and field

procedures on the precision of an environmental measurement. They can also provide information on the

heterogeneity of a sampling site. Field duplicate samples are collected immediately after collection of the



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original sample using the same collection method. Sampling personnel will be careful to collect the field

duplicate samples as close as possible to the locations of original samples. Field duplicate samples will be

collected every other sampling event. Duplicate field measurements will also be taken every other

sampling event.

MS/MSD samples are laboratory QC samples collected in the field. For aqueous samples, MS/MSD

samples require twice the normal sample volume for inorganic analyses. Section 2.5.2.2 describes

MS/MSD samples.

2.5.2 Laboratory Quality Control Requirements

STAT will follow its internal QA procedures and any additional QA procedures specific to the analytical

methods that will be used. Attachment A provides a copy of STAT’s QA manual and laboratory SOPs.

The laboratory QA officer is responsible for ensuring that all laboratory internal QC checks are conducted

in accordance with the laboratory’s QA manual and SOPs, and with the requirements of this QAPP. This

section contains brief descriptions of the laboratory QC samples to be analyzed by STAT.

2.5.2.1 Laboratory Control Samples

An LCS or blank spike originates in the laboratory as deionized water that has been spiked with standard

reference materials of known concentration. An LCS is analyzed to verify the accuracy of the analytical

system at a frequency of one per analytical batch. LCSs are prepared and analyzed using the same

procedures as field samples at the frequency prescribed in the individual analytical method. Method- and

laboratory-specific protocols will be followed to assess the usability of the data if LCS percent recovery

results (used to determine accuracy) or RPD results (used to determine precision) are outside established

acceptance limits.

2.5.2.2 Matrix Spike and Matrix Spike Duplicates

MS and MSD samples are analyzed, when appropriate, to evaluate the suitability of an analytical method

for a particular environmental sample matrix. The MS sample is prepared using a known concentration of

target analytes added to an aliquot of the field sample. The additional sample volume collected by the

field team will be used to create these samples. The samples will be spiked when they are prepared for

analysis at the laboratory. MS and MSD results are used to measure the efficiency of all of the steps of the

analytical method in recovering target analytes from an environmental sample matrix. The percent

recoveries will be calculated for each spiked analyte and used to evaluate analytical accuracy. The RPD



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between spiked sample results will be calculated to evaluate precision. Precision is based on comparison

of the results for duplicate and original analyses. For inorganic analyses, a matrix duplicate may be

analyzed in place of an MSD. MS and MSD samples are analyzed at a frequency of 1 per 20 or fewer

investigative samples. If the MS and MSD percent recovery results used to assess accuracy or the RPD

results used to assess precision are outside the established acceptance limits, method- and laboratory-

specific protocols will be followed to evaluate data usability.

2.5.3 Laboratory Quality Control Procedures

The laboratory will establish SQLs and standard laboratory RLs adjusted for the characteristics of

individual samples. The SQL is a chemical-specific level that a laboratory should be able to routinely

detect and quantify in a given sample matrix. The SQLs should correspond to the lowest calibration

standard analyzed during the initial instrument calibration for the specific method. The SQL takes into

account changes in the preparation and analytical methodology that may alter the ability to detect an

analyte, including changes such as use of a smaller sample aliquot or dilution of the sample extracts,

digestates, or distillates. The laboratory will calculate and report SQLs for all environmental samples.

2.6 INSTRUMENT AND EQUIPMENT TESTING, INSPECTION, AND MAINTENANCEREQUIREMENTS

This section outlines testing, inspection, and maintenance procedures for field equipment and instruments

and for laboratory instruments. This section discusses general requirements that apply to field and

laboratory equipment, and field-specific and laboratory-specific requirements.

2.6.1 General Requirements

For most instruments, preventive maintenance is performed in accordance with procedures and schedules

recommended in (1) the instrument manufacturer’s literature or operating manual, or (2) SOPs associated

with particular applications of the instrument.

In some cases, testing, inspection, and maintenance procedures and schedules will differ from the

manufacturer’s specifications or SOPs. Differences can occur when a field instrument is used to make

critical measurements or when the analytical methods associated with a laboratory instrument require

more frequent testing, inspection, and maintenance.



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2.6.2 Field Equipment and Instruments

Field equipment will be rented from Field Environmental Instruments, Inc. (Fields). Tetra Tech has a

contract with Fields and has successfully used Fields equipment on similar projects. Fields will be

responsible for thoroughly checking and calibrating field equipment and instruments before shipment or

transport to Tetra Tech prior to field activities. Copies of testing, inspection, and maintenance procedures

will be shipped to Tetra Tech with the equipment and instruments. After the equipment and instruments

arrive, the field technicians will assume responsibility for testing, inspection, and maintenance.

Detailed information regarding maintenance and servicing of field instruments is available in the

instruction manual of the specific instrument used. Field personnel will record service and maintenance

information in field logbooks. Specific preventive maintenance procedures will follow the manufacturer’s

recommendations. Following use, field equipment will be properly decontaminated before it is returned to

Fields. Critical spare parts such as tape, paper, pH probes, electrodes, batteries, and battery chargers will

be kept on site to minimize equipment downtime. Backup instruments, equipment, and additional spare

parts will be available on site or within a 1-day shipping period to avoid delays in the field schedule.

2.6.3 Laboratory Instruments

STAT will follow a maintenance schedule for each instrument used to analyze samples collected from the

watershed areas. All instruments will be serviced at scheduled intervals necessary to optimize factory

specifications. Routine preventative maintenance and major repairs will be documented in a maintenance

logbook. STAT also maintains an equipment tracking form for each instrument that documents identity;

date in service; manufacturer’s name, model number, and serial number; current location; and

preventative maintenance schedule. A list of critical spare parts for each instrument will be identified by

the STAT and requested from the manufacturer. These spare parts will be stored at the laboratory for

availability and use to reduce downtime.

2.7 INSTRUMENT CALIBRATION AND FREQUENCY

This section describes procedures for maintaining the accuracy of field equipment and laboratory

instruments used for field tests and laboratory analyses. The equipment and instruments should be

calibrated before each sampling event or, when not in use, on a scheduled periodic basis.



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2.7.1 Calibration of Field Instruments

This section describes calibration procedures and frequency for maintaining the accuracy of instruments

used for obtaining field measurements. All calibrations along with instrument serial numbers will be

documented and recorded in field logbooks.

Each instrument will be examined to certify that it is in good operating condition. This examination

includes checking the manufacturer’s operating manual to ensure that all maintenance requirements are

being observed. Field notes from previous sampling trips will be reviewed so that notations on any prior

equipment problems are not overlooked and so that all necessary repairs to equipment have been carried

out.

Calibration of field instruments will be performed at the intervals specified by the manufacturer or more

frequently as conditions dictate. Field measurements will be made with a Horiba U-10 Water Quality

Checker or similar device. If an internally calibrated field instrument fails to meet calibration/checkout

procedures, it will be returned to the manufacturer for service. The Horiba U-10 Water Quality Checker

can be calibrated automatically for all four parameters (pH, conductivity, turbidity, and DO)

simultaneously, or manual calibration can be completed for each parameter individually. According to the

instruction manual included in Attachment B, manual calibration is more accurate, but the auto-

calibration procedure should be sufficient for most measurement operations. Tetra Tech will perform

manual calibration before and after each sampling event and will use the auto-calibration procedure as

necessary. Calibration procedures are included in the instruction manual in Attachment B, and a summary

of manual calibration procedures for each parameter is presented below.

pH

1. Wash the unit’s probe two to three times using deionized or distilled water.

2. Complete a zero calibration using a pH 7 standard solution (use the “UP” and “DOWN” keys toselect the value of the pH 7 standard solution at the temperature of the sample).

3. Complete a span calibration using either a pH 4 or pH 9 standard solution (use the “UP” and“DOWN” keys to select the value of the standard solution at the temperature of the sample).



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Conductivity

1. Prepare three concentrations (0.005, 0.05, and 0.5 N) of potassium chloride standard solution forthe span calibration.


3. Complete a zero calibration in atmospheric air; no solution is needed.

4. Complete a span calibration by washing the probe two to three times in the standard solution andplacing the unit probe in a beaker of each standard solution to calibrate the meter at a range of0 to 1, 1 to 10, and 10 to 100 millisiemens per centimeter

Turbidity

1. Prepare a standard solution of 800 Nephelometric turbidity units for the span calibration.


3. Complete a zero calibration using deionized or distilled water.

4. Complete a span calibration using the standard solution of 800 Nephelometric turbidity units.

DO

1. Prepare a sodium sulfite solution for the zero calibration.

2. Complete the zero calibration using the sodium sulfite solution.

3. Complete the span calibration using deionized or tap water that has been saturated with oxygen inair from an air pump.

Field measurements will be made with Flowatch Flow Meter or similar device. If an internally calibrated

field instrument fails to meet calibration/checkout procedures, it will be returned to the manufacturer for

service. The instruction manual is included in Attachment B.

2.7.2 Calibration of Laboratory Equipment

All laboratory equipment will be calibrated according to the STAT QA manual (see Attachment A).

Instruments will be calibrated prior to use to establish its ability to meet the QC guidelines contained in

the test method for the instrument. Routine calibration is conducted at the frequency recommended in the

test method.

Laboratory analyses will be conducted in accordance with approved analytical methods and will follow

the calibration procedures and frequencies specified in the relevant method. Calibration procedures and

requirements will also be provided, as appropriate, for laboratory support equipment, such as balances,



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mercury thermometers, pH meters, and other equipment used to take chemical and physical

measurements. All laboratory equipment used to analyze samples collected under this project will be

calibrated based upon written SOPs maintained by the laboratory. Calibration records (including the dates

and times calibration and the names of the personnel performing the calibration) will be filed at the

location where the analytical work is performed and maintained by the laboratory personnel performing

QC activities.

2.8 REQUIREMENTS FOR INSPECTION AND ACCEPTANCE OF SUPPLIES ANDCONSUMABLES

Supplies and consumables can be received either prior to sampling or at the sampling site. When supplies

are received prior to sampling, the project manager or designee will inspect the condition of all supplies

before the supplies are accepted for use on a project. If the supplies do not meet the acceptance criteria,

deficiencies will be noted on the packing slip and purchase order. The item will be returned to the vendor

for replacement or repair. When supplies are received in the field, the sampling team leader will inspect

them in accordance with the acceptance criteria. Any deficiencies or problems will be noted in the field

logbook. Deficient items will be returned for immediate replacement.

STAT will provide certified clean containers for all analyses. The containers will be inspected prior to

use, and any defective containers will be replaced before the sampling event begins.

Solvents and reagents used by the laboratory in all analytical procedures will be documented in a

laboratory logbook. At a minimum, information regarding the manufacturer, lot number, date received,

date opened, and date prepared should be included. Solvents and reagents will be tested for contamination

before use. The results of this procedure and any other quality inspections will be documented in a

laboratory logbook.

The laboratory will regularly check the temperatures of all refrigerators used to store project samples,

standards, and other consumables, and will document temperatures measured in a laboratory logbook.

Thermometers used to monitor temperatures will be subject to verification against a National Institute of

Standards and Technology-certified thermometer at a frequency prescribed in the laboratory’s QA

manual. Unless otherwise directed by the project manager, unused samples will be stored for a minimum

of 60 days following submittal of analytical data.



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2.9 NON-DIRECT MEASUREMENTS

Tetra Tech is collecting new data to fill in data gaps identified and supplement previously collected data

discussed in the Stage 1 reports. The previously collected data for each segment were obtained from the

following sources:

U.S. Department of Agriculture (USDA)

USEPA

U.S. Geological Survey (USGS) National Water Information System (NWIS) database

IEPA

The Stage 1 report for the watershed summarizes and analyzes existing water quality data. The report

recommends additional data collection through sampling because the existing data were not recent (within

the past 10 years). The sampling sites and frequencies for this project are based on Stage 1 report

recommendations. The samples will be primarily collected from existing sites as shown in Table 4 and

Figures 3 and 4. The existing and new data will be combined for TMDL development.

2.10 DATA MANAGEMENT

Data for this project will be obtained from a combination of sources, including field measurements and

laboratory analyses of collected water samples. The data gathering process requires a coordinated effort

and will be conducted by project staff members in conjunction with all potential data producers.

The Tetra Tech sampling team leader will be responsible for review, transfer, and storage of all data

collected in the field. The sampling team leader will maintain documentation of sampling, logging, and

field measurements, and will note any deviations from the QAPP or SOPs.

Data obtained from STAT will be in the form of an electronic data deliverable in addition to the required

hard-copy analytical data package. Formal verification (or validation) of data will be conducted before

associated results are presented or used for subsequent activities. Tetra Tech will validate 10 percent of

the analytical data to ensure that the confirmatory data are accurate and defensible, unless otherwise

directed by IEPA. As a part of the data validation process, the electronic data deliverables will be

reviewed against the hard-copy deliverables to ensure the accurate transfer of data. In addition, the hard



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copy will be evaluated for errors in the calculation of results. After the data validation, standard data

qualifiers can be placed on the data to indicate data usability. These qualifiers will be placed into the

electronic data file. Upon approval of the data set with the appropriate data qualifiers, the electronic data

will be released to the project manager for reporting.

After data validation and release of data, the project manager will use the data for project report

preparation. Tetra Tech will compile all relevant and verified laboratory analytical data into an electronic

database using Microsoft Access or Excel 2000. The analytical results will be evaluated for QA/QC and

reduced for assessment purposes. Data will be evaluated throughout the project to ensure that procedures

are adequate and numbers are reasonable. In addition, Tetra Tech will organize laboratory data into a

tabular format that can easily be incorporated into a Geographic Information System (GIS). Tetra Tech

will provide field data in a format consistent with the data requirements of the TMDL project. All data

will be stored in a specific project folder on Tetra Tech’s internal drive. The drive is password protected

with only Tetra Tech personnel having access. Tetra Tech maintains project documents and records for a

minimum of 10 years.



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3.0 ASSESSMENT AND OVERSIGHT

This section discusses assessment and oversight reports of field and laboratory activities during data

collection and analysis. Section 3.1 includes assessment and response actions, and Section 3.2

summarizes reports to management.

3.1 ASSESSMENT AND RESPONSE ACTIONS

Assessments of field and laboratory procedures are conducted to support data quality and encourage

continuous improvement in the systems that support environmental data collection. This section discusses

both field and laboratory assessments as well as corrective action procedures to any QA issues.

3.1.1 Field Assessments

Generally, field assessments or audits are conducted early in the project so that any quality issues can be

resolved before large amounts of data are collected; however, no assessments or audits have been planned

or budgeted for this project. If IEPA desires to conduct its own assessments of project activities, the Tetra

Tech project manager will coordinate with the IEPA WAM regarding the times and locations of the

assessments.

In lieu of an assessment or audit, Tetra Tech will conduct a procedural review to coincide with the first

sampling event. The procedural review will be conducted by the project manager and QA officer with the

sampling staff prior to data collection and will cover sample collection and handling techniques, SOPs

and documentation requirements, health and safety, and any unique aspects of this project.

3.1.2 Laboratory Assessments

Performance and system assessments can be conducted to audit analytical work. Performance assessments

are quantitative checks on the quality of a measurement system. Performance assessments for a laboratory

may be accomplished by submitting reference materials as blind reference samples, which are samples

with known concentrations that are submitted to a laboratory without informing the laboratory of the

known concentration. System assessments are qualitative reviews of different aspects of analytical work

to check on the use of appropriate QC measures and the functioning of the QA system. No laboratory

assessments are currently funded or scheduled for this project; however, IEPA could conduct a laboratory

performance or system assessment on its own.



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3.1.3 Field Corrective Action Procedures

If an assessment is conducted and findings are made indicating problems, field corrective action

procedures will depend on the type and severity of the finding. Tetra Tech classifies assessment findings

as either deficiencies or observations. Deficiencies are findings that may have a significant impact on data

quality and that will require corrective action. Observations are findings that do not directly affect data

quality but are suggestions for consideration and review. The project manager, sampling team leader, and

QA officer will hold a teleconference to discuss any deficiencies and the appropriate steps to resolve each

one by completing the following:

Determine when and how the problem developed

Assign responsibility for problem investigation and documentation

Select the corrective action to eliminate the problem

Develop a schedule for completing the corrective action

Assign responsibility for implementing the corrective action

Document and verify that the corrective action has eliminated the problem

Notify IEPA of the problem and the corrective action taken

3.1.4 Laboratory Corrective Action Procedures

Internal laboratory procedures for corrective action and descriptions of out-of-control situations that

require corrective action are contained in the laboratory QA manual in Attachment A. At a minimum,

corrective action will be implemented when any of the following three conditions occurs: (1) control

limits are exceeded, (2) method QC requirements are not met, or (3) sample holding times are exceeded.

The laboratory will report out-of-control situations to Tetra Tech within 2 working days after they are

identified. In addition, the laboratory project manager will prepare and submit a corrective action report to

the Tetra Tech project manager. This report will identify the out-of-control situation and the steps that the

laboratory has taken to rectify the situation and to prevent its recurrence.



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3.2 REPORTS TO MANAGEMENT

Effective management of environmental data collection operations requires timely assessment and review

of measurement activities. It is essential that open communication, interaction, and feedback be

maintained among all project participants, including (1) the Tetra Tech QA and QC officers, project

manager, and sampling team leader; (2) the STAT laboratory project manager and QA officer, and (3) the

IEPA WAM and QA officer, as appropriate. The sampling team leader will notify the project manager

and Tetra Tech QC officer of any QA issues related to field sampling activities and will discuss any

necessary corrective actions to resolve the issues. If there are significant quality issues, the Tetra Tech

QAO may be consulted to initiate corrective action investigation and identification of potential remedies,

but most corrective actions are readily addressed at the task level between the QCO and sampling team

leader in consultation with the project manager, and will be discussed in subsequent quality assurance

discussion in data reports. The STAT project manager will notify the Tetra Tech project manager if any

significant problems occur during sample analysis. The Tetra Tech project manager will prepare monthly

progress reports for IEPA that will address any QA issues and facilitate timely communication of these

issues.



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4.0 DATA VALIDATION AND USABILITY

This section describes the procedures used to review and verify field and laboratory data collected.

Section 4.1 discusses data review, verification, and validation. Section 4.2 includes verification and

validation methods. Section 4.3 addresses reconciliation with DQOs.

4.1 DATA REVIEW, VERIFICATION, AND VALIDATION

Validation and verification of data generated during field activities are essential to obtaining data of

defensible and acceptable quality. Field and laboratory measurement data reduction and review

procedures and requirements are specified in SOPs in Attachment B.

Field personnel will record, in a field logbook and data collection sheets, all raw data from chemical and

physical field measurements. The project manager has primary responsibility for (1) verifying that field

measurements were made correctly, (2) confirming that sample collection and handling procedures

specified in the QAPP were followed, and (3) ensuring that all field data reduction and review procedures

requirements are followed. The project manager is also responsible for assessing preliminary data quality

and for advising IEPA of any potential QA/QC problems with field data.

STAT will complete data reduction for laboratory measurements and will complete an in-house review of

all laboratory analytical results. The laboratory QA officer will be responsible for ensuring that all

laboratory data reduction and review procedures follow the requirements stated in this QAPP. The

laboratory QA officer will also be responsible for assessing data quality and for advising the Tetra Tech

QA officer of possible QA/QC problems with laboratory data.

4.2 VERIFICATION AND VALIDATION METHODS

This section outlines the basic data validation procedures that will be followed for all field and laboratory

measurements. The following subsections identify personnel who are responsible for data validation, and

general data validation procedures.



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4.2.1 Data Validation Responsibilities

Tetra Tech is responsible for validation of analytical data provided by STAT. The QA officer has primary

responsibility for coordinating Tetra Tech’s data validation activities. Tetra Tech will validate 10 percent

of all STAT laboratory data. Data validation will be completed by one or more experienced data

reviewers.

4.2.2 Data Validation Procedures

Tetra Tech data reviewers will conduct a systematic review of the data on the basis of spike, duplicate,

and blank sampling results provided by the laboratory. The data review will identify any out-of-control

data points and omissions. Tetra Tech data reviewers will evaluate laboratory data for compliance with

the following information:

Holding times

Blanks

MS/MSD recovery results

LCS results

Field duplicate sample results

Other laboratory QC requirements specified by the method

Detection limits

Analyte quantitation

Sample results verification

Overall assessment of data for a sample delivery

Tetra Tech will review analytical data in general accordance with USEPA’s “National Functional

Guidelines for Superfund Inorganic Data Review” (USEPA 2013). In addition, the QC requirements set

out in this document and the analytical methods will be used as criteria for validation.

4.3 RECONCILIATION WITH DATA QUALITY OBJECTIVES

After water quality data have been reviewed and results verified and validated in accordance with the

procedures described above, the data must be further evaluated to determine whether the DQOs have been

met. Tetra Tech will systematically assess data quality and data usability. This assessment may include

the following:



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Review of the sampling design and sampling methods to verify that these were implemented asplanned and are adequate to support project objectives

Review of project-specific data quality indicators for precision, accuracy, representativeness,completeness, comparability, and quantitation limits to determine whether acceptance criteriahave been met

Review of project-specific DQOs to determine whether they have been achieved by the datacollected

Evaluation of any limitations associated with the decisions to be made based on the data collected

Because this project is intended to supplement existing data and fill data gaps identified in the Stage 1

reports, data collected using methods specified in this QAPP should be sufficient for TMDL development

of the segments discussed in Section 1.3. The final report for the project will discuss any potential

impacts of the review findings on data usability and will clearly define any limitations associated with the

data and how any such limitations might affect the development of TMDLs.



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REFERENCES

Tetra Tech. 2014. “Pecatonica River Total Maximum Daily Load and Load Reduction Strategies.”February.

U.S. Environmental Protection Agency (USEPA). 2006. “Guidance on Systematic Planning Using theData Quality Objectives Process (QA/G-4).” EPA/240/B-06/001. Office of EnvironmentalInformation (OEI). Washington, DC. February.

USEPA. 2001. “USEPA Requirements for Quality Assurance Project Plans (QA/R-5).” EPA/240/B-01/003. OEI. Washington, DC. March. Reissued May 2006.

USEPA. 2013. “National Functional Guidelines for Inorganic Superfund Data Review.” EPA 540-R-13-001. Office of Superfund Remediation and Technology Innovation. Washington, DC. October.


ATTACHMENT

ATTACHMENT A

STAT ANALYTICAL CORP. QUALITY ASSURANCE MANUAL AND SOPs

This attachment includes the following documents:

1. STAT Quality Assurance Manual

2. STAT - SOP: Total Kjeldahl Nitrogen (TKN) – Block Digestion with Semi-Automated Skalar

3. STAT - SOP: Total Ammonia Analysis

4. STAT – SOP: Automated NO3/NO2, NO2 AND NO3 Analysis by SM 4500-NO3 I

5. STAT - SOP: Total Dissolved Solids(TDS), Total Suspended Solids(TSS), and Total

Solids(TS)


ATTACHMENT

ATTACHMENT B

INSTRUMENT INSTRUCTION MANUALS AND SOPs

This attachment includes the following documents:

1. Horiba U-10 Instruction Manual

2. Flowatch Instruction Manual

3. Tetra Tech SOP No. 009 - Surface Water Sampling

4. Tetra Tech SOP No. 010 - Groundwater Sampling

5. Tetra Tech SOP No. 011 – Field Measurement of Water Temperature

6. Tetra Tech SOP No. 012 – Field Measurement of pH

7. Tetra Tech SOP No. 013 – Field Measurement of Specific Conductance

8. Tetra Tech SOP No. 024 - Recording of Notes in Field Logbook

9. Tetra Tech SOP No. 061 - Field Measurement of Groundwater Indicator Parameters

Analysis Corporation

STAT

Policy Statement

STAT Analysis Corporation This Quality Manual summarizes the policies and operational procedures associated with STAT Analysis Corporation in Chicago, Illinois. Specific protocols for sample handling and storage, chain-of-custody, and laboratory analysis, data reduction, corrective action, and reporting are described. All policies and procedures have been structured in accordance with the current National Environmental Laboratory Accreditation Conference (NELAC) standards (current as of the date of this publication), current American Industrial Hygiene Association (AIHA-LAP, LLC) Policy (current as of the date of this publication), National Voluntary Laboratory Accreditation Program (NVLAP) standards adopted in National Institute of Standards and Technology (NIST) Handbook 150, 2006 Edition, the requirements of the Consumer Products Safety Commission (CPSC), and International Standards Organization/International Electrotechnical Commission (ISO/IEC) 17025 (2005) regulations, guidance, and technical standards. The laboratory management is committed to comply with these standards. NVLAP has issued specific requirements for referencing the NVLAP term, logo, and symbol (NIST Handbook 150, 2006). STAT uses the NVLAP term and symbol for purposes of announcing the accredited status and for use on reports that describe testing within the scope of accreditation. STAT complies with the conditions detailed in NIST Handbook 150, Annex A. STAT Analysis does not use or reference the logo from any other accrediting authority. This manual has been prepared in accordance with the guidance documents available from Accreditating organizations. Further details on these policies and procedures are contained in SOPs and related documents. This Quality Manual, SOPs, and related documentation describe the laboratory’s management system policies related to quality. The purpose of this Quality Assurance Manual is to describe the quality management system in place at STAT Analysis Corporation. It is STAT’s policy to keep abreast of policy revisions issued by accrediting agencies and to implement changes within a reasonable time frame by revising this QAM and other appropriate SOPs in order to be compliant with existing accrediting agency policies. The QA Director monitors and tracks the schedule for policy updates based on notification by accreditation agencies. After identifying the changes to be addressed, the management team meets to create, plan and develop the implementation schedule. The QA Director oversees the implementation within the scheduled deadline. STAT Analysis Corporation performs chemical analyses for inorganic and organic constituents, microbiological analyses, and asbestos analyses in various matrices and products. The objective of STAT Analysis Corporation’s quality management system is to produce data that is scientifically valid and of known and documented quality in accordance with standards developed by NELAC, ISO/IEC 17025, AIHA-LAP, LLC, NIST/NVLAP, CPSC and any applicable federal or state government entity’s regulations or requirements. STAT Analysis Corporation conducts all business with integrity and in an ethical manner. The laboratory management is committed to good professional practice, to the quality of its environmental

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testing in servicing its customers, and to continually improve the effectiveness of the management system. All personnel involved with testing activities within the laboratory must review this quality manual. It is the responsibility of each staff member, manager, director, and owner to perform their duties with the highest ethical standards and professional conduct to ensure compliance with this Quality Manual and related documentation. Surendra N. Kumar, Ph.D. Bruce Gallant, Laboratory President/CEO Director





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Table of Contents 1. INTRODUCTION.......................................................................................................................7

2. LABORATORY ORGANIZATION and MANAGEMENT STRUCTURE ........................8 2.1 Staff Qualifications and Responsibilities...................................................................................8 2.2 Approved Signatories ..............................................................................................................12 2.3 New Work Requirements.........................................................................................................13 2.4 Departures from Policies and Procedures ................................................................................13

3. DOCUMENT CONTROL........................................................................................................14

4. GENERAL QUALITY CONTRO L PROCEDURES ..........................................................14 4.1 Introduction..............................................................................................................................15 4.2 Laboratory Apparatus and Instruments ...................................................................................15 4.3 Laboratory Supplies.................................................................................................................16 4.4 Laboratory Hazardous Wastes Handling and Disposal Procedures.........................................17 4.5 Selection and Purchasing of Services and Supplies.................................................................17

5. VERIFICATION PROCEDURES..........................................................................................18 5.1 Introduction..............................................................................................................................18 5.2 Traceability of Calculations.....................................................................................................18 5.3 Performance Testing................................................................................................................21 5.4 Precision ..................................................................................................................................26 5.5 Accuracy ..................................................................................................................................27 5.6 Annual Analytical Performance Summary..............................................................................27

6. METHODOLOGY ...................................................................................................................28

7. PHYSICAL FACILITIES and INSTRUMENTATION .......................................................28 7.1 Facilities...................................................................................................................................28 7.2 Equipment................................................................................................................................29 7.3 Equipment Maintenance Program ...........................................................................................29

8. SAMPLE RECEIPT and ACCEPTANCE.............................................................................30 8.1 Introduction..............................................................................................................................30 8.2 Sample Acceptance Policy ......................................................................................................31 8.3 Sample Acceptance Policy Differences...................................................................................31 8.4 Chain-of-Custody Form...........................................................................................................31 8.5 Standard Operating Procedure – Sample Receipt/Custody .....................................................31 8.6 Policy for Disposal of Laboratory Samples.............................................................................31

9. SAMPLE RECORDS, DATA REVIEW and DATA HANDLING......................................32 QA 001 Quality Assurance Manual

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9.1 Sample Logging.......................................................................................................................32 9.2 Analytical Data Review and Handling ....................................................................................36 9.3 Computerized Analytical Data System....................................................................................33 9.4 Reporting .................................................................................................................................35

10. CORRECTIVE AND PREVENTIVE ACTIONS .................................................................35 10.1 Corrective Action……………………………………………………………………....35 10.2 Preventive Action………………………………………………………………..……..36

11. QUALITY EXCEPTION/ CASE NARRATIVE ...................................................................37

12. COMPLAINTS .........................................................................................................................37

13. CONFIDENTIALITY ..............................................................................................................37

14. INTERNAL AUDITS ...............................................................................................................37

15. MANAGEMENT REVIEW of the QUALITY SYSTEM.....................................................38

16. TRAINING ................................................................................................................................38

17. DATA INTEGRITY .................................................................................................................38

18. SUB-CONTRACTING.............................................................................................................40

19. LABORATORY SAFETY .......................................................................................................40 19.1 Introduction..............................................................................................................................40 19.2 General.....................................................................................................................................40 19.3 Sample Receiving and Login...................................................................................................41

20. DEFINITIONS ..........................................................................................................................42

Appendix 1 Summary of Changes from QAM Revision 11………………………………………61 Appendix 2 Organizational Chart....................................................................................................64 Appendix 3 STAT SOPs....................................................................................................................65 Appendix 4 Instrumentation.............................................................................................................74 Appendix 5 Sample Bottle Types and Preservation .......................................................................82 Appendix 6 Sample Acceptance Policy............................................................................................86 Appendix 7 Ethics Policy and Data Integrity Agreement..............................................................88





STAT

Attachment 1 Facility Diagram............................................................................................................90 Attachment 2 Chain of Custody for NELAC Samples ......................................................................91 Attachment 3 Chain of Custody for Lead AIHA-LAP, LLC Samples.............................................92 Attachment 4 Chain of Custody for Asbestos Samples .....................................................................93 Attachment 5 Chain of Custody for Microbiology Samples .............................................................94 Attachment 6 Example of Notice of Confidentiality for Emails .......................................................95 Attachment 7 Example of Notice of Confidentiality for Facsimiles .................................................96





STAT

1. INTRODUCTION

It is the policy of STAT Analysis Corporation (STAT) to produce analytical results of the highest degree of repeatability, precision, and accuracy in a laboratory that employs state of the art analytical instrumentation operated by highly skilled, qualified, motivated, and responsible analysts. The laboratory management is committed to follow NELAC, AIHA-LAP, LLC,DOD, CPSC NIST/NVLAP, and ISO/IEC 17025 requirements. This Quality Manual is based on NELAC, ISO 17025, NIST/NVLAP and AIHA-LAP, LLC standards. All employees are to be trained and committed to following the requirements herein. The primary purpose of this document is to establish and maintain uniform operational and quality control guidelines for operations that affect the quality of the data produced in this laboratory. The establishment of, and adherence to, uniform elements of an intra-laboratory quality control program are essential to the production of reliable analytical data. The QA/QC requirements for all relevant preparation and analytical methods, and any verified modifications of such, used in this laboratory are described in this manual or described in relevant Standard Operating Procedures (SOPs). While the implementation of a quality assurance policy is a management function, each individual has a responsibility for the operational aspects of quality control. It is the individual responsibility of each analyst and his/her supervisor to monitor quality control indicators and to provide for corrective actions when necessary. These corrective actions can range from routine corrective action to stopping work until the nonconformity has been resolved. Appropriate communication processes, such as training, seminars, and one-on-one instructions are used to train personnel regarding the effectiveness of the management system. Personnel are trained regarding relevance and importance of their activities and how they contribute to the achievement of the objectives of the management system. Personnel are trained on the importance of meeting customer requirements as well as statutory and regulatory requirements. Laboratory management ensures that the integrity of the management system is maintained when changes are planned and implemented. This manual and the quality control protocols described herein are not to be viewed as all-inclusive. Rather, they serve as a basic foundation on which to build stronger quality assurance/quality control program. It is the policy of this laboratory to use the most stringent controls whether dictated by methodologies and SOPs, accrediting bodies, or Quality Assurance Project Plans (QAPP). STAT reviews the QAM annually. The QAM is updated whenever the need for changes or updates is required. Each SOP will be reviewed whenever the need for changes or updates are required. The need for changes may arise due to availability of new or improved technologies or changes published in the reference method.. The current revision of the SOP will be compared to the reference method for technical and procedural merit to determine if any changes are necessary. Furthermore, as part of Internal Audit, each SOP is reviewed and need for changes or updates determined.





STAT

This revision (Rev. 14) of the QAM was developed by modifying Rev.13 of the QAM. Summary of the changes made is presented in Appendix 1. An electronic file containing new text in color and deleted text identified as strike-outs is archived on the network. 2. LABORATORY ORGANIZATION and MANAGEMENT STRUCTURE

Hi-Tek Environmental Inc., d/b/a, STAT Analysis Corporation (STAT), FEIN 36-4128978, was incorporated in December 1996. The laboratory is located at 2242 W. Harrison Street, Chicago, IL 60612. An electronic keypunch provides limited access to this building. It is company policy that all employees must be free from commercial, financial and other pressures that might adversely interfere with the quality of their work. All employees must be aware that customer relations and service are an integral part of their job description. To prevent the possibility of staff being placed under pressure by customers or other sections of the laboratory, reporting relationships have been established to isolate staff from this pressure. The responsibilities of the employee in dealing with the customer will be specified in order to maintain independence of judgment and integrity. The Organizational Chart for STAT is shown in Appendix 2. 2.1 Staff Qualifications and Responsibilities This section will show that STAT have personnel, who, irrespective of other responsibilities, have the authority and the resources to fulfill their responsibilities, including the development, implementation, maintenance, and continuous improvement of the management system. They also have the resources to identify departures from the management system or other SOPs and to initiate corrective actions to minimize or prevent such departures.

2.1.1 President/CEO- ensures that those who hold the positions of Laboratory Director, Technical Manager, and Quality Assurance Director , meet the requirements of NELAC, ISO 17025, NIST/NVLAP, and AIHA-LAP, LLC.

2.1.2 Key Personell

2.1.2 .1 Laboratory Director

Duties The Laboratory Director has the overall responsibility for analytical and operational activities of the laboratory. The director will be responsible for supervision (and appointment of supervisors) of laboratory personnel and ensuring that sufficient numbers of qualified staff are employed to supervise and perform the work of the laboratory. The Director will be responsible for production and quality of data reported by the laboratory.





STAT

Qualifications The Laboratory Director should have a minimum of 2 years experience managing a laboratory. He or she shall have earned a bachelor’s degree, or higher, in chemistry.

2.1.2.2Technical Manager Duties The Technical Manager, under the general direction of the laboratory director, is responsible for the appropriateness of the technical background of all tests performed by the laboratory and to insure the laboratory’s compliance with the NELAC and ISO 17025 standards.. The development, validation and approval of new methods is overseen by the Technical Manager in coordination with Department Managers and the Quality Assurance Director. The Technical Manager has the responsibility to monitor performance standards in quality assurance and quality control and monitoring the validity of the analyses performed and the data generated in the laboratory to assure quality data. This individual is part of the whole corrective action process and is responsible for the final approval of any corrective actions performed at the laboratory. He/she shall be available during at least 50 percent of the laboratory operating hours to address technical issues for laboratory staff and customers and acceptable onsite supervision must be demonstrated. The Technical Manager maintains the LIMS. The Technical Manager provides proper educational direction to laboratory staff. The Technical Manager’s responsibilities meet those defined for the Technical Manager in NELAC Chapter 4.1.1.1, NIST Handbook 150 Section 4.1, and AIHA-LAP, LLC Section 2A.5.1.1

The Technical Manager ensures that all laboratory personnel possess the necessary educational and technical background appropriate to the job they perform. By signing the Demonstration of Capability statement, the Technical Manager certifies that the laboratory analyst has met the requirements to perform the specific test method analysis.

In the event that the Technical Manager is absent for more than 15 consecutive calendar days, the Technical Manager will appoint the Laboratory Director as a temporary replacement. In the event that the Technical Manager is absent for more than 20 business days (for AIHA-LAP, LLC) or for more than 35 business days (For TNI/NELAC), the acting Technical Manager or the Quality Assurance Director will notify the Accrediting Authorities (IEPA, AIHA-LAP, LLC, NVLAP, ORELAP, Utah DEP, Kentucky DEP) in writing within 20 business days. This notification requirement shall be in effect if the Technical Manager,





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the EMPAT Technical Manager, the QA Director, the EMPAT QA Manager, or an analyst who is the only staff member that performs a test, are absent for reasons of extended family leave, illness, temporary disability, etc.

Qualifications The Technical Manager should have a minimum of 4 years experience in an environmental laboratory. He or she shall have earned a bachelor’s degree, or higher, in chemistry with a minimum of 24 college semester credit hours in chemistry. 2.1.2.3 EMPAT Technical Manager Duties The EMPAT Technical Manager, under the general direction of the laboratory director, is responsible for the appropriateness of the technical background of all tests performed by the microbiological laboratory. The EMPAT Technical Manager has the responsibility to monitor performance standards in quality assurance and quality control and monitoring the validity of the analyses performed and the data generated in the laboratory to assure quality data. The EMPAT Technical Manager is located on site and has the responsibility for the function and administration of the day-to-day operation of the microbiological laboratory. The EMPAT Technical Manager provides proper educational direction to microbiological laboratory staff. The EMPAT Technical Manager, or designee, functions as the approved signatory. Qualifications The EMPAT Technical Manager should have a minimum of 2 years experience in a microbiological environmental laboratory. He or she shall have earned a bachelor’s degree, or higher, in microbiology, biology, or related life science, with a minimum of 20 college semester credit hours in microbiology. 2.1.2.4 Quality Assurance Director Duties: The Quality Assurance Director (or Manager) has the responsibility for the maintenance, coordination and continuous improvement of the Quality Assurance and Quality control (QA/QC) program for the laboratory and to insure the laboratory’s compliance with the NELAC and ISO 17025 standards. The QA Director is responsible for training all new employees on their first day of employment in the importance of the QAM, the ethics policy and other issues as specified in SOP 1230 Section 14.1. The QA Director functions as the Data Integrity officer and reviews and approves all analytical SOPs or test methods. The QA Director is responsible for conducting or arranging an annual internal audit of the entire laboratory operation and technical systems, as described in SOP 006 Management Review of the Quality System, to gauge the effectiveness of the Quality System and to determine if opportunities for improvement are present.





STAT

The Quality Assurance Director is responsible for the day-to-day monitoring of the laboratory quality systems as well as the data review procedures for the laboratory and also acts as the Lab’s Data Integrity Officer by implementing a program to detect and deter illegal or improper actions by the laboratory or staff. The QA Director reports directly to the President/CEO and is independent from the Technical Manger.

In the event that the QA Director is absent for more than fifteen consecutive calendar days, the President/CEO will appoint either the Technical Manager or the Laboratory Director as a temporary replacement.

Qualifications The Quality Assurance Director must have a minimum of a bachelor’s degree in natural or physical sciences and have documented training or experience in QA/QC and statistical procedures. He/she also must have a general knowledge of the analytical test methods. 2.1.2.5 EMPAT Quality Assurance Manager

Duties The EMPAT Laboratory Quality Assurance Manager has the responsibility for the maintenance and coordination of the quality assurance and quality control (QA/QC) program for the microbiological laboratory. The EMPAT Laboratory QA Manager is responsible for the data review procedures for the laboratory and re-analyzing five percent of all samples. The EMPAT Laboratory QA Manager will also provide genus/species identification when needed. The EMPAT Laboratory QA Manager is responsible for conducting an annual internal audit of the microbiological laboratory operation. Qualifications The EMPAT Laboratory QA Manager must have a minimum of a bachelor’s degree in microbiology, biology, or related life science. The EMPAT Laboratory QA Manager must have a minimum of six months of relevant microbiological laboratory experience and familiarity with microbiological QA/QC. ` 2.1.2.6 Department and Project Managers

Duties

Department Managers are responsible for supervising analysts, analysts in training, and technicians. They are responsible for reviewing and verifying data produced by analysts in training and technicians. Project Managers are responsible for primary customer contact. They review and approve customer’s reports for completeness and adherence to all project specific criteria.





STAT

Qualifications Department Managers must have a minimum of a bachelor’s degree in natural or

physical sciences, enough course work to qualify for a minor in chemistry, and have at least one year of experience in the analyses pertaining to the applicable fields of testing.

Project Managers must have a minimum of a bachelor’s degree in natural or

physical sciences and have at least one year of experience in the analyses of environmental samples.

2.1.3 Non-Key Personnel

2.1.3.1 Analysts

Duties The analyst is responsible, under the direction of the Department Manager, for the applicable analyses of the samples submitted to the laboratory. Analysts shall be responsible for complying with all quality assurance and quality control requirements pertaining to their technical functions.

Qualifications The analyst shall have a bachelor’s degree (or equivalent), or an associates degree with one year experience, or greater than two years experience with experience in natural or physical sciences. Analysts will have one year of full-time employment in the environmental testing field, and have documented proof of technical proficiency via in-house training at STAT, including an Initial Demonstration of Capability (IDOC). Analysts shall have demonstrated ability to produce reliable results through accurate analysis of certified reference materials (CRMs), proficiency testing samples, or in-house quality control samples. Their performance must be documented. Instrumentation Analysts must have four hours of equipment manufacturer training or two-week apprenticeship under an experienced analyst. 2.1.3.2 Analyst in Training

Analyst in training must meet the requirements of Technician while in process of meeting the requirements of Analyst. 2.1.3.3 Technician

Duties The technician is responsible for carrying out the designated activities related to the analysis of materials submitted to the laboratory and works under the direct supervision of the Department Manager or Analyst.





STAT

Qualifications The Technician shall have a minimum of a high school diploma or equivalent. Technicians will have documented proof of technical proficiency via in-house training at STAT, including an IDOC. Instrumentation Technicians must have four hours of equipment manufacturer training or two-week apprenticeship under an experienced analyst.

2.2 Approved Signatories

All analysts that have passed training for a particular analysis can sign off on data either as analyst or secondary review (as appropriate). All customer correspondence is to be signed either by the Laboratory Director, Technical Manager, Department Managers, or Project Managers as appropriate. For asbestos and microbiology, analysts sign reports. Quotes can be generated and signed by the President/CEO, Laboratory Director or Project Manager (unless specific approval is given to another employee by the named individuals). All bid proposals are to be signed by the President/CEO, Laboratory Director, Project Managers or designee.

2.3 New Work Requirements All new analyses must undergo a thorough review prior to release. The Laboratory Director, Technical Manager, Quality Assurance Director , and Department Manager may undertake this review. This review may include:

• Staff and appropriate equipment are available as well as appropriate workspace to perform the task.

• Standard Operating Procedure must be in place. • Initial Demonstration of Capability (IDOC) must be performed. • Method Detection Limit Study (if applicable) must be performed. • A Blind Quality Control Sample must be satisfactorily completed, if available.

The procedure to review new work and new test method analyses is outlined in SOP 220 Customer Service.

2.4 Departures from Policies and Procedures

All laboratory personnel are instructed to follow the policies and procedures as outlined in the Quality Assurance Manual and supporting laboratory documentation. On occasion, departures from these policies and procedures may be taken. Any such departures must be fully defined, documented, and approved by the Technical Manager or the President/CEO. If the departure is considered a permanent change, a new revision of the laboratory’s quality documentation may be necessary.





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Any modifications to reference test methods are listed in Section 5 of the test method SOPs. These modifications are approved by management as indicated by the signatures on the SOP cover page.

Minor modifications to test methods for particular samples are allowed if these modifications are fully documented. An example follows:

The test method SOP states that a 30-gram soil sample is extracted and analyzed for Semi-Volatile Organic compounds. The submitted sample weighs only 10 grams. The analyst notes in the logbook that the minimum amount of sample was not available for analysis. The customer agrees that the sample can be analyzed as submitted. The final reporting limit for this sample will be elevated due to limited sample size.

3. DOCUMENT CONTROL

All internal and external documents that form STAT Analysis Management System are tracked. Documents are assigned a unique document number, revision and effective date noted. Controlled documents (SOPs) are also listed with all individuals who have been issued these documents (including external customers). This document, QA 001 Quality Assurance Manual Revision 14, is a controlled document. The procedure to maintain and control laboratory documents is outlined in SOP 005 Document Control. Controlled copies of the SOPs, Quality Manual and other documents are located in each room in a controlled binder of the laboratory for personnel to use. The documents referenced in SOP 005 include software (e.g. excel spreadsheets and reporting templates, instrument operating software), instrument operation manuals, and other internal and external source documents. Lists of internal and external source documents, softwares, and instruction manuals are updated, if necessary, following annual review or following purchase of new equipment. As these documents are updated and revised, the QA department will replace each controlled copy with the revision in the controlled binders. The original hardcopy document is archived and all superceded controlled copies are destroyed (see SOP 240 Archiving). The computer file is archived via the computer network and will include all the changes to the document. Spreadsheets and other STAT generated electronic documents are tracked through the Master Document Spreadsheet List which is located in \\Harrison\d\Quality Control\\pinaki-littlefield\tracking\tracking-Master Document List, which contains spreadsheet title and revision number. All laboratory notebooks are considered to be controlled documents.

4. GENERAL LABORATORY PRACTICES All aspects of laboratory operations are documented in Standard Operating Procedures

(SOPs). Each page of these SOPs will contain 1) SOP Number, 2) Revision Number, 3) Effective Date, and 4) current page number of the total number of pages in the document. This is described in SOP 100, SOP on SOPs.

QA 001 Quality Assurance Manual




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4.1 Introduction Intrinsic to the production of quality analytical data is the quality of laboratory services available to the analyst. Without adequate quality control being exercised with regard to facilities, services, laboratory environment, instrumentation, and laboratory supplies, an analyst cannot be expected to produce reliable analytical data. Access to the laboratory is restricted to STAT employees only, unless accompanied by a STAT employee. Recognizing the necessity of maintaining control over general laboratory operation, the subsequent sections outline provisions for maintaining the quality laboratory support services.

4.2 Laboratory Apparatus and Instruments

All support equipment is maintained in proper working order. All water baths, refrigerators, freezers, ovens, balances, pH meters, thermometers, mechanical pipettes, and the conductivity meter must be verified in accordance with SOP 1040 General Laboratory Practices (GLP) and/or the analytical SOP. Where possible, calibration and reference standards, traceable to national standards of measurement, are used in the laboratory to calibrate and/or verify the test equipment. These calibration and reference standards are only used for calibration and/or verification purposes. The laboratory uses an independent calibration service to perform an annual check of the balances and an annual check of the mechanical pipettes. In addition, an independent calibration service is used to perform a calibration check of the NIST reference thermometer at least every five years or as required by the manufacturer or calibration certificate. Vendors and service suppliers need to provide traceability of their products to NIST or to another recognized national standard of measurement. Criteria for identifying valid service suppliers and vendors and determining valid products are discussed in SOP 1330, Purchasing. Instructions for support equipment operations are found in STAT SOP 1040 General Laboratory Procedures. 4.2.1 Water baths 4.2.2 Refrigerators and freezers 4.2.3 Ovens 4.2.4 Balances 4.2.5 pH meters 4.2.6 Thermometers

Unless otherwise specified by regulatory methodology, it is the policy of STAT to use only non-mercury containing thermometers in all laboratory operations.

4.2.7 Mechanical Pipettes . 4.2.8 Plastic Tubes





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4.2.9 Weights 4.2.10 Conductivity meter 4.2.9 4.2.11 Incubators 4.2.12 Autoclaves

Record temperature, pressure, and time maintained during each autoclave use per SOP 1130.

4.3 Laboratory Supplies

4.3.1 Glassware Glassware used in general laboratory operations must be of high quality borosilicate glass. Volumetric glassware must be of Class “A” quality, except where the method specifies plastic volumetric flasks. Procedures for cleaning laboratory glassware are described in STAT SOP 1020 Laboratory Glassware Cleaning.

4.3.2 Chemicals, Reagents, Solvents and Gases

The quality of chemicals, reagents, solvents, standards and gases used in the laboratory is determined by the sensitivity and specificity of the analytical techniques being used. Reagents of lesser purity than specified by a method will not be used.

Reagents, chemicals, solvents, and standard reference materials (excluding high-demand items) should be purchased in quantities to minimize extended shelf storage.

All reagents, chemicals, solvents, and standard reference materials are initialed and dated when received, when opened or prepared, and discard when outdated, or when evidence of discoloration or deterioration is detected (STAT SOP 1010 Analytical Standards and Reagents Receipt and Preparation).

4.3.3 Laboratory Reagent Water

The laboratory reagent water system is tap water that is processed through a carbon-filtering tank and two mixed-beds ion exchange tanks. This water is checked daily to ensure that it has at least 1 megohm-cm resistivity (≤ 1 umhos/cm conductivity) at 25oC and recorded in conductivity logbook (STAT SOP 4200 Conductivity and SOP 1040 General Laboratory Practices). Reagent water blanks are performed with each water batch to monitor for potential contamination.





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4.4 Laboratory Hazardous Wastes Handling and Disposal Procedures

It is the policy of STAT Analysis to collect, store, package, label, ship and dispose of hazardous wastes in a manner which ensures compliance with all Federal, State and local laws, regulations, and ordinances. These procedures are designed to minimize employee exposure to hazards associated with laboratory-generated hazardous wastes and to afford maximum environmental protection (STAT SOP 1130 Waste Disposal).

4.5 Selection and Purchasing of Services and Supplies Goods and services are purchased from qualified companies and individuals. The purchased items may be chemicals, consumable items, equipment, calibration services, repair services, sub-contract laboratory services, consultant services, and building and environmental services. The laboratory maintains a list of qualified and approved vendors, suppliers, sub-contractors, consultants, and contractors. Service suppliers are deemed qualified if they have ISO 17025 accreditation in combination with ISO Guide 34 and a certificate bearing the seal of accreditation from an ILAC signatory. Purchased supplies and reagents and consumable materials that affect the quality of tests and/or calibrations are not used until they have been inspected or otherwise verified as complying with ISO 17025 accreditation. Actions taken to check compliance are documented. A sub-contractor, usually a testing laboratory, provides test reports to STAT that is used to supplement the information sent to STAT’s customers. A sub-contractor may perform test methods that are not currently being performed at STAT, or may serve as an adjunct to the testing methodology already in place at STAT. Sub-contractors are deemed qualified if they possess accreditation from the National Environmental Laboratory Accreditation Program (NELAP), American Industrial Hygiene Association (AIHA-LAP, LLC), Environmental Laboratory Accreditation Program (ELAP), National Voluntary Laboratory Accreditation Program (NVLAP), American Association for Laboratory Accreditation (A2LA), or from some other nationally recognized accreditation body. If there is no independent means to qualify a potential vendor or supplier, the following procedure is used: Obtain qualification statements, obtain a list of references or customers, and send inquiries to these parties to obtain written information concerning the quality of materials and services rendered. Contact the Better Business Bureau (BBB) to determine if any complaints have been filed. A request or a purchase order may be made to a vendor to supply a small lot of material to be qualified using STAT in-house test methodology. A request or a purchase order may be made to a supplier to perform a service that will be independently verified by an already approved supplier. If this qualifications procedure is deemed successful, the vendor or supplier may be added to the approved list. The results of this evaluation is recorded on the Vendor Evaluation Form (SOP 1330 Purchasing, Form #3,) STAT will determine the best value for its expenditures if two equally qualified and approved vendors or suppliers offer the same materials or services.





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5. VERIFICATION PROCEDURES

5.1 Introduction

It is the objective of STAT to provide our customers with data that is of known and documented quality consistent with the analytical methods and SOPs listed in Appendix 3. This is accomplished with the use of traceable calibrations and documentation of this traceability with external reference samples. Where possible, calibration and reference standards, traceable to national standards of measurement, are used in the laboratory to calibrate and/or verify the test equipment. These calibration and reference standards are only used for calibration and/or verification purposes.

5.2 Traceability of Calibrations Each analytical process undergoes the following to document calibrations used in the

laboratory:

5.2.1 Initial Demonstration of Capability: Each analyst to determine the range of instrument operation, if applicable, and to demonstrate precision and accuracy, analyzes a series of laboratory control standards. This study is signed by the analyst, Department Supervisor, the QA Director, and the Technical Manager. See the specific requirements in SOP 1230 Training and analytical SOPs.

5.2.2 Initial Calibration Determination: Based on the Initial Demonstration of

Capability (IDOC), an initial calibration is performed. The ICAL determination must meet the criteria specified in the analytical SOP.

If the regulatory limit is stated or defined for a particular analysis or test parameter, the laboratory’s policy is to perform the analysis using a calibration standard at or below the defined regulatory limit.

5.2.3 Initial Calibration Verification: The Initial Calibration Verification is

immediately performed to determine the validity of the initial calibration. This standard is from a second source, if available. Concentrations and acceptance criteria are specified in the relevant analytical SOP.

5.2.4 Method Detection Limit Study: The laboratory performs an MDL study prior to

instituting a new procedure/analysis and a LOD/LOQ study yearly thereafter. MDL study is not applicable for some tests, e.g., pH, odor, temperature, etc. These procedures are outlined in STAT SOP 1210 Method Detection Limits.





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5.2.5 Quality Control Check Sample: External reference standards that are analyzed as an unknown by the analyst. This provides an independent check of the analytical process. These results may be placed in the analysts’ training file. See section 5.3.2.2 for more details. The laboratory maintains a reference slide and spore collection of each microbiological sample identified. Because microbiological analyses measures constantly changing living organisms, these organisms are inherently variable. STAT SOP 005 Document Control contains references used in this laboratory.

5.2.6 Continuing Calibration Verification: A calibration standard is prepared and

analyzed when an initial calibration is not performed. At a minimum, a calibration check is analyzed at the beginning and at the end of each analytical batch. Organic internal standard methods are an exception where the calibration check is analyzed only at the beginning of the analytical sequence. Refer to the analytical SOPs for frequency and acceptance criteria. If a calibration check fails the appropriate SOP stated criteria, and routine corrective action fails to produce a second calibration check within acceptance criteria, then the initial calibration and initial calibration verification is performed. All samples analyzed since the last calibration check was in control will be re-analyzed, except in those instances where the calibration check was exceeded high (high bias) and there are non-detect results for the corresponding analyte in the samples associated with the calibration check. Those non-detects may be reported.

5.2.7 Method Blank Determination: A method blank is performed once per preparation

batch per matrix type. The method blank is a negative control. A method blank is acceptable if it does not contain an analyte of interest at a concentration greater than the highest of the following: the reporting limit, 10% of the regulatory limit for that analyte, or 10% of the measure concentration for that analyte in any environmental sample in the batch. Some approved test methods do not require method blanks (e.g., pH, temperature, conductivity, etc.) Refer to the individual analytical SOP for acceptance criteria.

5.2.8 Analytical Reagent Blank: Analytical reagents, without media, shall be prepared

and analyzed, when applicable, with each batch of samples, using the same procedure that is used for field samples.

5.2.9 Field Blank: It is recommended that customers of the laboratory supply

specimens of blank sampling media from the same source lot as was used for collecting the field samples. A field blank from this source lot can help determine possible contamination of an analyte during handling and shipping procedures.

5.2.10 Continuing Calibration Blank (Inorganic): Inorganic SOPs require continuing

calibration blanks analyzed each time a calibration check is analyzed. The same criteria are used as specified for method blanks (5.2.7). All samples analyzed





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since the last continuing calibration blank that was in control will be re-analyzed, except in those instances where there are non-detected results for the corresponding analyte in the samples associated with the continuing calibration blank. Those non-detected results may be reported.

5.2.11 Interference Check Standards (ICS): ICSs used in ICP-MS analysis checks for

metal complex interferents (e.g. Ar, C, Cl, etc) with a similar mass of low concentration analytes. The appropriate analytical SOP contains specific instructions for analysis of these standards.

5.2.12 System Tuning Verification (GC/MS and ICP/MS): The GC/MS is hardware

tuned before performing the initial and continuing calibrations. Refer to the individual analytical SOP for acceptance criteria.

5.2.13 Internal Standard Area Monitoring (GC/MS and ICP/MS): Internal standards are

monitored to determine the quality of the injection process. Criteria are in the appropriate analytical SOP with corrective action specified.

5.2.14 Laboratory Control Standard: Laboratory Control Standard (or Sample) (LCS) is

performed at least once per preparation batch per matrix. The LCS and MS/MSD are positive controls that measure the percent recovery (5.5) of the analytes added prior to preparation/analysis. They provide the assurance that the analytical system is capable of measuring the analytes specified. If the LCS does not meet control limits specified in the SOP, analysis is halted and corrective action taken to bring the system under control, including re-preparation of all samples in the batch associated with the out-of-control LCS. LCS is not performed when spiking solutions are not available, e.g., color, odor, temperature, dissolved oxygen, or turbidity.

5.2.15 Surrogate or System Monitoring Compounds (Organic): Surrogate compounds

are added to most organic chromatography methods. Surrogates indicate that sample preparation and analysis are within the appropriate method SOP criteria. Specific SOPs have procedures handling out-of-control situations, including sample re-extraction/re-analysis.

5.2.16 Matrix Spike/Matrix Spike Duplicate: Matrix Spike/Matrix Spike Duplicate

analysis is similar to LCS analysis (5.2.14) except it is performed on customer samples. The MS/MSD shall be prepared once per preparation batch of 20 or less samples per matrix type. If more than 20 samples are prepared a second MS/MSD shall be prepared after the twentieth sample.. Samples specified for MS/MSD analysis by customers will be selected if so indicated. MS/MSDs indicate the effect of the sample matrix on the precision and accuracy of the results generated using the selected method. This information does not determine the validity of the entire batch. For cases where the sample cannot be divided (e.g., wipes, air samples, not enough sample provided by customer) and thus a MS/MSD pair





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cannot be prepared for the preparation batch, an LCS/LCSD pair is analyzed to measure precision.

5.2.17 The laboratory will maintain a reference slide collection of asbestos types with

various asbestos concentrations from previous NIST Proficiency Analytical Testing rounds. Standard Reference Materials (SRMs) are purchased from NIST for calibrations.

5.2.18 Duplicate Analysis (for analyses not suitable for spiking): Samples that are not

suitable for MS/MSD analysis will be analyzed in duplicate. A Laboratory Control Standard Duplicate (LCSD) will also be performed for tests not suitable for matrix spike analysis or duplicate analysis (e.g. wipes, air samples, etc.). Relative Percent Difference (5.4) is calculated and compared to control criteria listed in the approved method SOP.

5.2.19 The laboratory maintains performance records to document the quality of data

that is generated. Method accuracy for samples is assessed and records maintained. STAT generates in-house acceptance limits and compares method performance data to the reference method criteria. The in-house control limits are generated based on a minimum of 20 data points. Parameters for which control limits are generated include, but not limited to, LCS, Surrogate recovery, and MS/MSD recoveries. Acceptance limits are developed based on three standard deviation from the average recovery and warning limits are developed based on two standard deviation from the average recovery. Control limits for the method parameters are generated by the QA Director in consultation with the Technical Manager, Laboratory Director, and Department Manager. Control limits are distributed to the analysts via updates to the LIMS control charts. The control limits are calculated based on in-house performance data. In-house generated data is compared to the specifications of the reference method. If the in-house limits are within the specifications of the reference method, the control limits are updated in LIMS. If the in-house limits are not within specifications, an investigation is performed to determine the cause(s) of the problem and a corrective action is completed. The analysis may continue until enough data points are collected to regenerate new control limits. Any QC data generated outside of reference method limits during that time frame, is flagged.

5.3 Performance Testing Samples

5.3.1 Introduction As part of the laboratory’s Quality Assurance program, an independent means of assessing laboratory accuracy for its performance in the various test methodologies has





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been developed. The Performance Testing Program analyzes Performance Testing (PT) samples on a routine basis. These samples, are of an unknown concentration to the analyst who performs the test. The purpose of analyzing these samples is to determine whether the analyst/laboratory can produce analytical results within specified acceptance criteria.

For analysis of all PT samples, with the exception of the EMPAT fungal direct examination program, the laboratory’s procedure is as follows:

• Upon receipt, the Performance Testing Samples are treated as any other sample submitted to the laboratory. They are logged into the system and assigned a unique laboratory number. A LIMS work order is generated and samples are distributed to the analysts. The samples are then prepared and analyzed in the same manner as any other submitted samples using the same procedures, equipment, and laboratory personnel. After the data review process, test results are recorded in the LIMS. A final report is generated and results are reported to the Technical Manager, Quality Assurance Director and Laboratory Director. Depending upon the type of PT sample, the final report is then submitted to the PT provider or evaluated in-house. After evaluation, either by the PT provider or by the QA Manager, the report is filed in the QA Manager’s office.

• For PT sample studies that are used for accreditation purposes, the evaluation report, copies of the PT study report forms, copies of all support documentation, and copies of any corrective action investigations and resolutions, are kept in the QA Manager’s files. This allows easy reconstruction and review of this data by the accrediting authority during on-site audits. This data, along with any electronic records, is kept at a minimum of five years from the date of the evaluation report received from the PT provider. This time frame may be increased to comply with any additional regulatory program requirements.

• All analysts participate in the PT process. Successful analyses are used to obtain accreditation or to maintain the laboratory’s current scope of accreditation. They may also be used to update employee-training records (continuing DOC), or to demonstrate to customers or other interested third parties that the laboratory is capable of producing quality data.

• For unacceptable results, or results that are in-control but are continually statistically biased high or low, corrective action must be taken to determine the cause of the problem. This is accomplished by the corrective action process (SOP QA 230 Corrective Action). For PT sample studies that are used for accreditation purposes, copies of any corrective action investigations and resolutions are available to accrediting authorities.

• For the EMPAT fungal direct examination program, the analyst views and identifies the unknown samples on-line. On a quarterly basis, the laboratory has access to 20 different digital images for identification of spores.

• The laboratory will notify its customers and interested third parties, in writing, of any change to the laboratory’s scope of accreditation (addition or deletion of analytes or fields of testing).





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The laboratory has established policies in reference to the analysis of PT samples. They are as follows:

• PT samples are treated and analyzed in the same manner as other sample submitted to the laboratory.

• The laboratory does not send any PT sample, or portion of a PT sample, for which it seeks to obtain accreditation or maintain its current accreditation to another laboratory for analysis.

• The laboratory does not knowingly accept PT samples or portions of PT samples from other laboratories for any analyses for which the sending laboratory seeks accreditation or is accredited.

• Laboratory personnel do not communicate with any other individuals from any other laboratories concerning PT samples.

• Laboratory personnel do not attempt to obtain the assigned value or analyte concentration of any PT sample from the PT provider.

5.3.2 NELAC Performance Samples

The PT program is divided into two sections.

5.3.2.1 External Evaluation of Performance Sample The first section of the program is dedicated to the analysis of PT samples for compliance with accreditation programs such as NELAC. The PT samples for this section of the program are of an unknown concentration to all laboratory personnel (blind to the laboratory). At a minimum of two times per year (approximately every six months), PT samples for each field of testing (each analyte/method/matrix) are purchased from a Proficiency Testing Oversight Body/Proficiency Testing Provider Accreditor (PTOB/PTPA) approved PT provider, when available. After analysis, a report is submitted to the PT provider for evaluation. The Technical Manager, Quality Assurance Director and Laboratory Director are responsible for the accuracy and the format of the report submitted to the PT provider. In order to initially obtain and to currently maintain accreditation, the laboratory must be successful in the analysis of these samples in two of the three most recent rounds of testing. If there is a failure to successfully analyze a particular analyte or supplemental testing is warranted, the laboratory must wait at least 30 days before analyzing additional samples. To maintain accreditation, the laboratory will continue to analyze samples at the prescribed frequency (two PT studies for each PT field of testing per year) unless there is a change in the program or in the environmental regulations. It will maintain a history of at least two acceptable PT studies for each PT field of testing out of the most recent three studies. The laboratory authorizes the PT provider to release the results of the laboratory’s performance (sample results and acceptable/not acceptable status) on any of the PT samples directly to any accrediting authority, NELAP, and the PTOB/PTPA.





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5.3.2.2 In-House Evaluation of Performance Samples The second section of the program is for in-house evaluation of analyst performance. The PT samples for this section of the program are of an unknown concentration to the analyst performing the test (blind to the analyst). The QA Manager purchases these samples that include the true analyte concentration and performance acceptance limits. The QA Manager does not divulge this information to any of the laboratory personnel. PT samples are purchased from a PTOB/PTPA approved PT provider or another provider that can provide samples that are traceable to NIST, when available. After analysis, a report is submitted to the QA Manager for evaluation. The successful analyses of these samples may be used as documentation for the analysts continuing Demonstration of Capability in the applicable test methods.

5.3.3 AIHA-PAT - Performance Samples For purposes of this program, an industrial hygiene laboratory is defined as a laboratory that analyzes samples or materials for the purpose of evaluating occupational exposure or contamination resulting from occupational activities. The laboratory participates in three programs for accreditation: 1) the AIHA-PAT Industrial Hygiene Laboratory Accreditation Program (IHLAP) for accreditation of industrial hygiene laboratories; 2) the AIHA-PAT Environmental Lead Laboratory Accreditation Program (ELLAP) for accreditation of laboratories performing lead analysis and, the AIHA PAT Environmental Microbiology Laboratory Accreditation Program (EMLAP). For the ELLAP program, the laboratory analyzes PAT samples in the following Fields of Testing: airborne particulates, dust wipes, paint chips and soil. The purpose of the PAT program is to ensure that the laboratory meets established performance criteria for the analysis of industrial hygiene samples. This laboratory chooses to participate in the four rounds of performance samples per year. AIHA-PAT PT programs are performance based and the programs do not specify the use of any particular analytical method when analyzing PT samples, except for asbestos by PCM. Proficiency testing samples shall be analyzed using the same analytical procedure used to test customer samples. The laboratory shall be responsible for the timely and proper submission of all PT sample results to the AIHA-PAT. The laboratory shall submit data using the AIHA Data Entry Portal on the AIHA web site. The data must be entered into the system by the specified deadline. An unreported result is classified as an outlier unless the AIHA-LAP, LLC has pre-approved nonparticipation. The AIHA-PAT shall provide the PT reports to each participating laboratory forty-five days after the close of the PT round. Accredited laboratories shall maintain these records for use during the assessment process. The laboratory is responsible for notifying the AIHA-PAT of any changes in laboratory status that may affect the receipt of PT samples/information, such as a change in address or named recipient.





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A result that is outside the statistical control limits determined for the Industrial Hygiene Performance Analytical Testing (IHPAT) or Environmental Lead Performance Analytical Testing (ELPAT) Environmental Microbiology Performance Analytical Testing (EMPAT) round is classified as nonconforming work.

5.3.3.1 IHPAT Round Performance Samples Proficiency is determined Field of Testing by Field of Testing and round by round. A laboratory is rated proficient for a given round for the applicable Field of Testing (FoT) if there is not more than twenty-five (25) percent deficiency for a given Field of Testing for that round. A laboratory is rated as proficient for the FoT if it passes two out of three consecutive test rounds. The laboratory shall have participated in at least two (2) PT rounds to be considered for accreditation. When PT samples are analyzed by more than one analyst, averaging the results for reporting is not permitted. A single analyst’s results are reported. 5.3.3.2 ELPAT Round Performance Samples A laboratory is rated proficient for the applicable FoT if there are not more than 25% cumulative outliers reported in the last four consecutive PT rounds in which the laboratory has participated at the time of accreditation or no outliers reported in the last two consecutive PT rounds. The laboratory shall have participated in at least two (2) PT rounds to be considered for accreditation. 5.3.3.3 EMPAT Round Performance Samples In order to maintain accreditation, the laboratory must be 85 % successful in the analysis of microbiology samples in the three most recent rounds of testing. To maintain accreditation, the laboratory will continue to analyze samples at the prescribed frequency (three PT studies for each PT field of testing per year) unless there is a change in the program or in the environmental regulations. It will maintain a history of at least 85 % acceptable PT studies for each PT field of testing out of the most recent three studies. 5.3.3.4 Inhouse PT (Demonstration of Competency, DOC) for Fields of Testing not covered by AIHA-LAP, LLC

Twice a year, a set of four media will be spiked at various levels by the QA director or designee. Spike levels will be given to the Department Manager. The blind samples will be run by the analyst and results evaluated against current in house limits for LCS recovery. The PT round will be considered passing for the FoT consisting of a single analyte if at least three out of four samples meet the LCS recovery acceptance limits. For FoTs containing multiple analytes, a sample is considered passing if 75% of the analytes meet the LCS recovery acceptance limits. Seventy-five percent of the samples must pass for the round to be considered passing. Results are evaluated by the QA Director for continuance of the FoT. Results are kept on file with the Department Manager. If a round fails, the round must be retested, four new samples are prepared/analyzed for each





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analyte and reevaluated. A laboratory is rated as proficient for the FoT if it passes two out of three consecutive test rounds. The laboratory shall have participated in at least two (2) PT rounds to be considered for accreditation. The laboratory will notify AIHA-LAP, LLC if it fails two out of three consecutive rounds and follow AIHA-LAP, LLC’s instruction for further action. Further details for each FoT are included in corresponding SOPs.

5.3.4 NVLAP Performance Samples

The PT program is divided into two sections. The first section of the program is dedicated to the analysis of PT samples for compliance with accreditation programs such as NIST/NVLAP. The PT samples for this section of the program are of an unknown concentration to all laboratory personnel (blind to the laboratory). PT samples for each field of testing are provided by NVLAP, generally, at a frequency of two times per year (approximately every six months). After analysis, a report is submitted to the PT provider for evaluation. The analysts, Technical Manager, Quality Assurance Director and Laboratory Director are responsible for the accuracy and the format of the report submitted to the PT provider. In order to initially obtain and to currently maintain accreditation, the laboratory must score less than 150 points on two out of the last three consecutive proficiency testing rounds. To maintain accreditation, the laboratory will continue to analyze samples at the prescribed frequency (two PT studies for each PT field of testing per year) unless there is a change in the program or in the environmental regulations. The laboratory authorizes the PT provider to the release the results of the laboratory’s performance (sample results and acceptable/not acceptable status) on any of the PT samples directly to the NIST/NVLAP. The second section of the program is for in-house evaluation of analyst performance. This is accomplished by a round-robin program. Asbestos samples are distributed to numerous laboratories and analysis is summarized and distributed to all participants. After analysis, a report is submitted to the QA Manager for evaluation. The successful analyses of these samples may be used as documentation for the analysts continuing Demonstration of Capability in the applicable test methods.

5.4 Precision

Precision is expressed as percent relative standard deviation and is calculated by the formula: % RSD = S x 100

X

Where: S = Standard Deviation X = Mean





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Precision can also be expressed as relative percent difference and is calculated by the formula: % RPD = D x 100

X

Where: D = Difference between measurements X = Mean

Percent difference is calculated by the formula: %D = (X-Y) x 100

X

Where: X = Initial Measurement Y = Comparison Measurement

5.5 Accuracy

Accuracy is expressed as percent recovery and calculated by the formula: (Y – X)/Z x 100 = % Recovery Where: X = concentration in unspiked sample. Y = concentration in spiked sample. Z = theoretical spike concentration

5.6 Analytical Performance Summary

Quality control data are reviewed on a continuous basis. During the review, percent RSD, percent RPD, upper warning and control limits of precision data and percent recovery of accuracy data are evaluated against established control limits. If a statistically significant trend is observed, then warning and control limits may be updated, and documented in Addendum to the SOP.

Annually, a summary report of the laboratory's analytical performance is prepared. Contained in this report are: the precision data (average percent RSD or RPD, upper warning and control limits), and accuracy data (average total percent recovery of spiked samples, reference samples, and performance audit samples). The Quality Assurance Director prepares this summary and it is reviewed by the Technical and the Laboratory Director prior to distribution for use.





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6. METHODOLOGY

Test method SOPs are based upon nationally recognized test method references such as the United States Environmental Protection Agency (USEPA), National Institute for Occupation Safety and Health (NIOSH), NIST/NVLAP, Standard Methods (American Public Health Association, American Water Works Association, Water Environment Federation), CPSC and American Society for Testing and Materials (ASTM). These test methods are used for sample analyses, and the related sample handling and storage activities are appropriate and consistent with the required quality and accuracy deemed necessary for customers and their decision-making processes concerning environmental regulations and compliance. The laboratory uses the most stringent standard as stated in the reference test method or as specified in the applicable regulation.

Appendix 3 contains a table of the laboratory’s scope of test methods and SOPs.

7. PHYSICAL FACILITIES AND EQUIPMENT 7.1 Facilities

STAT has over 12,000 square feet of state-of-the-art laboratory facilities. An electronic key-punch provides limited access to this building. The laboratory space and ventilation system was specifically refurbished to achieve the critical needs of an environmental laboratory. For example, laboratories for air toxics and volatiles analyses are positively pressurized and are supplied with fresh air that is carbon filtered. Environmental lead is digested and analyzed in a laboratory separate from bulk lead samples (paint chips, dust, etc) to prevent cross contamination. Separate laboratories are provided for microbiology, optical microscopy and electron microscopy. Three organic extraction laboratories occupy nearly 1400 square feet of space and allow for extraction of air, water and soil with room for further expansion. A facility lay-out is provided in Appendix 4. There is no other testing facility being utilized other than the permanent lab premises. The rooms are dedicated to specific laboratory testing departments and administrative offices. The physical environment (temperature, humidity, lighting, and ventilation) is adequate to perform all testing methodologies. Temperature is monitored and controlled by individual thermostats in each room. Ventilation hoods are monitored as part of the laboratory safety program. Any problems encountered with the physical accommodations are immediately brought to the attention of the Technical Manager or the Laboratory Director. The building engineer is then notified to take immediate corrective action to remedy any problems.

As part of the Internal Audit Process (SOP 1220 Internal Quality Assurance Audit), the QA Manager is required to monitor the laboratory’s facilities to ensure that the facilities are adequate and that personnel are in compliance with laboratory policies. Those areas audited include the following:

• Ventilation: hoods checked and tagged per the Chemical Hygiene Plan QA 001 Quality Assurance Manual




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• Room temperature: monitor the TCLP extraction area • Voltage surge suppressors to protect computer network and critical

instrumentation • Separation of incompatible areas is maintained • Personnel movement is limited to prevent cross-contamination • Good housekeeping practiced - items reviewed: benches, floors, hood used

properly, clutter, glassware cleaning space and storage, bottle/container storage • Waste storage area is reviewed to ensure safe practices • Air Monitoring for Spores in Microbiology Laboratory: Background

contamination is to be checked periodically (once every Quarter). If growth of Aggressive spores is observed, all areas of the laboratory are cleaned. The air system is checked, and if necessary, filter is replaced. Cleaning will continue until no background contamination is detected.

• Air Monitoring for Asbestos: Background contamination is to be checked periodically (once every Quarter) by taking air samples from areas where asbestos is handled, such as sample receiving, bulk asbestos analysis Laboratory, and PCM and Transmission Electron Microscopy (TEM) Laboratory. Samples are analyzed by TEM. If presence of asbestos is confirmed, all areas of the laboratory are cleaned. Cleaning will continue until no background contamination is detected.

• Background Monitoring for Lead in Lead Laboratory: Background contamination is to be checked periodically (once every Quarter). If lead is observed, all areas of the laboratory are cleaned. Cleaning will continue until no background contamination is detected.

7.2 Equipment

The major equipment in use at STAT Analysis Laboratory is listed in Appendix 4. The equipment list is under the control of the Quality Assurance Director . The list is updated as required whenever new equipment is purchased or current equipment is permanently removed from service.

7.3 Equipment Maintenance Program

Proper maintenance of laboratory instrumentation is a key to longevity of the instrumentation, as well as providing the analyst with equipment capable of producing reliable analyses. The analysts and on occasion, vendor specialists, share the responsibility for maintenance and repair of all STAT Analysis Laboratory equipment. Specific maintenance requirements are found in the analytical SOPs. Therimary elements of the equipment maintenance program include:

• All major equipment receives a daily check for such things as: cooling fan operation, pump operation, indicator readings, mechanical checks, clean air filters, etc.

• Service schedules are established for performing routine preventative maintenance on all major equipment items.





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• Records are maintained for all instrument repairs (See individual instrument maintenance logbooks).

• A conservative inventory of critical spare parts is maintained for high-use instrumentation.

• Vendor operation and maintenance manuals are maintained for laboratory instrumentation.

Any equipment that is found to be defective is taken out of service. The equipment is tagged by the person making the judgment and marked “Out of Service;” the person applies their initials and dates the tag. This action is noted in the maintenance logbook. The department supervisor is notified of this action. If deemed necessary, a corrective action report is initiated to determine if the malfunctioning equipment has potentially generated data that is suspect. The equipment is not put back into service until repairs are made and the equipment is shown to be performing properly after calibration and/or verification procedures have been successfully completed and documented in the maintenance logbook.

8. SAMPLE RECEIPT and ACCEPTANCE

8.1 Introduction Complete documentation of the sample collection and handling process is an extremely important aspect of a regulatory monitoring effort. Formal chain-of-custody procedures provide a written record of sample traceability, accountability and serve to validate sample integrity. All samples received by STAT Analysis are controlled by these procedures. For more information see STAT SOP 300 (Sample Receiving and Login Procedure).

Appendix 5 contains a table of acceptable sample containers with sample preservation requirements for analyses listed in section 6. Sample collection is typically a function of our customer’s activities. STAT does not provide sampling services. STAT’s customers deliver samples to the laboratory for testing. However, STAT will attempt to ensure compliance with all applicable ISO/IEC 17025, NIST/NVLAP, AIHA-LAP, LLC, and NELAC requirements. STAT requests customers to submit field blanks with their samples, where applicable. A summary of STAT’s written sample acceptance policy will be made available to sample collectors. Data from samples that do not meet the sample acceptance criteria will be unambiguously flagged to define the nature of the variance. Sampling procedures for collection of subsamples are described within each method’s Standard Operating Procedure (SOP).

8.2 Sample Acceptance Policy





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Please refer to Appendix 6 for a detailed description of STAT’s Sample Acceptance Policy. It becomes the customer’s responsibility to distribute the sample acceptance policy to all field collection personnel. STAT Analysis Corp endeavors not to reject samples for analysis the is is accreditred to perform except for reasons of safety, radioactivity or the requirement to maintain a legal Chain of Custody. NOTE: STAT Analyses will not accept samples that require legal Chain-of-Custody.

8.3 Sample Acceptance Policy Differences 8.3.1 Additional Requirements for NELAC Samples :

8.3.1.1.1 Liquid Samples for volatiles analyses do not contain headspace.

8.4 Chain-of Custody Form A Chain-of Custody (COC) should accompany every sample that is received for analysis by STAT Analysis. If the COC is not present, the customer will be notified and the exception noted on the Sample Log and Checklist/Receipt Form (Sample Receiving and Login Procedure). (Attachments 2-4 list examples of COC forms.)

8.5 Standard Operating Procedure – Sample Receipt/Custody The sample custodian or a designated alternate receives samples. Receiving and Login Procedure. STAT accepts samples between the hours of 8 AM to 8 PM, Monday through Friday. STAT has a secured sample drop box outside the building for samples that do not require preservation and can fit inside the box. For samples that arrive after hours, the sample custodian will receive the samples the next business day. 8.5.1 For specific details refer to SOP 300 Sample Receiving. is

8.6 Policy for Disposal of Laboratory Samples Samples and their extracts will normally be disposed of within (STAT SOP 1130 Waste Disposal) 90 days from receipt of samples or in accordance with individual SOPs. The exception to this will be when a sample hold request is implemented. A disposal report will be generated and provided to designated staff as appropriate for samples characterized as non-hazardous (routine environmental). Sample disposal of the routine environmental samples should be completed by the appropriate analyst within 2 weeks from disposal report distribution. The routine environmental samples will be disposed of in the following manner: Refer to STAT SOP 1130 Waste Disposal for specific procedures





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9. SAMPLE RECORDS, DATA REVIEW AND DATA HANDLING

Sample accountability through the analytical process can be divided into five major elements: (1) initial sample logging, (2) sample preparation, (3) data acquisition, (4) data review, and (5) documentation/storage. The location of the sample and data records is discussed in SOP 1000 Control and Use of Laboratory Notebooks and in SOP 240 Archiving. Sample records must be able to reproduce the resultant analytical data. It is management’s responsibility to ensure that all analytical and operational activities of the laboratory are properly and sufficiently documented. This is accomplished through the periodic audit and review processes as outlined in SOP 1220 Internal Quality Assurance Audit and SOP 006 Management Review of the Quality System. All data, whether manually generated or electronically generated, and final reports are available to the accrediting authority (NELAC, AIHA-LAP, LLC, etc.).

The following sections outline current sample and data documentation and review procedures.

9.1 Sample Logging

Samples received at STAT with accompanying identification and COC are logged into the Laboratory Information Management System. The sample custodian, or designate, signs the laboratory receipt section of the COC. Each sample, and each sub-sample appropriately preserved, is assigned a unique sample ID. 9.2 Analytical Data Review and Handling All raw analytical and instrument control data generated in the laboratory are either entered into bound data books or kept as strip charts, or in instruments computer hardcopy, tape, CD-ROM, or disk. The analyst reviews the data initially and all data entries checked 100% and then the data under goes a second review by a technical peer or supervisor. Errors, or potential errors, are investigated and corrected as necessary. The analytical section manager, Project Manager, Technical Manager, or Laboratory Director, for consistency of data and for assuring customer’s needs are met, performs final review. Refer to STAT SOP 1250 Data Review. Information contained in these data logbooks includes the following: Work Order Number, Sample number, parameter, date of preparation or analysis, analyst, and all pertinent instrument identification with analytical conditions. For non-computerized instruments all calibration data, all readout data, calculations, final concentration, and quality control data should be recorded in the logbook.





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9.3 Computerized Analytical Data System 9.3.1 All sample results are entered into the STAT Analysis Laboratory Information

management System (LIMS). Sample preparation, as appropriate, will also be entered in LIMS.

9.3.2 For NELAC and IH/Lead samples, all appropriate Quality Control data associated with these results are entered into the LIMS, including, but not limited to, Initial Calibration, Initial Calibration Verification, Continuing Calibration Verification, Continuing Calibration Blank, Method Blanks, Laboratory Control Standards, Matrix Spike/Matrix Spike Duplicate, Internal Standard Recoveries, and Surrogate Recoveries.

9.3.3 For all other samples, the quality control information is entered into a separate

database or spreadsheet. The information is stored under a unique batch identification number. This information may include: Initial Calibration, Initial Calibration Verification, Continuing Calibration Verification, Continuing Calibration Blank, Method Blanks, Laboratory Control Standards, and Matrix Spike/Matrix Spike Duplicate recoveries as applicable.

9.3.4 Analytical Data Processing. All final analytical results are calculated after entry into the analytical results database.

9.3.5 Analytical Backlogs can be generated through the LIMS system. Sample Status will be updated to complete after results are calculated. Samples that are complete will no longer appear on an analytical backlog report. The work order will only be available for Final Report after all sample results have been calculated and subjected to the Quality Control Validation Process.

9.4 Reporting

Final results of all analyses are provided in a standard computerized report format and forwarded to the requester (customer) with cover memorandum. Remarks should be used with reported data to alert the user to some specific conditions that affects the data (e.g., holding times missed, samples diluted to remove interferences, etc.). Exceptions to this report format must be noted and have approval of the Technical Manager or Laboratory Director.

For modified methods, reports are generated by appending an “M” to the method identifier. Amendments or corrections to the issued test report are only made in the form of a revised document that includes the statement “This report is revised to reflect changes made after the initial report was issued” in the cover letter or in the case narrative.





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Customers are notified immediately, in writing, of any event that cast doubt on the correctness or validity of the laboratory’s calibrations, or test results given in any test report or amendment to a report. Such events might include: identification of defective measuring, identification of defective test equipment, or audit findings.

Test results are certified to meet all requirements of NELAC, NVLAP, and AIHA-LAP, LLC standards, or reasons are stated if they do not meet these standards. Sample results are, generally, not blank corrected. Readers are referred to the specific analytical SOPs for details regarding blank correction. If analysis requires blank correction, then the blank used for correction, as well as its value, are noted in the case narrative. In addition to the items mentioned, below, in 9.4.1 (7), the analytical report will make the following statements: 1. The report shall not be reproduced except in its entirety, unless written

approval has been obtained from the laboratory. 2. The results of this report relate only to the samples tested. 3. The laboratory certifies that the test results meet all requirements of IEPA

code, Title 35, Subtitle: A, NELAP/Part 186 or NIST Handbook 150 (2006 Edition) or the AIHA-LAP, LLC Policy Document, current revision.

4. Accredited and non-accredited analyses will be distinguished. 9.4.1 Reporting Requirements

The Analytical Report will only be issued in its entirety. The Report will include: 1. A Title, e.g.: Analytical Report, STAT Work Order # or STAT Batch #. 2. Date, name and address of laboratory, phone number and name of contact

person (with signature) and laboratory accreditation number. The person signing the report is accepting responsibility for the content of the report;

3. A unique Work Order Number and the total number of pages in the report, with all pages sequentially numbered;

4. Name and address of customer and project identification; 5. Description and unambiguous identification of the sample(s) including the

customer identification code, date of sample receipt, date and time of sample collection;

6. Clear identification (including lab name and accreditation number) of any sample results that were generated by a subcontracted laboratory;

7. Case Narrative outlining any sample acceptance outliers and /or sample results with any failures or deviations from approved SOPs including the use and definitions of data qualifiers; as well as reporting uncertainties as required.

8. Identification of approved test method with date of sample preparation, sample preparation method, and/or analysis;





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9. Identification of reporting units, such as mg/L, mg/Kg, mg/Kg–dry, ppbv, µg/filter µg/wipe, mg, µg, wt. %, or µg/m3;

10. Measurements, examinations and derived results, supported by tables, graphs, sketches and photographs as appropriate, and any failures identified;

11. A statement to the effect that sample results relate only to the analytes of interest tested or to the sample as received by the laboratory;

12. Reference to sampling procedures if performed by the laboratory; 13. Identification of analytical methods, including “M” for modified methods,

to reflect the methods listed in STAT’s FoTs from various accrediting agencies.

9.4.2 Reporting Differences

9.4.2.1 NELAC Differences 9.4.2.2 Clear identification of numerical results with values outside the

quantitation limits. 10. CORRECTIVE AND PREVENTIVE ACTIONS Non-conforming work arises out of the analytical process. Corrective and Preventive actions are mechanisms for identifying and correcting Nonconforming work. Quality control data are evaluated, and if data are found to be outside control limits, corrective actions are taken to correct the problem and to prevent incorrect data from being reported. Corrective/preventive actions are tracked through LIMS in the same manner.

10.1 Corrective Action

Routine corrective action will be taken at any time during the analytical process as

outlined in the quality control sections of each SOP. These types of out-of-control situations include such things as: instrument calibration outliers, blank contamination, poor laboratory control standard recovery, poor surrogate recovery, poor matrix spike/ matrix spike duplicate recovery or RPD, etc. These situations require immediate corrective action. These required actions are specified in each analytical SOP. All routine corrective actions taken are documented by the analyst on the raw data or appropriate checklist including their initials and date, to assure traceability of corrective actions performed. All nonconforming data are recorded in a database in a way that they can be reviewed and assessed for recurrence. The database documents all nonconforming and conforming events, which can be reviewed to identify incidences of warning limit and control limit exceedances. Multiple exceedances of warning limits may trigger preventive action. Similarly, multiple exceedances of control limits will trigger corrective action. When instances arise that are not covered by the routine corrective action procedures in the applicable analytical SOP, the analyst must bring the issue to the attention of the Department and the QA Manager. The issues will be discussed with the





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appropriate staff, the best corrective action determined, performed, documented in the raw data and reported to the customer in a case narrative.”

Some out-of-control situations require a more formal corrective action process. They may be the result of internal or external audits, out-of-control proficiency testing analysis, continuing control chart outliers, or even the inability to produce analytical results on time. These situations require a more stringent process. This process may involve technicians, analysts, and laboratory management. The Quality Assurance Director monitors this process (STAT SOP QA 230 Corrective Action). Essential steps in this process include documentation of the following:

• Identification of the problem. • Assigning a tracking number to the Corrective Action. • Assigning personnel to investigate the problem. • Uncovering the root cause of the problem. • Correcting the problem. • Monitoring the corrective action. • Documentation of the corrective action.

Corrective Actions are resolved in a time frame relative to the severity of the defined problem. Some corrective actions may need to be immediately implemented in order for production to continue. Other corrective actions may require a certain amount of time in order to complete a full investigation. An appropriate time frame for completion of the corrective action is discussed with the affected parties. All corrective action investigations are to be completed within a two-week time frame unless unusual circumstances are documented that would extend this deadline. Corrective Actions investigations involve assigning an individual to investigate and determine the cause of the problem. 10.2 Preventive Action Preventive actions are pro-active processes to identify opportunities for improvement rather than a reaction to the identification of problems. Preventive actions will be taken upon identification of needed improvements and potential sources of nonconformity. Action plans will be developed, implemented, and monitored to reduce the likelihood of the occurrence of such nonconformities and to improve on existing procedures. As part of the preventive action, operational procedures will be reviewed. Data review may also be conducted that include trend and risk analyses and proficiency-testing results.

Steps in the preventive action process may include:

• Identification of the source of nonconformity or needed improvements. • Assigning personnel to investigate • Reviewing operational procedures. • Implementing needed improvements or procedure to avoid potential

nonconformity.





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• Monitoring the preventive action. • Documentation of the preventive action. • Assigning a tracking number to the Preventive Action

11. QUALITY EXCEPTION REPORT/CASE NARRATIVE

Some out-of-control situations are not correctable (e.g., silver matrix recovery when certain levels of chloride are present or VOA system monitoring compound recoveries on samples containing activated carbon). The Quality Exception report is executed and included in the case narrative of the analytical final report (STAT SOP QA 230 Corrective Action).

12. COMPLAINT

Customer complaints are logged and resolved by project managers as outlined in STAT SOP 220 Customer Service. STAT seeks feedback from its customers so that improvements can be made to the management system, testing and calibration activities, and customer service.

13. CONFIDENTIALITY All customers, including government entities, are entitled to all aspects of their project to

be considered confidential. To protect national security concerns and proprietary rights, STAT Analysis will ensure customer confidentiality. No aspects of customer project can be released to others without the expressed written consent of the customer. All data, electronic media, and reports are considered confidential

A Notice of Confidentiality is affixed to outgoing e-mails and facsimiles transmittals.

Examples of these can be viewed in Attachments 5 and 6, respectively. 14. INTERNAL AUDITS The Laboratory will undergo an annual internal audit, or more frequently if warranted.

The Quality Assurance Director will take the lead in this activity. If the Quality Assurance Director is responsible for analytical activity, another member of the management team will audit that area. These activities are outlined in STAT SOP 1220 Internal Quality Assurance Audit. As part of the internal audit, STAT will keep abreast of policy revisions issued by accrediting agencies and to implement changes within a reasonable time frame by revising this QAM and other appropriate SOPs in order to be compliant with existing accrediting agency policies. STAT will contact the accrediting authorities to acquirethe current checklist prior to conducting the internal audit.





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15. MANAGEMENT REVIEW of the QUALITY SYSTEM

STAT strives continually to improve the effectiveness of its management system through the use of the quality policy, quality objectives, audit results, data analysis, corrective and preventive actions, and management review. This document, and the entire Quality Systems, is reviewed yearly. This process and procedures for development and submittal of quality assurance reports to management are outlined in STAT SOP 006 Management Review of Quality Systems. In addition to the annual report, quarterly quality assurance reports are developed and submitted to management. Finding from management reviews include recommended actions for improvement and the actions are carried out within a reasonable time frame and documented.

Changes made to appendices of this document will not constitute a revision to this

Quality Assurance Manual. 16. TRAINING STAT ensures that all employees will have proper training for their job. A training file is

maintained for each employee (STAT SOP 1230 Training (for NELAC/AIHA-LAP, LLC)). It is the responsibility of STAT Management to ensure all employees are educated on ethical and legal responsibilities, as well as, the punishment and penalties for improper, unethical, or illegal actions. Every employee is expected to read, understand, and sign a code of ethics statement.

The need for training beyond initial training on analytical SOPs will be assessed on a case-by-case basis. The department manager and laboratory director will determine if additional training is needed. The introduction of a new technique is an example of the need for additional training. The effectiveness of the training actions is evaluated by the trainer.

17. DATA INTEGRITY

STAT’s management is committed to support and implement specific requirements of the data integrity program. STAT’s procedures ensure that management and personnel are free from any undue internal and external commercial, financial, and other pressures and influences that may adversely affect the quality of their work. STAT promotes a culture of receptive environment where all employees can privately discuss ethical issues or report items of ethical concern. Such discussions are kept confidential, if need to be. The data integrity system includes four elements discussed below.

• Data Integrity Training: STAT has a training program in place for new employee orientation and on an annual basis for all employees to prevent breaches of ethical behavior. Written training material includes Appendix 7. Topics include:





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- Discussion regarding all data integrity procedures, data integrity training documentation, data integrity monitoring, and procedure documentation.

- Employees are trained on STAT’s responsibility to produce data that is scientifically valid, defensible, and of known and documented quality in accordance with all applicable federal, State, and local laws and regulations consistent with accepted professional and analytical practices in a manner that justifies the public trust. The employees are required to understand the critical need for honesty and full disclosure in all analytical reporting.

- Employees are provided specific examples of unethical behavior including improper data manipulations, adjustment of instrument time clocks, and inappropriate changes in samples, software, analytical conditions or concentrations of standards.

- Personnel are trained to inform STAT of any accidental or intentional reporting of non-authentic data by the employee or other employees. Employees are trained not to comply with instructions, requests, or direction by any manager or representative of management to perform any improper laboratory practices. Employees are trained to immediately report such event to all appropriate members of management including department manager, the Laboratory Director, the QA Manager and President/CEO, excluding such individuals who participated in such perceived improper instruction, request, or directive.

- Employees are required to understand that any infractions to the data integrity procedures will result in a detailed investigation. Any allegation of misconduct will be promptly investigated in an unbiased and confidential manner by an investigative team designated by the President. Investigation could lead to very serious consequences for the employee including immediate termination. The investigation, including any supporting documentation, actions and resolution, will be recorded and archived by the QA Director.

- Analysts are trained on proper documentation in Case Narratives where analytical data may be useful, but are partially deficient.

• Signed data integrity documentation for all employees: The initial data integrity

training and the annual refresher training have a space for employee signature to verify that the employee has participated in the training and understands his or her obligations related to data integrity issues (see Appendix 7: Ethics Policy and Data Integrity Agreement.).

• In-depth periodic monitoring of data integrity: STAT is committed to document

all activities associated with generating valid data. All tasks from sample receipt to issue of analytical reports are tracked and reviewed. Some examples of data monitoring activities include:

- Documentation and secondary review of sample log-in





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- Documentation and review of all sample preparation activities in specific logbooks

- Primary and secondary review of all analytical data - Primary and secondary review of all manual integration - Further review of all of the above steps by project manager and/or Quality

Manager - Calibration of measuring devices, such as thermometers, balances,

weights, and pipettes.

• Data Integrity Procedure documentation: All aspects of the data integrity procedures are documented. These include documenting all data monitoring activities. All customer communications are recorded. As discussed above, data integrity training material are developed and documented. Actions arising from data integrity issues, whether technical or ethical in nature, are documented.

18. SUB-CONTRACTING Any sub-contracting of accredited analytical work must be to another NELAC, ISO

17025, NVLAP, DOD or AIHA-LAP, LLC (or other ILAAC signatory) accredited laboratory with the appropriate fields of testing, approved test methods and analytes. STAT retains on file a copy of the certificates issued to the sub-contracting laboratory. The customer will be notified in writing of the intention to sub-contract analytical work. The analytical report contains the name and accreditation number of the sub-contracted laboratory. STAT maintains a record of all laboratories to which we subcontract analytical work. See STAT SOP 220 Customer Service for additional information.

19. LABORATORY SAFETY

19.1 Introduction

All STAT employees must accept the responsibility for acting in accordance with safety rules and practices and for reporting any observed safety hazard. This section highlights some general guidelines and rules that specifically apply to the analytical laboratory. Therefore, in addition to adhering to guidelines, each person is trained in, and expected to read, understand, and follow STAT SAP 003 Chemical Hygiene Plan.

19.2 General (additional requirements are detailed in STAT SAP 003 Chemical

Hygiene Plan)

• Lab coats and safety glasses should be worn at all times in the laboratory. The only exception to this is when personnel are working at computer terminals or microscopes. Lab coats are left in the laboratory. Latex or nitrile gloves are worn when chemical or samples are handled.





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• When working in any of the laboratories, it is recommended that all jewelry be removed and that personnel wash their hands frequently. Always wash hands thoroughly when leaving the laboratory.

• All containers should be labeled as to contents, with particular care to note corrosive or hazardous materials.

• There will be no eating, drinking, or smoking in any of the laboratories.

• An inventory of all chemicals used in the laboratory will be maintained.

• The Safety Officer will conduct a quarterly safety inspection of the laboratory.

• All work areas should be cleaned at the end of each workday. Spills should be

cleaned up immediately.

• Samples should be in laboratories only during preparation and analysis; other wise keep them in the storage area.

• New personnel must be familiarized with safety practices, location of safety

equipment, and made aware of possible hazards in the areas in which they will be working.

• Use safety guards where appropriate when using electrical equipment or

ventilation/fume hood systems. 19.3 Sample Receiving and Login

When possible, determine the source of the samples and any special hazards that might be associated with them. Some samples, when sealed in containers will build up pressure. Samples that indicate pressure should be brought to the attention of the Safety Officer or Laboratory Management.





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20. DEFINITIONS Acceptance Criteria: specified limits placed on characteristics of an item, process, or service defined in requirement documents. (NELAP) Acceptance Limits: Established mathematical data quality limits for analytical method performance. (AIHA-LAP, LLC) Accreditation: the process by which an agency or organization evaluates and recognizes a laboratory as meeting certain predetermined qualifications or standards, thereby accrediting the laboratory. In the context of the National Environmental Laboratory Accreditation Program (NELAP), this process is a voluntary one. (NELAC) A formal recognition that a facility meets AIHA LAP,LLC Policy Requirements to carry out specific tasks or specific types of tests. (AIHA-LAP, LLC) Accreditation Body: The territorial, state, or federal agency having responsibility and accountability for environmental laboratory accreditation and which grants accreditation. Accredited Laboratory: A testing laboratory that has been evaluated and granted accreditation covering a specific measurement or task, usually for a specific property or analyte, and for a specified period of time. (AIHA-LAP, LLC) Accrediting Authority: The Territorial, State, or federal agency having responsibility and accountability for environmental laboratory accreditation and which grants accreditation (NELAC)[1.5.2.3] Accrediting Authority Review Board (AARB): five voting members from Federal and State Accrediting Authorities and one non-voting member from USEPA, appointed by the NELAP Director, in consultation with the NELAC Board of Directors, for the purposes stated in 1.6.3.e. (NELAC) Accreditation Field of proficiency Testing: Same as “Field of Proficiency Testing.” Accuracy: The degree of agreement between an observed value and an accepted reference value. Accuracy includes a combination of precision and bias. See “Precison” and “Bias” a data quality indicator. (QAMS) (AIHA LAQAP) Addendum: Attachment to a document that contains new or altered text. AIHA: American Industrial Hygiene Association Aliquot See “Subsample” (AIHA-LAP, LLC) Analysis: The qualitative or quantitative determination of a property or analyte in a substance or material. (AIHA-LAP, LLC) Analysis Date: The calendar date of analysis associated with the analytical result reported for an accreditation or experimental field of proficiency testing. Analyst: the designated individual who performs the "hands-on" analytical methods and associated techniques and who is the one responsible for applying required laboratory practices and other pertinent quality controls to meet the required level of quality. (NELAC) Analytical Run: For chemical analyses, an analytical run consists of all samples processed continuously using an item of instrumentation or equipment. Such samples are analyzed applying the same set of standard calibration data. (AIHA-LAP, LLC) Analytical Sensitivity: The lowest concentration that can be detected by the method, based upon the amount or portion of sample analyzed (e.g., for methods involving a count = 1 raw count per





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amount or portion of sample analyzed, calculated and expressed in the final reporting units) (AIHA-LAP, LLC). Analytical Uncertainty: A subset of measurement uncertainty that includes all laboratory activities performed as part of the analysis. (NELAP) Applicant Laboratory or Applicant: the laboratory or organization applying for NELAP accreditation. (NELAC) Approved Signatory: Person who is recognized by a laboratory as competent and authorized by the laboratory management to sign test reports. (AIHA-LAP, LLC) Asbestos: A commercial term applied to the asbestiform varieties of six different minerals. The asbestos types are chrysotile, amosite, crocidolite, and asbestiform anthophyllite, asbestiform tremolite, and asbestiform actinolite. The properties of asbestos that caused it to be widely used commercially are: 1) its ability to be separated into long, thin, flexible fibers; 2) high tensile strength; 3) low thermal and electrical conductivity; 4) high chemical and mechanical durability; and 5) high heat resistance. Assessment: the evaluation process used to measure or establish the performance, effectiveness, and conformance of an organization and/or its systems to defined criteria (to the standards and requirements of NELAC). (NELAC) Assessment Criteria: the measures established by NELAC and applied in establishing the extent to which an applicant is in conformance with NELAC requirements. (NELAC) Assessment Team: the group of people authorized to perform the on-site inspection and proficiency testing data evaluation required to establish whether an applicant meets the criteria for NELAP accreditation. (NELAC) Assessor: One who performs on-site assessments of accrediting authorities and laboratories’ capability and capacity for meeting NELAC requirements by examining the records and other physical evidence for each one of the tests for which accreditation has been requested. (NELAC) Assessor: A person who conducts technical systems audits. Used interchangeable with site visitor, and auditor. (AIHA-LAP, LLC) Assessor Body: the organization that actually executes the accreditation process, i.e., receives and reviews accreditation applications, reviews QA documents, reviews proficiency testing results, performs on-site assessments, etc., whether EPA, the State, or contracted private party. (NELAC) ASTM: American Society for Testing and Materials Audit: a systematic and independent examination of facilities, equipment, personnel, training, procedures, record-keeping, data validation, data management, and reporting aspects of a system to determine whether QA/QC and technical activities are being conducted as planned and whether these activities will effectively achieve quality objectives. Batch: Environmental samples that are prepared and/or analyzed together with the same process and personnel, using the same lot(s) of reagents. A preparation batch is composed of one to 20 environmental samples of the same NELAC-defined matrix, meeting the above-mentioned criteria and with a maximum time between the start of processing of the first and last sample in the batch to be 24 hours. An analytical batch is composed of prepared environmental samples (extracts, digestates or concentrates) that are analyzed together as a group. An analytical batch can include prepared samples originating from various environmental matrices and can exceed 20 samples. (NELAC Quality Systems Committee)





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A group of samples that are processed in one operation: considered to be a uniform, discrete unit (AIHA-LAP, LLC) Bias: A systematic error manifested as a consistent positive or negative deviation from the known true value. (AIHA-LAP, LLC) The systemic or persistent distortion of a measurement process, which causes errors in one direction (i.e. the expected sample measurement is different from the sample’s true value). (NELAP) Blank: a sample that has not been exposed to the analyzed sample stream in order to monitor contamination during sampling, transport, storage or analysis. The blank is subjected to the usual analytical and measurement process to establish a zero baseline or background value and is sometimes used to adjust or correct routine analytical results. Blanks include: Field Blank: blank prepared in the field by filling a clean container with pure de-ionized water and appropriate preservative, if any, for the specific sampling activity being undertaken. (EPA OSWER) Instrument Blank: a clean sample (e.g., distilled water) processed through the instrumental steps of the measurement process; used to determine instrument contamination. (EPA-QAD) Method Blank: a sample of a matrix similar to the batch of associated samples (when available) that is free from the analytes of interest and is processed simultaneously with and under the same conditions as samples through all steps of the analytical procedures, and in which no target analytes or interferences are present at concentrations that impact the analytical results for sample analyses. (NELAC) Reagent Blank: (method reagent blank): a sample consisting of reagent(s), without the target analyte or sample matrix, introduced into the analytical procedure at the appropriate point and carried through all subsequent steps to determine the contribution of the reagents and of the involved analytical steps. (QAMS) Blind Sample: a sub-sample for analysis with a composition known to the submitter. The analyst/laboratory may know the identity of the sample but not its composition. It is used to test the analyst or laboratory’s proficiency in the execution of the measurement process. (NELAC) A sample submitted for analysis with a composition and identity known to the submitter, but unknown to the analyst, and used to evaluate proficiency in the execution of the measurement process. (AIHA-LAP, LLC) Calibration: A set of operations used: (1) to determine the value of a reference standard or reference material to a stated uncertainty; or (2) to determine the accuracy of the reading of a test device to a stated uncertainty. (AIHA-LAP, LLC) A set of operations that establish, under specified conditions, the relationship between values of quantities indicated by a measuring instrument or measuring system, or values represented by a material measure or a reference material, and the corresponding values realized by standards. (1) In calibration of support equipment, the values realized by standards are established through the use of reference standards that are traceable to the International system of units (SI). (2) In calibration according to methods, the values realized by standards are typically established through the use of reference materials that are either purchased by the laboratory with a certificate of analysis or purity, or prepared by the laboratory using support equipment that has been calibrated or verified to meet specifications. (NELAP)





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Calibration Curve: The mathematical relationship between the known values, such as concentrations, of a series of calibration standards and their instrument response. (NELAC) A graphical relationship between the known values for a series of calibration standards and instrument responses. The levels of the calibration standards should bracket the range of measurements. (AIHA) Calibration Method: a defined technical procedure for performing a calibration. (NELAC) Calibration Standard: a substance or reference material used for calibration (NELAC) Certification: Procedure by which a third party gives written assurance that the competence of a person, organization, or other entity to perform a function or service conforms to specified requirements. (AIHA-LAP, LLC) Certified Reference Material (CRM): Reference material accompanied by a certificate, having a value, measurement uncertainty, and stated metrological traceability chain to a national metrology institute.. (NELAC) A reference material that has one or more of its property values established by a technically valid procedure, and is accompanied by or traceable to a certificate or other documentation issued by a certifying body. (AIHA-LAP, LLC) Chain-of-Custody: Definitive evidence (a record) of the persons who had possession or custody of the sample(s) for all periods of time, as it moved from the point of collection to the final analytical result. (AIHA-LAP, LLC) Chain-of-Custody Form: Record that documents the possession of the samples from the time of collection to receipt in the laboratory. This record generally includes: the number and types of containers, the mode of collection; the collector; time of collection; preservation; and requested analyses. Check Sample: An uncontaminated sample matrix spiked with a known amount of analyte, usually from the same source as the calibration standard. It is generally used to establish the stability of the analytical system, but also may be used to assess the performance of all or a portion 2 of the measurement system. (AIHA-LAP, LLC) Clean Air Act: the enabling legislation in 42 U.S.C. 7401 et seq., Public Law 91-604, 84 Stat. 1676 Pub. L. 95-95, 91 Stat., 685 and Pub. L. 95-190, 91 Stat., 1399, as amended, empowering EPA to promulgate air quality standards, monitor and to enforce them. (NELAC) Client: See Customer. Comparability: Refers to the ability to compare data from different sources with a degree of confidence. Completeness: Refers to the amount of data that is successfully collected with respect to that amount intended in the study design. Comprehensive Environmental Response, Compensation and Liability Act (CERCLA/Superfund): the enabling legislation in 42 U.S.C. 9601-9675 et seq., as amended by the Superfund Amendments and Reauthorization Act of 1986 (SARA), 42 U.S.C. 9601et seq., to eliminate the health and environmental threats posed by hazardous waste sites. (NELAC) Confidential Business Information (CBI): information that an organization designates as having the potential of providing a competitor with inappropriate insight into its management, operation or products. NELAC and its representatives agree to safeguard identified CBI and to maintain all information identified as such in full confidentiality. Confirmation: verification of the identity of a component through the use of an approach with a different scientific principle from the original method. These may include, but are not limited to:





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Second column confirmation Alternate wavelength Derivatization Mass spectral interpretation Alternative detectors or Additional cleanup procedures. (NELAC) Conformance: an affirmative indication or judgment that a product or service has met the requirements of the relevant specifications, contract, or regulation; also the state of meeting the requirements. (ANSI/ASQC E4-1994) Contributor: a participant in NELAC who is not a Voting Member. Contributors include representatives of laboratories, manufacturers, industry, business, consumers, academia, laboratory associations, laboratory accreditation associations, counties, municipalities, and other political subdivisions, other federal and state officials not engaged in environmental activities, and other persons who are interested in the objectives and activities of NELAC. (NELAC)[Art III, Const] Control Chart: A graph of some measurement plotted over time or sequence of sampling, together with control limit(s) and, usually, a central line and warning limit(s). (AIHA-LAP, LLC) Corrective Action: the action taken to eliminate the causes of an existing nonconformity, defect or other undesirable situation in order to prevent recurrence. (ISO 8402) All activities taken, whether unsuccessful or not, to eliminate the cause(s) of an existing nonconformity or deficiency in order to prevent recurrence. (AIHA-LAP, LLC) Customer: Any person or organization that engages the services of a laboratory. Used interchangeably with “client” in this and other quality system documents. Data Audit: a qualitative and quantitative evaluation of the documentation and procedures associated with environmental measurements to verify that the resulting data are of acceptable quality (i.e., that they meet specified acceptance criteria). (NELAC) Data Reduction: the process of transforming raw data by arithmetic or statistical calculations, standard curves, concentration factors, etc., and collation into a more useable form. (NELAC) Deficiency: A failure to comply with the requirements of the AIHA-LAP, LLC accreditiaion programs or the laboratory’s own stated management system requirements.A failure to comply with a requirement of the AIHA Accreditation Program(s) or a laboratory’s own stated quality system requirements. (AIHA-LAP, LLC) Delegate: any environmental official of the States or the Federal government not sitting in the House of Representatives, who is eligible to vote in the House of Delegates. (NELAC) Demonstration of Capability: a procedure to establish the ability of the analyst to generate analytical results of acceptable accuracy and precision. (NELAC) Denial: The decision not to granta laboratory initial accreditation. (AIHA-LAP, LLC.)Detection Limit: the lowest concentration or amount of the target analyte that can be identified, measured, and reported with confidence that the analyte concentration is not a false positive value. See Method Detection Limit. (NELAC) Determination: An analysis with a qualitative result. (AIHA-LAP, LLC) Deviation: A departure from written procedures, test methods, contracts or any other standard operating procedure that is part of the laboratory Quality Assurance System. (AIHA-LAP, LLC)





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Document Control: the act of ensuring that documents (and revisions thereto) are proposed, reviewed for accuracy, approved for release by authorized personnel, distributed properly and controlled to ensure use of the correct version at the location where the prescribed activity is performed. (ASQC) Duplicate Samples: Two samples taken from and representative of the same population and carried through all steps of the sampling and analytical procedures in an identical manner. Duplicate samples are used to assess variance of the total method including sampling and analysis. (AIHA-LAP, LLC) Environmental Laboratory Advisory Board (ELAB): a Federal Advisory Committee, with members appointed by EPA and composed of a balance of non-state, non-federal representatives, from the environmental laboratory community, and chaired by an ELAB member. (NELAC)[1.6.2] Environmental Lead Laboratory Accreditation Program (ELLAP): This AIHA-LAP,LLC program complies with the requirements of the EPA National Lead Laboratory Accreditation Program (NLLAP) Laboratory Quality System Requirements (LQSR) and also conforms to the ISO/IEC 17025 Standard and ISO/IEC Guide 58 requirements. (AIHA-LAP, LLC) Environmental Lead Proficiency Analytical Testing (ELPAT): Required quarterly quality assurance lead samples of various matrices analyzed by accredited and participating laboratories as a way to determine laboratory testing proficiency of the ELLAP Results are evaluated by AIHA-PAT, LLC and are used to determine laboratory proficiency. AIHA-LAP, LLC) Environmental Monitoring Management Council (EMMC): an EPA Committee consisting of EPA managers and scientists, organized into a Policy Council, a Steering Group, ad hoc Panels, and work groups addressing specific objectives, established to address EPA-wide monitoring issues. (NELAC) Equipment: All physical items (including software and instruments) in the facility used in the performance of analytical testing. (AIHA-LAP, LLC) Equipment Log: A chronological record of preventive and emergency maintenance performed on any equipment. The logs include a record of calls, service technician summaries, records of calibration by the manufacturer, routine user maintenance, and other information as required by these policies. (AIHA-LAP, LLC) Experimental Field of Proficiency Testing (Experimental FoPT): Analytes for which a laboratory is required to analyze a PT sample if they seek or maintain accreditation for the field of accreditation but for which successful analysis is not required in order to obtain or maintain accreditation. Federal Insecticide, Fungicide and Rodenticide Act (FIFRA): the enabling legislation under 7 U.S.C. 135 et seq., as amended, that empowers the EPA to register insecticides, fungicides, and rodenticides. (NELAC) Federal Water Pollution Control Act (Clean Water Act, CWA): the enabling legislation under 33 U.S.C. 1251 et seq., Public Law 92-50086 Stat. 816, that empowers EPA to set discharge limitations, write discharge permits, monitor, and bring enforcement action for non-compliance. (NELAC) Field Blank: An analyte-free matrix carried to the sampling site, exposed to the sampling conditions (e.g., bottle caps removed), returned to the laboratory, treated as a sample, and carried through all steps of the analysis. For example, a clean culture media plate, sorbent tube, or a clean filter could be used as a field blank. The field blank, which should be treated just like the





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sample, evaluates possible effects attributable to shipping and field handling procedures. (AIHA-LAP, LLC) Field of Accreditation: Those matrix, technology/method, and analyte combinations for which the accreditation body offers accreditation. (NELAC) Field of Proficiency Testing (FoPT):Analysis for which a laboratory is required to successfully analyze a PT sample in order to obtain or maintain accreditation, collectively defined as: matrix, technology/method, analyte. FoT: Field of Testing Finding: an assessment conclusion referenced to a laboratory accreditation standard and supported by objective evidence that identifies a deviation from a laboratory accreditation standard requirement. (NELAC) Governmental Laboratory: as used in these standards, a laboratory owned by a Federal, state, or tribal government; includes government-owned contractor-operated laboratories. (NELAC) Holding Times (Maximum Allowable Holding Times): The maximum times that samples may be held prior to analysis and still be considered valid or not compromised. (40 CFR Part 136) The maximum time that can elapse between two specified activities. (NELAC) Inspection: an activity such as measuring, examining, testing, or gauging one or more characteristics of an entity and comparing the results with specified requirements in order to establish whether conformance is achieved for each characteristic. (ANSI/ASQC E4-1994) Interim Accreditation: temporary accreditation status for a laboratory that has met all accreditation criteria except for a pending on-site assessment which has been delayed for reasons beyond the control of the laboratory. (NELAC) Inter-laboratory Comparisons: Evaluation of tests on the same or similar items by two or more laboratories. (AIHA-LAP, LLC) Internal Quality Control: Routine activities and checks, such as periodic calibrations, duplicate analyses and matrix spikes that are included in routine internal procedures to control the accuracy and precision of measurements. Internal Standard: A known amount of standard added to a test portion of a sample as a reference for evaluating and controlling the precision and bias of the applied analytical method. (NELAC) Laboratory: a body that calibrates and/or tests. (ISO 25) An entity that tests, either at a fixed site, mobile facility or field operations facility. (AIHA-LAP, LLC) Laboratory Accreditation Programs (AIHA-LAP, LLC) General term referring to any AIHA_LAP, LLC program established to maintain standards of performance for laboratories analyzing samples and evaluating exposures to hazardous agents. (AIHA-LAP, LLC) Laboratory Assessment: An onsite evaluation of a laboratory for the purpose of conducting a technical systems audit to assess compliance with AIHA accreditation requirements and technical competence to perform the testing for which the Lab is seeking accreditation. (AIHA-LAP, LLC) Laboratory Control Sample (however named, such as laboratory fortified blank, spiked blank, or QC check sample): Laboratory Control Sample (LCS)/Method Spike Sample: A matrix-based reference material with an established concentration obtained from a source independent of the instrument calibration and traceable to NIST or other similar reference materials. The LCS is carried through the entire procedure from sample preparation through





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analysis as if it were a field sample. The purpose of the LCS is to evaluate bias of the method. (AIHA-LAP, LLC) A sample matrix, free from the anlytes of interest, spiked with verified known amounts of analytes or a material containing known and verified amounts of analytes and taken through all sample preparation and analytical steps of the procedure unless otherwise noted in a reference method. It is generally used to establish intra-laboratory or analyst specific precision and bias to assess the performance of all or portion of the measurement system. (NELAC) Laboratory Control Sample Duplicate (LCSD)/Method Spike Sample Duplicate: A duplicate of the LCS. (AIHA-LAP, LLC) Laboratory Duplicate: aliquots of a sample taken from the same container under laboratory conditions and processed and analyzed independently. (NELAC) Laboratory Quality Assurance Program(s) (LAP-LLC): General term referring to any AIHA program or programs established to maintain the highest possible standards of performance for analysts and/or laboratories analyzing samples and evaluating exposures to hazardous agents. (AIHA-LAP, LLC) Legal Chain-of-Custody Protocols: procedures employed to record the possession of samples from the time of sampling through the retention time specified by the client or program. These procedures are performed at the special request of the client and include the use of a Chain of Custody Form that documents the collection, transport, and receipt of compliance samples by the laboratory. In addition, these protocols document all handling of the samples within the laboratory. (NELAC) Limit(s) of Detection (LOD): A laboratory’s estimate of the minimum amount of an analyte in a given matrix that an analytical procedure can reliably detect in their facility. (NELAP) Limit(s) of Quantitation (LOQ): The minimum levels, concentrations, or quantities of a target variable (e.g., target analyte) that can be reported with a specific degree of confidence. (NELAC) Manager (however named): the individual designated as being responsible for the overall operation, all personnel, and the physical plant of the environmental laboratory. A supervisor may report to the manager. In some cases, the supervisor and the manager may be the same individual. (NELAC) Matrix: the substrate of a test sample.

Field of Accreditation Matrix: these matrix definitions shall be used when accrediting a laboratory (see Field of Accreditation).

Drinking Water: any aqueous sample that has been designated a potable or potential potable water source. Non-Potable Water: any aqueous sample excluded from the definition of Drinking Water matrix; includes surface water, groundwater, effluents, water treatment chemicals, and TCLP or other extracts. Solid and Chemical Materials: includes soils, sediments, sludges, products and by-products of an industrial process that results in a matrix not previously defined. Biological Tissue: any sample of a biological origin such as fish tissue, shellfish, or plant material. Such samples shall be grouped according to origin. Air and Emissions: whole gas or vapor samples including those contained in flexible or rigid wall containers and the extracted concentrated analytes of interest





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from a gas or vapor that are collected with a sorbent tube, impinger solution, filter, or other device. (NELAC).

Quality System Matrix: These matrix definitions are an expansion of the field of accreditation matrices and shall be used for purposes of batch and quality control requirements. These matrix distinctions shall be used:

Aqueous: any aqueous sample excluded from the definition of Drinking Water matrix or Saline/Estuarine source; includes surface water, groundwater, effluents, and TCLP or other extracts. Drinking Water: any aqueous sample that has been designated a potable or potential potable water source. Saline/Estuarine: any aqueous sample from an ocean or estuary, or other salt-water source such as the Great Salt Lake. Non-aqueous Liquid: any organic liquid with <15% settleable solids. Biological Tissue: any sample of a biological origin such as fish tissue, shellfish, or plant material. Such samples shall be grouped according to origin. Solids: includes soils, sediments, sludges and other matrices with >15% settleable solids. Chemical Waste: a product or by-product of an industrial process that results in a matrix not previously defined. Air and Emissions: whole gas or vapor samples including those contained in flexible or rigid wall containers and the extracted concentrated analytes of interest from a gas or vapor that are collected with a sorbent tube, impinger solution, filter, or other device. (NELAC)

The component or substrate (e.g., soil, air or charcoal tube) that contains the analyte of interest. (AIHA-LAP, LLC)

Matrix Duplicate: A replicate matrix prepared in the laboratory and analyzed to obtain a measure of precision. (NELAC) Matrix Spike (spiked sample or fortified sample): a sample prepared, taken through all sample preparation and analytical steps of the procedure unless otherwise noted in a reference method, by adding a known amount of target analyte to a specified amount of matrix sample for which an independent test result of target analyte concentration is available. Matrix spikes are used, for example, to determine the effect of the matrix on a method's recovery efficiency. (NELAC) An aliquot of sample, or sample media, spiked with a known concentration of target analyte(s). The spiking occurs prior to sample preparation and analysis. (AIHA-LAP, LLC) Matrix Spike Duplicate (spiked sample or fortified sample duplicate): A replicate matrix spike prepared in the laboratory and analyzed to obtain a measure of the precision of the recovery for each analyte. (NELAC) May: denotes permitted action, but not required action. Measurement Quality Objectives (MQOs): The desired sensitivity, range, precision, and bias of a measurement. Measurement System: A method, as implemented at a particular laboratory, and which includes the equipment used to perform the test and the operator(s). Method: see Test Method Method Blank: An unexposed sampling media or reagent(s), not taken to the field or shipped, but carried through the complete sample preparation and analytical procedure. The blank is used





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to assess possible background contamination from the analytical process. This blank may also be referred to as a laboratory blank. (AIHA-LAP, LLC) Method Detection Limit (MDL): the minimum concentration of a substance (an analyte) that can be measured and reported with 99% confidence that the analyte concentration is greater than zero and is determined from analysis of a sample in a given matrix containing the analyte. (40 CFR Part 136, Appendix B) The minimum concentration of an analyte that, in a given matrix and with a specific method, has a 99 percent probability of being identified, qualitatively or quantitatively measured, and reported to be greater than zero. (AIHA-LAP, LLC) Method Performance: A general term used to document the characteristics of a method. These characteristics usually include method detection limits, linearity, precision, accuracy and bias and uncertainty of measurement. See Acceptance Limits. (AIHA-LAP, LLC) Must: denotes a requirement that must be met. (Random House College Dictionary) National Accreditation Database: the publicly accessible database listing the accreditation status of all laboratories participating in NELAP. (NELAC) National Institute of Standards and Technology (NIST): A federal agency of the US Department of Commerce’s Technology Administration that is designed as the United States national metrology institute (NMI). (NELAC) National Environmental Laboratory Accreditation Conference (NELAC): a voluntary organization of State and Federal environmental officials and interest groups purposed primarily to establish mutually acceptable standards for accrediting environmental laboratories. A subset of NELAP. (NELAC) National Environmental Laboratory Accreditation Program (NELAP): the overall National Environmental Laboratory Accreditation Program of which NELAC is a part. (NELAC) National Voluntary Laboratory Accreditation Program (NVLAP): a program administered by NIST that is used by providers of proficiency testing to gain accreditation for all compounds/matrices for which NVLAP accreditation is available, and for which the provider intends to provide NELAP PT samples. (NELAC) Negative Control: measures taken to ensure that a test, its components, or the environment do not cause undesired effects, or produce incorrect test results. (NELAC) NELAC Standards: the plan of procedures for consistently evaluating and documenting the ability of laboratories performing environmental measurements to meet nationally defined standards established by the National Environmental Laboratory Accreditation Conference. (NELAC) NELAP Recognition: the determination by the NELAP Director that an accrediting authority meets the requirements of the NELAP and is authorized to grant NELAP accreditation to laboratories. (NELAC) Nonconformity: Noncompliance with any quality assurance policy, procedure, or specification. Nonconforming work results from an analysis event in which the QC results are not within acceptance limits and/or method specifications are not met. (AIHA-LAP, LLC) Non-governmental Laboratory: any laboratory not meeting the definition of the governmental laboratory. (NELAC) Performance Audit: the routine comparison of independently obtained qualitative and quantitative measurement system data with routinely obtained data in order to evaluate the proficiency of an analyst or laboratory. (NELAC)





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Performance Based Measurement System (PBMS): a set of processes wherein the data quality needs, mandates or limitations of a program or project are specified and serve as criteria for selecting measurement processes which will meet those needs in a cost-effective manner. (NELAC) Policy: An organization’s written statement of commitment to implement a management program element. (AIHA-LAP, LLC) Positive Control: measures taken to ensure that a test and/or its components are working properly and producing correct or expected results from positive test subjects. (NELAC) Precision: The degree to which a set of observations or measurements of the same property, obtained under similar conditions, conform to themselves; a data quality indicator. Precision is usually expressed as standard deviation, variance or range, in either absolute or relative terms. (NELAC) The degree to which a set of observations or measurements of the same property, usually obtained under similar conditions, conform to themselves. Precision is often expressed as standard deviation, variance or range, in either absolute or relative terms. (AIHA-LAP, LLC) Preventive Action: A planned activity to identify, recognize and control potential sources of nonconformity and to introduce needed improvements. (AIHA-LAP, LLC) Procedure: A written set of instructions that describe how to implement a policy requirement, or how to carry out a specific task. (AIHA-LAP, LLC) A specified way to carry out an activity or process. Procedures can be documented or not. (NELAC) Preservation: Any condition under which a sample must be kept in order to maintain the chemical and/or biological integrity prior to analysis. (NELAC) Primary Accreditation Body (Primary AB): The accreditation body responsible for assessing a laboratory’s total quality system, on-site assessment, and PT performance tracking for fields of accreditation. (NELAC) Proficiency Analytical Testing (PAT): Refers to any proficiency analytical testing program(s), such as the programs established under the Analytical Quality Programs. See Inter-laboratory Comparisons. (AIHA-LAP, LLC) Proficiency Testing (PT): A means to evaluate a laboratory’s performance under controlled conditions relative to a given set of criteria, through analysis of unknown samples provided by an external source. (NELAC) Proficiency Testing Oversight Body/Proficiency Testing Provider Accreditor (PTOB/PTPA): an organization with technical expertise, administrative capacity and financial resources sufficient to implement and operate a national program of PT provider evaluation and oversight that meets the responsibilities and requirements established by NELAC standards. (NELAC) Proficiency Testing (PT): Refers to any proficiency testing program(s),such as the programs established under the Analytical Quality Programs. (AIHA-LAP, LLC) Proficiency Testing Program (PT Program): the aggregate of providing rigorously controlled and standardized environmental samples to a laboratory for analysis, reporting of results, statistical evaluation of the results and the collective demographics and results summary of all participating laboratories. (NELAC) Proficiency Testing Provider (PTP): Aperson or organization accredited by the TNI-approved Proficiency Testing Provider Accreditor to operate a TNI-compliant PT program. (NELAC)





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Proficiency Testing Provider Accreditor (PTPA): An organization t5hat is approved by TNI to accredit and monitor the performance of proficiency testing providers. (NELAC) Proficiency Testing Sample (PT Sample): A sample, the composition of which is unknown to the laboratory and is provided to test whether the laboratory can produce analytical results within the specified acceptance criteria. (NELAC) Proficiency Testing Study (PT Study): A single complete sequence of circulation of proficiency testing samples to all participants in a proficiency test program. PT Study Opening Date: The calendar date that a PT sample is first made available to any laboratory by a PT provider. PT Study Closing Date: The calendar date for which analytical results for a PT sample shall be received by the PT provider from the laboratory. Protocol: a detailed written procedure for field and/or laboratory operation (e.g., sampling, analysis) that must be strictly followed. (NELAC) Quality: The suitability of a product or service for use, as perceived by the user. (AIHA-LAP, LLC) Quality Assurance: An integrated system of management activities involving planning, implementation, assessment, reporting and quality improvement to ensure that a process, item, or service is of the type and quality needed and expected by the client. (NELAC) An integrated system of activities involving planning, quality control, quality assessment, reporting, and quality improvement to ensure a product or service meets defined standards of quality within a stated level of confidence. (AIHA-LAP, LLC) Quality Assurance [Project] Plan (QAPP): a formal document describing the detailed quality control procedures by which the quality requirements defined for the data and decisions pertaining to a specific project are to be achieved. (EPA-QAD) Quality Control: The overall system of technical activities that measures the attributes and performance of a process , item, or service against defined standards to verify that they meet the stated requirements established by the customer; operational techniques and activities that are used to fulfill requirements for quality; also the system of activities and checks used to ensure that measurement systems are maintained within prescribed limits, providing protection against “out of control” conditions and ensuring that the results are of acceptable quality.. (NELAC) Technical activities whose purpose is to measure and control the quality of a product or service so that it meets the needs of users. The aim is to provide quality that is satisfactory, adequate, dependable and economical. (AIHA-LAP, LLC) Quality Control Sample: A sample used to assess the performance of all or a portion of the measurement system. One of any number of samples, such as CRM, a quality system matrix fortified by spiking, or actual samples fortified by spiking, intended to demonstrate that a measurement system or activity is in control. (NELAC) Quality Manager: The Quality Manger is responsible for implementation of the Quality Management System with direct access to the highest levels of management. The Quality Manger is responsible for planning and organizing audits. Quality Management System: System to establish a quality policy and quality objectives and to achieve those objectives. Quality Manual: a document stating the management policies, objectives, principles, organizational structure and authority, responsibilities, accountability, and implementation of an





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agency, organization, or laboratory, to ensure the quality of its product and the utility of its product to its users. (NELAC) A document stating the quality policy, quality system and internal quality control procedures of the laboratory. (AIHA-LAP, LLC) Quality System: a structured and documented management system describing the policies, objectives, principles, organizational authority, responsibilities, accountability, and implementation plan of an organization for ensuring quality in its work processes, products (items), and services. The quality system provides the framework for planning, implementing, and assessing work performed by the organization and for carrying out required QA and QC activities. Quantitation Limits: levels, concentrations, or quantities of a target variable (e.g., target analyte) that can be reported at a specified degree of confidence. (NELAC) Range: the difference between the minimum and the maximum of a set of values. (EPA-QAD) Raw Data: The documentation generated during sampling and analysis. This documentation includes, but not limited to, field notes, electronic data, magnetic tapes, untabulated sample results, QC sample results, print outs of chromatograms, instrument outputs, and handwritten records. (NELAC) Recognition: previously known as reciprocity. The mutual agreement of two or more parties (i.e., States) to accept each other’s findings regarding the ability of environmental testing laboratories in meeting NELAC standards. (NELAC)[1.5.3] Reference Material: Material or substance one or more of whose property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to materials. (NELAC) A material or substance, one or more properties of which are sufficiently homogeneous and well established to be used to monitor instrument and method performance. AIHA PAT samples may be used as reference materials. (AIHA-LAP, LLC) Reference Method: a method of known and documented accuracy and precision issued by an organization recognized as competent to do so. (NELAC) Reference Standard: Standard used for the calibration of working measurement standards in a given organization or at a given location.NELAC) A substance or reference material used to calibrate an instrument. Reference standards shall be NIST traceable or equivalent and of the highest quality available at the location. (AIHA-LAP, LLC) Reference Toxicant: the toxicant used in performing toxicity tests to indicate the sensitivity of a test organism and to demonstrate the laboratory’s ability to perform the test correctly and obtain consistent results (see Chapter 5, Appendix D, section 2.1f). (NELAC) Relative Percent Difference (RPD): A term defined as RPD = ((R1 – R2)/R) x 100 where R1 – R2 represents the absolute difference of two (2) values and R represents the average of the two (2) values. (AIHA-LAP, LLC) Relevant Degree: A program of collegiate study that is appropriate to the applicable accreditation program. (AIHA-LAP, LLC) Replicate Analyses: the measurements of the variable of interest performed identically on two or more sub-samples of the same sample within a short time interval. (NELAC) Reporting Limit: The lowest concentration of analyte in a sample that can be reported with a defined, reproducible level of certainty. This value is based on the low standard used for





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instrument calibration. For environmental lead analyses, the reporting limit must be at least twice the MDL. (AIHA-LAP, LLC) Representativeness: Refers to the degree to which the data collected accurately reflect the population, group or medium being sampled. Requirement: denotes a mandatory specification; often designated by the term “shall”. (NELAC) An essential criterion necessary for accreditation. (AIHA-LAP, LLC) Resource Conservation and Recovery Act (RCRA): the enabling legislation under 42 USC 321 et seq. (1976), that gives EPA the authority to control hazardous waste from the “cradle-to-grave”, including its generation, transportation, treatment, storage, and disposal. (NELAC) Revocation: the total or partial withdrawal of a laboratory’s accreditation by an accreditation body. (NELAC) The formal, permanent removal of a laboratory’s accreditation for noncompliance with AIHA accreditation requirements. (AIHA-LAP, LLC) Removal of the accredited status of a laboratory if the laboratory is found to have violated the conditions for accreditation. (NIST) Run: A set of consecutive measurements performed on different samples. (AIHA-LAP, LLC) Safe Drinking Water Act (SDWA): the enabling legislation, 42 USC 300f et seq. (1974), (Public Law 93-523), that requires the EPA to protect the quality of drinking water in the U.S. by setting maximum allowable contaminant levels, monitoring, and enforcing violations. (NELAC) Sample: for instrumental analyses, a sample is defined as an analytical determination. Thus a Continuing Calibration Verification Standard (CCV) is analyzed after every ten determinations, regardless of the type of sample (QC sample or test sample). For those test methods that require the analysis of an Initial or Continuing Calibration Blank (ICB or CCB) after the ICV or CCV analysis, the ICB or CCB is not counted as a determination. In addition, if a reagent/solvent blank analysis (rinse blank) is performed to ensure that carryover from a highly concentrated sample has not contaminated the system, this is not counted as a determination. For certain analyses (i.e., GC/MS), the requirement to analyze a CCV is per number of hours, not per number of determinations. Sample Log: A document where sample identification, date received, customer, etc., are noted when samples arrive at the laboratory. The log is part of the sample tracking system. See Sample Tracking. (AIHA-LAP, LLC) Sample Tracking: procedures employed to record the possession of the samples from the time of sampling until analysis, reporting, and archiving. These procedures include the use of a Chain of Custody Form that documents the collection, transport, and receipt of compliance samples to the laboratory. In addition, access to the laboratory is limited and controlled to protect the integrity of the samples. (NELAC) Sample Tracking: A documentation system of following a sample from receipt at the laboratory, through sample processing nd analysis, to final reporting. The system includes unique numbering, or bar coding labels, and the use of a Sample Log. (AIHA-LAP, LLC) Sampling: Activity related to obtaining a representative sample of the object of conformity assessment, according to a procedure. (NELAC) Secondary Accrediting Authority: the Territorial, State or federal agency that grants NELAC accreditation to laboratories, based upon their accreditation by a NELAP-recognized Primary Accrediting Authority. See also Recognition and Primary Accrediting Authority. (NELAC)[1.5.2.3]





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Selectivity: The ability to analyze, distinguish, and determine a specific analyte or parameter from another component that may be a potential or that may behave similarly to the target analyte or parameter within the measurement system. (NELAC) Sensitivity: the capability of a method or instrument to discriminate between measurement responses representing different levels (e.g., concentrations) of a variable of interest. (NELAC) Shall: denotes a requirement that is mandatory whenever the criterion for conformance with the specification requires that there is no deviation. This does not prohibit the use of alternative approaches or methods for implementing the specification so long as the requirement is fulfilled. (ANSI) Should: denotes a guideline or recommendation whenever noncompliance with the specification is permissible. (ANSI) Spike: a known mass of target analyte added to a blank sample or sub-sample; used to determine recovery efficiency or for other quality control purposes. (NELAC) SRM (NIST Standard Reference material): A reference material certified and distributed by the National Institute of Standards and Technology. Standard: The document describing the elements of laboratory accreditation that has been developed and established within the consensus principles of standard setting and meets the approval requirements of standard adoption organizations procedures and policies. (NELAC) A substance or material with properties believed to be known with sufficient accuracy to permit its use to evaluate the same property of another. In chemical measurements, it often describes a solution or substance commonly prepared by the analyst to establish a calibration curve or the analytical response function of an instrument. (AIHA-LAP, LLC) Standard Administrative Procedure (SAP): a written procedure that details administrative operations that thoroughly prescribes actions to be taken Standard Operating Procedures (SOPs): A written document which details the method for an operation, analysis, or action, with thoroughly prescribed techniques and steps. SOPs are officially as the methods for performing certain routine or repetitive tasks. (NELAC) A written document that details the procedures of an operation; an analysis or action whose techniques and procedures are thoroughly prescribed, and which are accepted as the procedure for performing certain routine or repetitive tasks. (AIHA-LAP, LLC) Standard Reference Material (SRM): a certified reference material produced by the U.S. National Institute of Standards and Technology or other equivalent organization and characterized for absolute content, independent of analytical method. (EPA-QAD) A certified reference material produced by the U.S. National Institute of Standards and Technology (NIST) and characterized for absolute content independent of analytical method. It is accompanied by a certificate that reports the results of the characterization and the intended use of the material. (AIHA-LAP, LLC) Standardization: The process of establishing the quantitative relationship between a known mass of target material and the measurement system (example, instrument response). See Calibration and Calibration curve. The term may also refer to activities that establish provisions for common and repeated use of accreditation policies to achieve an optimum level of conformity. (AIHA-LAP, LLC) Statistical Minimum Significant Difference (SMSD): the minimum difference between the control and a test concentration that is statistically significant; a measure of test sensitivity or power. The power of a test depends in part on the number of replicates per concentration; the





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significance level selected, e.g., 0.05, and the type of statistical analysis. If the variability remains constant, the sensitivity of the test increases as the number of replicates is increased. (NELAC) Stock Solution: A concentrated solution of analyte(s) or reagent(s) prepared and verified by prescribed procedure(s), and used for preparing calibration standards. See Calibration Standard. (AIHA-LAP, LLC) Study: This term refers to a PT study or supplemental PT study. Supplemental Proficiency Testing Study (Supplemental PT Study): A PT sample that may be from a lot previously released by a PT provider that meets the requirements for supplemental PT samples given in Volume 3 of TNI Standard but that does not have a pre-determined opening date and closing date. Subsample: A representative portion of a sample; a subsample may be taken from any location or a field sample; in analytical chemistry, an “aliquot.” (AIHA-LAP, LLC) Suggestion: Suggested activity or advice for improving laboratory performance often made during a site assessment. A suggestion is not a requirement. (AIHA-LAP, LLC) Supervisor (however named): the individual(s) designated as being responsible for a particular area or category of scientific analysis. This responsibility includes direct day-to-day supervision of technical employees, supply and instrument adequacy and upkeep, quality assurance/quality control duties and ascertaining that technical employees have the required balance of education, training and experience to perform the required analyses. (NELAC) Surrogate: a substance with properties that mimic the analyte of interest. It is unlikely to be found in environment samples and is added to them for quality control purposes. (QAMS) Suspension: the temporary removal of a laboratory’s accreditation for a defined period of time, which shall not exceed six (6) months or the period of accreditation, whichever is longer, in order to allow the laboratory time to correct deficiencies or area of nonconformance with the Standard. (NELAC) A temporary removal of the accredited status of a laboratory when it is found to be out of compliance with specific program requirements. (AIHA-LAP, LLC) Technical Director: individual(s) who has overall responsibility for the technical operation of the environmental testing laboratory. (NELAC) Technical Systems Audit: A thorough, systematic, onsite, qualitative evaluation of facilities, equipment, personnel, training, procedures, record keeping, data validation, data management and reporting aspects of a total quality system. (AIHA-LAP, LLC) Technology: A specific arrangement of analytical instruments, detection systems, and/or preparation techniques. Test: a technical operation that consists of the determination of one or more characteristics or performance of a given product, material, equipment, organism, physical phenomenon, process or service according to a specified procedure. The result of a test is normally recorded in a document sometimes called a test report or a test certificate. (ISO/IEC Guide 2-12.1, amended) A technical operation that consists of determining one or more elements in a sample according to a specified procedure. (AIHA-LAP, LLC) Test Method: Specified technical procedure for performing a test. See Standard Operating Procedure (AIHA-LAP, LLC)





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A body of procedures and techniques for performing an activity (e.g., sampling, chemical analysis, quantification), systematically presented in the order in which they are to be executed. (NELAC). Testing Laboratory: a laboratory that performs tests. (ISO/IEC Guide 2-12.4) Test Sensitivity/Power: the minimum significant difference (MSD) between the control and test concentration that is statistically significant. It is dependent on the number of replicates per concentration, the selected significance level, and the type of statistical analysis (see Chapter 5, Appendix D, section 2.4.a). (NELAC) TNI PT Board: A board consisting of TNI members or affiliates, appointed by the TNI Board of Directors, which is responsible for the successful implementation and operation of the TNI Proficiency Testing Program. The duties of the TNI PT Board are defined in the TNI PT Board Charter. Tolerance Chart: A chart in which the plotted quality control data is assessed via a tolerance level (e.g. +/- 10% of a mean) based on the precision level judged acceptable to meet overall quality/data use requirements instead of a statistical acceptance criteria (e.g. +/- 3 sigma) (applies to radiobioassay laboratories). (ANSI) Toxic Substances Control Act (TSCA): the enabling legislation in 15 USC 2601 et seq., (1976), that provides for testing, regulating, and screening all chemicals produced or imported into the United States for possible toxic effects prior to commercial manufacture. (NELAC) Traceability: The ability to trace the history, application, or location of an entity by means of recorded identifications. In a calibration sense, traceability relates measuring equipment to national or international standards, primary standards, basic physical constants or properties, or reference materials. In a data collection sense, it relates calculations and data generated throughout the project back to the requirements for the quality of the project. (NELAC) Property of the result of a measurement or the value of a standard whereby it can be related to stated references, usually international or national standards, through an unbroken chain of comparisons all having stated uncertainties. (NIST) The process of documenting the value of a reference material or standard as related to NIST standards or equivalent through an unbroken chain of comparisons with stated uncertainties. (AIHA-LAP, LLC) Uncertainty of Measurement: Result of the evaluation aimed at characterizing the range within which the true value of a test result is estimated to lie, generally within a given likelihood. (AIHA-LAP, LLC) Parameter, associated with the result of a measurement that characterizes the dispersion of the values that could reasonably be attributed to the measurand. (NIST) United States Environmental Protection Agency (EPA): the federal governmental agency with responsibility for protecting public health and safeguarding and improving the natural environment (i.e., the air, water, and land) upon which human life depends. (US-EPA) Validation: the process of substantiating specified performance criteria. (EPA-QAD) The process of confirming specified method performance criteria. (AIHA-LAP, LLC) Verification: confirmation by examination and objective evidence that specified requirements have been met. (NELAC) NOTE: In connection with the management of measuring equipment, verification provides a means for checking that the deviations between values indicated by a measuring instrument and corresponding known values of a measured quantity are consistently smaller than the maximum





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allowable error defined in a standard, regulation or specification peculiar to the management of the measuring equipment. The result of verification leads to a decision either to restore in service, to perform adjustment, to repair, to downgrade, or to declare obsolete. In all cases, it is required that a written trace of the verification performed shall be kept on the measuring instrument’s individual record. Confirmation by examination and provision of evidence that specified requirements have been met. (AIHA-LAP, LLC) Voting Member: officials in the employ of the Government of the United States, and the States, the Territories, the Possessions of the United States, or the District of Columbia and who are actively engaged in environmental regulatory programs or accreditation of environmental laboratories. (NELAC)





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Appendix 1

Summary of Changes from Rev 13

• Addition to the Introduction stating that the individual analyst has the responsibility to

monitor quality control indicators and to initiate corrective action that can include stopping work if necessary.

• Added a reference to Consumer Products Safety Commission (CPSC) to the Policy Statement and to Section I: Introduction Revised the Duties of the Quality Assurance Director (2.1.2.4) to bring them into agreement with DOD requirements and the requirement to insure compliance with ISO 17025.

• Revised Duties of Technical Manager (2.1.2.2) to include the requirement to insure compliance with ISO 17025.

• Revised sections 4.2 and 4.2.6 to require calibration of the NIST Traceable Thermometer at least every five years.

• Minor editorial revisions.





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APPENDIX 2: Organizational Chart





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APPENDIX 3: STAT SOPs

ADMINISTRATIVE SOPs SOP Number STAT SOP ADMINISTRATIVE PROCEDURES 005 SOP 005 Document Control 006 SOP 006 Management Review of Quality System 100 SOP 100 SOP on SOPs 230 SOP QA 230 Corrective Action 240 SOP 240 Archiving1000 SOP 1000 Control and Use of

Laboratory Notebooks 1010 SOP 1010 Analytical Standards and Reagents Receipt and

Preparation 1020 SOP QA 1020 Laboratory Glassware Cleaning 1040 SOP 1040 General Laboratory Practices 1210 SOP 1210 Method Detection Limits 1220 SOP 1220 Internal Quality Assurance Audit 1230 SOP 1230 Training 1250 SOP 1250 Data Review 1255 SOP 1255 Manual Integration 1270 SOP 1270 Uncertainty SAFETY DEPARTMENT 003 SOP QA 003 Chemical Hygiene Plan 1130 SOP 1130 Waste Disposal CUSTOMER SERVICE DEPARTMENT 220 SOP 220 Customer Service 300 SOP 300 Sample Receiving and Login Procedures 1330 SOP 1330 Purchasing INFORMATION TECHNOLOGY DEPARTMENT 1400 SOP 1400 LIMS 1500 SOP 1500 Computer Network





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APPENDIX 3 (cont.'d) NELAC APPROVED TEST METHODS

Laboratory Test Method STAT SOP SW846 9095A SOP 2010 Paint Filter Liquids Test by EPA Method 9095A SW846 1311 SOP 2125 Leaching Procedures (Toxicity Characteristic

Leaching Procedure (EPA Method 1311)) SW846 1312 SOP 2125 Leaching Procedures (Synthetic Precipitation

Leaching Procedure (EPA Method 1312)) SW846 3005A SOP 3005 SW848 3005 Acid Digestion of Waters for Total

Recoverable or Dissolved Metals for Analysis by FLAA, ICP, or ICP-MS

SW846 3620B SOP 3060 Florisil Clean up for PCBs and Pesticides (EPA

Method 3620B) SW846 3660B SOP 3070 Sulfur & Sulfuric Acid/Permanganate Cleanup

for PCBs and Pesticides (EPA Method 3660B & 3665A) SW846 3665A SOP 3070 Sulfur & Sulfuric Acid/Permanganate Cleanup

for PCBs and Pesticides (EPA Method 3660B & 3665A) SW846 3050B SOP 3110 SW846 3050B Acid Digestion of Sediment,

Sludges, and Soils for Metals Analysis by FLAA, ICP, or ICP-MS

SW846 3050B SOP 3115 Extraction of High Volume Filters SW846 3630C SOP 3330 Silica Gel Cleanup for Semi-Volatile Organics

(EPA Method 3630C) SW846 3510C SOP 3500 Extractions of Samples for Semi-Volatile

Organic Analyses (EPA Methods 3510C, 3520C, 3540, 3545, 3550B, 3580A, 8151A)

SW846 3540 SOP 3500 Soxhlet Extraction: Extractions of Samples for

Volatile and Semi-Volatile Organics (EPA Methods 3510C, 3520C, 3540, 3545, 3550B, 3580A, 8151A)





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APPENDIX 3 (cont.’d) NELAC APPROVED TEST METHODS

Laboratory Test Method STAT SOP SW846 3545 SOP 3500 Pressurized Fluid Extraction: Extractions of

water nonsoluble or slightly soluble Semi-Volatile Organics (EPA Methods 3510C, 3520C, 3540, 3545, 3550B, 3580A, 8151A)

SW846 3550B SOP 3500 Extractions of Samples for Semi-Volatile

Organic Analyses (EPA Methods 3510C, 3520C, 3550B, 3580A, 8151A)

SW846 3580A SOP 3500 Extractions of Samples for Semi-Volatile


SW846 8151A SOP 3500 Extractions of Samples for Semi-Volatile


SW846 9012A SOP 3610 Total and Amenable Cyanide: Distillation by

EPA 9012A SW846 Ch. 7 SOP 3615 Reactive Cyanide and Sulfide: Distillation by

SW 846, Chapter 7. SW846 9065 SOP 3620 Phenolics: Distillation by EPA 9065. SW846 8260B SOP 4000 Volatile Organic Compounds by Gas

Chromatography/Mass Spectrometry (GC/MS) (EPA Methods 5030B/5035/ 8260B)

SW846 8270C SOP 4020 Semi-Volatile Organic Compounds by Gas

Chromatography/Mass Spectrometry (GC/MS) (EPA Method 8270C)

SW846 8081A SOP 4050 Organochlorine Pesticides & PolyChlorinated

Biphenyl by Gas Chromatography/Electron Capture Detector (EPA Methods 8081A/8082)

SW846 8082 SOP 4050 Organochlorine Pesticides & PolyChlorinated

Biphenyl by Gas Chromatography/Electron Capture Detector (EPA Methods 8081A/8082)





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Laboratory Test Method STAT SOP ASTM Method D-4059 SOP 4051 PolyChlorinated Biphenyl by Gas

Chromatography/Electron Capture Detector (ASTM Method D-4059)--DRAFT

SW846 8321A SOP 4080 ChloroPhenoxy Herbicides by HPLC (EPA

Method 8321A) SW846 8015M SOP 4090 Total Petroleum Hydrocarbons by GC/FID SW846 1010 SOP 4105 Ignitibility by EPA 1010/ ASTM D93-02

Pensky-Martens Closed Cup and ASTM D1310 Tag Open Cup- DRAFT

SW846 9040B SOP 4210 pH of Aqueous, Soil and Waste Samples by EPA

Method 9040B, 9045C, 150.1 SW846 9045C SOP 4210 pH of Aqueous, Soil and Waste Samples by EPA

Method 9040B, 9045C, 150.1 SW846 8270C SIM SOP 4500 Polynuclear Aromatic Compounds by Gas

Chromatography/Mass Spectrometry (GC/MS) with Selective Ion Monitoring (SIM) (EPA Method 8270C SIM)

SW846 6020 SOP 4510 Metals Analysis by Inductively Coupled

Plasma- Mass Spectrometry (EPA Method 6020 and EPA Method IO-3.5)

SW846 7470A SOP 4530 Mercury in Water, Solid or Semisolid Water

(Manual Digestion/Automated Analysis Cold-Vapor Technique (EPA Method 7470A & 7471A)

SW846 7471A SOP 4530 Mercury in Water, Solid or Semisolid Water

(Manual Digestion/Automated Analysis Cold-Vapor Technique (EPA Method 7470A & 7471A)

SW846 3060A SOP 4600 Automated Hexavalent Chromium Analysis by

EPA Method 7196A and 3060A SW846 7196A SOP 4600 Automated Hexavalent Chromium Analysis by

EPA Method 7196A and 3060A





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Laboratory Test Method STAT SOP SW846 9012A SOP 3610 Total and Amenable Cyanide: Distillation by

9012A SW846 Chapter 7.3.3.2 SOP 3615 Reactive Cyanide and Sulfide: Distillation by

SW846 Chapter 7 SW846 9065 SOP 3620 Phenolics 4AAP: Distillation by EPA 9065 EPA 415.1 SOP 4630 Total Organic Carbon By EPA 415.1 SW846 9012A SOP 4710 Automated Cyanide Analysis by EPA 9012A SW846 9066 SOP 4715 Automated Phenols – Analysis by EPA 9066 846 9034 SOP 4725 Automated Sulfide Analysis by EPA 376.2 and

EPA 9034 EPA 410.4 SOP 4260 Chemical Oxygen Demand by EPA 410.4 SW846 9023 TOX, EOX in Soils and Waters by SW846 9023 and 9020-

DRAFT





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APPENDIX 3 (cont’d) AIHA TEST METHODS

Laboratory Test Method STAT SOP NIOSH 7300 SOP 4515 Elements by ICP-MS by NIOSH 7300 -DRAFT NIOSH 6009 SOP 4535 Mercury in Air Monitoring Cartridges by -

NIOSH 6009 NIOSH 7082 SOP 4550 Lead Analysis of Lead by Atomic Absorption

Direct Aspiration (NIOSH 7082, EPA IO-3.2, and EPA 7420)

OSHA 07, NIOSH SOP 4700 Organic Vapors in Air Monitoring Cartridges by

Gas Chromatography (5515, 1400, 1501, 1500, 2000, NIOSH 7400 SOP 5100 Asbestos and Other Fibers by PCM NIOSH 5515 SOP 4701 Polynuclear Aromatic Hydrocarbon in Air

Monitoring Cartridges by GC/MS with Selective Ion Monitoring

NIOSH 5503 SOP 4702. Polychlorinated biphenyls in Air Monitoring

Cartridges by Gas Chromatography. OSHA 0500, 0600 SOP 4040 Sampling And Analysis of Ambient Air for

Total Suspended Particulate Matter (SPM) And PM10 Using High Volume (HV) Sampler

SOP 6110 SOP 6110 Analysis of Non-Viable Microbiological Air

Samples SOP 6120 SOP 6120 Analysis of Viable Microbiological Air Samples SOP 6210 SOP 6210 Analysis of Non-Viable Microbiological

Samples by Direct Examination SOP 6220 SOP 6220 Analysis of Viable Microbiological Swab and

Bulk Samples SOP 6310 Preparation of Media and Sterile Water





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APPENDIX 3 (cont.’d) AMBIENT AIR TEST METHODS (ORDEQ/NELAC)

Laboratory Test Method STAT SOP EPA IO-3.1 SOP 3115 Extraction of High Volume Filters SW846 3510, 3550B, 3580A SOP 3500 Extractions of Samples for Semi-Volatile


EPA TO-14A/15 SOP 4010 Volatile Organic Compounds in Ambient Air by

2-Stage Thermal Desorption/Gas Chromatography/Mass Spectrometry (GC/MS) (EPA Method TO-14A/TO-15)

EPA TO-14A/15 SOP 4011 Flow Calibration of Passive Air Sampling

Equipment EPA TO-13A SOP 4030 Determination of Polycyclic Aromatic

Hydrocarbons in Ambient Air Using Gas Chromatography/ Mass Spectrometry by EPA TO-13A

EPA IO-3.1 SOP 4040 Sampling And Analysis of Ambient Air for

Total Suspended Particulate Matter (SPM) And PM10 Using High Volume (HV) Sampler

EPA IO-3.5 SOP 4510 Metals Analysis by Inductively Coupled

Plasma- Mass Spectrometry (EPA Method 6020 AND EPA Method IO-3.5)

IO-3.2, EPA 7420 SOP 4550 Analysis of Lead by Atomic Absorption Direct

Aspiration (NIOSH 7082, EPA IO-3.2, and EPA 7420)





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APPENDIX 3 (cont.’d) NIST/NVLAP METHODS

5200 SOP 5200 Polarized Light Microscopy (PLM) Analysis 5330 SOP 5300 Transmission Electron Microscopy (TEM) Sample

Analysis

OTHER TEST METHODS ASTM E1664 SOP 2000 Total Recoverable Oil & Grease by ASTM E1664

and EPA 9071B - DRAFT SW846 9071B SOP 2000 Total Recoverable Oil & Grease by ASTM

E1664 and EPA 9071B - DRAFT ATSM D4979 SOP 2040 Color, Order, Physical Description by ASTM

D4979 - DRAFT ASTM 5058-90 SOP 2080 Compatibility of Screening Analysis - DRAFT ASTM 3987-85 SOP 2125 Leaching Procedures (ASTM D3987-85

Leaching Procedure) EPA350.1 SOP 3250 Ammonia Distillation by EPA 350.1 - DRAFT ASTM D93-80 SOP 4105 Ignitibility by EPA 1010 Pensky-Martens

Closed Cup and ASTM D93-80 Open Cup – DRAFT SW846 9050A SOP 4200 Conductivity (Specific Conductance) EPA 150.1 SOP 4210 pH of Aqueous, Soil and Waste Samples (EPA

Method 9040B, 9045C, 150.1) SM 4500 SOP 4250 Ammonia as N in Soil and Water by SM 4500 EPA 410.4 SOP 4260 Chemical Oxygen Demand by EPA 410.4 SM 5210B Biological Oxygen Demand (BOD) and Carbonaceous BOD

(CBOD)





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APPENDIX 3 (cont.’d) OTHER TEST METHODS

Laboratory Test Method STAT SOP SM 45001 SOP 4420 Nitrates and Nitrites in Soils and Water by SM

4500 FR, I EPA 353.2 SOP 4420 Nitrates and Nitrites in Soils and Water by EPA

EPA 353.2 SM 2320B Alkalinity Analysis EPA 365.2 SOP 4450 Ortho-phosphate in Soils and Waters by EPA

365.2 - DRAFT EPA 160.4 SOP 4480 % Ash, FOC, % Solids and % Moisture by EPA

160.4, ASTM D2974, ASTM D2216, and ASTM 3550B ASTM D2974 SOP 4480 % Ash, FOC, % Solids and % Moisture by EPA

160.4, ASTM D2974, ASTM D2216, and ASTM 3550B ASTM D2216 SOP 4480 % Ash, FOC, % Solids and % Moisture by EPA

160.4, ASTM D2974, ASTM D2216, and ASTM 3550B – ASTM 3550B SOP 4480 % Ash, FOC, % Solids and % Moisture by EPA

160.4, ASTM D2974, ASTM D2216, and ASTM 3550B EPA 160.1 SOP 4482 Total Dissolved, Total Settleable Solids, and

Total Solids by EPA 160.1 EPA 160.2, and SM 2540 B-G EPA 160.2 SOP 4482 Total Dissolved, Total Settleable Solids, and

Total Solids by EPA 160.1 EPA 160.2, and SM 2540 B-G. SM 2540 B-G SOP 4482 Total Dissolved, Total Settleable Solids, and

Total Solids by EPA 160.1 EPA 160.2, and SM 2540 B-G. EPA 376.2 SOP 4725 Automated Sulfide Analysis by EPA 376.2 and

EPA 9034





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APPENDIX 4: INSTRUMENTATION Equipment Manufacturer Model # Serial # Dept.

5890 Series II GC 2950A27820

5971U MSD 3050A01584

GC/MS (SVOC-1) Hewlett Packard

6890 AS 3409A34948-3

SVOC

6890N GC US00033560

5973N MSD US9014004

GC/MS (SVOC-2) Agilent

7683N AS US95310985

SVOC

6890N GC US00037515

5973N MSD US03340461


7683N AS US01012145

SVOC

6890N GC US00042823

5973N MSD US10440761


7683N AS US11618674

SVOC

6890N GC CN52734690

5975N MSD US52430277


7683N AS CN5272615

SVOC

GC/MS (SVOC-6) Agilent 7890GC; 5975C MSD; 7683B AS

CN10705003/US83130313/CN83250642

SVOC

5890 Series II GC 3140A39325 GC/FID Hewlett Packard

6890 AS 3113G06781-3

SVOC

GC/FID2 Agilent 7890A GC; 7683B AS CN10724063/CN83250636

SVOC

GC/ECD PCB1 Agilent 6890N GC

7683N AS US00034720 US00411387

Pest/PCB

GC/ECD PCB2

Agilent 6890N GC 7683N AS

CN10445022 CN44731379

Pest/PCB

GC/ECD PCB3

Agilent 6890N GC 7683 AS

CN10606009 CN62239870

Pest/PCB

6890 GC US00023185 GC/MS (VOC-1) Hewlett Packard

5973 MSD US82311186

VOC

5890 Series Plus GC 2939A08878 GC/MS (VOC-2) Hewlett Packard

5971 MSD 3050A01916

VOC

6890N GC US00033670 GC/MS (VOC-3) Agilent

5973N MSD US03340480

VOC

6890N GC US00042820 GC/MS (VOC-4) Agilent

5973N MSD US10440768

VOC

GC/MS (VOC-5) Agilent 6890 GC CN10516053 Air Toxics





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Agilent 5973 MS US44621448

Tekmar 14-ACAN-000 AS US05130007

6890 GC CN 10716027 5975C MS US 71235770

GC/MS (VOC-6) Agilent

Autocan 12 US 07100004

Air Toxics

Agilent 6890 US00001664 Tekmar 14-3100-OEL 241003

VOA-7 (GC FID/PID)

Varian Archon 13383

Air Toxics

GCFID HP 5890 3033A31565 Air Toxics 600 Controller SX5MM0449M

Pump MX5KM3223M HPLC 1 Waters

717 Autosampler MX5EM4621M

SVOC

G1311A Pump DE14917955

G1313A Autosampler DE14918512

G1322A Degasser DE14918512

G1316A Column Heater DE14926164

G1314A VWD JP11616431

HPLC 2

Agilent 1100

G1321A Fluorescence Det. DE14904016

SVOC

Hot Plate VWR Dynatherm 33918 ASB

Purified HEPA Filter Enclosure

Labconoco 3730000 02022032A-31 ASB

Sonicator Branson 2510 RLA1203942170 ASB

Balance-2 Mettler Toledo B303 1114032438 Micro

Analytical Balance-6

Mettler AE160 B81560 LEAD

Autosampler Perkin-Elmer AS90 507910 (8621) LEAD

Block Digestors CPI 05 C0530 293 LEAD

FLAA Perkin-Elmer PE Analyst 300 041S9110115 LEAD

Pyromultimagnestir

Labline 1268 058950057 LEAD


Mettler AB104-S 1128422933 METALS

Autosampler on ICP-MS1

CETAC ASX510 090007A5X5 METALS

Autosampler on ICP-MS2

Cetac ASX510 020230ASX METALS

Block Digestors CPI Int. - A METALS

Block Digestors CPI Int. - B METALS

Chiller on ICP-MS1

Neslab M75 102025049 METALS

Chiller on ICP-MS2

Neslab CFT-100 100175035 METALS

Kwikool AC Kwikool SWAC 2411 4480 METALS





STAT


High Vacuum Pump

Edwards E2M5 17915F METALS

ICP-MS-1 Agilent 7500i JP93200201 METALS

ICP-MS-2 Agilent 7500i JP13200437 METALS

Mercury Analyzer

CETAC M-6000A 060003MAS METALS

Water Bath VWR 1204 23005 METALS

Class Safety Enclosure

Labconoco 3730001 020220239A MICRO

Colony Counter Leica 3327 0002411463YPO003 MICRO

Conductivity Meter

VWR 61161-362 230355432 MICRO

Crystal Panel Viewer

Becken-Dickison BD-BBL 050604-1499 MICRO

Fluorescence Analysis Chamber

Spectriline CM-10 147858 MICRO

Fluorescence Analysis Chamber

UVP CC-10 95-00724 MICRO

Fume Enclosure Mystaire 100 MICRO

Fume Enclosure Mystaire FE100 MICRO

Furnace Thermolyne 48000 480911020760 MICRO

Hot plate VWR Dynatherm 0687 MICRO

Hot plate VWR Dynatherm 0686 MICRO

Hot Plate/ Stirrer VWR 371 2258 MICRO

Incubator (I-1) VWR 1510E 120060-2 MICRO

Incubator (I-2) VWR 1516E 04070804 MICRO

Microscope Olympus CX31 RBSFA 2M03757 MICRO

Microscope Olympus CH2 7L0064 MICRO

Microscope Olympus BH-2 223905 MICRO



Mini Vortex VWR 945300 14263 MICRO

pH /Temp. Meter 340

Beckman 511210 4585 MICRO

Sealer Index Quanti-Tray 89-10894-02 3510R MICRO

Smart Cycler II Cephid 900-0057 200306 MICRO

Refrigerator #10 Jordan AB-4-6 PR52858-99H RECEIVE

Refrigerator #6 Jordan AB-4-6 PR52857-99H RECEIVE

Refrigerator #7 NORPOLE NPGR2 RECEIVE





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Refrigerator #8 Jordan AB-4-6 PR5381-00A VOC

Autosampler Varian 8200 8200-09311 STORAGE

Autosampler Varian SPS-5 95061148 STORAGE

Autosampler (VOC1)

Varian Archon 13037 STORAGE

FLAA Varian SpectrAA 200 31-100838-00 STORAGE

Hot plate Thermolyne Cimarec-3 66196070461 STORAGE

HPLC Pump Hewlett Packard 1050 STORAGE

Power Pack Varian SIPS/PP1 94111272 STORAGE

Purge & Trap (VOC2)

HP 1909 3432A10143 STORAGE

Sample introduction

Varian SIPS 1 95021096 STORAGE

Sonicator Branson 450 BI0009670 STORAGE

Spect 20 Baush & Lomb 33.31.72 1152868 STORAGE

TCLP tumblers Millipore Agitator 10 455VS4045 STORAGE

TCLP tumblers Millipore Agitator 10 455VS4049 STORAGE

Water Bath Precision Scientific 180 26AX-6 STORAGE

Desktop Centrifuge

Becton-Dickinson Compact II 31000253 SVOC

Fume enclosure Labconco 69000 020697466M SVOC

Fume enclosure Labconco 69000 020697440M SVOC

GC/ECD Varian 3600 3600-02846 SVOC

Heaters Glas Col TM106 158714a to 29A SVOC

Mini Vortex VWR 1945300 23007 SVOC

N2 Solvent Concentrator

Labconco 79100-00 991292324C SVOC


Labconco 79100-00 000593233D SVOC


Labconco 79100-00 000893763E SVOC


Labconco 79100-00 000893764E SVOC

Refrigerator #78 GE TAX4DNCAWH 32373 SVOC

Refrigerator 13 Kenmore 253.6072101 WA2001629 SVOC

Sonicator Branson 450 BI120061 SVOC



Top Loading Balance-4

Mettler Toledo PM300/49 F64687 SVOC





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APPENDIX 4: INSTRUMENTATION Equipment Manufacturer Model # Serial # Dept. Autosampler

(VOC2) Varian Archon 13037 VOC

Autosampler (VOC3)

Varian Archon 13176 VOC

Autosampler (VOC4)


Autosampler (VOC1)


Flow Meter Agilent ADM 1000 US06L31632 VOC

Freezer #0 GE FUM5SAARWH H2115897 VOC

Freezer #12 Kenmore 253.234.24101 WB32231534 VOC

Freezer #9 GE FUM5SAARWH V21100784 VOC

Fume enclosure Labconco 6900000 020697464M VOC

Purge & Trap (VOC1)

Tekmar 3100 US 01107021 VOC

Purge & Trap (VOC3)

Tekmar 3000 98019001 VOC

Purge & Trap (VOC4)

Tekmar 14-8900-00T US04356005 VOC

Refrigerator #14 Kenmore 56491601100 30200594 VOC

Sonicator Branson 2510 RLA070151006D VOC

Balance-1 Mettler Toledo PB403-S 1128192065 VOC

Vacuum Pump for VOC 2

Edwards E2M2 68877 VOC

Gas leak detector GPW-MAC 21-070 S20308 Air Tox

Gas leak detector GPW-MAC 21-050 J47706 VOC

Dessicator (D-1) Nalgene 5317-0180 Cat. 24987-056 WET


Mettler-Toledo AB304-S 1125191416 Metals

Box Furnace Lindberg Blue BF51828C-1 009L-516875-OL WET

COD Reactor Hach 4500 0107000022043 WET

Conductivity Meter

VWR 61161-362 230109686 WET

Digital Hygrometer/Ther

mometer

Control Company 35519-049 240130982 WET

Digital Hygrometer/Ther

mometer

Control Company 35519-049 240160719 WET

Environ Chamber Environmental Chamber Company

Tenney TH Jr 11863-528 WET

Flash Point Precision 74537 S03198 WET

Hot Plate/ Stirrer VWR 325 0868 WET

Hot Plate/ Stirrer VWR 325 0869 WET





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Magnetic stirrer VWR VWR 200 58940-158 WET

Mini-Cyanide Distillation

System

RGW Instruments R-3166MS-100 2 WET

pH/mV/Temp Meter Series 20

Cole Palmer 570002-30 EP20/18094 WET

Phi240 pH/Temp Meter

Beckman Phi-340 3532 WET

QuickChem FIA Lachat 8000 A83000-1663 WET Spect 20 Baush & Lomb 33.31.72 0115280 WET

Stirrer VWR 205 7251 WET

Stirrer VWR 941006 6090 WET Stirrer VWR 941006 6096 WET Stirrer VWR 941006 6097 WET

Stirrer VWR 941006 6085 WET Stirrer VWR 941006 6093 WET Stirrer VWR 941006 6094 WET

TCLP tumblers Analytical Technologies 42RBFC1-E3 0685CPF0018 WET TCLP tumblers Millipore Agitator 10 455RY4029 WET

TOC/TOX Euroglass TOC 1200 2000.137 WET

Balance-12 Mettler PB1502-S 1126341459 WET Top Loading

Balance-7 Mettler BD202 4846 WET Top Loading

Balance-8 Mettler PB602 1113242526 WET

Balance-11 Mettler-Toledo 1129140668 SVOC

Balance-13 Mettler PB403 1129262406 Air Tox

Ba;ance 14 Mettle-Toledo AG-204 1118121901 WET

Transite Oven Blue M 11TA S3585 WET XYZ

Autosampler Lachat ASX 500 020122 ASX WET

Refri/Freezer 17 Kenmore WET

Refrigerator 16 ABSOCOLD SVOC

Refrigerator 18 Kenmore SVOC

Refri/Freezer 19 Kenmore SVOC

Refri/Freezer 20 Kenmore SVOC

Refri/Freezer 21 Kenmore Hallway

Refrigerator 22 Kenmore Micro

Refri/Freezer 23 Kenmore Air Tox Refri/Freezer

R12 Kenmore Micro QA 001 Quality Assurance Manual




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BOD Incubator VWR Micro

Incubator-3 Micro

Walk-in room

Manufacturer Equipment Model # Serial # Lab Olympus

Microscope CX31 2M03757 Micro Olympus

Microscope CX21 4J00403 Micro Bransonic

Ultrasonic Bath 2210R-MT RLA94060-072C ABS JEOL Electron Microscope JEM-100CX II EM156150-260

ABS JEOL Vacuum Evaporator JEE-4X EM300059-376

ABS Ladd Carbon rod Sharpener 30285 89-01-014

ABS

Olympus Microscope CH-2 9H0036

ABS Olympus PLM scope BH-2 H62105-00214

ABS Olympus PLM scope BH-2 HS2805-2000

ABS

Olympus Stereoscope 399597

ABS

Olympus Stereoscope SZX2 344125

ABS SPI Plasma Asher 11005 1586

ABS Thermolyne Muffle Furnace 48000 480911020760

ABS Olympus PCM Microscope CH-2 H92607-0318

ABS Oxford PCM filter fixer QuickFix 10931

ABS VWR

Hot plate / Stirrer 371 2258 ABS

VWR Hotplate Dylatherm 33918432 (cat.#) ABS

VWR Hotplate Dylatherm 33918432 (cat.#) ABS

VWR Mini Vortex 945300 14203 ABS

VWR Water Bath 1203 1103897 ABS





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VWR Incubator 1 NA 1200602 Micro



Edwards High Vacuum Pump E2M5 17915F

ABS

Thermolyne Furnace 48000 480911020760 ABS

VWR BOD Incubator Model 2020 08006510 Metals

CEM MARS Microwave Oven R907501 MD1078 Metals

SPEX CertiPrep Freezer/Mills 6850-115 02021 Metals

SPEX CertiPrep AUTOEXTRACTOR 6814 10020 Metals

HAAKE SHAKER WATERBATH SWB20 920057 Metals

YSI Dissolved Oxygen meter 10D 100381 Metals

Cimarec hotplate HP131535 1757090481029 Metals

VWR hotplate VWR 97042-654 110510001 Metals





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APPENDIX 5 Sample Bottles and Preservation

WATER

METALS

Parameter Container Preservative Holding Time General, dissolved Plastic Filtered on site, 6 months (500 mL) HNO3 to pH<2

General, total Plastic HNO3 to pH<2 6 months

Chromium, hexavalent Plastic Cool 4°C 24 hours

Mercury Plastic HNO3 to pH<2 28 days

CONVENTIONAL PARAMETERS

Parameter Container Preservative Holding Time

Acidity Plastic Cool 4°C 14 days

Alkalinity Plastic Cool 4°C 14 days

Ammonia Plastic H2SO4 to pH<2, Cool 4°C 28 days

BOD Plastic Cool 4°C 48 hours

Bromide Plastic None 28 days

Chloride Plastic None 28 days

Chlorine Plastic Cool 4°C Analyze Immediately

Chromium Plastic Cool 4°C 24 hours





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COD Plastic H2SO4 to pH<2, Cool 4°C 28 days

APPENDIX 5 (cont’d) Sample Bottles and Preservation



Color Plastic Cool 4°C 48 hours

Conductivity Plastic Cool 4°C 28 days

Cyanide, Total or Amenable Plastic NaOH to pH>12, Cool 4°C 14 days

Cyanide, Reactive Plastic NaOH to pH>12, Cool 4°C 14 days

Fluoride Plastic None 28 days

Hardness, Total Plastic HN03 to pH<2 6 months Nitrate/Nitrite Plastic H2S04 to pH<2, Cool 4°C 28 days Nitrate Plastic Cool, 4°C 48 hours Nitrite Plastic Cool, 4°C 48 hours Oil & Grease Glass H2SO4 to pH<2, Cool 4°C 28 days

pH Plastic None Analyze Immediately

Phenols Glass H2S04 to pH<2, Cool 4°C 28 days

Phosphorus, Ortho Plastic Cool 4°C 48 hours

Phosphorus, Total Plastic H2S04 to pH<2, Cool 4°C 28 days

Silica Plastic Cool 4°C 28 days

Solids, Dissolved Plastic Cool 4°C 7 days

Solids, Suspended Plastic Cool 4°C 7 days

Solids, Total Plastic Cool 4°C 7 days

Solids, Settleable Plastic Cool 4°C 48 hours





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Solids, Volatile Plastic Cool 4°C 7 days

Sulfate Plastic Cool 4°C 28 days

Sulfide Plastic NaOH to pH>9, 7 days

Cool 4°C

Sulfide, Reactive Plastic NaOH to pH>9, 7 days Cool 4°C Sulfite Plastic None Analyze Immediately Surfactants, MBAS Plastic Cool 4°C 48 hours Turbidity Plastic Cool 4°C 48 hours Total Organic Carbon (TOC) Plastic H2S04 to pH<2, Cool 4°C 28 days Total Organic Halogens Glass H2S04 to pH<2, Cool 4°C 28 days (TOX)

ORGANICS

Parameter Container Preservative Holding Time HPLC Pesticides Glass vial 1.2 mL Chloroacetic acid 28 Days (Aldicarb / Carbonfuran) Cool 4°C EDB/DBCP Glass vial Cool 4°C 28 Days Endothall Glass Cool 4°C 7 days extraction 1-day analysis Pesticides and PCBs Glass Cool 4°C 7 days extraction 40 days analysis Petroleum Hydrocarbons Glass H2S04 to pH<2, Cool 4°C 28 days





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ORGANICS

Parameter Container Preservative Holding Time Phenoxyacid Herbicides Glass Cool 4°C 7 days extraction 40 days analysis Phthalate Esters Glass Cool 4°C 7 days extraction 40 days analysis Polynuclear Aromatic Glass Cool 4°C 7 days extraction Hydrocarbons 40 days analysis GC/MS Semivolatiles Glass Cool 4°C 7 days extraction 40 days analysis Total Petroleum Glass Cool 4°C 7 days extraction Hydrocarbons 40 days analysis Volatile Organics 40 ml Glass HCl to pH<2 14 days

SOIL

ALL PARAMETERS


All except VOA 2, 4, 8 or Cool 4°C See individual SOP 32 oz Glass Volatile Organics ENCORE* Cool 4°C 48 Hours Volatile Organics NaHSO4/ Cool 4°C 14 Days Methanol *Or equivalent





STAT

Appendix 6: STAT Analysis Sample Acceptance Policy Chain of Custody Requirements: All samples must be submitted with a completed Chain-of-Custody

(COC) form filled out in ink. Please print legibly. The following information should be included:

1) Client Information: Company name and contact information. 2) Client Project Name or Number. 3) Sampler’s name. 4) Sample identification or location. 5) Date and Time of collection. 6) Matrix type. 7) Preservation type: Including chemical preservation as well as thermal preservation.

Environmental samples require thermal preservation and the temperature requirement for shipment/storage is 0.1-6ºC.

8) Total number of containers. 9) Requested analyses or reference to quote or other documentation specifying analysis. 10) Turn Around Time. 11) Special remarks: Includes any additional sample analysis requirements such as reporting limits, if

the samples are considered hazardous or contaminated, etc. 12) Signatures including date/time of all persons who have handled or possessed the samples. 13) If applicable, Purchase Order number, quote or other billing information.

Sampling/Container Requirements:

1) All samples must be labeled properly with unique identification in indelible ink, on water-resistant labels and correspond with the information on the COC. Date and time of sampling and preservation type should also be present on the label. Deviations between the sample number on the COC and sample containers will be noted on the sample receipt checklist.

2) All samples must be received in appropriate containers required by the analytical test methods and be received in good condition without any signs of damage or contamination. If the sampler suspects the outside of the container has been contaminated, it is imperative to notify the laboratory so that appropriate action can be taken to prevent cross contamination of samples.

3) Containers must have sufficient sample volume for analysis, with proper preservation. If QC is required (MS/MSD), additional sample must be submitted. Chemical preservation (pH) is checked at log in or by the analyst. Insufficient volume and improper preservation will be noted on the sample receipt checklist. Please see attachment for container and volume requirements.

4) All samples should be received within the analytical test method specified holding times. Hold time violations will be noted in the analytical report. For analysis with short hold time, please submit the sample with adequate time for analysis and notify your project manager when the sample will be arriving.

If a sample must be analyzed on a rush basis in order to meet hold time, additional rush surcharges may be applied.

NOTE: Sample containers provided by STAT Analysis may contain small amounts of chemical preservatives as required by the analytical test method and labeled as such. Please take necessary precautions when using these sample bottles. Be sure to cap bottles tightly before shipment. When shipping samples to STAT Analysis:





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1) Enclose completed COC form in sealed zip-lock bag in order to prevent water damage from melting ice.

2) Ensure that the sample cooler is sealed properly with tape to avoid opening while in transit. 3) Ensure that there is enough ice or cooling material (ice is preferred over ‘Blue Ice’) in order to

maintain required temperature preservation (0.1-6ºC). Samples received out of temperature compliance will be noted on the COC or sample receipt checklist.

4) Ensure that there is enough packing material in cooler to prevent damage to sample containers while in transit. Fill empty space in the cooler with bubble wrap or other packing material.

5) Be sure that samples containers are properly sealed so that water from melting ice does not enter the sample container. Shipping sample containers in sealed zip-lock bags can help prevent this.

6) Use extra packing material when shipping water samples. It is best to individually wrap glass water containers with bubble wrap or packing paper and then place in zip-lock bags.

NOTE: Samples that do not meet the above criteria will be flagged in an unambiguous manner defining the nature and substance of the variation. This will be noted on the final report.





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Appendix 7 Ethics Policy and Data Integrity Agreement

Ethics Policy and Data Integrity Agreement

It is STAT Analysis Corporation’s responsibility to produce data that is scientifically valid, defensible, and of known and documented quality in accordance with all applicable federal, State, and local laws and regulations consistent with accepted professional and analytical practices in a manner that justifies the public trust. STAT Analysis Corporation conducts all business with integrity and in an ethical manner. It is the responsibility of each staff member, manager, director, and owner to perform their duties with the highest ethical standards and professional conduct to ensure compliance with this Quality Manual and related documentation. The STAT Analysis Corporation laboratory has a Quality Assurance Manual designed to insure that work performed in the laboratory is accurate, precise, complete, comprehensive, reproducible and reflects the need of the customer/client while satisfying the requirements of appropriate State and Federal regulations. STAT Analysis Corporation will not offer any analysis for which we cannot demonstrate consistent quality and defensible analyses. Any allegation of misconduct will be promptly investigated in an unbiased and confidential manner by an investigative team designated by the President/CEO. The investigation including any supporting documentation, actions and resolution will be recorded and archived by the QA Manager. I. I understand the high standards of integrity required of me with regard to the duties I perform and

the data I report in connection with my employment at STAT Analysis Corporation. II. I state that I am free from any commercial, financial or other pressures and do not have any

conflicts of interests, which might adversely affect my duties at STAT Analysis Corporation. Laboratory analysts will not have any direct customer contact except with the approval of laboratory management, this includes but is not limited to telephone calls, emails, facsimiles, audits, etc.

III. I agree that in the performance of my duties at STAT Analysis Corporation:

a. I agree to read, understand, sign and comply with all the policies and procedures detailed in the latest revisions of the Quality Assurance Plan and SOPs at all times;

b. I will not intentionally report data that are not the actual values obtained without collaborating data acceptable to the laboratory’s Standard Operating Procedures. All modifications will be properly documented;

c. I will not invent data (dry lab) this includes raw data, support equipment calibrations; quantitative reports, LIMS etc.

d. I will not adjust the area of a peak in chromatography to bypass QC criteria (peak shaving or adding);

e. I shall not intentionally report the dates and times of data analyses that are not the actual dates and times of data analyses (time traveling);

f. I shall not intentionally represent another individual’s work as my own; g. I understand that if my job includes supervisory responsibilities, I shall not instruct, request,

or direct any subordinate to perform any laboratory practice, which is unethical or improper.





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IV. I will not compare or disclose results for any Performance Testing (PT) sample, or other similar QA or QC requirements, with any employee of any other laboratory, prior to the required submission date of the results to the person, organization, or entity supplying the PT sample.

V. I will not divulge customer names or their results outside of the company except to those parties

designated as an approved customer representative. VI. I agree to inform STAT Analysis Corporation of any accidental or intentional reporting of non-

authentic data by other employees or by myself in a timely manner. I understand that if any manager or representative of management instructs, requests, or directs me to perform any of the aforementioned improper laboratory practices (I – V), or if I am in doubt or uncertain as to whether or not such laboratory practices are proper, I will not comply, but I must immediately report such event to all appropriate members of management including my manager, the Laboratory Director, the QA Manager and President/CEO, excluding such individuals who participated in such perceived improper instruction, request, or directive.

I understand that failure to follow company policies and procedures, and failure to follow federal, State and local law, may result in discipline, up to and including termination. If I have knowledge of a non-compliant incident and do not report it, I will be subject to disciplinary measures up to and including termination. If I retaliate or in any way punished another employee for reporting a violation, I will be subject to discipline, up to and including termination.

____________________________________________________________________________ (Employee’s Signature) (Dated) ____________________________________________________________________________ (Print Name) ____________________________________________________________________________ (Witness Signature) (Dated) ____________________________________________________________________________ (Print Name) NOTE: This Ethics Policy/Data Integrity Agreement must be signed at the time of hire and re-signed between January 1 and January 15 of every year. Such signature is a condition of continued employment and failure to sign will result in immediate termination of employment.





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ATTACHMENT 1 Facility Diagram





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ATTACHMENT 2

Example Chain of Custody for NELAC Samples





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ATTACHMENT 3 Example Chain of Custody for Pb AIHA Samples





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ATTACHMENT 4 Example Chain of Custody for Asbestos Samples





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ATTACHMENT 5

Microbiology Chain of Custody





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Attachment 6 Example of Notice of Confidentiality for E-mail








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Attachment 7 Example of Notice of Confidentiality for Facsimiles

Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 1 of 14

First Environmental Laboratories

Standard Operating Procedure

Title: Total Kjeldahl Nitrogen (TKN) – Block Digestion with Semi-Automated Skalar Regulatory References: EPA 600/4-79-020, Method 351.2 R.2.0. (1993) Matrices: aqueous (wastewater and ground water), non-aqueous liquid, solids(soil/sediment), chemical wastes Regulatory Limits: NA Sample Collection, Preservation, Shipment, and Storage Sample Collection: All samples shall be collected using an appropriate sampling plan and properly preserved containers. The volume collected should be sufficient to insure a representative sample, allow for replicate analysis (if required), and minimize waste disposal. All samples should be held at 4oC until time of analysis. Preservation: pH <2 using H2SO4, all samples should be held at 4oC until time of analysis. Shipment: Samples should be shipped in a manner permitting continuation of storage at 4oC. Storage: Samples are stored prior to analysis at 4oC. Container: 250 cc plastic for aqueous samples or 4oz jar for solid samples Single Analysis Sample Volume: 25 mL or 2g Holding Time: 28 days (Range) Reporting Limit - Upper End: 1.0 mg/L – 10.0 mg/L Note: The range can be extended by diluting the sample Summary of Method: Samples are digested in a block digestor with sulfuric acid and copper sulfate as a catalyst. The digestion recovers nitrogen components of biological origin, such as amino acids, proteins, and peptides, as ammonia, but may not recover the nitrogenous compounds of some industrial wastes. Nitrate is not recovered. The digested sample is injected onto the automated flow injection analyzer where its pH is controlled by raising it to a known, basic pH by neutralization with a concentrated buffer. This in-line neutralization converts the ammonium cation to ammonia, and also prevents undue influence of the sulfuric acid matrix on the pH-sensitive color reaction. The color reaction of the automated procedure for the determination of Total Nitrogen is based on the modified Berthelot reaction; ammonia is chlorinated to monochloramine which reacts with salicylate to 5-aminosalicylate. After oxidation and oxidative coupling a green colored complex is formed. The reaction is catalyzed by nitroprusside, sodium hypochlorite is used for chlorine donation. The absorption of the formed complex is measured at 660 nm.

First Environmental Laboratories, Inc.

Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 2 of 14 1. Instrumentation / Apparatus / Glassware 1.1. SA 5640 Block Digester with Controller 1.2. SA 5395 75 mL Digester Tubes 1.3. Hengar Granules for smooth boiling, non-selenized 1.4. SA 4000-01 Sans++ Analyzer 1.5. SA 1074 Random Access Auto Sampler 1.6. The Skalar Sans++ custom method designed for this instrument details cartridge components and consumables. Part numbers for consumables can be found in the catalog titled, “The Skalar Continuous Flow Analyzers Components and Accessories Booklet.” 1.7. SA1033 Disposable sample tubes, 10mL 1.8. Analytical balance capable of accurately weighing 0.0001g 1.9. Top loading balance capable of accurately weighing 0.1g 1.10. Maintenance is performed in accordance with procedures documented in the appropriate maintenance log book / file. 2. Reagents All reagents should be prepared from reagent grade materials using deionized water and volumetric glassware. 2.1. Digestion Solution: Dissolve 134 grams of potassium sulfate and 7.3 grams of cupric sulfate into 500 mL of DI water. Slowly add 134 mL of conc. H2SO4. Let cool and dilute volumetrically to 1 liter. Expiration Date: 1 month NFPA Diamond Safety Information for Sulfuric Acid (H2SO4): Health (blue) 3 / Reactivity (yellow) 2 /Hazard (white) no-water 2.2. Sodium Chloride Solution: Dilute 2 mL of FFD6 into a 1L volumetric flask with DI water. Mix. Expiration Date: 1 week (FFD6 is purchased from Skalar Analytical / Catalog #13908) 2.3. Stock Potassium Sodium Tartrate Solution: Dissolve 200 grams of potassium sodium tartrate (C4H4O6KNa – 4H2O) into 800 mL DI water. Dilute volumetrically to 1 liter. Expiration Date: 1 month 2.4. Stock Buffer Solution: Dissolve 134 grams of di-sodium hydrogen phoshate (Na2HPO4) into 800 mL of DI water. Add 20 grams of sodium hydroxide (NaOH). Dilute volumetrically to 1 liter. Expiration Date: 1 month NFPA Diamond Safety Information for Sodium Hydroxide (NaOH): Health (blue) 3 / Reactivity (yellow) 1 2.5. Sodium Hydroxide (5M): Dissolve 200 grams of sodium hydroxide (NaOH) into 800 mL of DI water. Dilute volumetrically to 1 liter. Expiration Date: 1 year NFPA Diamond Safety Information for Sodium Hydroxide (NaOH): Health (blue) 3 / Reactivity (yellow) 1


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 3 of 14 2.6. Buffer Solution: Mix 250 mL of Stock Potassium Sodium Tartrate Solution and 200 mL of Stock Buffer Solution into 200 mL of DI water. Add 110 mL of Sodium Hydroxide (5M) and mix. Dilute volumetrically to 1 liter. Expiration Date: 1 week NFPA Diamond Safety Information for Sodium Hydroxide (NaOH): Health (blue) 3 / Reactivity (yellow) 1 2.7. Salicylate-Nitroprusside Solution: Disslove 150 grams of sodium salicylate (C7H5NaO3) and 0.3 grams of sodium nitroprusside (Na[Fe(CN)5NO]2H2O) into 800 mL DI water. Dilute volumetrically to 1 liter. Expiration Date: 1 week 2.8. Hypochlorite Solution (5%): Purchased. Expiration Date: per manufacturer’sinstructions. NFPA Diamond Safety Information for Hypochlorite Solutions: Health (blue) 2 2.9. Hypochlorite Solution: Dilute 18.0 mL of sodium hypochlorite solution (5%) into 80 mL of DI water. Dilute volumetrically to 250mL. Expiration Date: 3 days 2.10. Rinsing Liquid: Dilute 400 mL of digestion solution into 600 mL of DI water. Dilute volumetrically to 1 liter. Expiration Date: 1 week NFPA Diamond Safety Information for Sulfuric Acid (H2SO4): Health (blue) 3 / Reactivity (yellow) 2 /Hazard (white) no-water 3. Standards All reference standards, purchased stock, purchased neat solutions, all intermediate solutions, and all working standards used more than one day, must be traceable to their source and method of preparation. Log books are kept documenting the preparation of standards from the “mother” source. Each reference, stock, intermediate and multiple use working standard is assigned a unique number and entered into the appropriate Standards Tracking Log. This unique number will also be applied to the label and the calibration certificate. The calibration certificate documents the traceability to national standards of measurement and is retained for reference. 3.1. 1,000 mg/L Total Nitrogen Stock Standard: Purchased as a prepared reagent. Expiration date: per manufacturer’s labeling. Source: ERA Catalog No. 985 Note: Ammonia Nitrogen is the stock used for Total Kjeldahl Nitrogen 3.2. 2,4,6,8,10 mg/L Total Kjeldahl Nitrogen Stock Standard for Calibration Curve: Add 0.2,0.4,0.6,0.8,1.0 mL of 1000 mg/L Total Kjeldahl Nitrogen stock to 60 mL of DI water + 40 mL of digestion solution. Expiration Date: 1 day 3.3. 1,000 mg/L Total Kjeldahl Nitrogen Second Source Stock Standard: Dissolve 3.819g of anhydrous ammonium chloride (NH4Cl), dried at 1050C for 2 hours, in DI water and dilute to 1 liter volumetrically. Expiration date: one year. 3.4. 5.0 mg/L CCVS: Add 0.500 mL of 1,000 mg/L second source stock to 60 mL of DI water + 40 mL of digestion solution. Expiration date: I month. 3.5. 1.0 mg/L Reporting Limit Verification Standard (RLVS): Add 100 uL of 1000 mg/L second source stock to 60 mL of DI water + 40 mL of digestion solution. Expiration date: I month.


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 4 of 14 3.6. Procedure Blank (PB): Add 25mL of DI water into 75 mL digester tube. Required to be processed with samples through digestion. 3.7. 10.0 mg/L Laboratory Control Sample (LCS): Add 0.250 mL of 1000 mg/L second source stock to 25 mL of DI water into 75 mL digester tube. Required to be processed with samples through digestion. 3.8. To Spike the Sample: Add 100 ul of 1000 mg/L second source stock to 25 ml of sample. The sample is now spiked with 1.0 mg/L of Total Kjeldahl Nitrogen. 3.9. Recommended source for PE samples is ERA or equivalent. 4. Analytical Procedure 4.1. Interferences 4.1.1. High nitrate concentrations (10x or more than the TKN level) result in low TKN values. If interference is suspected, samples should be diluted and reanalyzed. 4.1.2. Method interferences may be caused by contaminants in the reagent water, reagents, glassware, and other sample processing apparatus that bias the analyte response high. 4.2. Digestion Procedure 4.2.1. Wash all digester tubes in hot soapy water and rinse three times with DI water. Even glassware that has been washed the night before can pick up contaminants over night. All glassware must be washed and rinsed immediately prior to usage to avoid such contaminants. 4.2.2. Pipet 25 mL of sample into digester tubes. For soils and sludge use 0.5g to 25 mL of DI water. Add 3-4 boiling chips. 4.2.3. Pipet 10 mL of digestion solution into each digester tube. 4.2.4. Place digester tubes into digestion block and turn power on. 4.2.5. Press the start button on digestion block. Samples will digest for 1 hour at approximately 140oC. Then, the samples will digest for 1 hour at approximately 170oC. At this point, most of the water will be boiled off. Then finally, the samples will digest for 2.5 hours at approximately 380oC. The digestion block control panel will control all the temperature changes at the appropriate set times. 4.2.6. When the samples are finished digesting the unit will beep. Turn the power off and carefully take out the digester tubes and place in a cooling rack. The tubes will be very hot so where oven mitts. Be sure to let the samples cool off under the hood. 4.2.7. Ten minutes after the samples have been cooled, dilute with approximately 15-20 mL of DI water. Vortex mix each tube. This is very critical because the sample will harden on the bottom of the tube if water is added too late.


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 5 of 14 4.2.8. Dilute to a 25 mL volume, using a graduated cylinder. The samples are now ready to be analyzed on the instrument. If the samples are not going to be analyzed immediately, place a rubber stopper on each digester tube and store samples at 4oC. 4.3. Determinative Procedure 4.3.1. Filter all turbid samples through a glass micro fiber filter paper before pouring into sample tubes. 4.3.2. A calibration curve is analyzed each day samples are analyzed. 4.3.3. An aliquot of rinsing solution processed through the analyzer serves as the reagent/calibration blank and monitors the reagents for contamination. Frequency: daily at the beginning of the run, every ten samples throughout the run, and at the end of the run. 4.3.4. An aliquot of 5.0 mg/L CCVS processed through the analyzer monitors the performance of the determinative procedure. Frequency: daily at the beginning of the run, every ten samples throughout the run, and at the end of the run. 4.3.5. A reporting limit standard of 1.0 mg/L processed through the analyzer monitors the performance of the determinative procedure. Frequency: daily at the beginning of the run. 4.3.6. An aliquot of PB processed through the colorimetric analysis monitors the performance of the digestion procedure. Frequency: one per every 20 samples. 4.3.7. An aliquot of 10.0 mg/L LCS processed through the colorimetric analysis monitors the performance of the alkaline digestion procedure. Frequency: one per every 20 samples. 4.3.8. Duplicate spiked aliquots of sample (MS/MSD) monitor the precision and accuracy of the procedure for a specific matrix. Frequency: 1/10 samples or less of the same matrix. See Section 3.8. for instructions on how to spike the sample. 4.3.9. General Description of Procedure See bench reference for start up procedures for more detailed instructions. • After samples are poured up turn on computer, interface, and auto sampler. • Open Flow Access software. • Use remote control icon to open valves, start pumps, and turn on detector lamps. • Open raw data viewer in order to see when baseline stabilizes. • Set up sample table definition. • Check dilution range. • If running overnight, enable time program shut down with correct day of run. • Start analysis.


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 6 of 14 • Check to see the curve is in correct calibration after the calibration curve peaks are shown on the raw data

viewer. 4.3. Calculation The calculation module automatically calculates the concentration of the samples in mg/L. The analyst must calculate any predilution factors. Autodilutions are included in the calculations performed by the instrument. 4.4. Reporting Limits 4.4.1. The routine reporting limit for an aqueous sample is 1.0 mg/L. The routine reporting limit for a solid sample is 25 mg/kg. 4.4.2. Reporting limits are normally 3-10 times the method detection limit. During method validation, regulatory criteria are also compared to the proposed reporting limit to ensure that the reporting limit meets the regulatory criteria. Refer to the SOP titled, “Method Detection Limit” (#109) for details regarding the determination of the method detection limit.


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 7 of 14 5. Quality Control Indicator Assessment 5.1. Each quality control indicator (QCI) must be assessed for compliance with the following criterion on a real time basis. When applicable, the percent recovery and/or the relative percent difference (RPD) is also recorded on the raw data/lab book form.

Quality Control Indicator (QCI)

Frequency Acceptance Criteria (Specification or Statistical

Requirement)

Initial Corrective Action Final Action / Data Qualification

Method Detection Limit Study (MDL)

See MDL SOP #109 for details

See QC Table Notes 1

Initial method validation and each time there is a significant change in the test method that affects how the test is performed. or when a change in instrumentation occurs that affects the sensitivity of the analysis, provided the reporting limit is equal to the low standard in the calibration curve, or a reporting limit verification standard is run daily.

The calculated MDL must be greater than 1/10th the MDL spiking concentration and greater than “0”, and the MDL spiking concentration must be greater than the calculated MDL. Minimum of 7 replicates.

Re-analyze and re-process MDL for analytes that fail to meet acceptance criteria.

Do not report results below the MDL.

Initial Demonstration of Capability (IDC)

See IDC/IDMP SOP #106 for details

Initial method validation and each time there is a significant change in the instrumentation, personnel, matrix or test method that affects the sensitivity of the analysis.

The source and concentration of IDC may vary depending on the purpose of the study. %R = 80-120

Re-analyze and re-process IDC for analytes that fail to meet acceptance criteria.

IDC/IDMP criteria must be met prior to sample analysis.

Calibration Curve See Calibration Curves

Inorganic #102 for details and validation file for historic performance

Daily at the beginning of every new run.

cc = 0.995, back calculation of percent recovery within 10% of true value

Identify problem(s) and re-analyze the calibration curve.

Sample analysis must not begin until criteria are met.

Initial Calibration Verification (2nd source)

Immediately following the curve +10% or within stated limits as supplied by manufacturer (95% confidence limit)

Re-evaluate the calibration curve to verify that all criteria have been met.

Data can only be released for analytes that have passed the ICVS criteria.



Reagent Blank / Continuing Calibration

Blanks

Daily at the beginning, end, and after every 10th samples

Less than the reporting limit. If RB/CCB and samples have concentrations >RL, then the RB/CCB <10% of the sample concentration.

Check for contamination problems and/or instrument drift. Re -run the CCB and evaluate the sample results with respect to the CCB. Reanalyze samples as determined by this evaluation.

The data may be reported with the appropriate data qualifier. Flag samples that have analyte concentrations less than 10 times the concentration found in the applicable blank.

Continuing Calibration Standard (CCVS) -

concentration middle of range

Daily at the beginning, end, and after every 10th samples

Specification: + 10% Statistical Control: 3 standard deviations for the control limit and 2 standard deviations for the warning limit

Re-run the CCVS and evaluate the sample results with respect to the CCVS result. Reanalyze samples as determined by this evaluation.

Data can only be released for analytes that have passed the CCVS criteria.

Reporting Limit Verification Standard - concentration equaling

the reporting limit

Daily at the beginning @ a concentration equaling the reporting limit

Specification: + 25 Re-run the RLVS and evaluate the sample results with respect to the RLVS. Reanalyze samples as determined by this evaluation.

Results for positive samples can be reported. Results of non-detect samples need to be documented in the case narrative prepared by the analyst and included in the project file

Procedure Blank (PB) (or Method Blank) See Table Notes 3

Per batch See Table Note 4

Less than the reporting limit. If PB and samples have concentrations >RL, then the PB must be <10% of the sample concentration.

Check for contamination problems. Evaluate the sample results with respect to the PB. Reanalyze samples as determined by this evaluation.

If samples are not reprocessed, the data may be reported with the appropriate data qualifier. Flag samples that have analyte concentrations less than 10 times the concentration found in the applicable blank.

Laboratory Control Standard (LCS) -

concentration upper end of range

Per batch See Table Note 4

Specification: + 20% Statistical Control: 3 standard deviations for the control limit and 2 standard deviations for the warning limit

Determine cause of problem and re-prepare and re-analyze the affected samples.

Results of analytes failing to meet acceptance criteria need to be documented in the case narrative prepared by the analyst and included in the project file.



Matrix Spike / Matrix Spike Duplicate

(MS/MSD) - concentration 20 to 50

percent of range See Table Note 5

Per batch Selection of sample for MS/MSD is arbitrary See Table Note 4

Specification: +10% Recovery and RPD 20 Statistical Control: 3 standard deviations for the control limit and 2 standard deviation for the warning limit

Evaluate the LCS with respect to the MS/MSD. If the LCS was acceptable, evaluate sample for matrix interferences. Examine the sample for homogeneity. Evaluate the spike concentration vs. native analyte concentration. If the concentration of analyte is >4x the spike concentration, then the spiking level is insignificant to the sample. Evaluate the sample for the presence of interferences by re-analyzing the sample and the MS at a dilution. Acceptable spike recovery indicates the presence of interference.

The information from the MS/MSD is sample/matrix specific and is not normally used to determine the validity of an entire batch. No action is taken on out of control MS/MSD data alone to qualify an entire batch

QC Table Notes:

1. Detection Limit

• Detection limit shall be initially determined for the compounds of interest in each test method in a matrix in which there are not target analytes nor interferences at a concentration that would impact the results or the detection limit must be determined in the matrix of interest.

• Detection limits must be determined each time there is a change in the test method that affects how the test is performed, or when a change in instrumentation occurs that affects the sensitivity of the analysis.

• All sample processing steps of the analytical method shall be included in the determination of the detection limit.

2. If a QCI fails to meet accept criteria, the analyst will prepare a case narrative documenting the failure and the associated decisions regarding reanalysis vs. acceptance of the data. The case narrative will be added to the project file. Project management will review case narratives during the preparation of the final report and make final decisions regarding data flagging requirements.

3. Definition of Method Blank: (per NELAC Glossary 2002 Standard) a sample of a matrix similar to the batch of associated samples (when available) that is free from the analytes of interest and is processed simultaneously with and under the same conditions as samples through all steps of the analytical procedures, and in which no target analytes or interferences are present at concentration that impact the analytical results for sample analyses. Synonymous with procedure blank (PB).

4. Definition of Batch: (per NELAC Glossary 2002 Standard) environmental samples that are prepared and/or analyzed together with the same process and personnel, using the same lot(s) of reagents. A preparation batch is composed of one to 20 environmental samples of the same NELAC-defined matrix, meeting the above mentioned criteria and with a maximum time between the start of processing of the first and last sample in the batch to be 24 hours. An analytical batch is composed of prepared environmental samples (extracts,


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 10 of 14 digestates or concentrates) which are analyzed together as a group. An analytical batch can include prepared samples originating from various environmental matrices and can exceed 20 samples.

5. Definition of Matrix: (per NELAC Glossary 2002 Standard) the substrate of a test sample.

• Aqueous: any aqueous sample excluded from the definition of Drinking Water matrix or Saline/Estuarine source. Includes surface water, groundwater, effluents, and TCLP or other extracts.

• Drinking Water: any aqueous sample that has been designated a potable or potential potable water source.

• Solids: includes soils, sediments, sludges, and other matrices with >15% settleable solids.

• Chemical Waste: a product or by-product of an industrial process that results in a matrix not previously defined.

Analyte Concentration Standard 1

mg/L

Concentration Standard 2

mg/L


mg/L


mg/L


mg/L TKN 2.00mg/L 4.00mg/L 6.00mg/L 8.00mg/L 10.00mg/L


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 11 of 14 5.2. Method Performance 5.2.1. Method performance data can be found in EPA 600/R-93/100, Method 351.2 Section 13.0. Internal performance data will be collected in accordance with SOP #112, “Statistical Control”. 5.2.2. Prior to the use of this method on analytical samples, the method must be validated with an Initial Demonstration of Method Performance (IDMP) (also known as an Initial Demonstration of Capability (IDC)) and a Method Detection Limit Study (MDL). The IDMP and MDL requirements are summarized in section Table 5 of this SOP. The determinative procedure in this SOP must be used for the associated IDMP and MDL. The IDMP and MDL are detailed in SOP #106 and #109 respectively. 5.2.3. Refer to SOP #129, “Summary of Quality Control Indicators – Inorganics & Organics” for additional information regarding QCIs. Note: this is a training document, therefore, if information in this document conflicts with information in the method SOP, the method SOP takes precedence. 6. Notes 6.1. Tips and Hints 6.1.1. See historical data to make dilutions ahead of time. This prevents the calibration from being thrown off due to highly contaminated samples. 6.1.2. The autoanalyzer will re-analyze the sample following a sample that required a dilution. This procedure allows the analyst to check for carry-over. 6.1.3. Sentry File is used for storage of all data. Scan the data on the copier and then upload it into the proper cabinet in Sentry file. 6.1.4. Standard Methods for the Examination of Water and Wastewater, Standard Methods, 21st Edition, Method 4500 Norg–D, Block Digestion and Flow Injection Analysis Standard Methods, 22nd Edition, Method 4500 Norg–D, Block Digestion and Flow Injection Analysis 7. Definitions Where appropriate, definitions have been provided in this SOP. If additional clarification is required, refer Section 20 of the Quality Assurance Manual. 8. Safety The toxicity or carcinogenicity of each reagent used in this method have not been fully established. Each chemical should be regarded as a potential health hazard and exposure to these compounds should be as low as reasonably achievable. Material Safety Data Sheets (MSDS) are available for review. All reagents should be appropriately labeled. Always wear safety glasses for eye protection, protective clothing and observe proper mixing when working with chemicals and potentially hazardous samples. Additional information can be found in the laboratories’ Chemical Hygiene Plan. Copies of specific MSDS can be obtained from various websites on an as needed basis.


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 12 of 14 9. Pollution Prevention Pollution prevention is defined in EPA documents as any technique that reduces or eliminates the quantity or toxicity of waste at the point of generation. First Environmental Laboratories, Inc. uses reduced volume procedures, where feasible, in order to comply with EPA guidance. The laboratory continuously assesses new technology that assists in the reduction or elimination of waste. 10. Waste Management The analysis of samples inevitably produces various wastes. When possible, First Environmental Laboratories, Inc. minimizes all releases from hoods and bench operations. Wastes, which cannot be neutralized or made innocuous, are collected and disposed of in an appropriate manner. Additional information can be found in the laboratories’ Chemical Hygiene Plan, SOP #901, “Sample Disposal,” and SOP #902, “Waste Disposal.” 11. References The analyst is required to have read and understood various supporting documents including regulatory method references, First Environmental’s Quality Assurance Manual, First Environmental’s Chemical Hygiene Plan, and non-method SOPs that support QA activities.

SOP #102, “Calibration Curves – Inorganics.” Note: this is a training document, therefore, if information in this document conflicts with information in the method SOPs, the method SOP takes precedence.

SOP #129, “Summary of Quality Control Indicators – Inorganics and Organics.” Note: this is a training document, therefore, if information in this document conflicts with information in the method SOP, the method SOP takes precedence.

SOP #106, “Initial Demonstration of Capability / Initial Demonstration of Method Performance.”

SOP #109, “Method Detection Limits.”

SOP #112, “Statistical Control.”

SOP #118, “Measurement Traceability & Calibration.”

SOP #123, “Sample Instructions & Materials.”

SOP #901, “Sample Disposal”

SOP #902, “Waste Disposal”

First Environmental’s Quality Assurance Manual

First Environmental’s Chemical Hygiene Plan

“Method of Soil Analysis”, 2nd Edition, American society of Agronomy/Soil Science Society of America.

Skalar Method Bench Reference


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 13 of 14 12. Approvals

Reviewed for Technical Accuracy by: Joy Geraci

Reviewed for Quality Assurance Compliance by: Lorrie Walker Implementation Date: 01/20/14 End Use Date:__________________


Filename: u:\methods\sops\conv\436.3 tkn skalar.doc Date Revised: 01/20/14 Revision No.: 3 Page 14 of 14 Appendix to Automated Methods Ammonia Method 350.1R2.0 Chloride Method 4500 Cl-E Cyanide Method 335.4R1.0 Nitrate Method 353.2R2.0 Phenol Method 5330B,C Sulfate Method 375.2R2.0 TOC Method 5310C TKN Method 351.2R2.0 CAR to IEPA on site audit conducted August 13-15, 2008 Automated Nitrate (Skalar) 353.2 #7. Finding: For the method 353.2 (nitrate) SOP there is no mention of the linear dynamic range (LDR) that is required in the test method. Need to perform and document an initial LDR and verify every six months. Need to retain record of initial LDR and verifications. The assessor suggests performing the initial LCR (i.e., expanded calibration curve over entire linear range) and then every six months compare response of current calibration curve points or highest point to the LCR. If response of standard(s) is within +10% agreement then acceptable. Response: A curve is performed each time a run is initiated; the acceptance criteria for the correlation coefficient must be 0.995 or better. It is verified using a second source standard at the mid-range of the curve; the acceptance criteria is + 10% of the true value. If the low standard in the curve is greater than the reporting limit, a standard at the reporting limit is also analyzed. If samples exceed the high standard, they are diluted to fall within the range of analysis and re-analyzed. The linear range for the analysis was established during initial method validation based upon the method procedures and information provided by Skalar. Their information is based on knowledge of the chemistry and instrument performance AND the desired sensitivity for the procedure. Extending the curve would potentially degrade the reporting limit. All the controls and documentation is in place on a per run basis proving that that analysis of samples is valid. An LDR analysis will NOT be run every 6 months. CAR was accepted via e-mail on 10/06/08. See attached.

Reviewed for Technical Accuracy by: Joy Geraci

Reviewed for Quality Assurance Compliance by: Lorrie Franklin Implementation Date: 10/07/08 End Use Date: _____________________



SOP 4250 Ammonia Analysis Revision 00

Effective Date: November 26, 2008 Page 2 of 28

STAT

Table of Contents Title Page ...................................................................................................................................1 Table of Contents.......................................................................................................................2 1. Identification of Test Methods .......................................................................................3 2. Applicable Matrix or Matrices .......................................................................................3 3. Detection Limits.............................................................................................................3 4. Scope and Application...................................................................................................3 5. Summary of Test Method ..............................................................................................3 6. Definitions ......................................................................................................................4 7. Interferences...................................................................................................................4 8. Safety .............................................................................................................................4 9. Equipment and Supplies ................................................................................................5 10. Reagents and Standards .................................................................................................5 11. Sample Collection, Preservation, Shipment and Storage ...............................................7 12. Quality Control ..............................................................................................................7 13. Calibration and Standardization.....................................................................................8 14. Procedure .....................................................................................................................11 15. Data Reduction, Calculations and Loading .................................................................13 16. Method Performance....................................................................................................14 17. Pollution Prevention.....................................................................................................15 18. Data Assessment and Criteria for Quality Control Measures ......................................15 19. Corrective Actions for Out-Of-Control Data ...............................................................16 20. Contingencies for Handling Out-Of-Control Or Unacceptable Data ..........................17 21. Waste Management......................................................................................................17 22. References ....................................................................................................................17 23. Forms, Figures, Tables, Diagrams, Flowcharts, Attachments or Validation Data ......18 APPENDIX A TROUBLESHOOTING .....................................................................19 APPENDIX B CREATING A METHOD..................................................................20 APPENDIX C DQM PLAN .......................................................................................23 APPENDIX D MANIFOLD DIAGRAM...................................................................25 APPENDIX E MANIFOLD INSTALLATION/REMOVAL....................................26 APPENDIX F MAINTENANCE SCHEDULE .........................................................28




STAT

1.0 Identification of Test Method

SOP Title: Ammonia Analysis is also known as Ammonia in the laboratory records.

2.0 Applicable Matrix or Matrices

This method is used to determine the concentration of Ammonium ion in aqueous samples, wastes, and leachates. This method is used to quantify the concentration of ammonia from the distillation procedure detailed in STAT SOP 3250 Ammonia Distillation by 4500-NH3 B

3.0 Detection Limits

The lab follows the procedure found in 40CFR Part 136B to determine the MDL for each matrix type on an annual basis. See the STAT Analysis SOP 1210 for the MDL procedure, frequency and acceptance criteria. The MDLs measured by the lab and all supporting documentation are in the laboratory QA files for review.

The laboratory determined MDL must always be less than the reporting limit (RL). The RL will usually range from three to ten times the laboratory measured MDL but this relationship may vary dependent on dilution of sample aliquots, matrix interferences, moisture adjustments (in solid samples), or method-specified requirements.

For the Phenate Method, the applicable range for aqueous samples is 0.05 to 5 mg/L and the applicable range for soil samples is 2.5 to 250 mg/Kg (as received basis). The applicable reporting level for titration of aqueous samples is 1 mg/L and for soils is 50 mg/kg (as received basis). Sample distillates with concentrations greater than the highest calibration standard are diluted and then reanalyzed. Samples with high concentrations of ammonia may also be redistilled using a smaller sample size and then analyzed.

4.0 Scope and Application

The method, based on Standard Methods 4500-NH3 H and C, is designed for the analysis of aqueous distillates for ammonia. Samples and QC samples are distilled prior to analysis. The distillation procedure described in SOP 3250 Ammonia Distillation by 4500-NH3 is designed for the determination of ammonia in aqueous solutions, solid waste materials, or effluents. This method is not applicable to oil or multiphasic samples or samples not amenable to the distillation procedure. This method may be performed using an Automated Phenate Method or the Titrimetric Method. For the automated method, it is restricted to use by or under the supervision of analysts experienced in the use of the Lachat Auto Analyzer.

5.0 Summary of Method

The Automated Method is based on Berthelot reaction of the distillate with alkaline phenol, then with sodium hypochlorite to form indophenol blue. Sodium nitroprusside (nitroferricyanide) is




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added to enhance sensitivity. The absorbance of the reaction product is measured at 630 nm, and is directly proportional to the original ammonia concentration in the samples. The Titrimetric Method is based on titration with sulfuric acid until indicator turns a pale lavender.

Method Modifications from Reference This SOP reflects the reduced volume version of the method. Reduced volume versions of this method that use the same reagents and molar ratios are acceptable provided they meet the quality control and performance requirements stated in the method. Degassing to remove air bubbles is performed only if it is noticed that there are air spikes during analysis by the Phenate Method.

6.0 Definitions

The STAT Analysis Corporation Quality Assurance Manual (QAM) contains the definitions of standard terms used in this SOP.

7.0 Interferences

7.1 Interferences are eliminated or reduced by using the distillation procedure described in SOP 3250 Ammonia Distillation by 4500-NH3 B.

7.2 Calcium and Magnesium ions may precipitate if present in sufficient concentration. EDTA

(Ethylenediamine Tetraacetate) is added to the sample in line in order to prevent this problem 7.3 Oxidizing agents such as chlorine, detected by the liberation of iodine upon acidification in

the presence of potassium iodide, are removed immediately after sampling by the addition of an excess of sodium arsenite. If chlorine is not removed, the ammonium compounds may be partially oxidized and the results may be low.

7.4 Method interference may be caused by contaminants in the reagent water, reagents,

glassware, and other sample processing apparatus that bias analyte response. 8.0 Safety

8.1 All samples must be assumed as hazardous and appropriate precautions taken during handling.

8.2 Safety glasses, gloves, lab coats and closed toe shoes are to be worn. 8.3 Other safety precautions must be conducted in accordance with the SAP 003 Chemical

Hygiene Plan. Other actions can also be applied if deemed necessary. A reference file of material safety data sheets (MSDS) is available in the laboratory for personnel involved in an analysis using chemicals.




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8.4 The toxicity or carcinogenicity of each reagent used in this method has not been fully established. Each chemical should be regarded as a potential health hazard and exposure should be as low as reasonably achievable. Cautions are included for materials known to be extremely hazardous.

8.5 The following chemicals have the potential to be highly toxic or hazardous, for detailed

explanation consults the MSDS. 8.5.1 Phenol is toxic and hygroscopic. Use extreme caution when handling this material. 8.5.2 Sulfuric acid is a strong oxidizer and sodium hydroxide is a strong reducing agent. Use

extreme caution when handling these materials. Avoid eye and skin contact. Wash exposed areas immediately with copious amounts of water.

8.5.3 Sodium Nitroferricyanide is toxic. Use extreme caution when handling this material. Avoid contact with acids which will releases cyanide gas.

9.0 Equipment and Supplies

9.1 LaCHAT AutoAnalyzer consisting of the following components: 9.1.1 Autosampler Cetac 9.1.2 Reagent Pump 9.1.3 System Unit Lachat 8000 9.1.4 Computer 9.1.5 Printer

9.2 Centrifuge Tubes, 50 mL graduated 9.3 Volumetric Flasks, Class A: 1000mL, 250mL, 100mL, 50mL, 25mL with stoppers 9.4 Autopipetter: 0.010 to 0.10 mL, 0.10 to 1.0 mL, 1.0 to 5.0 mL

9.5 Test Tubes, 15 mL and Tube Racks 9.6 Plastic and glass bottles for solution storage

9.7 Burette: 50 mL. with 0.1 mL graduations

9.8 Beaker: 250 mL.

10.0 Reagents and Standards

The following reagents and standards are required to perform this procedure. When instructions are given on how to prepare a specific volume of a reagent or standard, larger or smaller volumes can be prepared as needed so long as the final concentrations remain the same. Any other deviations from the reagents or standards listed in this SOP could be detrimental to the quality of the data produced. Such deviations would have to be approved and documented (see 230 Corrective Action SOP).

10.1 Instructions for labeling and record keeping of reagents and standards are contained in SOP

1010 Analytical Standards and Reagents Receipt and Preparation.




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10.2 Reagents - In methods where the purity of reagents is not specified, analytical reagent grade shall be used. Reagents of lesser purity than those specified by the test method shall not be used.

10.3 Use ammonia-free reagent water (1 Mohm) for all solutions. Degas reagents with helium if

necessary to prevent bubble formation.

10.4 Reagent 1. Sodium Phenolate: In a 1-liter volumetric flask, dissolve 88 ml of 88% liquefied phenol, or 83 g crystalline phenol in 600 ml reagent water. While stirring, slowly add 32 g Sodium Hydroxide (NaOH for Nitrogen determination), cool, dilute to the mark with reagent water and invert to mix. Do not degas this reagent.

10.5 Reagent 2. Sodium Hypochlorite: In a 500-ml volumetric flask, mix 109 mL regular

Clorox © Bleach (6% sodium hypochlorite) with 125 mL. of DI water. Invert to mix.

10.6 Reagent 3. Buffer: In a 1-liter volumetric flask, dissolve 50.0 g Disodium Ethylenediamine Tetraacetate Dihydrate (Na2EDTA*2H2O) and 5.0 g Sodium Hydroxide (Nitrogen Determination grade) in approximately 900 ml reagent water. Mix until dissolved and dilute to the mark.

10.7 Reagent 4. Sodium Nitroprusside: To a 1-liter volumetric flask, dissolve 3.5 g Sodium

Nitroprusside (Sodium Nitroferricyanide). Dilute to the mark with reagent water and invert to mix.

10.8 Reagent 5. Carrier and Diluents (0.20% H2SO4): To a 1-liter volumetric flask, add

approximately 900 ml reagent water and 2 ml concentrated Sulfuric Acid. Dilute to the mark with reagent water and invert to mix.

10.9 Reagent 6. 0.02 N Sulfuric Acid (Titrant)

10.10 Standards for Phenate Method

10.10.1 At least one of the standards must be traceable to a NIST traceable source when

available. The manufacturer should include a certificate of analysis for each standard. If one is not provided, contact the manufacturer. Retain all certificates in the designated binder (see SOP 1010 Analytical Standards and Reagents Receipt and Preparation).

10.10.2 Standards must be prepared volumetrically using class-A volumetric glassware, calibrated micropipettes, or gas tight syringes. Do not use disposable pipettes to prepare standards.

10.10.3 Nitrogen Stock Calibration Standard: 1000 mg Nitrogen/L: Commercially Purchased. Store per manufacturer’s recommendations and shelf life. If shelf life is not stated, then this solution may be used for twelve months if stored in the original container at 0.1 - 6oC and shows no sign of deterioration.

10.10.4 Intermediate Ammonia Calibration Solution: 100 mg Nitrogen/L: Dilute 5 ml of Ammonia Stock Standard to 50 ml with 0.20% H2SO4 (Reagent 5). Invert to mix. This solution may be used for six months if stored at 0.1 - 6oC and shows no sign of deterioration.

10.10.5 Stock ICV/CCV Nitrogen Standard (2ndSource) 1000 mg Nitrogen/L: Commercially purchased. Store per manufacturer’s recommendations and shelf




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life. If shelf life is not stated, then this solution may be used for twelve months if stored in the original container at 0.1 - 60C and shows no sign of deterioration.

10.10.6 Intermediate (ICV/CCV) Ammonia Standard 100 mg Nitrogen/L: Dilute 5 ml of Stock ICV/CCV Standard to 50 ml with 0.20% H2SO4 (Reagent 5), invert to mix. This solution may be used for six months if stored at 0.1 - 60C and shows no sign of deterioration.

10.10.7 Working ICV STD, 1 mg Nitrogen/L: Dilute 0.5 ml of Intermediate ICV/CCV STD to 50 ml with 0.20% H2SO4 (Reagent 5). Prepare this solution fresh daily.

10.10.8 Working CCV STD, 2.5 mg Nitrogen/L: Dilute 1.25 ml of Intermediate ICV/CCV STD to 50 ml with 0.20% H2SO4 (Reagent 5). Prepare this solution fresh daily.

10.10.9 The Calibration Standards are prepared according to Table 1 below. Add listed volumes of the Intermediate Ammonia Calibration Standard to each flask, and dilute to mark with 0.20% H2SO4 (Reagent 5). Cap and mix will.

Table 1 Ammonia Calibration Standards

Calibration Standard Concentration, mg

Nitrogen/L

Amount of Intermediate Calibration

Standard mL

Concentration of Intermediate Calibration

Standard, mg/L

Final Volume, mL

mg Nitrogen

per 50 mL

5 2.5 100 50 0.25 2.5 1.25 100 50 0.125 1 0.5 100 50 0.05

0.5 0.25 100 50 0.025 0.1 0.05 100 50 0.005

0.05 0.025 100 50 0.0025 0.01 0.005 100 50 0.0005

0 0 0 50 0 11.0 Sample Collection, Shipment, Preservation and Storage

Samples shall be placed on ice immediately after collection. The holding time is 28 days for a refrigerated sample (0.1 - 6oC) with proper chemical preservation (pH < 4). Distillation and analysis must occur within the 28 days period to be compliant.

12.0 Quality Control

The following details the QC requirements that apply to this analysis. Each Quality Control Indicator (QCI) provides information pertaining to either method or individual sample performance. Our goal is to produce defensible data of known and documented quality.

The results of these QCI samples are used to assess the acceptability of data.

12.1 Blanks

Method Blank analysis is performed to determine if any contamination is present in the analytical process and is used to evaluate acceptance of the batch of samples. A method




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blank shall be prepared once per preparation batch of 20 or less samples per matrix type If more than 20 samples are prepared a second blank shall be prepared after the twentieth sample. The method blank shall be processed through all preparatory steps used for the samples, including cleanup procedures. The blank shall be analyzed using the same instrument and conditions as the samples.

12.2 Laboratory Control Sample (LCS)

The LCS is used to evaluate the performance of the total analytical system, including all preparation and analysis steps. The LCS shall be prepared once per preparation batch of 20 or less samples per matrix type. If more than 20 samples are prepared a second LCS shall be prepared after the twentieth sample. The LCS shall be processed through all preparatory steps used for the samples, including cleanup procedures. The LCS shall be analyzed using the same instrument and conditions as the samples.

12.3 Duplicates

Duplicates of field samples or of the LCS must be prepared in compliance with the method requirements and client directives. Note: The analysis of the Matrix Spike Duplicate (MSD) is used as a substitute for the laboratory duplicate.

12.4 Matrix Spike and Matrix Spike Duplicate (MS/MSD)

MS/MSDs indicate the effect of the sample matrix on the precision and accuracy of the results generated using the selected method. This information does not determine the validity of the entire batch. MS/MSD’s must be analyzed at a minimum of 1 per 20 samples per matrix per preparation procedure, or as specified by the required test method. For cases where the sample cannot be divided (e.g., wipes, air samples, not enough sample provided by customer) and thus a MS/MSD pair cannot be prepared in the preparation batch, an LCS/LCSD pair is prepared and analyzed to measure precision.

The MS/MSD pair shall be processed through all preparatory steps used for the samples. They shall be analyzed using the same instrument and conditions as the samples.

13.0 Calibration For the Phenate Method

Initial Calibration (ICAL) In addition to achieving the reference method requirements for the minimum number of calibration standards and the acceptance criteria (statistics) for calibration curve fit, the following ICAL criteria also apply:

13.1 The ICAL must be a minimum of 5 standards, not including a blank. 13.2 The ICAL must be verified with a second source standard (ICV) prior to the analysis of

samples. 13.3 Results of samples not bracketed by the ICAL range must be qualified on the final report. If

possible, dilute the sample or distill a smaller amount and reanalyze in order to achieve a result within the calibrated range of the instrument.




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13.4 The lowest calibration standard may establish the reporting limit: RL = 0.05 mg/L for waters and 2.5 mg/Kg for soils (as received basis). The RL must be greater than or equal to the detection limit.

13.5 Samples must be quantitated from the initial calibration curve and may not be quantitated

from any instrument CCV. Initial Calibration Verification (ICV) In addition to the method requirements, the following ICV criteria also apply:

13.6 Must be a second source standard from the ICAL standards or from a different manufacturer lot number.

13.7 Must be traceable to NIST when available.

13.8 Must be analyzed when an ICAL is not performed on the day of analysis, prior to sample

analysis.

13.9 Initial Calibration Blank (ICB): (0.2% H2SO4) Analyzed immediately after the ICV. Acceptance limits are ± RL.

Continuing Calibration Verification (CCV) In addition to the method requirements, the following CCV criteria also apply: May be analyzed at the beginning of the batch to check the CCV recovery.

13.10 Must be analyzed after every 10 samples and at the end of each analytical batch.

13.11 If the CCV results obtained are outside the acceptance criteria, corrective actions must be performed. If routine corrective actions fail to produce an acceptable second consecutive (immediate) CCV, then either the lab has to demonstrate performance after corrective action with two consecutive successful CCVs, or a new ICAL must be performed. If the instrument has not demonstrated acceptable performance, sample analyses cannot continue until a new ICAL is established and verified with an ICV. However, sample data associated with an unacceptable CCV may be reported as qualified data under the following special conditions:

13.11.1 When the acceptance criteria for CCV are exceeded high, i.e., high bias, and there are

associated samples that are non-detects, then those non-detects may be reported. Otherwise the samples affected by the unacceptable calibration verification must be reanalyzed after a new ICAL has been established, evaluated and accepted.

13.11.2 When the acceptance criteria for the CCV are exceeded low, i.e., low bias, those

sample results may be reported if they exceed a maximum regulatory limit/decision level. Otherwise the samples affected by the unacceptable verification must be reanalyzed after a new ICAL is established and verified with an ICV.

13.11.3 When the acceptance criteria for the CCV are exceeded and it is not possible to

reanalyze the sample due to limited sample quantity AND a new sample cannot be obtained by the laboratory, the data may be reported with the appropriate data qualifiers if the client has been contacted and agrees, in writing, to accept the qualified data.




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13.12 Continuing Calibration Blank (CCB): (0.2% H2SO4) Analyze immediately after the CCV. Acceptance limits are ± RL.

13.13 Records: Initial and Continuing Calibration Records will contain, at a minimum, the

following: 1. Calibration date 2. Test method 3. Instrument 4. Analysis date 5. Each analyte name 6. Analyst's initials or signature 7. Standard Concentration (appropriate units) and number of standards 8. Response (appropriate units) 9. Calibration curve or response factor 10. Evaluation of and Statistics for ICAL curve fit in order to judge calibration curve

acceptance 11. Evaluation of and Acceptance Limits for ICV analysis in order to judge calibration curve

acceptance 12. Evaluation of and Acceptance Limits for CCV analysis in order to judge continuing

calibration acceptance 13. Calibration Standards and Reagent Solutions IDs

Calibration Acceptance Summary:

Table 2 Calibration Requirements

QCI Frequency Standards Control Limits Corrective Action ICAL Daily or as needed, Minimum 5

standards, see Table 1 for concentrations

r = 0.995 Correct problem then repeat initial calibration

ICV After each new ICAL And at the beginning of each analytical run.

1.0 mg/L ± 10% of true value Correct problem then repeat initial calibration

ICB After each ICV 0.2% H2SO4 ± reporting limit Correct problem then repeat initial calibration

CCV Beginning (optional), every 10 samples, and end of the batch

2.5 mg/L ± 10% of true value Correct problem then repeat CCV or repeat initial calibration

CCB After each CCV 0.2% H2SO4 ± reporting limit Correct problem then repeat CCV or repeat initial calibration

Support Equipment: Autopipettes - Check autopipette to ensure standardization is within control limits (see SOP 1040 General Laboratory Practices for Pipette Calibration).

Balances - Be sure the balance is checked prior to use and performance criteria are met (see SOP 1040 General Laboratory Practices for Calibration of Balances).




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14.0 Procedure (14.1 through 14.11 for the Phenate method)

14.1 Instrument Start Up 14.1.1 Turn on the power to all modules by turning on the power strip and allow the

autosampler to perform its startup routine. Wait until the autosampler stops with the probe above the wash bath.

14.1.2 If necessary, install the manifold on the channel you want to run. (See Appendix E.) 14.1.3 Make all the injection fluidic connections. 14.1.4 Make all the cell fluidic connections. 14.1.5 Set all pump tubes on the pump. (Varies method to method.) 14.1.6 Run reagent water through all the lines to make sure there are no leaks. 14.1.7 If there are no leaks, put actual reagents in line. 14.1.8 ALWAYS start pumping Buffer Solution FIRST. 14.1.9 Pour the calibration Standards into Standard vials, and place into the autosampler

Standards Rack. 14.1.10 Pour the Samples into test tubes and place into the Sample Rack. 14.1.11 If necessary, insert the interference filter into the upper slot in the detector. 14.1.12 Turn on the Heater by increasing the Set Point to 600C. Press the Set Point Key (Left

of the arrow keys) until the display shows the letters SP for Set Point. Press the big arrow keys for setting the temperature, press the ENTER key to save the information. Press the Set Point key once. The display will show the current temperature in Celsius. The red light will be lit when the heater is ON.

14.2 Software Set up

14.2.1 Double click on the Omnion FIA icon. Then click OK. The autosampler probe should go into the wash bath and the dilutor activity may be heard, the injection valves may turn to the inject state if they were not already there.

14.2.2 Log In with your user name and password. [User name: demo with no password will also get you in]. The Main Menu should appear.

14.2.3 From the Main Menu click on the Instrument button labeled FIA Instrument 1. Each valve allocated to this instrument will be cycled in turn from Load to Inject and back to Inject again. Omnion will automatically open the last Method and Tray that was used. (The names will appear at the top in the title bar.).

14.3 Open the Ammonia Method (To Create a Method see Appendix B)

14.3.1 Click on the Method button, or from the Main Menu click on File , then Open Method. This will open the Open Method Dialog window.

14.3.2 Double click on the method file you want to open: Ammonia met. or click once then click on OK.

14.3.3 From the Main Menu click on the Instrument button labeled FIA Instrument 1. Each valve allocated to this instrument will be cycled in turn from Load to Inject and back to Inject again. Omnion will automatically open the last Method and Tray that was used. (The names will appear at the top in the title bar.)

14.4 Opening and Editing the TRAY

14.4.1 Click on the Tray button or from the Main Menu, click on File, then Open Tray. 14.4.2 Click twice on the name of the tray you wish to open. (Ammonia tray) The First rows

of the tray spreadsheet are blue. This denotes that these samples are actually Calibration Standards. This is from the method and will not change. The Sample Type is Cal Std.




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And the Level is NEVER 0; it will be a number from 1 to 14 (This will match the level in the Analyte Table in the method.) The Cup Number (Cup #) refers to the cup number in the Standard Rack and will be a number between 1 and 14.

14.4.3 Edit the Sample ID. Using the mouse, move the pointer to the cell and click once; type in the new ID. In the Sample Rack Loading Aid (Top Left) the sample cup you are editing will be in green.)

14.4.4 The Cup Numbers (Cup #) for sample will can be anything from 1 to 90. 14.4.5 The Level column is 0 for all samples of Sample Type Unknown 14.4.6 The Reps for samples and standards is 1 or 2. 14.4.7 To Schedule manual QC See Appendix C (DQM Plan)

14.5 Click on the Run Tray button. (Or from the Main Menu, click on Tray then Run Tray.)

14.5.1 Leave the Method and Tray boxes empty to use the ones that are active (open). 14.5.2 In the Data File box enter the name for your run, (i.e. 981006Ca. YYMMDD C (for

Calibration) and a (for number of the run... a b c...).) The extension *.fdt (FIA Data) is used by default.

14.5.3 The Autosampler Position refers to the autosampler sample rack position: 1, 2 or 3. 14.5.4 Skip Recalibration Block Box can be checked when you want to run a tray that

contains Cal standards and samples but you want only want to run samples 14.5.5 While the tray is processing, you can view the peaks and runtime report. 14.5.6 If the baseline does not appear on the screen change Display options. 14.5.7 Click Method, then Display Options 14.5.8 Specify the channel: 1. 14.5.9 Specify the voltage scale on the Y-axis (i.e. -1 to 3). 14.5.10 Click OK.

14.6 Analyze samples for Ammonia. Click on the RUN button. The tray will start running. After

the pump is allowed to pump at a normal speed for the period specified it the method, pump timing, the autosampler will move to the first calibration standard. The Standards and samples are done in Row order (on the computer screen), no matter where they are located on the autosampler tray.

14.7 While running you will see a STOP sign on the tool bar. To suspend the tray click on the

STOP sign. The Tray will pause and the computer gives you the choices of aborting or resuming the tray. At the end of the tray, after the last sample ID entered is reported, the sample probe should return to the rinse position and the STOP button will turn back into the RUN button.

14.8 If baseline drifts or other problems with precision arise, clean the manifold using the

following procedure. Place all reagent lines in reagent water for 5 min. Place all reagent lines in 1 M Hydrochloric Acid (1 volume concentrated HCl added to 11 volumes of reagent water) and pump for 10 min. Rinse with reagent water for 30 min.

14.9 System Shutdown Procedure

14.9.1 Remove the reagent transmission lines and place into the rinse solution and pump for 5 minutes at standard speed. 14.9.2. Place the lines into reagent water and allow the system to rinse 5 to 10 minutes at standard speed.




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14.9.3 Remove the lines from the reagent water and allow all liquid to be pumped out of the manifold. 14.9.4 Turn off the pump and release the pump tube cartridges tension. Press the tube cartridges holders on the sides of the Isomatec pump. 14.9.5 Turn off the Heater by Reducing the Set Point to a temperature lower than room temperature. (e.g. 15°C). 14.9.6 Close all files 14.9.7 Switch off the master power strip

14.10 Documentation requirements. Record the following information in the appropriate logbook or data file. Include any deviations from this procedure.

14.10.1 Analyst initials, date [and time if required by the specific project or QAPP] of analysis, sample number or ID, initial sample volume or weight processed, final digestate volume, calibration standard sample or solution identifier, QC sample or solution identifier, reagent solutions identifiers, any dilution information, [beginning and ending times of analytical steps if required by the specific project or QAPP], data file name or batch ID, instrument method name, visual observations, and any other information as deemed necessary

14.10.2 Print out a copy of the calibration curve used and datafile (run sequence).

14.11 Routine Maintenance – Record all maintenance in the logbook. See Appendix F

14.12 Titrimetric Method: Fill burette with reagent upto the Zero mark (meniscus at 0). Place 50

mL. of the blank distillate in a beaker. Add titrant dropwise while swirling the beaker. Record amount of titrant used when color turns and remains lavender for 30 seconds. Repeat procedure for samples, LCS, MS/MSD.

15.0 Data Reduction, Calculations and Loading

15.1 The data system will then prepare a calibratio n curve by plotting response versus standard concentration. Sample concentration is calculated from the regression equation.

15.2 Report only those values that fall between the lowest and highest calibration standards.

Samples exceeding the highest standard must be diluted and reanalyzed. 15.3 Aqueous Samples: The concentration readout for aqueous sample distillates is mg Ammonia

as Nitrogen/L. It does not need further data reduction unless the initial sample volume was less than 50 mL. If less than 50 mL sample was distilled, calculate the concentration as follows: Concentration in mg Ammonia /L = readout * (50 ml/ initial sample volume analyzed in mL)

15.4 For sample results greater than the highest calibration standard, dilute the sample in a 10 mL

centrifuge tube using Reagent 5.

15.5 Pipette in the appropriate volume of sample into the tube, dilute to the mark with Reagent 5. Record the volume of distillate used for analysis. Dilution Factor = (10 mL/ distillate volume analyzed in mL). Use the dilution factor and calculate the concentration in aqueous samples as follows:




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Concentration in mg Ammonia /L = readout * (10 ml/ distillate volume analyzed in mL)

15.6 Soil Samples: The concentration readout for soil samples must be multiplied by the following factor: Factor = (50 / sample weight in g). Calculate the concentration in soil samples as follows: Concentration in mg Ammonia /Kg = readout * (50/ sample weight in g) For soil sample results greater than the highest calibration standard, follow the dilution procedure in section 15.4

15.7 Soil samples reported on a dry weight basis: The concentration is divided by the decimal

equivalent of the percent residue of the soil at 1050C. 15.8 Report results in mg Ammonia /L, or mg Ammonia /Kg.

15.9 The procedure for uploading data into the LIMS system is detailed in SOP 1400 LIMS.

15.10 For the Titrimetric Method,

Mg NH3-N/L = (A-B) x 280/mL. sample Where, A: Volume of H2So4 required for sample (mL) B: Volume of H2So4 required for blank (mL)

16.0 Method Performance

Demonstration of Capability (DOC) Note: Each analyst must demonstrate the ability to generate acceptable results with this method.

All parameters of interest must meet the method acceptance criteria before actual sample analysis begins. See SOP 1230 Training for the procedure to perform and document the DOC. The DOCs for the analysts performing this method are located in the analysts’ training form folders located in the QA office files. A quality control (QC) reference concentrate is required containing Ammonia at a concentration of 1-4 times the reporting limit. The QC reference sample is made using stock standards prepared independently from those used for calibration. For the Phenate Method, distillation is required. For the Titrimetric method, disrtillation is not required.

For each analyte, calculate the mean recovery (X), standard deviation (s), relative standard deviation (RSD), and the average % Recovery (%R). Compare X and s and %R with the corresponding acceptance criteria for accuracy and precision, respectively. Note: RSD must be equal to or less than 20% and the %R must be within 100 ± 20%. These limits are taken from established in-house criteria If RSD and %R for all analytes meet the acceptance criteria, the system performance is acceptable and analysis of actual samples can begin. If RSD or %R falls outside the range for accuracy and precision, then the system performance is unacceptable for that analyte and corrective action must be taken.




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Comparison to Reference Method Data There are no stated reference method criteria for ICV, LCS, Duplicate Sample or MS/MSD recoveries in Method 4500-NH3.

In-House Control Limits Method performance data is on file in the laboratory QC department. Comparison of method performance data for the laboratory to the reference method criteria occurs when laboratory in-house acceptance limits are generated. In-house generated data is compared to the specifications of the reference method. If the in-house limits are within the specifications of the reference method, the control limits are updated in LIMS. If the in-house limits are not within specifications, an investigation is performed to determine the cause(s) of the problem and a corrective action is completed. The analysis may continue until enough data points are collected to regenerate new control limits. Any QC data generated outside of reference method limits during that time frame is flagged.

The laboratory maintains performance records to document the quality of data that is generated. Method accuracy for samples is assessed and records maintained.

17.0 Pollution Prevention

The preparation of excessive volumes of laboratory reagents and standards shall be avoided so that waste and potential for pollution are minimized. Samples, reagents and standards shall be disposed in compliance with the laboratory waste disposal program and applicable waste disposal regulations. With the consent of the client, the samples may be returned to their origin for treatment.

Uncontaminated paper waste, glass and cans should be separated for recycling. Laboratory staff are required to protect the laboratory’s and our clients’ business information when disposing of recycling or waste from the facility.

18.0 Data Assessment and Criteria for Quality Control Measures

The laboratory maintains records to document the quality of data that is generated. Ongoing quality checks are compared with established performance criteria to determine if the results of analyses meet the performance characteristics of the method. The data review is conducted according to SOP 1250 Data Review.

Method Blank (MB) If the blank exceeds the RL (the lowest calibration standard), the source of contamination must be investigated and corrective actions taken. Affected samples must be reprocessed and reanalyzed or Data must be appropriately qualified if: 1) The concentration of a targeted analyte in the blank is at or above the reporting limit as

established by the SOP or by regulation, AND is greater than 1/10 of the amount measured in any sample .

2) The blank contamination otherwise affects the sample results as per the test method

requirements or the individual project data quality objectives.




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Laboratory Control Sample (LCS) The results of the individual batch LCS are calculated in percent recovery (%R) and compared to established acceptance criteria (in-house limits). LCS %R limits are 100 ± 20%. If the LCS is outside the acceptance criteria, the analytical system is “out-of-control”. Any affected samples associated with an out of control LCS must be reprocessed and reanalyzed or the results reported with appropriate data qualifiers.

Matrix Spikes The results from MS/MSD are primarily designed to assess the precision and accuracy of analytical results in a given matrix and are expressed as percent recovery (%R) and relative percent difference (RPD). See the STAT QAM, Section 5.4 for the calculation for RPD. Results are compared to established acceptance criteria (in-house limits). For aqueous samples, MS/MSD %R limits are 100 ± 25% and RPD limits are 20%. For soil samples, MS/MSD %R limits are 100 ± 25% and RPD limits are 20%. For matrix spike results outside established criteria corrective action must be documented, or the data for the spiked sample is reported with appropriate data qualifying codes.

Duplicates

The results from laboratory Duplicates are designed to assess the precision of analytical results in a given matrix and are expressed as relative percent difference (RPD). See the STAT QAM, Section 5.4 for the calculation for RPD. Results are compared to established acceptance criteria (in-house limits). RPD limits are 20%. For duplicates results outside established criteria corrective action must be documented, or the data for the duplicate sample is reported with appropriate data qualifying codes.

19.0 Corrective Actions for Out-of-Control Data

The process for handling corrective actions is found in SOP 230 Corrective Action.

If the CCV, MB, LCS/LCSD, MS/MSD, or lab duplicate recovery of any parameter falls outside the designated acceptance range, the laboratory performance for that parameter is judged to be out of control, and the problem must be immediately identified and corrected. The analytical result for that parameter in the samples is suspect and is only reported for regulatory compliance purposes with the appropriate corrective action form. Immediate corrective action includes reanalyzing all affected samples by using any retained sample before the expiration of the holding time. Final data results must be qualified in the client report for reported results not meeting the laboratory-defined criteria.

1) Review standards preparation logbooks. Check all calculations and ensure dilution factors are

properly recorded. 2) Re-prepare the suspected standard or QC sample to identify possible preparation errors of the

standard or QC sample.

3) Re-Analyze the samples when the CCV or LCS is not within acceptable limits.




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4) Perform routine preventative maintenance following manufacturer's specification. Record all maintenance in the instrument logbook.

20.0 Contingencies for Handling Out-of-Control Or Unacceptable Data

Every effort is made to prevent problems from occurring. When out of control or unacceptable data occurs the first option is to identify the problem and reanalyze the samples within the holding times. When this is not possible, the QA Manager and/or the Laboratory Director reviews data and discuss options with the client. Reanalysis or reporting the data with qualification is alternatives. Out-of-control or unacceptable data reported to the client must include the data qualifier, flag and discussion on the rationale for reporting.

The process for handling unacceptable and out of control data is found in section 11 of the Laboratory QAM. The reporting of data that is out of control must be approved and documented by Quality Assurance Manager and either the Technical Manager or the Laboratory Director.

21.0 Waste Management

The STAT Analysis Corporation SOP 1130 Waste Disposal identifies proper waste management practices for the chemicals and biological materials used in this procedure. Samples are stored and discarded accordance with SOP 1130 Waste Disposal.

22.0 References

22.1 Method 4500-NH3 B, H, and C. U.S. EPA, Standard Methods for the Examination of Water and Wastewater (20th Edition).

22.2 Determination of Total Recoverable Ammonia by Flow Injection Analysis. QuikChem Method 10-107-06-1-B.

22.3 STAT Analysis Corporation Quality Assurance Manual 22.4 STAT SOP 003 Chemical Hygiene Plan 22.5 STAT SOP 230 Corrective Actions 22.1 STAT SOP 1000 Control and Use of Laboratory Notebooks 22.2 STAT SOP 1010 Standard and Reagent Preparation 22.3 STAT SOP 1020 Glassware Cleaning 22.4 STAT SOP 1040 General Laboratory Procedures 22.5 STAT SOP 1130 Waste Disposal 22.6 STAT SOP 1210 Method Detection Limits (MDL’s) 22.7 STAT SOP 1230 Training 22.8 STAT SOP 1250 Data Review 22.6 STAT SOP 1400 LIMS 22.7 STAT SOP 3250 Ammonia Distillation by EPA 4500-NH3 B. 22.8 QuikChem 8000 Automated Ion Analyzer Omnion FIA Software. 22.9 QuikChem 8000 Automated Ion Analyzer Continuum Series “Flow Injection Analyzer”

Hardware Installation and System Operation.




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23.0 Forms, Figures, Tables, Diagrams, Flowcharts, Attachments or Validation Data

23.1 Appendix A Troubleshooting 23.2 Appendix B Creating a Method 23.3 Appendix C DQM Plan 23.4 Appendix D Manifold Diagram 23.5 Appendix E Manifold Installation/ Removal 23.6 Appendix F Maintenance Schedule




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Appendix A – Trouble Shooting

Keep all modules clean and dry at all times. Keep in Stock: Pump tubes orange White Red Red Gray Green Teflon tubing: 0.8 mm id Manifold

0.5 mm id Low Flow Manifold 0.6 mm id Restriction Coil O-rings Transmission Tubing

Routine Maintenance (See Appendix F for the Maintenance Schedule) Pump

n After each day rinse the cartridges in reagent water to wash any spills. Clean pump surfaces, except rollers, with a wet cloth. Dry all sur faces.

n If rusty clean rollers with steel wool. Apply silicon spray on a lint free cloth and holding it to the moving rollers to apply a light coat of silicon.

n Check for wear, cracks or acid damage on the cartridges ad holders. n Replace pump tubes that start to show signs of wear n If the pump tubes burst, clean all cartridges and holders, as well as, the pump,

immediately. n All surfaces should be kept clean. Use a damp cloth to clean the module surfaces.

Dry surfaces thoroughly. Valve Modules n Keep the instrument clean and dry at all times. n Replace o-rings once per month n When changing the o-rings, clean the valve ports with cotton swab and reagent water.

This will help remove any dirt or precipitate that may prevent a good seal. If a leak persists, replace the new o-rings and make sure the connector itself does not have precipitate on the thread.

n All surfaces should be kept clean. Use a damp cloth to clean the module surfaces. Dry all surfaces thoroughly.

n The internal sample loop valve will give thousands of injections without trouble. The rotor seal wears with use and is the only part that needs routine replacement.

Detector Modules and Flow Cell n If a flow cell appears to leak remove it immediately to keep all liquid form the

electronics inside the detector head. Instrument Troubleshooting

For problems with the instrument see the QuikChem 8000 Automated Ion Analyzer Continuum Series “Flow Injection Analyzer” Hardware Installation and System Operation Manual under the Troubleshooting Section.




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Appendix B – Creating A Method 1.1 Click on the Method button, or from the Main Menu click on File, then New Method. 1.2 Then Method will open and you will see the Analyte Table 1.3 Click on Analyte Name of channel and press backspace to delete. Enter the new analyte

name. If an analyte name is not present, the system will ignore that channel. 1.4 Fill out the analyte Table. Channel 1 Analyte Name Ammonia Concentration mg/L Level 1 5 Level 2 2.5 Level 3 1 Level 4 0.5 Level 5 0.1 Level 6 0.05 Level 7 0.01 Level 8 0 Calibration Rep Handling Average Calibration Fit Type 1st Order Polynomial Force Through Zero No Weighting Method None Concentration Scaling None Chemistry Direct Injection to Start Peak 41.8 s Peak Base Width 27.8 s % Width Tolerance 100% Threshold 10000 1.5 From the Main Menu, click on Method, then Valve Timing 1.6 Enter the Method Cycle Period. 60s 1.7 Sample Reaches the first valve 18s (For Standard Pump Sample Assembly) (travel

time from sample probe to port 6 usually 24 s if dilutor enter 28s) 1.8 Load Period 15s Load Time 0s Inject Period 45s Notice that Load Period + Injection Period = Cycle Period 1.9 Click OK 1.10 From the Main Menu, click on Method, then Sampler Timing. 1.11 The Sample Prep Sequence box is optional 1.12 Enter the Minimum Probe in Wash Period 5.0 s 1.13 Enter the Probe in Sample Period 24s




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1.14 Click OK. 1.15 From the Main Menu, click on Method, then Pump Timing 1.16 Check the Go to Standby on Idle box X 1.17 Enter Idle Before Standby 180.0s 1.18 Enter At Speed Before Analysis 45.0s 1.19 Click OK. 1.20 From the Main Menu, click on File, then Save Method As 1.21 The FIA Method File Header will appear. Write a method description (analyte and sample loop size) and click OK. (i.e. Ammonia Sample Loop XXX cm) 1.22 The Method Save As dialog box will appear. 1.23 C:\ Omnion\Methods\

Change the name to Ammonia.met II To Fine Tune the Method 1.0 After you have run a data. 1.1 Open a file from the main menu click on File, Open Data and click twice on the Data file

name, i.e. 981006Ca.fdt. 1.2 Load the original method form this data by clicking on the Data menu the Load Method. 1.3 You should see the peaks on the screen. 1.4 Click on Data then Reanalyze Data. (Or click on the Reanalyze button.) 2.0 Fine Tuning the Threshold 2.1 Look before and after the tray to see some baseline. 2.2 From the menu click on Method, then Graphical, Events, Programming... 2.3 Click on Threshold. 2.4 The Status bar will prompt you to “Select Start of Baseline Section”. 2.5 Set the cursor at the beginning of the baseline region and click once. 2.6 You will be prompted to “Select End of Baseline Section”. 2.7 Move the mouse pointer to the end of the baseline region and click again. 2.8 Omnion calculates a Threshold value. 2.9 Click on OK to enter the value in the Analyte Table of your method 3.0 Fine Tuning the Peak Base Width 3.1 From the menu click on Method, then Graphical Events Programming... 3.2 Click on Peak Base Width. 3.3 You will be prompted to “Select Start of Peak” 3.4 Set the cursor at the beginning of the high standard and click once. 3.5 You will be prompted to “Select End of Peak” 3.6 Move the cursor to the end of the peak and click again. 3.7 Omnion calculates a Peak Base Width. 3.8 Click on OK to enter the value in the Analyte Table of your method 4.0 Save these new method parameters by clicking on File, then Save Method As.




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5.0 Viewing a Method’s Calibration 5.1 Up to 4 replicates of each Standard can be applied to a method’s calibration. 5.2 If not already open, load the method form the data file by clicking on Data, Load Method. 5.3 Click on the button. (Or from the main menu click on Method, then Review Analyte

Calibration Curve. The Review Analyte Calibration window will appear. 5.4 Click Fit, and then Clear to ‘Clear’ the Calibration Replicate Table. 5.5 Click Exit. 5.6 Click the Analyze button. The re-analysis occurs exactly as it did in the actual tray run. 5.7 Click on the Review Calibration button again to see the curve. 6.0 Editing the Calibration 6.1 Clicking twice on any of the results in the calibration replicate Table will turn it red and

make it unused in the calibration. 6.2 To Use the point again, click twice on it again, and it will turn form red back to blue.




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Appendix C – DQM Plan DQM Plan Consists of one or several DQM sets. Each Set has one or more samples. The DQM has 3 sections; the DQM set box, the DQM Sample Box, and the Channel Data box. 1.0 Adding DQM Sets 1.1 Click Tray, then Load DQM. 1.2 In the DQM Set Box click on the drop-down button showing the DQM Set ID , type in a

new name. (Check Standards, Duplicates, Matrix Spikes) 1.3 For the Check Standards Set check the Automatic box X. 1.4 Click ADD to add the set. NOTE: Automatic Sets never have their sample info in the tray table and the samples are loaded in the standards rack. Manual sets have their sample info in the tray table and the samples are loaded in the sample rack. 2.0 Adding DQM Samples 2.1 In the DQM Sample Box, click on the drop-down button showing the DQM Sample ID

and type in a new name (ICB, ICV, CCV, CCB, Method Blank, Dup 1, Spike, Spike Dup)

2.2 Click on the Append button. 2.3 Replicates should be 2 2.4 Click on the drop-down button showing the Type and select the type of sample. (Blank,

Unspiked, Spiked, AbsChkStd, RelChkStd, Dup 1, Dup 2) 2.5 For the Automatic Check Samples enter the Standard Rack Cup. 3.0 Editing Channel Data information. 3.1 In the Channel Data Box, select the appropriate channel. 3.2 If you can’t see the Test 1 row, click on the Add Test button. 3.3 The Test Explanation spells out the test that will be done for this DQM Sample and

depends on what Type the DQM Sample is. 3.4 If the standard has a known concentration it needs to be entered in the Known Conc box

along with the Conc Units. 3.5 Enter the Test Limit. 10.000% difference. 3.6 Select a Fail Action from the drop-down menu. Recalibrate & Repeat, Alarm &

message . 3.7 Enter the Pass/ Fail Message. NOTE: A Test Passes if test value < = Test Limit A Test Fails if Test value > Test Limit 3.8 You can perform more then 1 test on each check sample. 4.0 Scheduling Automatic DQM Sets 4.1 From the Main Menu, click on Tray, then Auto DQM Schedule 4.2 Select the Auto DQM Set from the drop-down menu. 4.3 Check the box (es) for the frequency of the sample 4.4 Click OK.




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5.0 Inserting Manual DQM Sets 5.1 Click on the Tray Table button. 5.2 Click on the row number before which you want to insert the check sample. 5.3 From the Main Menu, click on Tray, then Manual DQM Insertion. 5.4 Click on the Manual DQM Set you wish to insert. 5.5 Enter the Sample ID’s of the DQM samples to reflect the actual identity of the samples.

(Note: The manual DQM sample rows are green.) 5.6 Renumber the Cup Numbers (Cup #) below the inserted Manual DQM Set by clicking

and dragging all the rows and cup numbers you wish to renumber. 5.7 Click on Tray, then Renumber Cups (or Ctrl-R) 5.8 Enter the Starting Number 5.9 Enter an Increment of 1. 5.10 Then click OK. 6.0 Calibration Pass/Fail Criteria 6.1 From the Main Menu, click on Method, then Calibration Failure Criteria 6.2 Select the appropriate channel. 6.3 Check the Minimum Correlation Coefficient (R2) Box and enter 0.995 6.4 Check the Maximum % Residual All Levels Box, and enter 10.0. 6.5 If the calibration passes, a message will be reported and the tray will continue to the nest

row. 6.6 If the calibration fails, a fail message will be reported and you will be given a choice to

Abort or continue the tray. 7.0 Save the DQM Plan 7.1 From the Main Menu, click File, then Save DQM Plan, or Save DQM Plan As... and

enter the File name Ammonia.dqm. The default extension is *.dqm.


SOP 4250 Automated Ammonia Analysis by EPA 4500 NH3 H Revision 00

Effective Date: March X, 2004 Page 25 of 28

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Appendix D – Manifold Diagram




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Appendix E – Manifold Installation/Removal Manifold Installation Procedure 1.0 Unwrap the transmission lines from around the manifold and place the manifold over the

sample-processing module. 1.1 Remove the transmission lines from the union on the 650 cm side of the heating unit,

insert both ends through the hole in the manifold and reseat the manifold onto the sample-processing module.

1.2 Make the Injection Valve Connections as follows: 1.3 Port 1 & 4 - The Sample Loop 0.8 mm i.d. length 75 cm. 1.4 Port 2 - Carrier line is connected to Port 2 -> from valve, disconnect from

Fitting and connect to port 2 0.8 mm id and 30 cm long. 1.4 Port 3 - 20 cm 0.8 mm id between port 3 and the fitting on the manifold

next to the label -> from valve where the carrier line was connected. 1.5 Port 5 - 15 cm 0.8 mm id. between port 5 and the waste line. 1.6 Port 6 - Sample Line. 130 cm (Varies method to method) connected to the

probe on the autosampler; pump tube adapter, and 20 cm tubing connected to port 6 of valve.

2.0 Flow Cell Top tubing connected to waste line. Bottom line connected to the fitting in the manifold next to the label to flow cell ->. Attach one of the lines from the heater to the union going to the flow cell. Attach the other heater line to the pyridine-barb. acid Tee-fitting.

3.0 Pump 3.1 Sample Line - Autosampler to injection valve 6. 3.2 Wash Line - Reagent water to wash reservoir on the autosampler 3.3 Reagents Lines- Varies from method to method sees Ammonia diagram. 3.4 On the Ismatec Pump Cartridges the arrows point towards the System Unit with the

tension lever on the left. 3.5 Place all of the reagents lines into corresponding containers or Reagent water. 3.6 Move tension levers to the maximum tension (Top Far Right Position) 3.7 Clamp down all pump tube cartridges. (Press down one side at a time.) 3.8 Move tension lever back from the top far right until it makes a clicking sound. 3.9 Set the reagent pump speed to 35. 3.10 Turn on the pump. 3.11 Depress the green button to turn the pump ON. The System Unit will take control over

the pump speed. (The yellow button is the override standby button.) 3.12 Check to confirm that the probe wash reservoir is filing with rinse water. 3.13 Check for Leaks on the manifold, va lve, flow cell or any of the connections. 3.14 Do NOT leave any pump tubes clamped down when the pump is shut off for more then a

few minutes. 3.15 To Remove cartridges, Press the sides of the pump holder on which the cartridge is

engaged. 4.0 Insert the interface filter into the detector module.




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II Manifold Removal Procedure 1.0 Rinse the manifold 1.1 Detach the manifold tubing from the manifold fitting that is connected to Port 3 at the

injection valve. Leave the piece of tubing attached to the injection valve. 1.2 Disconnect the carrier pump tube from Port 2 of the injection valve. Take this tubing and

connect it to the manifold fitting that was connected to Port 3. 1.3 Detach output of the manifold from union on the flow cell tubing leave the union

connected to the flow cell 1.4 Remove the back pressure loop, if necessary 1.5 Detach heating unit tubing from the manifold, and reconnect to the union underneath the

manifold (650 cm side.) 1.6 Remove all manifold pump tubes from cartridges. 1.7 Remove the interface filter from the detector module 1.8 Remove the sample loop from Port 1 & 4 valve 1.9 Remove manifold from the Sample Processing Module (Channel) 1.10 Carefully wrap the transmission lines around the manifold and store it in the plastic

bubble bag.




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Appendix F – Maintenance Schedule All listed maintenance is performed as needed. Following is a checklist of items along with the maintenance that may need to be performed. It is the instrument analyst’s responsibility to check the condition of the instrument daily and perform any necessary maintenance to insure the instrument is operating correctly. AutoSampler Clean Surfaces AutoDilutor Clean Surfaces Prime dilutor with reagent water after using any other diluent Pump Clean Surfaces Rinse cartridges Detector Dry and clean all Surfaces System Unit Keep Dry and Clean Injection Valves Clean Ports and valve connections Autosampler Clean rods/ moving parts Pump Replace pump tubes as needed Clean pump tube adapters Manifold Clean union and tee as needed Injection valves Replace o-rings Manifold Replace o-rings Manifold Check all tubing and replace as needed Flow Cells Check and replace flares and o-rings as needed Computer Clean hard drive


SOP 4420 Automated Nitrate/Nitrite Analysis Revision 00

Effective Date: December 23, 2008 Page 2 of 25

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Table of Contents Title Page 1 Table of Contents 2 1. Identification of Test Methods 3 2. Applicable Matrix or Matrices 3 3. Detection Limits 3 4. Scope and Application 3 5. Summary of Test Method 3 6. Definitions 3 7. Interferences 4 8. Safety 4 9. Equipment and Supplies 4 10. Reagents and Standards 5 11. Sample Collection, Preservation, Shipment and Storage 6 12. Quality Control 6 13. Calibration and Standardization 8 14. Procedure 10 15. Data Reduction, Calculations and Loading 13 16. Method Performance 13 17. Pollution Prevention 14 18. Data Assessment and Criteria for Qua lity Control Measures 14 19. Corrective Actions for Out-Of-Control Data 15 20. Contingencies for Handling Out-Of-Control Or Unacceptable Data 15 21. Waste Management 16 22. References 16 23. Forms, Figures, Tables, Diagrams, Flowcharts, Attachments or Validation Data 16 APPENDIX A TROUBLESHOOTING 17 APPENDIX B CREATING A METHOD 18 APPENDIX C DQM PLAN 20 APPENDIX D MANIFOLD DIAGRAM 22 APPENDIX E MANIFOLD INSTALLATION/REMOVAL 23 APPENDIX F MAINTENANCE SCHEDULE 25




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1.0 Identification of Test Method SOP Title: Automated NO3/NO2, NO2 AND NO3 Analysis by SM 4500-NO3 I

2.0 Applicable Matrix or Matrices This method is used to determine the concentration of Nitrate/Nitrite as – mg N/L in aqueous samples, soils, wastes, and leachates. The lab follows the procedure found in 40CFR Part 136B to determine the MDL for each matrix type on an annual basis. See the STAT Analysis SOP 1210 for the MDL procedure, frequency and acceptance criteria. The MDLs measured by the lab and all supporting documentation is in the laboratory QA files for review. 3.0 Detection Limits The laboratory determined MDL must always be less than the reporting limit (RL). The RL will usually range from three to ten times the laboratory measured MDL but this relationship may vary dependent on dilution of sample aliquots, matrix interferences, or method-specified requirements.

The applicable range for aqueous samples is 0.2 - 20 mg N/L. The MDL for NO2 is 0.0321 mg N/L. The MDL of NO3 is 0.0857 mg N/L. The reporting limit for NO2 and NO3 is 0.2 mg N/L. 4.0 Scope and Application The method is designed for the analysis of aqueous samples. This method is restricted to use by or under the supervision of analysts experienced in the use of the Lachat Auto Analyzer. Note: Each analyst must demonstrate the ability to generate acceptable results with this method. 5.0 Summary of Method Nitrate is quantitatively reduced to nitrite by passage of the sample through a copperized cadmium column. Nitrite is determined by diazotizing with sulfanilamide followed by coupling with N-(1-naphthyl) ethylenediamine dihydrochoride. Absorbance of the color at 520 nm is proportional to the nitrate+nitrite in the sample. Nitrite alone can be determined by turning off the cadmium column. Nitrate is determined by subtracting nitrite results from nitrate plus nitrite results. Method Modifications from Reference Degassing to remove air bubbles is performed only if it is noticed that there are air spikes during analysis. 6.0 Definitions The STAT Analysis Corporation Quality Assurance Manual (QAM) contains the definitions of standard terms used in this SOP.




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7.0 Interferences

7.1 Residual chlorine can interfere by oxidizing the cadmium reduction column. Samples that contain large concentrations of oil and grease will coat the surface of the cadmium.

7.2 Sample turbidity may interfere. Turbidity can be removed by filtration through a 0.45 pore diameter membrane filter prior to analysis.

7.3 Low results can be obtained for samples that contain high concentration of iron and copper.

8.0 Safety


8.2 Safety glasses, gloves, lab coats and closed toe shoes are to be worn. 8.3 Other safety precautions must be conducted in accordance with the Chemical Hygiene Plan.

Other actions can also be applied if deemed necessary. A reference file of material safety data sheets (MSDS) is available in the laboratory for personnel involved in an analysis using chemicals.

8.4 The toxicity or carcinogenicity of each reagent used in this method has not been fully established. Each chemical should be regarded as a potential health hazard and exposure should be as low as reasonably achievable. Cautions are included for materials known to be extremely hazardous.

8.5 The following chemicals have the potential to be highly toxic or hazardous, for detailed explanation consults the MSDS.

Cadmium granules Ammonium hydroxide Sodium hydroxide Phosphoric acid Sulfanilamide 9.0 Equipment and Supplies

9.1 LaCHAT AutoAnalyzer consisting of the following components: 9.1.1 Autosampler Cetac 9.1.2 Reagent Pump 9.1.3 System Unit Lachat 8000 9.1.4 Computer 9.1.5 Printer

9.2 Centrifuge Tubes, 50 mL graduated 9.3 Volumetric Flasks, Class A: 1000mL, 250mL, 100mL, 50mL, 25mL with stoppers 9.4 Autopipetter: 0.010 to 0.10 mL, 0.10 to 1.0 mL, 1.0 to 5.0 mL

9.5 Test Tubes, 15 mL and Tube Racks 9.6 Plastic and glass bottles for solution storage




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10.0 Reagents and Standards The following reagents and standards are required to perform this procedure. When instructions are given on how to prepare a specific volume of a reagent or standard, larger or smaller volumes can be prepared as needed so long as the final concentrations remain the same. Any other deviations from the reagents or standards listed in this SOP could be detrimental to the quality of the data produced. Such deviations would have to be approved and documented (see 230 Corrective Action SOP).

10.1 Instructions for labeling and record keeping of reagents and standards are contained in SOP 1010 Standard and Reagent Preparation.

10.2 Reagents - In methods where the purity of reagents is not specified, analytical reagent grade

shall be used. Reagents of lesser purity than those specified by the test method shall not be used.

10.3 Use reagent water (1 Mohm) for all solutions. Degas reagents with helium if necessary to

prevent bubble formation.

10.4 Reagent 1. 15 N Sodium Hydroxide: Add 150 g NaOH very slowly to 250 ml of DI water. Cool and store in a plastic bottle.

10.5 Reagent 2 Sulfanilamide color reagent: In a 1 L volumetric flask add approximately 600

mL DI water, 100 mL 85% phosphoric acid, 40 g sulfanilamide, and 1.0 g N-(1-naphthyl) ethylenediamine dihydrochloride (NED). Dilute to the mark, and mix. Store in dark bottle. This solution is stable for one month.

10.6 Reagent 3. Ammonium Chloride Buffer: In a 1 liter volumetric flask dissolve 85.0 g ammonium chloride and 1.0 g Disodium Ethylenediamine Tetraacetate Dihydrate (Na2EDTA*2H2O) in about 800 ml water. Dilute to the mark and mix until dissolved. Adjust the pH to 8.5 with 15 N sodium hydroxide solution. This solution is stable for 6 month

10.7 Standards

10.7.1 At least one of the standards must be traceable to a NIST traceable source when available. The manufacturer should include a certificate of analysis for each standard. If one is not provided, contact the manufacturer. Retain all certificates in the designated binder (see SOP 1010 Reagent Receiving).

10.7.2 Standards must be prepared volumetrically using class A volumetric glassware, calibrated micropipettes, or gas tight syringes. Do not use disposable pipettes to prepare standards.

10.7.3 Nitrate Nitrogen Stock Calibration Standard: 1000 ppm NO3-N: Commercially Purchased. Store per manufacturer’s recommendations and shelf life. If shelf life is not stated, then this solution may be used for twelve months if stored in the original container at 0.1 - 6oC and shows no sign of deterioration.

10.7.4 Nitrite Nitrogen Stock Calibration Standard: 1000 ppm NO2-N: Commercially Purchased. Store per manufacturer’s recommendations and shelf life. If shelf life is not stated, then this solution may be used for twelve months if stored in the original container at 0.1 - 6oC and shows no sign of deterioration.

10.7.5 Nitrate Nitrogen Stock ICV/CCV Standard: 1000 ppm NO3-N: Commercially Purchased. Store per manufacturer’s recommendations and shelf life. If shelf life is




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not stated, then this solution may be used for twelve months if stored in the original container at 0.1 - 6oC and shows no sign of deterioration.

10.7.6 Nitrite Nitrogen Stock Calibration ICV/CCV Standard: 1000 ppm NO2-N: Commercially Purchased. Store per manufacturer’s recommendations and shelf life. If shelf life is not stated, then this solution may be used for twelve months if stored in the original container at 0.1 - 6oC and shows no sign of deterioration.

10.7.7 Working ICV STD, 5 ppm: Dilute 0.25 ml of Stock ICV/CCV STD to 50 ml DI. Prepare this solution fresh daily.

10.7.8 Working CCV STD, 10 ppm: Dilute 0.5 ml of Stock ICV/CCV STD to 50 ml with DI. Prepare this solution fresh daily.

10.7.8.1For LCS, 0.5 mL of 1000 ppm, dilute 0.5 mL of 1000mg/L in 50 mL of reagent water.

10.7.8.2For MS/MSD, dilute 0.5 of 1000 ppm in 50 mL of sample. 10.7.9 The Calibration Standards are prepared according to Table 1 below. Add listed

volumes of the Stock Calibration Standard to each flask, and dilute to mark with DI. Cap and mix will.

Table 1 Nitrate/Nitrite Calibration Standards

Calibration Standard Concentration, mg/L

Amount of Stock Calibration

Standard mL

Concentration of Stock Calibration Standard, mg/L

Final Volume, mL

20 1.0 1000 50 10 0.5 1000 50 5 0.25

1000 50

1 0.05 1000 50 .4 0.02 1000 50 .2 0.01 1000 50 0 0 0 50

11.0 Sample Collection, Shipment, Preservation and Storage Samples shall be placed on ice immediately after collection. The holding time is 28 days for a refrigerated sample (0.1 - 6oC) for total nitrate/nitrite with proper chemical preservation (pH < 4). The holding time for nitrate or nitrite is 48 hours from time of collection. 12.0 Quality Control The following details the QC requirements that apply to this analysis. Each Quality Control Indicator (QCI) provides information pertaining to either method or individual sample performance. Our goal is to produce defensible data of known and documented quality. The results of these QCI samples are used to assess the acceptability of data.




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12.1 Blanks

Method Blank analysis is performed to determine if any contamination is present in the analytical process and is used to evaluate acceptance of the batch of samples. A method blank shall be prepared once per preparation batch of 20 or less samples per matrix type (see Section 6 for definition of a prep batch). If more than 20 samples are prepared a second blank shall be prepared after the twentieth sample. The method blank shall be processed through all preparatory steps used for the samples, including cleanup procedures. The blank shall be analyzed using the same instrument and conditions as the samples.

12.2 Laboratory Control Sample (LCS)

The LCS is used to evaluate the performance of the total analytical system, including all preparation and analysis steps. The LCS shall be prepared once per preparation batch of 20 or less samples per matrix type. If more than 20 samples are prepared a second LCS shall be prepared after the twentieth sample. The LCS shall be processed through all preparatory steps used for the samples, including cleanup procedures. The LCS shall be analyzed using the same instrument and conditions as the samples.

12.3 Duplicates

Duplicates of field samples or of the LCS must be prepared in compliance with the method requirements and client directives. Note: The analysis of the Matrix Spike Duplicate (MSD) is used as a substitute for the laboratory duplicate. In those cases when there is insufficient sample to perform either a duplicate analysis or MSD analysis, the duplicate analysis of the LCS (LCS/LCSD) is used to judge the precision of the analytical results.

12.4 Matrix Spike and Matrix Spike Duplicate (MS/MSD)

MS/MSDs indicate the effect of the sample matrix on the precision and accuracy of the results generated using the selected method. This information does not determine the validity of the entire batch. MS/MSDs must be analyzed at a minimum of 1 per 20 samples per matrix per preparation procedure, or as specified by the required test method. If an MS/MSD pair is not analyzed in the preparation batch, an LCS/LCSD pair is analyzed.

Samples chosen for matrix spiking are rotated among different clients and/or different client projects. This is accomplished through communication between the Department Manager and the analyst. In addition, designated samples, as indicated by client request or contract requirement, are matrix spiked.

The MS/MSD pair shall be processed through all preparatory steps used for the samples. They shall be analyzed using the same instrument and conditions as the samples.




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13.0 Calibration and Standardization Initial Calibration (ICAL) In addition to achieving the reference method requirements for the minimum number of calibration standards and the acceptance criteria (statistics) for calibration curve fit, the following ICAL criteria also apply:

13.1 The ICAL must be a minimum of 5 standards, not including a blank. 13.2 The ICAL must be verified with a second source standard (ICV) prior to the analysis of

samples. 13.3 Results of samples not bracketed by the ICAL range must be qualified on the final report. If

possible, dilute the sample or extract and reana lyze in order to achieve a result within the calibrated range of the instrument.

13.4 The lowest calibration standard may establish the reporting limit: RL = 0.2mg/L. The RL

must be greater than or equal to the detection limit. 13.5 Samples must be quantitated from the initial calibration curve and may not be quantitated

from any instrument CCV. Initial Calibration Verification (ICV) In addition to the method requirements, the following ICV criteria also apply:

13.6 Must be a second source standard from the ICAL standards or from a different manufacturer lot number.

13.7 Must be traceable to NIST when available.

13.8 Must be analyzed when an ICAL is not performed on the day of analysis, prior to sample

analysis. Continuing Calibration Verification (CCV) In addition to the method requirements, the following CCV criteria also apply:

13.9 May be analyzed at the beginning of the batch to check the CCV recovery. 13.10 Must be analyzed after every 10 samples and at the end of each analytical batch. 13.11 If the CCV results obtained are outside the acceptance criteria, corrective actions must be

performed. If routine corrective actions fail to produce an acceptable second consecutive (immediate) CCV, then either the lab has to demonstrate performance after corrective action with two consecutive successful CCVs, or a new ICAL must be performed. If the instrument has not demonstrated acceptable performance, sample analyses cannot continue until a new




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ICAL is established and verified with an ICV. However, sample data associated with an unacceptable CCV may be reported as qualified data under the following special conditions:

13.11.1 When the acceptance criteria for CCV are exceeded high, i.e., high bias, and there are

associated samples that are non-detects, then those non-detects may be reported. Otherwise the samples affected by the unacceptable calibration verification must be reanalyzed after a new ICAL has been established, evaluated and accepted.

13.11.2 When the acceptance criteria for the CCV are exceeded low, i.e., low bias, those

sample results may be reported if they exceed a maximum regulatory limit/decision level. Otherwise the samples affected by the unacceptable verification must be reanalyzed after a new ICAL is established and verified with an ICV.

13.11.3 When the acceptance criteria for the CCV are exceeded and it is not possible to

reanalyze the sample due to limited sample quantity AND a new sample cannot be obtained by the laboratory, the data may be reported with the appropriate data qualifiers if the client has been contacted and agrees, in writing, to accept the qualified data.

13.12 Records: Initial and Continuing Calibration Records will contain, at a minimum, the

following:

1. Calibration date 2. Test method 3. Instrument 4. Analysis date 5. Each analyte name 6. Analyst's initials or signature 7. Standard Concentration (appropriate units) and number of standards 8. Response (appropriate units) 9. Calibration curve or response factor 10. Evaluation of and Statistics for ICAL curve fit in order to judge calibration curve

acceptance 11. Evaluation of and Acceptance Limits for ICV analysis in order to judge calibration curve

acceptance 12. Evaluation of and Acceptance Limits for CCV analysis in order to judge continuing

calibration acceptance 13. Calibration Standards and Reagent Solutions IDs




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Calibration Acceptance Summary:

Table 2 Calibration Requirements

QCI Frequency Standards Control Limits Corrective Action ICAL Daily or as needed, Minimum 5 standards,

see Table 1 for concentrations

r = 0.995 Correct problem then repeat initial calibration

ICV After each new ICAL And at the beginning of each analytical run.

5.0 mg/L ± 10% of true value Correct problem then repeat initial calibration

CCV Beginning (optional), every 10 samples, and end of the batch

10.0 mg/L ± 10% of true value Correct problem then repeat CCV or repeat initial calibration

ICB After ICV Reagent water <RL Correct problem then repeat CCV or repeat initial calibration

CCB After CCV Reagent water <RL Correct problem then repeat CCV or repeat initial calibration

Support Equipment Autopipettes - Check autopipette to ensure standardization is within control limits (see SOP 1040 for Pipette Calibration). Balances - Be sure the balance is checked prior to use and performance criteria are met (see SOP 1040 for Calibration of Balances). 14.0 Procedure

14.1 Instrument Start Up

14.1.1 Turn on the power to all modules by turning on the power strip and allow the autosampler to perform its startup routine. Wait until the autosampler stops with the probe above the wash bath.

14.1.2 If necessary, install the manifold on the channel you want to run. (See Appendix E.) 14.1.3 Make all the injection fluidic connections. 14.1.4 Make all the cell fluidic connections. 14.1.5 Set all pump tubes on the pump. (Varies method to method.) 14.1.6 Run reagent water through all the lines to make sure there are no leaks. 14.1.7 If there are no leaks, put actual reagents in line. 14.1.8 ALWAYS start pumping Buffer Solution FIRST. 14.1.9 Pour the calibration Standards into Standard vials, and place into the autosampler

Standards Rack. 14.1.10 Pour the Samples into test tubes and place into the Sample Rack. 14.1.11 If necessary, insert the interference filter into the upper slot in the detector.

14.2 Software Set up




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14.2.1 Double click on the Omnion FIA icon. Then click OK. The autosampler probe should go into the wash bath and the dilutor activity may be heard, the injection valves may turn to the inject state if they were not already there.

14.2.2 Log In with your user name and password. [User name: demo with no password will also get you in]. The Main Menu should appear.

14.2.3 From the Main Menu click on the Instrument button labeled FIA Instrume nt 1. Each valve allocated to this instrument will be cycled in turn from Load to Inject and back to Inject again. Omnion will automatically open the last Method and Tray that was used. (The names will appear at the top in the title bar.)

14.3 Open the Nitrate/Nitrite Method (To Create a Method see Appendix B)

14.3.1 Click on the Method button, or from the Main Menu click on File , then Open Method.

This will open the Open Method Dialog window. 14.3.2 Double click on the method file you want to open: Nitrite/Nitrate me t. or click once

then click on OK. 14.3.3 From the Main Menu click on the Instrument button labeled FIA Instrument 1. Each

valve allocated to this instrument will be cycled in turn from Load to Inject and back to Inject again. Omnion will automatically open the last Method and Tray that was used. (The names will appear at the top in the title bar.)

14.4 Opening and Editing the TRAY

14.4.1 Click on the Tray button or from the Main Menu, click on File, then Open Tray. 14.4.2 Click twice on the name of the tray you wish to open. Nitrate/Nitrite) The First rows of

the tray spreadsheet are blue. This denotes that these samples are actually Calibration Standards. This is from the method and will not change. The Sample Type is Cal Std. And the Level is NEVER 0, it will be a number from 1 to 14 (This will match the level in the Analyte Table in the method.) The Cup Number (Cup #) refers to the cup number in the Standard Rack and will be a number between 1 and 14.

14.4.3 Edit the Sample ID. Using the mouse, move the pointer to the cell and click once; type in the new ID. In the Sample Rack Loading Aid (Top Left) the sample cup you are editing will be in green.)

14.4.4 The Cup Numbers (Cup #) for sample will be anything between 1 to 90. 14.4.5 The Level column is 0 for all samples of Sample Type Unknown 14.4.6 The Reps for samples and standards is 1 or 2. 14.4.7 To Schedule manual QC See Appendix C (DQM Plan)

14.5 Click on the Run Tray button. (Or from the Main Menu, click on Tray then Run Tray.)

14.5.1 Leave the Method and Tray boxes empty to use the ones that are active (open). 14.5.2 In the Data File box enter the name for your run. i.e. 981006Ca. YYMMDD C (for

Calibration) and a (for number of the run... a b c...) The extension *.fdt (FIA Data) is used by default.

14.5.3 The Autosampler Position refers to the autosampler sample rack position; 1, 2 or 3. 14.5.4 Skip Recalibration Block Box can be checked when you want to run a tray that

contains Cal standards and samples but you want only want to run samples 14.5.5 While the tray is processing, you can view the peaks and runtime report. 14.5.6 If the baseline does not appear on the screen change Display options. 14.5.7 Click Method, then Display Options




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14.5.8 Specify the channel: 1. 14.5.9 Specify the voltage scale on the Y axis (i.e. -1 to 3). 14.5.10 Click OK.

14.6 Analyze samples for Total Nitrate/Nitrite by turning flow to the cadmium column on.

Analyze samples for Nitrite by turning cadmium column off. Click on the RUN button. The tray will start running. After the pump is allowed to pump at a normal speed for the period specified it the method, pump timing, the autosampler will move to the first calibration standard. The Standards and samples are done in Row order(on the computer screen), no matter where they are located on the autosampler tray.

14.7 While running you will see a STOP sign on the tool bar. To suspend the tray click on the

STOP sign. The Tray will pause and the computer gives you the choices of aborting or resuming the tray. At the end of the tray, after the last sample ID entered is reported, the sample probe should return to the rinse position and the STOP button will turn back into the RUN button.

Note : Cadmium Column always should be filled with buffer solution. Run buffer solution before turning off column, and after turning on column.

14.8 System Shutdown Procedure

14.8.1 Remove the reagent transmission lines and place into the rinse solution and pump for 5

minutes at standard speed. 14.8.2 Place the lines into reagent water and allow the system to rinse 5 to 10 minutes at

standard speed. 14.8.3 Remove the lines from the reagent water and allow all liquid to be pumped out of the

manifold. 14.8.4 Turn off the pump and release the pump tube cartridges tension. Press the tube cartridges

holders on the sides of the Isomatec pump. 14.8.5 Close all files 14.8.6 Switch off the master power strip

14.9 Documentation requirements. Record the following information in the appropriate logbook or

data file. Include any deviations from this procedure.

14.9.2 Analyst initials, date [and time if required by the specific project or QAPP] of analysis, sample number or ID, initial sample volume or weight processed, final digestate volume, calibration standard sample or solution identifier, QC sample or solution identifier, reagent solutions identifiers, any dilution information, [beginning and ending times of analytical steps if required by the specific project or QAPP], data file name or batch ID, instrument method name, visual observations, and any other information as deemed necessary

14.9.3 Print out a copy of the calibration curve used and datafile (run sequence).

14.10 Routine Maintenance – Record all maintenance in the logbook. See Appendix F




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15.0 Data Reduction, Calculations and Loading

15.1 The data system will then prepare a calibration curve by plotting response versus standard concentration. Sample concentration is calculated from the regression equation.

15.2 Report only those values that fall between the lowest and highest calibration standards.

Samples exceeding the highest standard must be diluted and reanalyzed or qualified.

15.3 Aqueous Samples: The concentration readout for aqueous samples is mg Nitrates/Nitrites as Nitrogen/L. It does not need further data reduction.

15.4 For sample results greater than the highest calibration standard, dilute the sample using DI to

bring within range.

15.5 The procedure for uploading data into the LIMS system is detailed in SOP 1400 LIMS.

15.6 Nitrite can be determined without cadmium column.

NO3/NO2 – NO2 = NO3 (Total – Nitrite = Nitrate) 16.0 Method Performance Demonstration of Capability (DOC) All parameters of interest must meet the method acceptance criteria before actual sample analysis begins. See SOP 1230 Training for the procedure to perform and document the DOC. The DOCs for the analysts performing this method are located in the analysts’ training form folders located in the QA office files. A quality control (QC) reference concentrate is required containing Nitrates/Nitrites at a concentration of 0.2 mg/L the Reporting level using the ICV/LCS solution. The QC reference sample is made using stock standards prepared independently from those used for calibration. For each analyte calculate the mean recovery (X) and standard deviation (s) and the average % Recovery (%R). Compare X and s and %R with the corresponding acceptance criteria for accuracy and precision, respectively. Note: For aqueous samples, X must be within 0.2 ± 0.04 mg/L and s must be less than 0.1mg/L and %R must be within 100 ± 20These limits are taken from established in-house criteria If X and s and %R for all analytes meet the acceptance criteria, the system performance is acceptable and analysis of actual samples can begin. If X or %R falls outside the range for accuracy, or s exceeds the precision limit, then the system performance is unacceptable for that analyte and corrective action must be taken. Comparison to Reference Method Data In-House Control Limits Method performance data is on file in the laboratory QC department. Comparison of method performance data for the laboratory to the reference method criteria occurs when laboratory in-house acceptance limits are generated. In-house generated data is compared to the specifications of the




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reference method. If the in-house limits are within the specifications of the reference method, the control limits are updated in LIMS. If the in-house limits are not within specifications, an investigation is performed to determine the cause(s) of the problem and a corrective action is completed. The analysis may continue until enough data points are collected to regenerate new control limits. Any QC data generated outside of reference method limits during that time frame is flagged. The laboratory maintains performance records to document the quality of data that is generated. Method accuracy for samples is assessed and records maintained. 17.0 Pollution Prevention The preparation of excessive volumes of laboratory reagents and standards shall be avoided so that waste and potential for pollution are minimized. Samples, reagents and standards shall be disposed in compliance with the laboratory waste disposal program and applicable waste disposal regulations. With the consent of the client, the samples may be returned to their origin for treatment.

Uncontaminated paper waste, glass and cans should be separated for recycling. Laboratory staff are required to protect the laboratory’s and our clients’ business information when disposing of recycling or waste from the facility. 18.0 Data Assessment and Criteria for Quality Control Measures The laboratory maintains records to document the quality of data that is generated. Ongoing quality checks are compared with established performance criteria to determine if the results of analyses meet the performance characteristics of the method. The data review is conducted according to SOP 1250 Data Review. Method Blank (MB) If the blank exceeds the RL (the lowest calibration standard), the source of contamination must be investigated and corrective actions taken.

Affected samples must be reprocessed and reanalyzed or Data must be appropriately qualified if:

1) The concentration of a targeted analyte in the blank is at or above the reporting limit as

established by the SOP or by regulation, AND is greater than 1/10 of the amount measured in any sample.

2) The blank contamination otherwise affects the sample results as per the test method

requirements or the individual project data quality objectives. Laboratory Control Sample (LCS) The results of the individual batch LCS are calculated in percent recovery (%R) and compared to established acceptance criteria (in-house limits). LCS %R limits are 100 ± 20%. If the LCS is outside the acceptance criteria, the analytical system is “out of control”. Any affected samples associated with an out




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of control LCS must be reprocessed and reanalyzed or the results reported with appropriate data qualifiers. Matrix Spikes The results from MS/MSD are primarily designed to assess the precision and accuracy of analytical results in a given matrix and are expressed as percent recovery (%R) and relative percent difference (RPD). See the STAT QAM, Section 5.4 for the calculation for RPD. Results are compared to established acceptance criteria (in-house limits). For aqueous samples, MS/MSD %R limits are 100 ± 25% and RPD limits are 20%. For soil samples, MS/MSD %R limits are 100 ± 25% and RPD limits are 20%. For matrix spike results outside established criteria corrective action must be documented, or the data for the spiked sample is reported with appropriate data qualifying codes. Duplicates The results from laboratory Duplicates are designed to assess the precision of analytical results in a given matrix and are expressed as relative percent difference (RPD). See the STAT QAM, Section 5.4 for the calculation for RPD. Results are compared to established acceptance criteria (in-house limits). RPD limits are 20%. For duplicates results outside established criteria corrective action must be documented or the data for the duplicate sample is reported with appropriate data qualifying codes.

19.0 Corrective Actions for Out-of-Control Data The process for handling corrective actions is found in SOP 230 Corrective Action. If the CCV, MB, LCS/LCSD, MS/MSD, or lab duplicate recovery of any parameter falls outside the designated acceptance range, the laboratory performance for that parameter is judged to be out of control, and the problem must be immediately identified and corrected. The analytical result for that parameter in the samples is suspect and is only reported for regulatory compliance purposes with the appropriate corrective action form. Immediate corrective action includes reanalyzing all affected samples by using any retained sample before the expiration of the holding time. Final data results must be qualified in the client report for reported results not meeting the laboratory-defined criteria.

1) Review standards preparation logbooks. Check all calculations and ensure dilution factors are properly recorded.

2) Re-prepare the suspected standard or QC sample to identify possible preparation errors of the

standard or QC sample.

3) Re-Analyze the samples when the CCV or LCS is not within acceptable limits.

4) Perform routine preventative maintenance following manufacturer's specification. Record all maintenance in the instrument logbook.

20.0 Contingencies for Handling Out-of-Control Or Unacceptable Data Every effort is made to prevent problems from occurring. When out of control or unacceptable data occurs the first option is to identify the problem and reanalyze the samples within the holding times.




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When this is not possible, the QA Manager and/or the Laboratory Director reviews data and discuss options with the client. Reanalysis or reporting the data with qualification is alternatives. Out of control or unacceptable data reported to the client must include the data qualifier, flag and discussion on the rationale for reporting.

The process for handling unacceptable and out of control data is found in section 11 of the Laboratory QAM. The reporting of data that is out of control must be approved and documented by Quality Assurance Manager and either the Technical Manager or the Laboratory Director.

21.0 Waste Management The STAT Analysis Corporation SOP 1130 Waste Disposal identifies proper waste management practices for the chemicals and biological materials used in this procedure. Samples are stored and discarded accordance with SOP 1130 Waste Disposal. 22.0 References

22.1 Method EPA 4500-NO3 I, U.S. EPA. Standard Methods for the Examination of Water and Wastewater (20th Edition).

22.2 Determination of Total Recoverable Nitrates/Nitrites by Flow Injection Analysis. QuikChem Method 10-107-04-1-A

22.3 . 22.1 STAT SOP 1040 General Laboratory Procedures 22.2 STAT SOP 1020 Glassware Cleaning 22.3 STAT SOP 1010 Standard and Reagent Preparation 22.4 STAT SOP 1000 Control and Use of Laboratory Notebooks 22.5 STAT SOP 230 Corrective Actions 22.6 STAT SOP 1400 LIMS 22.7 STAT SOP 1130 Waste Disposal 22.8 STAT SOP 003 Chemical Hygiene Plan 22.9 STAT SOP 1250 Data Review 22.10 STAT SOP 1230 Training 22.11 STAT SOP 1210 Method Detection Limits (MDLs) 22.12 STAT Analysis Corporation Quality Assurance Manual 22.13 QuikChem 8000 Automated Ion Analyzer Omnion FIA Software. 22.14 QuikChem 8000 Automated Ion Analyzer Continuum Series “Flow Injection Analyzer”

Hardware Installation and System Operation. 23.0 Forms, Figures, Tables, Diagrams, Flowcharts, Attachments or

Validation Data

23.1 Appendix A Troubleshooting 23.2 Appendix B Creating a Method 23.3 Appendix C DQM Plan 23.4 Appendix D Manifold Diagram 23.5 Appendix E Manifold Installation/ Removal 23.6 Appendix F Maintenance Schedule




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Appendix A – Trouble Shooting

Keep all modules clean and dry at all times.

Routine Maintenance (See Appendix F for the Maintenance Schedule) Pump

n After each day rinse the cartridges in reagent Water to wash any spills. Clean pump surfaces, except rollers, with a wet cloth. Dry all surfaces

n If rusty clean rollers with steel wool. A light coat of silicon spray can be applied by spraying on a lint free cloth and holding it to the moving rollers

n Check for wear, cracks or acid damage on the cartridges ad holders n Replace pump tubes that start to show signs of wear n If the pump tubes burst, clean all cartridges and holders, as well as, the pump,

immediately. n All surfaces should be kept clean. Use a damp cloth to clean the module surfaces.

Dry surfaces thoroughly. Valve Modules n Keep the instrument clean and dry at all times. n Replace o-rings once per month n When changing the o-rings, clean the valve ports with cotton swab and reagent water.

This will help remove any dirt or precipitate that may prevent a good seal. If a leak persists, replace the new o-rings and make sure the connector itself does not have precipitate on the thread.

n All surfaces should be kept clean. Use a damp cloth to clean the module surfaces. Dry all surfaces thoroughly.

n The internal sample loop valve will give thousands of injections without trouble. The rotor seal wears with use and is the only part that needs routine replacement.

Detector Modules and Flow Cell n If a flow cell appears to leak remove it immediately to keep all liquid form the

electronics inside the detector head. Instrument Troubleshooting

For problems with the instrument see the QuikChem 8000 Automated Ion Analyzer Continuum Series “Flow Injection Analyzer” Hardware Installation and System Operation Manual under the Troubleshooting Section.




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Appendix B – Creating A Method 1.1 Click on the Method button, or from the Main Menu click on File, then New Method. 1.2 Then Method will open and you will see the Analyte Table 1.3 Click on Analyte Name of channel and press backspace to delete. Enter the new analyte

name. If an analyte name is not present the system will ignore that channel. 1.4 Fill out the analyte Table. Channel 1 Analyte Name Nitrates/Nitrites mg/L 1.3 From the Main Menu, click on Method, then Valve Timing 1.4 Enter the Method Cycle Period. 60s 1.5 Sample Reaches the first valve 18s (For Standard Pump Sample Assembly) (travel

time from sample probe to port 6 usually 24 s if dilutor enter 28s) 1.6 Load Period 15s Load Time 0s Inject Period 45s Notice that Load Period + Injection Period = Cycle Period 1.7 Click OK 1.8 From the Main Menu, click on Method, then Sampler Timing. 1.9 The Sample Prep Sequence box is optional 1.10 Enter the Minimum Probe in Wash Period 5.0 s 1.11 Enter the Probe in Sample Period 24s 1.12 Click OK. 1.13 From the Main Menu, click on Method, then Pump Timing 1.14 Check the Go to Standby on Idle box X 1.15 Enter Idle Before Standby 180.0s 1.16 Enter At Speed Before Analysis 45.0s 1.17 Click OK. 1.16 From the Main Menu, click on File, then Save Method As 1.17 The FIA Method File Header will appear. Write a method description (analyte and

sample loop size) and click OK. (i.e. Ammonia Sample Loop XXX cm) 1.18 The Method Save As dialog box will appear. 1.19 C:\ Omnion\Methods\

Change the name to Ammonia.met II To Fine Tune the Method 1.0 After you have run a data. 1.1 Open a file from the main menu click on File, Open Data. and click twice on the Data file

name. i.e. 981006Ca.fdt.




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1.2 Load the original method form this data by clicking on the Data menu the Load Method. 1.3 You should see the peaks on the screen. 1.4 Click on Data then Reanalyze Data. (Or click on the Reanalyze button.) 2.0 Fine Tuning the Threshold 2.1 Look before and after the tray to see some baseline. 2.2 From the menu click on Method, then Graphical Events Programming... 2.3 Click on Threshold. 2.4 The Status bar will prompt you to “Select Start of Baseline Section”. 2.5 Set the cursor at the beginning of the baseline region and click once. 2.6 You will be prompted to “Select End of Baseline Section”. 2.7 Move the mouse pointer to the end of the baseline region and click again. 2.8 Omnion calculates a Threshold value. 2.9 Click on OK to enter the value in the Analyte Table of your method 3.0 Fine Tuning the Peak Base Width 3.1 From the menu click on Method, then Graphical Events Programming... 3.2 Click on Peak Base Width. 3.3 You will be prompted to “Select Start of Peak” 3.4 Set the cursor at the beginning of the high standard and click once. 3.5 You will be prompted to “Select End of Peak” 3.6 Move the cursor to the end of the peak and click again. 3.7 Omnion calculates a Peak Base Width. 3.8 Click on OK to enter the value in the Analyte Table of your method 4.0 Save these new method parameters by clicking on File, then Save Method As. 5.0 Viewing a Method’s Calibration 5.1 Up to 4 replicates of each Standard can be applied to a method’s calibration. 5.2 If not already open, load the method form the data file by clicking on Data, Load Method. 5.3 Click on the button. (or from the main menu click on Method, then Review Analyte

Calibration Curve. The Review Analyte Calibration window will appear. 5.4 Click Fit, then Clear. to ‘Clear’ the Calibration Replicate Table. 5.5 Click Exit. 5.6 Click the Analyze button. The re-analysis occurs exactly as it did in the actual tray run. 5.7 Click on the Review Calibration button again to see the curve. 6.0 Editing the Calibration 6.1 Clicking twice on any of the results in the calibration replicate Table will turn it red and

make it unused in the calibration. 6.2 To Use the point again, click twice on it again, and it will turn form red back to blue.




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Appendix C – DQM Plan DQM Plan

Consists of one or several DQM Sets. Each Set has one or more samples. The DQM has 3 sections; the DQM Set box, the DQM Sample Box, and the Channel Data box.

1.0 Adding DQM Sets 1.1 Click Tray, then Load DQM. 1.2 In the DQM Set Box click on the drop-down button showing the DQM Set ID, type in a

new name. (Check Standards, Duplicates, Matrix Spikes) 1.3 For the Check Standards Set check the Automatic box X. 1.4 Click ADD to add the set. NOTE: Automatic Sets never have their sample info in the tray table and the samples are loaded in the standards rack. Manual sets have their sample info in the tray table and the samples are loaded in the sample rack. 2.0 Adding DQM Samples 2.1 In the DQM Sample Box, click on the drop-down button showing the DQM Sample ID

and type in a new name (ICB, ICV, CCV, CCB, Method Blank, Dup 1, Spike, Spike Dup)

2.2 Click on the Append button. 2.3 Replicates should be 2 2.4 Click on the drop-down button showing the Type and select the type of sample. (Blank,

Unspiked, Spiked, AbsChkStd, RelChkStd, Dup 1, Dup 2) 2.5 For the Automatic Check Samples enter the Standard Rack Cup. 3.0 Editing Channel Data information. 3.1 In the Channel Data Box, select the appropriate channel. 3.2 If you can’t see the Test 1 row, click on the Add Test button. 3.3 The Test Explanation spells out the test that will be done for this DQM Sample and

depends on what Type the DQM Sample is. 3.4 If the standard has a known concentration it needs to be entered in the Known Conc box

along with the Conc Units. 3.5 Enter the Test Limit. 10.000% difference. 3.6 Select a Fail Action from the drop-down menu. Recalibrate & Repeat, Alarm &

message . 3.7 Enter the Pass/ Fail Message. NOTE: A Test Passes if test value < = Test Limit A Test Fails if Test value > Test Limit 3.8 You can perform more then 1 test on each check sample. 4.0 Scheduling Automatic DQM Sets 4.1 From the Main Menu, click on Tray, then Auto DQM Schedule 4.2 Select the Auto DQM Set from the drop-down menu. 4.3 Check the box (es) for the frequency of the sample 4.4 Click OK.




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5.0 Inserting Manual DQM Sets 5.1 Click on the Tray Table button. 5.2 Click on the row number before which you want to insert the check sample. 5.3 From the Main Menu, click on Tray, then Manual DQM Insertion. 5.4 Click on the Manual DQM Set you wish to insert. 5.5 Enter the Sample ID’s of the DQM samples to reflect the actual identity of the samples.

(Note: The manual DQM sample rows are green.) 5.6 Renumber the Cup Numbers (Cup #) below the inserted Manual DQM Set by clicking

and dragging all the rows and cup numbers you wish to renumber. 5.7 Click on Tray, then Renumber Cups (or Ctrl-R) 5.8 Enter the Starting Number 5.9 Enter an Increment of 1. 5.10 Then click OK. 6.0 Calibration Pass/Fail Criteria 6.1 From the Main Menu, click on Method, then Calibration Failure Criteria 6.2 Select the appropriate channel. 6.3 Check the Minimum Correlation Coefficient (R2) Box and enter 0.995 6.4 Check the Maximum % Residual All Levels Box, and enter 10.0. 6.5 If the calibration passes, a message will be reported and the tray will continue to the nest

row. 6.6 If the calibration fails, a fail message will be reported and you will be given a choice to

Abort or continue the tray. 7.0 Save the DQM Plan 7.1 From the Main Menu, click File, then Save DQM Plan, or Save DQM Plan As... and

enter the File name Ammonia.dqm. The default extension is *.dqm.


SOP 4250 Automated Ammonia Analysis Revision 00

Effective Date: March 1, 2004 Page 22 of 25

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Appendix D – Manifold Diagram




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Appendix E – Manifold Installation/Removal Manifold Installation Procedure 1.0 Unwrap the transmission lines from around the manifold and place the manifold over the

sample processing module. 1.1 Remove the transmission lines from the union on the 650 cm side of the heating unit,

insert both ends through the hole in the manifold and reseat the manifold onto the sample processing module.

1.2 Make the Injection Valve Connections as follows: 1.3 Port 1 & 4 - The Sample Loop 0.8 mm i.d. length 75 cm. 1.4 Port 2 - Carrier line is connected to Port 2 -> from valve, disconnect from

Fitting and connect to port 2 0.8 mm id and 30 cm long. 1.4 Port 3 - 20 cm 0.8 mm id between port 3 and the fitting on the manifold

next to the label -> from valve where the carrier line was connected. 1.5 Port 5 - 15 cm 0.8 mm is between port 5 and the waste line. 1.6 Port 6 - Sample Line. 130 cm (Varies method to method) connected to the

probe on the autosampler, pump tube adapter, and 20 cm tubing connected to port 6 of valve.

2.0 Flow Cell Top tubing connected to waste line. Bottom line connected to the fitting in the manifold next to the label to flow cell ->. Attach one of the lines from the heater to the union going to the flow cell. Attach the other heater line to the pyridine-Barb. Acid Tee fitting.

3.0 Pump 3.1 Sample Line - Autosampler to injection valve 6. 3.2 Wash Line - Reagent water to wash reservoir on the autosampler 3.3 Reagents Lines- Varies from method to method sees Ammonia diagram. 3.4 On the Ismatec Pump Cartridges the arrows point towards the System Unit with the

tension lever on the left. 3.5 Place all of the reagents lines into corresponding containers or Reagent water. 3.6 Move tension levers to the maximum tension (Top Far Right Position) 3.7 Clamp down all pump tube cartridges. (Press down one side at a time.) 3.8 Move tension lever back from the top far right until it makes a clicking sound. 3.9 Set the reagent pump speed to 35. 3.10 Turn on the pump. 3.11 Depress the green button to turn the pump ON. The System Unit will take control over

the pump speed. (The yellow button is the override standby button.) 3.12 Check to confirm that the probe wash reservoir is filing with rinse water. 3.13 Check for Leaks on the manifold, valve, flow cell or any of the connections. 3.14 Do NOT leave any pump tubes clamped down when the pump is shut off for more then a

few minutes. 3.15 To Remove cartridges, Press the sides of the pump holder on which the cartridge is

engaged. 4.0 Insert the interface filter into the detector module.




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Manifold Removal Procedure 1.0 Rinse the manifold 1.1 Detach the manifold tubing from the manifold fitting that is connected to Port 3 at the

injection valve. Leave the piece of tubing attached to the injection valve. 1.2 Disconnect the carrier pump tube from Port 2 of the injection valve. Take this tubing and

connect it to the manifold fitting that was connected to Port 3. 1.3 Detach output of the manifold from union on the flow cell tubing leave the union

connected to the flow cell 1.4 Remove the back pressure loop, if necessary 1.5 Detach heating unit tubing from the manifold, and reconnect to the union underneath the

manifold (650 cm side.) 1.6 Remove all manifold pump tubes from cartridges. 1.7 Remove the interface filter from the detector module 1.8 Remove the sample loop from Port 1 & 4 valve 1.9 Remove manifold from the Sample Processing Module (Channel) 1.10 Carefully wrap the transmission lines around the manifold and store it in the plastic

bubble bag.




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Appendix F – Maintenance Schedule All listed maintenance is performed as needed. Following is a checklist of items along with the maintenance that may need to be performed. It is the instrument analyst’s responsibility to check the condition of the instrument daily and perform any necessary maintenance to insure the instrument is operating correctly. AutoSampler Clean Surfaces AutoDilutor Clean Surfaces Prime dilutor with reagent water after using any other diluent Pump Clean Surfaces Rinse cartridges Detector Dry and clean all Surfaces System Unit Keep Dry and Clean Injection Valves Clean Ports and valve connections Autosampler Clean rods/ moving parts Pump Replace pump tubes as needed Clean pump tube adapters Manifold Clean union and tee as needed Injection valves Replace o-rings Manifold Replace o-rings Manifold Check all tubing and replace as needed Flow Cells Check and replace flares and o-rings as needed Computer Clean hard drive


SOP Title: TDS, TSS, TS Revision 00


\\Harrison\d\Quality Control\Quality Manual & SOPs\4000 Anaytical SOPs\SOP 4482\SOP4482 Percent Moisture.doc

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Table of Contents Title Page 1 Table of Contents 2 1. Identification of Test Methods 3 2. Applicable Matrix or Matrices 3 3. Detection Limits 3 4. Scope and Application 3 5. Summary of Test Method 3 6. Definitions 4 7. Interferences 4 8. Safety 5 9. Equipment and Supplies 5 10. Reagents and Standards 6 11. Sample Collection, Preservation, Shipment and Storage 6 12. Quality Control 6 13. Calibration and Standardization 7 14. Procedure 7 15. Data Reduction, Calculations and Loading 9 16. Method Performance 10 17. Pollution Prevention 11 18. Data Assessment and Criteria for Quality Control Measures 11 19. Corrective Actions for Out-Of-Control Data 12 20. Contingencies for Handling Out-Of-Control Or Unacceptable Data 12 21. Waste Management 13 22. References 13 23. Forms, Figures, Tables, Diagrams, Flowcharts, Attachments or Validation Data 13





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1.0 Identification of Test Method

SOP Title: Total Dissolved Solids(TDS), Total Suspended Solids(TSS), and Total Solids(TS) 2.0 Applicable Matrix or Matrices This method is applicable to the following matrices: drinking water, surface and saline water, solid, and multiphasic wastes.

3.0 Detection Limits

The applicable range for Total Suspended Solids (TSS) is 4 to 20,000 mg/L. The Method Detection Limit for TSS is 3.8 mg/L. The reporting limit for TSS is 8 mg/L.

The applicable range for Total Dissolved Solids (TDS) and Total Solids (TS) is 12 to 20,000 mg/L. The Method Detection Limit for TDS and TS is 3.1 mg/L. The reporting limit for TDS and TS is 6 mg/L.

The Method Detection Limits for Volatile solids (VS) and fixed solids (FS) have not been determined at this time.

4.0 Scope and Application

4.1 Solid analyses are important in the control of wastewater treatment processes. 4.2 Total Suspended Solids can include various materials including industrial wastes,

sewage, etc. and is often used to measure turbidity in water. 4.3 Total Dissolved Solids is used to estimate the quality of drinking water because it

represents the amount of dissolved ions in water. 4.4 Total Volatile Solids are those solids lost on ignition (heating to 550oC.) They are useful

because they give a rough approximation of the amount of organic matter present in the solid fraction of wastewater, activated sludge and industrial wastes

NOTE: Each analyst must demonstrate the ability to generate acceptable results with this method.

5.0 Summary of Test Method

5.1 Total Suspended Solids

The sample is shaken and filtered through a preweighed 1.5 micron glass filter, which is dried to a constant weight in an oven at 103-105oC. The trapped solids and filter are cooled in a desiccator, weighed, and calculations perform for TSS.





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5.2 Total Dissolved Solids The sample is shaken and filtered through a 1.5-micron glass filter. The filtrate is collected in a preweighed beaker. It is dried to a constant weight in an oven at 180 + 2oC, then cool to room temperature, weighed, and calculations perform for TDS.

5.3 Total Solids

The sample is shaken and poured through an evaporating dish and dried to a constant weight after oven drying at 103-105oC, cooled in a dessicator and weighed.

5.4 Method modifications from Reference –

Duplicate samples must be within 10% (5% - 2540C)

6.0 Definitions

The STAT Analysis Corporation Quality Assurance Manual (QAM) contains the definitions of standard terms used in this SOP.

Preparation batch - composed of one to 20 environmental samples of the same NELAC-defined matrix, meeting the above-mentioned criteria and with a maximum time between the start of processing of the first and last sample in the batch to be 24 hours (NELAC).

Analytical batch - composed of prepared environmental samples (extracts, digestates or concentrates) that are analyzed together as a group. An analytical batch can include prepared samples originating from various environmental matrices and can exceed 20 samples (NELAC).

Total Suspended Solids (TSS)-solids that are trapped by a filter, expressed as mg/L (also known as filterable residue)

Total Dissolved Solids (TDS) - (also known as non-filterable residue) -solids remaining after evaporation of a sample that has been passed through a filter, expressed as mg/L

Total Solids (TS) - (also known as Total Residue) –After oven drying at 103-105oC, expressed as mg/L

Fixed Solids (FS) – solids remaining from TSS after ignition at 550 oC, expressed as mg/L

Volatile Solids (VS) – solids lost after ignit ion at 550 oC, expressed as mg/L

7.0 Interferences

7.1 Highly mineralized waters with large amounts of calcium, magnesium, chloride and/or sulfate may be hygroscopic and require longer drying, desiccation, and rapid weighing.

7.2 Samples high in bicarbonate require a longer drying time at 180oC (for TDS) to insure

complete conversion of bicarbonate to carbonate.





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7.3 Too much residue in the aluminum dish can reduce the amount of water that can be evaporated during drying. Samples containing high amounts of minerals and other hygroscopic materials may require a smaller sample size to help insure removal of all moisture.

8.0 Safety


8.2 Safety glasses, gloves, lab coats and closed toe shoes are to be worn. 8.3 Other safety precautions must be conducted in accordance with the Chemical Hygiene

Plan. Other actions can also be applied if deemed necessary. A reference file of material safety data sheets (MSDS) is available in each room for personnel involved in an analysis using chemicals.

8.4 The toxicity or carcinogenicity of each reagent used in this method has not been fully

established. Each chemical should be regarded as a potential health hazard and exposure should be as low as reasonably achievable. Cautions are included for known extremely hazardous materials.

8.5 A reference file of material safety data sheets (MSDS) is available in the lab for personnel involved in any analysis using chemicals.

9.0 Equipment and Supplies

The following apparatus is recommended for performing this procedure. Equivalent items can be used, if with their use, the analytical and QA/QC requirements in this SOP can be met.

9.1 Whatman filters – AH 934 55mm, porosity: fine(1.5 microns) glass fiber filters

9.2 Disposable aluminum dishes – 75mm diameter

9.3 Porcelain crucibles – (31 x 26 mm) diameter x height (mL 10) and (35 x 29) (mL 15)

9.4 Oven for operation to 100 ± 5oC and 180 ± 5oC 9.5 Muffle furnace for operation up to 550 oC

9.6 250 mL, 500mL, and 1000mL graduated cylinders (Pyrex)

9.7 Forceps

9.8 Filter flask - 250 mL, 500mL

9.9 Analytical balance capable of weighing to + 0.0001g.





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9.10 Desiccant Blue (97% CaSO4 and 3% CoCl2) and white (100% CaSO4) A mixture of 10% blue and 90% white should be used in the desiccator. When the desiccant turns from blue to pink (indicating water absorption), heat in an oven at 180 oC overnight to drive off moisture.

9.11 Desiccator

9.12 Buchner funnels w/rubber stoppers-56mm (top diameter) 42mm (perforated diameter)

9.13 150, 250, 400 mL glass beakers (Pyrex)

9.14 Thermometer (-10oC to 260oC)

9.15 Steam bath

10.0 Reagents and Standards 10.1 Deionized water – ASTM type 2 reagent grade water

10.2 Sodium Chloride – (reagent grade) Dry in an oven at 180oC for 1 hour and store in a

tightly sealed container in a dessicator. Shelf life is 5 years.

10.3 Diatomaceous Earth (DE) - Dry in an oven at 180oC for 1 hour and store in a tightly sealed container in a dessicator. Shelf life is 5 years.

10.4 Stock solution for Laboratory Control Sample (LCS) for TDS/TSS /TS– Weigh out 2

grams of DE and 1 grams of sodium chloride. Add to 1000 ml of reagent water, mix well and store in a plastic bottle at room temperature. Shelf life is one year. T.V. for TSS is 2,000 mg/L and TDS is 1,000 mg/L.

11.0 Sample Collection, Preservation and Handling

Samples should be analyzed as soon as possible. No preservation is needed. Samples must be analyzed within seven days from the time of collection. Store at 0.1 – 6 oC until analysis.

12.0 Quality Control

12.1 Method Blank A Method Blank analysis is performed to determine if any contamination is present in the analytical process and is used to evaluate acceptance of the batch of samples. A Method Blank must be processed through the same conditions as the associated samples for TSS and TDS using reagent water. The Method Blank is of a similar matrix (e.g. reagent water) and is free of analytes of interest.





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12.2 Laboratory Control Sample (LCS) - The LCS is used to evaluate the performance of the total analytical system, including all preparation and analysis steps. The LCS is a controlled matrix (e.g., reagent water, Ottawa sand, glass beads, etc.), known to be free of analytes of interest, spiked with known and verified concentrations of analytes. Alternatively the LCS may consist of a media containing known and verified concentrations of analytes or as Certified Reference Material (CRM). All LCS analyte concentrations must be within the calibration range. The LCS must be analyzed at a minimum of once per preparation batch.

12.3 Duplicates - Duplicates are defined as replicate aliquots of the same sample taken

through the entire analytical procedure. The result from this analysis is an indication of the precision of the analytical method. The duplicate provides a usable measure of precision only when target analytes are found in the sample chosen for duplication. Duplicates are performed on replicate aliquots of actual samples. The duplicate analysis must be analyzed at a frequency of at least once per 20 samples per preparation batch.

12.4 MS/MSDs are not applicable to this method.

13.0 Calibration and Standardization

13.1 Balances need to be checked daily with the appropriate weights prior to use (refer to SOP 1040 General Laboratory Practices).

13.2 Thermometers - Check thermometers to ensure the calibration is not expired (refer to SOP 1040 General Laboratory Practices for Thermometer Calibration).

14.0 Procedure Analysis for all procedures should be done on a well-mixed sample. Remove any large objects or paper from the aliquot being used for the test. Note in the logbook that large objects were not included in the analysis. If analysis is requested by the customer on the complete sample, large object(s) must be cut or crushed to a small size in order to be included with the rest of the sample. Check with the Project Management or the Department Manager when testing any samples, which require processing as above.

Note: Always use clean forceps to transfer the filter.

14.1 Total Suspended Solids (TSS)

Filter Conditioning

14.1 Set up filtraton apparatus. Place the filter in the Buchner funnel, wet with reagent

water and apply vacuum. Pre-wash the filter with three 20 ml portions of reagent water and discard. When all water has been vacuumed through the filters, place the filters on aluminum weighing dishes in a 103° -105°C oven for 20 minutes to dry. (If volatile suspended solids are to be analyzed, move the dry filters into a preheated





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550°C muffle furnace for 15 minutes); if the volatile portion does not need to be determined, place the filters and aluminum weighing dishes into a desiccator to cool and skip to step 3.

14.2 Remove the filters and aluminum weighing dish from the muffle furnace and place

on a clean heat resistant surface. Allow to cool for one minute before placing in the desiccator.

14.3 Cool the filters to ambient temperature in the desiccator before use. Washed filters

and aluminum weighing dishes should be stored in a desiccator. 14.4 Record in the logbook the weight of a preconditioned filter and aluminum dish. Set

up the filtration unit. Using tweezers, transfer the filter to the buchner funnel. Wet the filter with reagent grade water and turn on the vacuum to seal the filter.

14.5 Shake the sample and pour 200 mL of sample into a 250 mL graduated cylinder

(note: For TSS, a different sample size may be used as long as the total amount of residue on the filter paper does not exceed 200 mgs). For the Method Blank analysis use at least as much reagent water as the volume in the samples.

14.6 Filter the sample and wash the filter paper and graduated cylinder with three

successive 10 mL volumes of reagent water. Wash the sides of the funnel to transfer all solids onto the filter paper. Continue the vacuum filtration until all the liquid has passed through and the filter appears dry. (Keep the filtrate if TDS is needed.)

14.7 Remove the filter and place on the aluminum dish. Dry at 103-105oC for at least 1

hour. Cool in a desiccator and record the weight in the logbook.

Note: The final weight should not be more than 200mg. If greater than this restart with a smaller sample size. 14.8 Place the filter and aluminum dish in the oven. Dry at 103-105oC for 15 minutes.

Cool in a desiccator and record the weight in the logbook.

14.9 Repeat this procedure until the change in the weight of the residue remains within 4% or less than 0.5 mg from one weighing to the next. (This is referred to as constant weight.)

Total Dissolved Solids (TDS)

14.10 Heat a clean glass beaker for one hour at 180 + 2oC in an oven. 14.11 Cool slightly and store in a desiccator until needed. 14.12 Weigh the beaker immediately prior to use. 14.13 Perform Step 14.1 14.14 Perform step 14.6 to obtain the filtrate. 14.15 Pour the filtrate into the beaker and rinse the filter flask three times with reagent

water.





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14.16 Place the beaker in the oven at 180 + 2oC. Evaporate to dryness for at least 1 hour.

14.17 Cool slightly and store in a desiccator until ambient temperature is reached. Record the weight in the logbook.

14.18 Repeat steps 14.15 and 14.16 until the change in the weight of the residue remains within 4% or less than 0.5 mg from one weighing to the next.

Total Solids (TS) 14.19 If volatile solids are to be measured ignite clean aluminum evaporating dish at 550 oC

for 1 hour in a muffle furnace. If only total solids are to be measured, heat a clean dish to 103-105 oC for one hour. Store cooled dish in dessicator. Weigh immediately before use.

14.20 Choose a sample volume that will yield a residue between 2.5 and 200 mg. Stir sample with magnetic stir bar and pipette a measured volume from the middle of the sample, but off center from the vortex to a preweigh dish. Evaporate to dryness in a drying oven. If necessary add successive sample portions to the same dish after evaporation and dry in oven. Oven temperature may need to be lowered to prevent boiling and splattering of sample during drying.

14.21 Dry for at least one hour at 103-105 oC. Cool dish and dessicate to ambient temperature. Record the weight and place in oven for 15 minutes. Remove, cool and dessicate. Reweigh and repeat drying until a constant weight is achieved.

Volatile Solids (VS)/ Fixed Solids (FS) 14.18 Record the weight of the dried filter, residue and aluminum dish from step 14.9 or

14.20 and place in a preheated muffle furnace at 550oC for 15 minutes. 14.19 Remove and let filter and aluminum dish cool partially in air until most of the heat

has been dissipated (about one minute). (Alternately place in oven at 105oC for at least 5 minutes).

14.20 Transfer to a desiccator for final cooling. Do not overload desiccator. Weigh the filter and aluminum dish as soon as it has cooled to ambient temperature.

14.21 Repeat cycle of igniting, cooling, desiccating, and weighing until a constant weight is obtained or until weight change is le ss than 4% or 0.5 mg, whichever is less.

15.0 Data Reduction, Calculations, and Loading

15.1 TSS as mg/L = (A-B) x 1000/ sample volume L

Where A = weight of filter and dish + residue in grams B = weight of filter and dish in grams

15.2 TDS as mg/L = (A-B) x 1000/sample volume L

Where A = weight of beaker + filtrate in grams B = weight of the beaker in grams





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15.3 Total Volatile Solids = (A-B) x 1000/ sample volume L

A = weight of residue + dish before ignition in grams B = weight of residue + dish or filter after ignition in grams

15.4 Total Fixed Solids = (B-C) x 1000/ sample volume L

B = weight of residue + dish or filter after ignition in grams C= weight of dish or filter in grams

The procedure for uploading data into the LIMS system is detailed in SOP 1400 LIMS. 16.0 Method Performance

All parameters of interest must meet the method acceptance criteria before actual sample analysis begins. See SOP 1230 Training for the procedure to perform and document the DOC. The DOCs for the analysts performing this method are located in the analysts’ training form folders located in the QA office files. A quality control (QC) reference concentrate is required for each procedure using the LCS Analyze four aliquots for TDS using the LCS standard stock. Dilute 24 mL of LCS stock to 1000mL with reagent water. Calculate the mean recovery (X) and standard deviation (s) and the average % Recovery (%R). Compare X and s and %R with the corresponding acceptance criteria for accuracy and precision, respectively. Note: X must be within 24 ± 4.8 mg/L and s must be less than 4.8 mg/L and %R must be within 100 ± 20%. Analyze four aliquots for TSS and using the LCS standard stock. Dilute 4 mL of LCS stock to 500mL with reagent water for each TSS aliquot. Calculate the mean recovery (X) and standard deviation (s) and the average % Recovery (%R). Compare X and s and %R with the corresponding acceptance criteria for accuracy and precision, respectively. Note: X must be within 16 ± 3.2 mg/L and s must be less than 3.2 mg/L and %R must be within 100 ± 20%. Analyze four aliquots for TS using the LCS standard stock. Dilute 48 mL of LCS stock to 1000mL with reagent water for each TS aliquot. Calculate the mean recovery (X) and standard deviation (s) and the average % Recovery (%R). Compare X and s and %R with the corresponding acceptance criteria for accuracy and precision, respectively. Note: X must be within 72 ± 7.2 mg/L and s must be less than 7.2 mg/L and %R must be within 100 ± 20% These limits are taken from established in-house criteria. If X and s and %R for all analytes meet the acceptance criteria, the system performance is acceptable and analysis of actual samples can begin. If any individual X or %R falls outside the range for accuracy, or any





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individual s exceeds the precision limit, then the system performance is unacceptable for that analyte and corrective action must be taken.

17.0 Pollution Prevention

Samples shall be disposed in compliance with the lab waste disposal program and applicable waste disposal regulations.

18.0 Data Assessment and Criteria for Quality Control Measures The laboratory must maintain records to document the quality of data that is generated. Ongoing data quality checks are compared with established performance criteria to determine if the results of analyses meet the performance characteristics of the method. When results of QC samples indicate atypical method performance, a calibration verification standard is used to confirm the measurements were performed in an in-control mode of operation. The data review is conducted according to SOP 1250 Data Review. Method Blank (MB) If the blank exceeds the RL (usually the lowest calibration standard), the source of contamination must be investigated and corrective actions taken.

Affected samples must be reprocessed and reanalyzed or Data must be appropriately qualified if:

1) The concentration of a targeted analyte in the blank is at or above the reporting limit as

established by the SOP or by regulation, AND is greater than 1/10 of the amount measured in any sample.

2) The blank contamination otherwise affects the sample results as per the test method requirements

or the individual project data quality objectives. Laboratory Control Sample (LCS) The results of the individual batch LCS are calculated in percent recovery (%R) and compared to established acceptance criteria (in-house limits). LCS %R limits are 100 ± 20% for both aqueous and soil samples. If the LCS is outside the acceptance criteria, the analytical system is “out of control”. Any affected samples associated with an out of control LCS must be reprocessed and reanalyzed or the results reported with appropriate data qualifiers. Matrix Spikes Not needed for these methods. Duplicates The results from laboratory Duplicates are designed to assess the precision of analytical results in a given matrix and are expressed as relative percent difference (RPD). See the STAT QAM, Section 5.4 for the





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calculation for RPD. Results are compared to established acceptance criteria (in-house limits). RPD limits are 20 %. For duplicates results outside established criteria corrective action must be documented, or the data for the duplicate sample is reported with appropriate data qualifying codes.

19.0 Corrective Actions for Out of Control Data The process for handling out of control data is found in SOP 230 Corrective Action.

If the Method Blank, LCS, or lab duplicate of any parameter falls outside the designated acceptance range, the laboratory performance for that parameter is judged to be out of control, and the problem must be immediately identified and corrected. The analytical result for that parameter in the samples is suspect and is only reported for regulatory compliance purposes with the appropriate corrective action form. Immediate corrective action includes reanalyzing all affected samples by using any retained sample before the expiration of the holding time. Final data results must be qualified in the client report for reported results not meeting the laboratory-defined criteria.

1) Review standards preparation logbooks. Check all calculations and ensure dilution factors are properly recorded.

2) Re-prepare the suspected standard or QC sample to identify possible preparation errors of the standard or QC sample.

3) Re-Analyze the samples when the LCS or Duplicate is not within acceptable limits. 4) Perform routine preventative maintenance following manufacturer’s specification.

Record all maintenance in the instrument logbook.

20.0 Contingencies for Handling Out-of-Control or Unacceptable Data Every effort is made to prevent problems from occurring. When out of control or unacceptable data occurs the first option is to identify the problem and reanalyze the samples within the holding times. When this is not possible, the QA Manager and/or the Laboratory Director review the data and discuss options with the client. Reanalysis or reporting the data with qualifications is an alternative. Out of control or unacceptable data reported to the client must include the data qualifier, flag and discussion on the rationale for reporting.

Holding time exceedance, or improper preservation are noted on the corrective action form and included on the final report.

20.1 The process for handling unacceptable and out of control data is found in the Laboratory QAM Section 11. The reporting of data that is out of control must be approved and documented by the Quality Assurance Manager and either the Technical Manager or the Laboratory Director.

20.2 Client Requested Modifications:

20.2.1 Clients must request modifications from the laboratory SOP in writing to the lab.

20.2.2 The Laboratory Director, Technical Manager and Quality Assurance Manager

will evaluate the requested client deviations; determine the feasibility of the deviation and the potential effects on the data.





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20.2.3 If it is determined that the laboratory will perform the requested deviations, the

Laboratory Director, Technical Manager and Quality Assurance Manager will decide if a method validation study is required.

20.2.4 The designated project manager will retain all documentation concerning the

requested deviation, including all correspondence with the client, in the client folder.

20.2.5 The final analytical report must include the statement “This report has analyses performed using client requested modifications”.

21.0 Waste Management The STAT Analysis Corporation SOP 1130 Waste Disposal identifies proper waste management practices for the chemicals and biological materials used in this procedure. Samples are stored and discarded accordance with SOP 1130 Waste Disposal.

.

22.0 References

22.1 Standard Test Methods for Moisture, Ash, and Organic Matter of Peat and Other Organic Soils, ASTM D 2974-87 (1987).

22.2 Standard Methods for the Examination of Water and Wastewater, 20th Edition (1998).

22.3 Methods for Chemical Analysis of Water and Wastewater, U.S. Environmental Protection Agency, EPA methods 160.1, 160.2, 160.3, 160.4

22.4 STAT SOP 1000 Control and Use of Laboratory Notebooks 22.5 SOP 1400 LIMS 22.6 STAT SOP 1210 Method Detection Limits (MDLs) 22.7 SOP 1040 General Laboratory Practices 22.8 STAT SOP 1020 Glassware Cleaning 22.9 STAT SOP 1250 Data Review 22.10 SOP 230 Corrective Actions 22.11 SOP 1130 Waste Disposal 22.12 SOP 1230 Training 22.13 SOP 003 Chemical Hygiene Plan 22.14 SOP 1010 Standard and Reagent Preparation 22.15 STAT Analysis Corporation Quality Assurance Manual

23. Forms, Figures, Tables, Diagrams, Flowcharts, Attachments or

Validation Data

None.

Impellers specifications› Regular size windspeed impeller: ø 20 mm, hole diameter ø 33 mm. Minimum sensitivity: < 3km/h - < 1m/s Precision : +/-2% ‘‘off-axis’’ error: +/-30° / +/-3% Operating temperature : -50°C to +100°C› Small size windspeed impeller: ø 12 mm, hole diameter ø 18 mm. Minimum sensitivity: < 3km/h - < 1m/s Precision: +/-2% ‘‘off-axis’’ error: +/-10° / +/-3% Withstood temperature: -50°C to +100°C› Water impeller: ø 60 mm Minimum sensitivity: < 0.3km/h - < 0.1m/s Precision: +/-2% ‘‘off-axis’’ error: +/-20° / +/-3%

Technical data› Sealed and weatherproof instrument› Thread on the bottom of the instrument for fixing to a tripod (1/4’’)› Speed resolution : 0.1 for all units (except in cm/s: 3cm/s)› Maximum speed: 150 km/h (except in cm/s: 999cm/s)› Thermometer precision : +/- 0.2°C› Thermometer resolution : 0.1°C› Power supply : 2 batteries, 1.5V AA Battery lifetime, at least 3 years with occasional use of the display backlight. To replace, loosen the three screws on the metal plate.› Weight : 210 grams (insubmersible)› Dimensions : ø66 X 137 mm› Warranty : 1 year› All cable are in PUR

WarrantyYour instrument has a one year warranty, against material or manufacturing defects, from JDC ELECTRONIC SA starting from the date of pur-chase. The warranty does not cover damage caused by incorrect use.The speed measuring principle of is based on the detection of a rotating magnetic field produced by an impeller. If the device is subject to a strong magnetic field produced by a transformer or motor, it may happen that the instrument shows undesirable values, without any rotation from the impeller.

More information is available on our website under www.jdc.ch.

Vous venez d’acquérir un appareil de haute précision, réalisé avec les technologies les plus modernes. Il a été conçu pour résister à un usage intensif. Cependant et afin de conserver son aspect et sa précision, nous vous recommandons de le traiter avec soin et de lire attenti-vement ce mode d’emploi.

Le système se compose au minimum de:› 1 boîtier d’affichage› 1 sonde› 1 hélice

Fonction des boutonsON : pression pendant 1s OFF : pression pendant 2s (non auto off)LIGHT : courte pression on et off UP : mode réglageSTART / STOP : mode chronomètreDOWN : mode réglageLAP / RESET : mode chronomètreSET / CAL : mode réglageRESET MEMORY : pression pendant 3s

ConfigurationPour entrer dans le mode configuration de votre appareil, il suffit de presser sur le bouton . Lorsqu’on presse une nouvelle fois sur le bouton , le système valide le réglage s’il y a eu une modification, sinon il passe au ré-glage suivant. Pour modifier les réglages, il faut utiliser les boutons et . Voici la manière de procéder pour les différents réglages de l’appareil.Unité de mesure de la vitesse des fluides et des gaz Les unités sélectionnables sont : knots, mph, km/h, m/s, fps, mph et cm/s. Une fois l’unité choisie, celle-ci reste affichée en haut à droite. Lorsqu’aucune unité n’est affi-chée, l’appareil se trouve en mode cm/s.Unité de mesure de la température Les unités sélectionnables sont : °F, °C, °F et °C .Réglage du temps de la moyenneLes temps sélectionnables sont : --- (pondération), 3’’, 6’’, 12’’, 30’’, 1’, 6’, 30’, 1:00’, 6:00’, 12:00’, 24:00’ ou Timer .Le mode Timer permet de mesurer la moyenne sur une durée définie entre un start (presser ) et un stop (pres-ser ), ce temps est affiché sur la ligne inférieure. Ce Timer permet également d’utiliser la fonction LapTime (presser , le symbole clignote). Le bouton per-met aussi de faire une mise à zéro du Timer. Celui-ci fonctionne de la même manière qu’un chronomètre standard.Réglage de l’affichage de la vitesse et de la températureLes affichages sélectionnables sont :---,MIN,AV,MAX.Lorsqu’on sélectionne AV, il s’agit de la moyenne pour la température et pour le vent. L’affichage des valeurs moyennes se fait toujours simultanément pour la vi-tesse (au milieu) et pour la température (en bas). Les autres modes (---,MIN,MAX) concernent uniquement la température.

Le réglage de l’affichage n’est pas disponible si l’unité sélectionnée est °F ou °C .Mesure de la vitesse d’écoulement d’un fluideVitesse instantanée (en haut) Vitesse maximum (au milieu)L’affichage de la vitesse maximale se fait sur la partie centrale. Il s’agit de la valeur maximale mesurée sur la durée de la moyenne. La valeur est mise à zéro lors d’un RESET de la mémoire.Vitesse moyenne (au milieu si le mode AV est sélectionné)

Mesure de la températureLe capteur de température est intégré à l’extremité de la sonde.Température instantanéeImportant : l’inertie thermique de la sonde agit directe-ment sur le temps de stabilisation de la mesure. Plus la différence de température est importante, plus ce temps sera long dans l’air.Pour la mesure dans l’eau, le temps de réaction sera très court.Température ressentieComme vous le savez certainement, les basses températures sont dangereuses pour le corps humain. Mais saviez-vous que le vent influence fortement les températu-res ressenties réellement par votre corps ? Par exemple, une température ambiante de 0°C et un vent de 30 km/h agissent comme une température de -13°C ! Le résultat du calcul de l’effet du vent sur la température s’appelle «température ressentie».Le vous calcule instantanément la température ressentie.Température minimumTempérature maximumDans ces deux modes, il s’agit de la valeur minimale ou maximale mesurée sur la durée de la moyenne. La valeur est mise à zéro lors d’un RESET de la mémoire. Ces valeurs ne sont pas données pour la température ressentie.Caractéristiques des sondesDisponible en 2 longueurs différentes, ces sondes sont indispensables pour y fixer des hélices de mesures.› Tige en aluminium télescopique, d’une longueur totale e 1,2 mètres pour mesurer dans les tubes de ventilation difficiles d’accès ou de grand diamètre, dans des rivières ou canalisations.› Tige en aluminium, longueur 10 cm. Pour transformer votre en anémomètre compact (s’utilise surtout avec les hélices pour gaz ø 20mm et ø 12mm)› Sonde avec hélice lestée à l’extrémité d’un câble de 15 mètres pour les mesures depuis une structure sur plombant la rivière.

' ''

You have just acquired a piece of high precision equi-pment which has been created using the most modern technology. It has been designed to stand up to inten-sive use. However, in order to maintain its appearance and its precision, we recommend that you treat it with care and read this manual carefully.

To work properly, the system has to include at least:

› 1 display unit› 1 probe› 1 impeller

Function of the buttonsON : press for 1 second OFF : press for 2 seconds (not auto off)LIGHT : press on and off brieflyUP : setting modeSTART / STOP : chronometer modeDOWN : setting modeLAP / RESET : chronometer modeSET / CAL : setting modeRESET MEMORY : press for 3 seconds

ConfigurationTo access the configuration mode of your instrument, just press on the button. Pressing the button once again cause the system to confirm the setting if there has been a change. If not then it goes to the next set-ting. To modify the settings the and buttons have to be used. Here is how to proceed with the different instrument settings.Speed measuring unit The units to be selected are : knots, mph, km/h, m/s, fps and cm/s. Once the unit is chosen, it remains displayed in the top right. If no other unit is chosen the instrument is set to the cm/s.Temperature measurement unit The units to be selected are : °F, °C, °F and °C .Setting the time of the average The times to be selected are : --- (weighting), 3’’, 6’’, 12’’, 30’’, 1’, 6’, 30’, 1:00’, 6:00’, 12:00’, 24:00’ or timer .The timer mode allows measurement of the average between start (press ) and stop (press ), this time is displayed on the lower lines. This timer allows the use of the LapTime function (press , the symbol flashes). The button also allows the timer to be re-set to zero. This works in the same way as a standard chronometer.Setting of the speed and temperature displays The displays to be selected are : ---, MIN, AV, MAX.If AV is selected, the average of temperature and wind are shown. The display of average values is always made simultaneously for the speed (at the centre) and temperature (at the bottom). The other modes (---, MIN, MAX) only concern the temperature.Setting of the display is not possible if the units selected are °F or °C .

Measuring air or liquid flowsInstantaneous speed (at the top) Maximum speed (at the centre)The display of the maximum speed is made at the central part. It is the maximum measured value of the time of the average. The value is reset to zero during a RESET of the memory.Average speed (at the center if AV is selected)

Measuring the temperature The temperature sensor is on the end of each probe.Instantaneous temperatureImportant : Thermal inertia of the instrument directly affects the stabilization time of the measurement. The greater the temperature difference, is the longer this time will be. This time will be shorter if the wind speed is higher.Wind-chill temperatureAs you know, exposure to low temperatures is potentially dangerous to the human body. But did you know that wind plays a significant part in how your body actually feels temperatures? For example, an ambient temperature of 0°C and a 30 km/h wind have the same effect on you as a temperature of -13°C! The result of the calculation of the effect of wind on the temperature is called the “wind-chill temperature”. The shows immediately the wind-chill.Minimum temperatureMaximum temperatureThese two modes show the min or max values measured over time of the average. The value is reset to zero during a RESET of the memory. These values are not those of the temperature felt by the body.Probe specificationsAvailable in 2 different lengths, these 2 probes are es-sential to install any impeller.› Aluminium telescopic rod, total length of 1.2m with 2 meters cable to measure in hard-to-reach ventilation shafts, air conditioning conduits, rivers flows and irrigation canals.› Aluminium small rod, 10 cm long to use your as a compact windmeter (mostly used with windspeed impellers ø 20mm and ø 12mm)› Probe with a 15 meters sounding cable with water- flow impeller, to measure water flow from bridges.

' ''

Caractéristiques des hélices› Hélice taille standard : gaz ø 20 mm, trou de passage ø 33 mm. Sensibilité minimum : < 3km/h - < 1m/s Précision : +/-2% Erreur ‘‘off-axis’’ : +/-30° / +/-3% Température d’utilisation : -50°C à +100°C› Hélice petite taille : gaz ø 12 mm, trou de passage ø 18 mm. Sensibilité minimum : < 3km/h - < 1m/s Précision : +/-2% Erreur ‘‘off-axis’’ : +/-10° / +/-3% Température d’utilisation : -50°C à +100°C› Hélice eau : ø 60 mm Sensibilité minimum : < 0.3km/h - < 0.1m/s Précision : +/-2% Erreur ‘‘off-axis’’ : +/-20° / +/-3%

Données techniques› Appareil étanche et résistant aux intempéries›Filetage sous l’appareil permettant sa fixation sur un trépied (1/4’’)› Résolution de la vitesse: 0.1 pour toutes les unités (sauf cm/s: 3cm/s)› Vitesse maximale: 150km/h (sauf cm/s: 999cm/s)› Précision du thermomètre : +/- 0.2°C› Résolution du thermomètre : 0.1°C› Alimentation : 2 piles 1.5V AA Autonomie des piles, au minimum 3 ans avec un usage occasionnel de l’éclairage de l’affichage. Pour le changement, dévisser les trois vis de la plaque métallique.› Poids : 210 grammes (insubmersible)› Dimensions : ø66 X 137 mm› Garantie : 1 année› Tous les câbles sont en PUR

GarantieVotre instrument est garanti par JDC ELECTRONIC SA pendant une année à partir de la date d’achat contre tout défaut matériel ou de fabrication. Sont exclus de cette garantie les dommages causés par une utilisation inadéquate.Le principe de mesure de la vitesse du est basé sur la détection du champ magnétique tournant produit par l’hélice. Si l’appareil est en présence d’un fort champ magnétique produit par un transformateur ou un moteur, il se peut que l’instrument indique des va-leurs non désirées, en l’absence de rotation de l’hélice.

Vous trouverez encore plus d’informations sur notre site internet www.jdc.ch.

FREN

JDC Electronic SARue des Uttins 40

1400 Yverdon-les-BainsSwitzerland

Phone: +41 24 445 21 21Fax: +41 24 445 21 23

Email: [email protected]

Website : www.jdc.ch



Phone: +41 24 445 21 21Fax: +41 24 445 21 23



++

Impellers specifications› Regular size windspeed impeller: ø 20 mm, hole diameter ø 33 mm. Minimum sensitivity: < 3km/h - < 1m/s Precision : +/-2% ‘‘off-axis’’ error: +/-30° / +/-3% Operating temperature : -50°C to +100°C› Small size windspeed impeller: ø 12 mm, hole diameter ø 18 mm. Minimum sensitivity: < 3km/h - < 1m/s Precision: +/-2% ‘‘off-axis’’ error: +/-10° / +/-3% Withstood temperature: -50°C to +100°C› Water impeller: ø 60 mm Minimum sensitivity: < 0.3km/h - < 0.1m/s Precision: +/-2% ‘‘off-axis’’ error: +/-20° / +/-3%

Technical data› Sealed and weatherproof instrument› Thread on the bottom of the instrument for fixing to a tripod (1/4’’)› Speed resolution : 0.1 for all units (except in cm/s: 3cm/s)› Maximum speed: 150 km/h (except in cm/s: 999cm/s)› Thermometer precision : +/- 0.2°C› Thermometer resolution : 0.1°C› Power supply : 2 batteries, 1.5V AA Battery lifetime, at least 3 years with occasional use of the display backlight. To replace, loosen the three screws on the metal plate.› Weight : 210 grams (insubmersible)› Dimensions : ø66 X 137 mm› Warranty : 1 year› All cable are in PUR

WarrantyYour instrument has a one year warranty, against material or manufacturing defects, from JDC ELECTRONIC SA starting from the date of pur-chase. The warranty does not cover damage caused by incorrect use.The speed measuring principle of is based on the detection of a rotating magnetic field produced by an impeller. If the device is subject to a strong magnetic field produced by a transformer or motor, it may happen that the instrument shows undesirable values, without any rotation from the impeller.

More information is available on our website under www.jdc.ch.

Vous venez d’acquérir un appareil de haute précision, réalisé avec les technologies les plus modernes. Il a été conçu pour résister à un usage intensif. Cependant et afin de conserver son aspect et sa précision, nous vous recommandons de le traiter avec soin et de lire attenti-vement ce mode d’emploi.

Le système se compose au minimum de:› 1 boîtier d’affichage› 1 sonde› 1 hélice

Fonction des boutonsON : pression pendant 1s OFF : pression pendant 2s (non auto off)LIGHT : courte pression on et off UP : mode réglageSTART / STOP : mode chronomètreDOWN : mode réglageLAP / RESET : mode chronomètreSET / CAL : mode réglageRESET MEMORY : pression pendant 3s

ConfigurationPour entrer dans le mode configuration de votre appareil, il suffit de presser sur le bouton . Lorsqu’on presse une nouvelle fois sur le bouton , le système valide le réglage s’il y a eu une modification, sinon il passe au ré-glage suivant. Pour modifier les réglages, il faut utiliser les boutons et . Voici la manière de procéder pour les différents réglages de l’appareil.Unité de mesure de la vitesse des fluides et des gaz Les unités sélectionnables sont : knots, mph, km/h, m/s, fps, mph et cm/s. Une fois l’unité choisie, celle-ci reste affichée en haut à droite. Lorsqu’aucune unité n’est affi-chée, l’appareil se trouve en mode cm/s.Unité de mesure de la température Les unités sélectionnables sont : °F, °C, °F et °C .Réglage du temps de la moyenneLes temps sélectionnables sont : --- (pondération), 3’’, 6’’, 12’’, 30’’, 1’, 6’, 30’, 1:00’, 6:00’, 12:00’, 24:00’ ou Timer .Le mode Timer permet de mesurer la moyenne sur une durée définie entre un start (presser ) et un stop (pres-ser ), ce temps est affiché sur la ligne inférieure. Ce Timer permet également d’utiliser la fonction LapTime (presser , le symbole clignote). Le bouton per-met aussi de faire une mise à zéro du Timer. Celui-ci fonctionne de la même manière qu’un chronomètre standard.Réglage de l’affichage de la vitesse et de la températureLes affichages sélectionnables sont :---,MIN,AV,MAX.Lorsqu’on sélectionne AV, il s’agit de la moyenne pour la température et pour le vent. L’affichage des valeurs moyennes se fait toujours simultanément pour la vi-tesse (au milieu) et pour la température (en bas). Les autres modes (---,MIN,MAX) concernent uniquement la température.

Le réglage de l’affichage n’est pas disponible si l’unité sélectionnée est °F ou °C .Mesure de la vitesse d’écoulement d’un fluideVitesse instantanée (en haut) Vitesse maximum (au milieu)L’affichage de la vitesse maximale se fait sur la partie centrale. Il s’agit de la valeur maximale mesurée sur la durée de la moyenne. La valeur est mise à zéro lors d’un RESET de la mémoire.Vitesse moyenne (au milieu si le mode AV est sélectionné)

Mesure de la températureLe capteur de température est intégré à l’extremité de la sonde.Température instantanéeImportant : l’inertie thermique de la sonde agit directe-ment sur le temps de stabilisation de la mesure. Plus la différence de température est importante, plus ce temps sera long dans l’air.Pour la mesure dans l’eau, le temps de réaction sera très court.Température ressentieComme vous le savez certainement, les basses températures sont dangereuses pour le corps humain. Mais saviez-vous que le vent influence fortement les températu-res ressenties réellement par votre corps ? Par exemple, une température ambiante de 0°C et un vent de 30 km/h agissent comme une température de -13°C ! Le résultat du calcul de l’effet du vent sur la température s’appelle «température ressentie».Le vous calcule instantanément la température ressentie.Température minimumTempérature maximumDans ces deux modes, il s’agit de la valeur minimale ou maximale mesurée sur la durée de la moyenne. La valeur est mise à zéro lors d’un RESET de la mémoire. Ces valeurs ne sont pas données pour la température ressentie.Caractéristiques des sondesDisponible en 2 longueurs différentes, ces sondes sont indispensables pour y fixer des hélices de mesures.› Tige en aluminium télescopique, d’une longueur totale e 1,2 mètres pour mesurer dans les tubes de ventilation difficiles d’accès ou de grand diamètre, dans des rivières ou canalisations.› Tige en aluminium, longueur 10 cm. Pour transformer votre en anémomètre compact (s’utilise surtout avec les hélices pour gaz ø 20mm et ø 12mm)› Sonde avec hélice lestée à l’extrémité d’un câble de 15 mètres pour les mesures depuis une structure sur plombant la rivière.

' ''

You have just acquired a piece of high precision equi-pment which has been created using the most modern technology. It has been designed to stand up to inten-sive use. However, in order to maintain its appearance and its precision, we recommend that you treat it with care and read this manual carefully.

To work properly, the system has to include at least:

› 1 display unit› 1 probe› 1 impeller

Function of the buttonsON : press for 1 second OFF : press for 2 seconds (not auto off)LIGHT : press on and off brieflyUP : setting modeSTART / STOP : chronometer modeDOWN : setting modeLAP / RESET : chronometer modeSET / CAL : setting modeRESET MEMORY : press for 3 seconds

ConfigurationTo access the configuration mode of your instrument, just press on the button. Pressing the button once again cause the system to confirm the setting if there has been a change. If not then it goes to the next set-ting. To modify the settings the and buttons have to be used. Here is how to proceed with the different instrument settings.Speed measuring unit The units to be selected are : knots, mph, km/h, m/s, fps and cm/s. Once the unit is chosen, it remains displayed in the top right. If no other unit is chosen the instrument is set to the cm/s.Temperature measurement unit The units to be selected are : °F, °C, °F and °C .Setting the time of the average The times to be selected are : --- (weighting), 3’’, 6’’, 12’’, 30’’, 1’, 6’, 30’, 1:00’, 6:00’, 12:00’, 24:00’ or timer .The timer mode allows measurement of the average between start (press ) and stop (press ), this time is displayed on the lower lines. This timer allows the use of the LapTime function (press , the symbol flashes). The button also allows the timer to be re-set to zero. This works in the same way as a standard chronometer.Setting of the speed and temperature displays The displays to be selected are : ---, MIN, AV, MAX.If AV is selected, the average of temperature and wind are shown. The display of average values is always made simultaneously for the speed (at the centre) and temperature (at the bottom). The other modes (---, MIN, MAX) only concern the temperature.Setting of the display is not possible if the units selected are °F or °C .

Measuring air or liquid flowsInstantaneous speed (at the top) Maximum speed (at the centre)The display of the maximum speed is made at the central part. It is the maximum measured value of the time of the average. The value is reset to zero during a RESET of the memory.Average speed (at the center if AV is selected)

Measuring the temperature The temperature sensor is on the end of each probe.Instantaneous temperatureImportant : Thermal inertia of the instrument directly affects the stabilization time of the measurement. The greater the temperature difference, is the longer this time will be. This time will be shorter if the wind speed is higher.Wind-chill temperatureAs you know, exposure to low temperatures is potentially dangerous to the human body. But did you know that wind plays a significant part in how your body actually feels temperatures? For example, an ambient temperature of 0°C and a 30 km/h wind have the same effect on you as a temperature of -13°C! The result of the calculation of the effect of wind on the temperature is called the “wind-chill temperature”. The shows immediately the wind-chill.Minimum temperatureMaximum temperatureThese two modes show the min or max values measured over time of the average. The value is reset to zero during a RESET of the memory. These values are not those of the temperature felt by the body.Probe specificationsAvailable in 2 different lengths, these 2 probes are es-sential to install any impeller.› Aluminium telescopic rod, total length of 1.2m with 2 meters cable to measure in hard-to-reach ventilation shafts, air conditioning conduits, rivers flows and irrigation canals.› Aluminium small rod, 10 cm long to use your as a compact windmeter (mostly used with windspeed impellers ø 20mm and ø 12mm)› Probe with a 15 meters sounding cable with water- flow impeller, to measure water flow from bridges.

' ''

Caractéristiques des hélices› Hélice taille standard : gaz ø 20 mm, trou de passage ø 33 mm. Sensibilité minimum : < 3km/h - < 1m/s Précision : +/-2% Erreur ‘‘off-axis’’ : +/-30° / +/-3% Température d’utilisation : -50°C à +100°C› Hélice petite taille : gaz ø 12 mm, trou de passage ø 18 mm. Sensibilité minimum : < 3km/h - < 1m/s Précision : +/-2% Erreur ‘‘off-axis’’ : +/-10° / +/-3% Température d’utilisation : -50°C à +100°C› Hélice eau : ø 60 mm Sensibilité minimum : < 0.3km/h - < 0.1m/s Précision : +/-2% Erreur ‘‘off-axis’’ : +/-20° / +/-3%

Données techniques› Appareil étanche et résistant aux intempéries›Filetage sous l’appareil permettant sa fixation sur un trépied (1/4’’)› Résolution de la vitesse: 0.1 pour toutes les unités (sauf cm/s: 3cm/s)› Vitesse maximale: 150km/h (sauf cm/s: 999cm/s)› Précision du thermomètre : +/- 0.2°C› Résolution du thermomètre : 0.1°C› Alimentation : 2 piles 1.5V AA Autonomie des piles, au minimum 3 ans avec un usage occasionnel de l’éclairage de l’affichage. Pour le changement, dévisser les trois vis de la plaque métallique.› Poids : 210 grammes (insubmersible)› Dimensions : ø66 X 137 mm› Garantie : 1 année› Tous les câbles sont en PUR

GarantieVotre instrument est garanti par JDC ELECTRONIC SA pendant une année à partir de la date d’achat contre tout défaut matériel ou de fabrication. Sont exclus de cette garantie les dommages causés par une utilisation inadéquate.Le principe de mesure de la vitesse du est basé sur la détection du champ magnétique tournant produit par l’hélice. Si l’appareil est en présence d’un fort champ magnétique produit par un transformateur ou un moteur, il se peut que l’instrument indique des va-leurs non désirées, en l’absence de rotation de l’hélice.

Vous trouverez encore plus d’informations sur notre site internet www.jdc.ch.

FREN



Phone: +41 24 445 21 21Fax: +41 24 445 21 23





Phone: +41 24 445 21 21Fax: +41 24 445 21 23



++

Developed and manufactured by:

JDC Electronic SASwitzerlandwww.jdc.ch

North American Sales & Support:

NTech USAPO Box 284

Holmen, WI [email protected]

608.498.4021

WIND METERS Xplorer 1: Wind speed only Xplorer 2: Adds Temperature Xplorer 3: Adds Digital Compass Xplorer 4: Adds Air Pressure and Altitude EOLE: “Cup-style” Wind Speed METEOS: “Cup-Style” Wind plus Temperature ATMOS: “Cup-Style” Wind, Temperature, Humidity

Products available through NTech USA:

OTHER PRODUCTS FLOWATCH: Flowofwater/fluids SPEEDWATCH: Wireless Boat Knotmeter POROSIMETER: Porosity of fabrics

SOP APPROVAL FORM TETRA TECH EM INC. ENVIRONMENTAL STANDARD OPERATING PROCEDURE SURFACE WATER SAMPLING SOP NO. 009 REVISION NO. 4 Last Reviewed: June 2009

6-19-09

Quality Assurance Approved

Date

Tetra Tech EM Inc. – Environmental SOP No. 009 Page 1 of 13Title: Surface Water Sampling Revision No. 4, June 2009

Last Reviewed: June 2009

1.0 BACKGROUND

Surface water sampling is conducted to determine the quality of surface water entering, leaving, or

affected by a site. Surface water bodies that can be sampled include streams, rivers, lakes, ponds,

lagoons, and surface impoundments. This standard operating procedure (SOP) discusses common

methods of collecting grab samples that represent water quality in a water body at a particular point in

time.

A series of grab samples also can be composited to represent water quality over a longer period of time.

Composite samples can be flow proportional or time proportional. The details of compositing water

samples are not included in this SOP.

1.1 PURPOSE

This SOP establishes the requirements and procedures for surface water sampling.

1.2 SCOPE

This SOP applies to surface water sampling and the instruments and methods used to collect the samples.

1.3 DEFINITIONS

Kemmerer Sampler: A messenger-activated water sampling device. Water flows through the device

until the release mechanism is triggered to close the container.

Peristaltic Pump: A rotary, positive-displacement pumping device characterized by its low suction and

rhythmic operation, and by the fact that the pump does not come into direct contact with the water being

sampled.

Pond Sampler: A sampling device fabricated by using an adjustable beaker clamp to attach a beaker to a

telescoping, heavy-duty aluminum pole.



1.4 REFERENCES

U.S. Environmental Protection Agency (EPA). 1977. “Procedures Manual for Ground Water Monitoring at Solid Waste Disposal Facilities.” EPA-530/SW-611. August.

EPA. 1980. “Samplers and Sampling Procedures for Hazardous Waste Streams.” EPA-600/2-80-018.

January. EPA. 1984. “Characterization of Hazardous Waste Sites — A Methods Manual, Volume II. Available

Sampling Methods.” Second Edition. EPA-600/4-84-076. December. EPA. 2002. “Surface Water Sampling.” Environmental Response Team SOP #2013 (Rev. #1.0,

12/17/02). On-Line Address: http://loostrom.com/kosov/separatasidor/usepasurfacewatersampling.pdf

EPA. 2007. “Operating Procedure – Surface Water Sampling.” Science and Ecosystem Support

Division. SCSDPROC-201-R1. November.

1.5 REQUIREMENTS AND RESOURCES

Surface water sampling requires a variety of procedures and instruments. The choice of procedure should

be determined by site-specific conditions, such as the type of surface water body, the sampling depth, and

the sample location’s distance from shore.

Samples can be collected from shallow depths by submerging the sample container. An intermediary

disposable collection container or one constructed of a nonreactive material also may be used. A pond

sampler, a peristaltic pump, or a Kemmerer sampler may be used to provide extended reach. The

following equipment may be required to sample surface water:

· Decontamination materials

· Sample containers and labels

· Point-source bailer

· Dipper

· Boat

· Pond sampler

· Peristaltic pump with batteries or power source

· Silicone tubing

· Heavy-wall Teflon® tubing



· Kemmerer sampler

· Bucket

· Logbook or field data sheets

· Chain-of-custody documentation

· Shipping materials

2.0 PROCEDURES

Safe access, handling, and other physical limitations should be influential factors during surface water

sampling. A site-specific sampling plan should delineate which of the procedures described below will be

used. Any deviations from the sampling plan should be recorded in the site-specific field logbook.

The following subsections provide detailed procedures for surface water sampling using specific

instruments and methods. In all cases, select a sampling location where the water quality will best

represent the water chemistry of the water body. Avoid stagnant or fast-moving areas. Do not sample

immediately downstream of incoming tributaries, because of the likelihood of incomplete mixing.

2.1 SURFACE WATER SAMPLING BY SUBMERGING SAMPLE CONTAINER

Samples from shallow depths should be collected by submerging the sample container. This method is

advantageous when the sample might be significantly altered during transfer from a collection vessel into

another container. This method should not be used for sampling lagoons or surface impoundments where

contact with contaminants is a potential concern.

The following procedure can be used for sampling surface water by submerging the sample container:

1. Place all equipment on plastic sheeting next to the sampling location. Sample containers should be selected in accordance with the requirements specified in the project-specific field work plan, field sampling plan, or quality assurance project plan (QAPP).

2. If required by the project, collect field parameter measurements using procedures in

relevant specific Tetra Tech SOPs and project-specific field sampling plan. Record this information on the field sheet or in the logbook.

3. A visual check for visible surface material (pond scum or ice) should be performed

before sampling. If present, surface water samples should be collected by directly



submerging the sample container (with lid still on) into the surface water at the specified sampling location. Avoid contacting the bottom of the water body with the sample container because this will disturb sediment that may interfere with the surface water sample. Once submerged, the lid should be removed to allow the container to fill with water below any visible material on the surface of the water. A visual check should be conducted during and after sample collection to ensure sample integrity. If no surface materials are present, sample as instructed below.

4. For stream sampling, sample the location farthest downstream first. In general, work

from zones suspected of low contamination to zones of high contamination. Orient the mouth of the sample container facing upstream while standing downstream so as not to stir up any sediment that would contaminate the sample. Avoid contacting the bottom of the water body with the sample container because this will disturb sediment that may interfere with the surface water sample.

5. For a larger body of surface water, such as a lake, collect samples near the shore, unless

boats are feasible and permitted. Collect samples from shallow depths by submerging the sample container. Avoid contacting the bottom of the water body with the sample container because this will disturb sediment that may interfere with the surface water sample. If sampling from a boat, collect the sample as far away as possible from the outboard engine to avoid possible fuel contamination.

6. If sediment samples are to be collected (using procedures in SOP No. 006 [Sludge and

Sediment Sampling]) with surface water samples, collect surface water samples at each location before collecting sediment samples to avoid contaminating the water samples with excess suspended particles generated during sediment sampling.

7. Continue delivery of the sample until the container is almost full. If sampling for volatile

organic compounds (VOC) or other analytical parameters requiring pre-preserved sample containers, the use of a transfer device is recommended so that the preservative is not displaced.

8. Preserve the sample in accordance with requirements specified in the project-specific

field work plan, field sampling plan, or QAPP. Ensure that a Teflon® liner is present in the cap of the sample container if required. Secure the cap tightly and affix a completed sample label to the container.

9. Complete all chain-of-custody documentation, field logbook entries, and sample

packaging requirements.



2.2 SURFACE WATER SAMPLING WITH TRANSFER DEVICE

A dipper, bailer, or other device made of inert material, such as stainless steel or Teflon®, can be used to

transfer liquid samples from their source to a sample container. This prevents contamination of the

outside of the sample container as a result of direct immersion in surface water. Depending on the

sampling application, the transfer device may be either disposed of or reused. If reused, the device should

be thoroughly rinsed and decontaminated in accordance with SOP 002 (General Equipment

Decontamination), prior to sampling a different source.

A transfer device can be used in most sampling situations, and is preferred when (1) direct contact or

physical access limitations pose a health and safety concern and (2) sample containers are pre-preserved.

However, direct collection by submerging the sample container is the preferred method when possible.

The following procedure can be used for sampling surface water with a dipper, bailer, or other transfer

device:

1 Place all equipment on plastic sheeting next to the sampling location. Sample containers should be selected in accordance with the requirements specified in the project-specific field work plan, field sampling plan, or QAPP.


relevant specific Tetra Tech SOPs. Record this information on the field sheet or in the logbook.

3. With minimal surface water disturbance, submerge a precleaned dipper, bailer, or other

transfer device.

4. Allow the device to fill slowly and continuously.

5. Retrieve the device from the surface water with minimal disturbance.

6. Remove the cap from the sample container. Slightly tilt the mouth of the container below the edge of the transfer device.

7. Empty the device slowly, allowing the sample to flow gently down the inside of the

container with minimal entry turbulence. Continue delivery of the sample until the container is almost full. If sampling for VOCs, the container must be completely filled leaving no head space.


field work plan, field sampling plan, or QAPP. Ensure that a Teflon® liner is present in



the cap of the sample container if required. Secure the cap tightly and affix a completed sample label to the container.



10. Decontaminate the transfer device prior to reuse or storage using the procedures in SOP No. 002 (General Equipment Decontamination).

2.3 SURFACE WATER SAMPLING WITH POND SAMPLER

A pond sampler may be used to collect liquid samples from ponds, pits, and lagoons (see Figure 1). A

pond sampler is easily and inexpensively fabricated. To construct a pond sampler, use an adjustable

clamp to attach a sampling beaker to the end of a two- or three-piece telescoping aluminum tube. The

telescoping tube serves as the handle. All nondisposable equipment should be cleaned before and after

each use.

The following procedure can be used for sampling surface water with a pond sampler:

1. Place all equipment on plastic sheeting next to the sampling location. Sample containers should be selected in accordance with the requirements specified in the project-specific field work plan, field sampling plan, or QAPP.



3. Assemble the pond sampler. Ensure that the sampling beaker, bolts, and nuts securing

the clamp to the pole are tightened properly.

4. Collect the sample by slowly submerging the precleaned beaker with minimal surface water disturbance.

5. Retrieve the pond sampler from the surface water with minimal disturbance.

6. Remove the cap from the sample container. Slightly tilt the mouth of the container below

the edge of the beaker.

7. Empty the beaker slowly, allowing the sample to flow gently down the inside of the container with minimal entry turbulence. Continue delivery until the container is almost full. If sampling for VOCs, the container must be completely filled leaving no head space.



8. Preserve the sample in accordance with requirements specified in the project-specific field work plan, field sampling plan, or QAPP. Ensure that a Teflon® liner is present in the cap of the sample container if required. Secure the cap tightly and affix a completed sample label to the container.



10. Decontaminate the pond sampler prior to reuse or storage using the procedures in SOP No. 002 (General Equipment Decontamination).

2.4 SURFACE WATER SAMPLING WITH PERISTALTIC PUMP

To extend reach in sampling efforts, a small peristaltic pump can be used (see Figure 2). A peristaltic

pump draws the sample through heavy-wall Teflon® tubing and pumps it directly into the sample

container. Use of a peristaltic pump allows the operator to reach out into a liquid body, to sample from a

depth or to sweep the width of a narrow stream. A battery-powered pump is preferable because it

eliminates the need for a direct current generator or an alternating current inverter.

If medical-grade silicone tubing is used in the peristaltic pump, it is suitable for sampling almost any

parameter, including most organics. However, some VOC stripping may occur and some sample material

may adhere to the tubing. Teflon® tubing may be used in place of silicone tubing on the intake side of the

pump to minimize the amount of sample adherence to the tubing. If tubing is to be reused, it should be

cleaned before and after each use following the procedures specified in SOP No. 002 (General Equipment

Decontamination). Depending on project requirements, it may be necessary to replace the Teflon® intake

tubing and the pump silicone tubing between sampling locations to prevent cross contamination.

Procedures for sampling surface water with a peristaltic pump are as follows:

1. Place all equipment on plastic sheeting next to the sampling location. Sample containers should be selected in accordance with the requirements specified in the project-specific field work plan, field sampling plan, or QAPP.



3. Install clean, medical-grade silicone tubing in the pump head according to the

manufacturer’s instructions. Allow enough tubing on the discharge side to facilitate



delivery of liquid into the sample container. Allow only enough tubing on the suction end for attachment to the intake line. This will minimize sample contact with the tubing.

4. Select the length of intake tubing needed to reach the required sample location. Attach it

to the intake side of the pump tubing. Heavy-wall Teflon® tubing of a diameter equal to that of the required pump tubing suits most applications. A heavier tubing wall will allow slightly greater lateral reach.

5. If possible, allow several liters of surface water to pass through the pump before

collecting the sample. Collect this purge volume. Return it to the source after the samples have been withdrawn.

6. Fill the sample container by allowing the pump discharge to flow gently down the inside

of the bottle with minimal entry turbulence. Continue delivery of the sample until the container is almost full.

7. If sampling for VOCs, the VOC sample must be collected using one of the “soda straw”

variations. Ideally, the tubing intake will be placed at the depth from which the sample is to be collected and the pump will be run for several minutes to fill the tubing with water representative of that interval. After several minutes, the pump is turned off and the tubing string is retrieved. The pump speed is then reduced to a slow pumping rate and the pump direction is reversed. After the pump is turned back on, the sample stream is collected into the VOC vials as it is pushed from the tubing by the pump. Care must be taken to prevent any water that was in contact with the peristaltic pump head tubing from being incorporated into the sample.





10. Allow the pump to drain, and then disassemble it. Decontaminate the tubing before reuse using the procedures in SOP No. 002 (General Equipment Decontamination), or dispose of it.

2.5 SURFACE WATER SAMPLING WITH KEMMERER SAMPLER

The Kemmerer sampler (see Figure 3) is used to collect surface water samples when the required sample

depth is greater than that which can be sampled with a pump. A Kemmerer sampler may be constructed

of various materials to be compatible with the required analytical technique. The sampler should be

cleaned before and after each use.



Procedures for sampling surface water with a Kemmerer sampler are as follows:

1. Place all equipment on plastic sheeting next to the sampling location. Sample containers should be selected in accordance with the requirements in specified in the project-specific field work plan, field sampling plan, or QAPP.



3. Inspect the body of the Kemmerer sampler to ensure that the drain line valve is closed, as

appropriate. Measure and mark the sample line (cable) at the desired sampling depth.

4. Open the sampler by lifting the upper stopper-trip head assembly.

5. Gradually lower the sampler into the surface water until the sample liquid reaches the sample line.

6. Place a messenger on the sample line and release it, closing the sampler.

7. Retrieve the sampler. Prevent accidental opening of the lower stopper by holding the

center rod of the sampler.

8. Rinse or wipe off the exterior of the sampler. Recover the sample by grasping the lower stopper and sampler body with one hand. Transfer the sample by lifting the upper stopper with the other hand and carefully pouring the contents into the sample container. If a drain line valve is present, hold the valve over the sample container, and open the valve slowly to release the sample.

9. Transfer the sample slowly, allowing it to flow gently down the inside of the container

with minimal entry turbulence. Continue delivery until the container is almost full. If sampling for VOCs, the container must be completely filled leaving no head space.





12. Decontaminate the Kemmerer sampler prior to reuse or storage using the procedures in SOP No. 002 (General Equipment Decontamination).



2.6 SURFACE WATER SAMPLING WITH BUCKET

A plastic bucket is used to collect surface water samples for measurement of water quality parameters

(such as pH, temperature, and conductivity) or classical water quality parameters (ammonia, nitrate-

nitrite, phosphorus, and total organic carbon). This method is not recommended for collecting samples

for chemical analysis. A bucket is commonly used to collect a sample when the water depth is too great

for wading, it is not possible to deploy a boat, or access is restricted (excessive vegetation or steep

embankments) and the water column is well mixed. The water body is usually accessed from a bridge.

The bucket is lowered by rope over the side of the bridge and, upon retrieval, the water is poured into the

appropriate sample containers.



FIGURE 1 POND SAMPLER



FIGURE 2 PERISTALTIC PUMP FOR LIQUID SAMPLING



FIGURE 3 KEMMERER SAMPLER

SOP APPROVAL FORM TETRA TECH EM INC. ENVIRONMENTAL STANDARD OPERATING PROCEDURE GROUNDWATER SAMPLING SOP NO. 010 REVISION NO. 4 Last Reviewed: June 2009

6-19-09

Quality Assurance Approved

Date

Tetra Tech EM Inc. - Environmental SOP No. 010 Page 1 of 16Title: Groundwater Sampling Revision No. 4, June 2009


1.0 BACKGROUND

Groundwater sampling may be required for a variety of reasons, such as to examine potable or industrial

water supplies, check for and track contaminant plume movement in the vicinity of a land disposal or spill

site, conduct Resource Conservation and Recovery Act (RCRA) compliance monitoring, or examine a

site where historical information is minimal or nonexistent, but where groundwater may be contaminated.

Groundwater is usually sampled through an in-place well, either temporarily or permanently installed.

SOP No. 020 (Monitoring Well Installation) provides guidance for installing new monitoring wells.

However, it can also be sampled anywhere groundwater is present, such as in a pit or a dug or drilled

hole.

1.1 PURPOSE

This standard operating procedure (SOP) establishes the requirements and procedures for determining the

quality of groundwater entering, leaving, or affected by site activities through groundwater sampling.

The samples are obtained by retrieving water from a well screened in the aquifer or aquifers underlying a

site.

1.2 SCOPE

This SOP provides general guidance for groundwater sampling activities conducted in the field. SOP

No. 015 (Groundwater Sample Collection Using Micropurge Technology) provides additional specific

guidance for using low-flow methods to collect groundwater samples.



1.3 DEFINITIONS

Bailer: A cylindrical sampling device with valves on either end, used to extract water from a well.

Bailers are usually constructed of an inert material such as stainless steel or polytetrafluoroethylene

(Teflon). The bailer is lowered and raised by means of a cable that may be cleaned and reused, or by

disposable rope.

Electrical Water Level Indicator: An electrical device that has a light or sound alarm connected to an

open circuit, used to determine the depth to liquid. The circuit is closed when the probe intersects a

conducting liquid. The wire used to raise and lower the probe is usually graduated.

Immiscible Phase: A liquid phase that cannot be uniformly mixed or blended with water. Heavy

immiscible phases sink, and light immiscible phases float on water.

Interface Probe: An electrical probe that determines the distance from the surface to air-water, air-

immiscible, or immiscible-water interfaces.

Purge Volume: The volume of water that needs to be removed from the well prior to sampling to ensure

that the sample collected is representative of the formation groundwater.

Riser Pipe: The length of well casing above the ground surface.

Total Well Depth: The distance from the reference measuring point (top of well casing or ground

surface) to the bottom of the well.

Water Level: The level of water in a well, measured as depth to water or as elevation of water, relative

to a reference mark or datum.

1.4 REFERENCES

U.S. Department of Energy. 1985. “Procedures for the Collection and Preservation of Groundwater and Surface Water Samples and for the Installation of Monitoring Wells: Second Edition.” Edited by N. Korte and P. Kearl. Technical Measurements Center, Grand Junction Projects Office. GJ/TMC-08.

U.S. Environmental Protection Agency (EPA). 1977. “Procedures Manual for Ground Water Monitoring at Solid Waste Disposal Facilities.” EPA-530/SW-611. August.



EPA. 1984. “Sampling at Hazardous Materials Incidents.” EPA Hazardous Response Support Division,

Cincinnati, 1984. EPA. 1995. “Groundwater Well Sampling.” Environmental Response Team SOP #2007 (Rev. #0.0,

01/26/95). http://www.ert.org/products/2007.PDF U.S. Geological Survey. 1984. “National Handbook of Recommended Methods for Water-Data

Acquisition” Reston, Virginia. Yeskis, D. and B. Zavala. 2002. Ground-Water Sampling Guidelines for Superfund and RCRA Project

Managers. U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response. Publication: EPA542-S-02-001. May. http://www.epa.gov/tio/tsp/download/gw_sampling_guide.pdf


There are various options available to obtain groundwater samples. The procedures are outlined in the

following section. The equipment needed to accomplish these procedures includes the following:

· Organic vapor detector with a flame ionization detector (FID) or a photoionization detector (PID)

· Pipe wrench and/or other tools needed to open monitoring wells (socket wrench, mallet,

etc.)

· Electrical water level indicator or interface probe

· Purging device (type needed depends on well depth, casing diameter, and type of sample desired; see sampling devices below)

· Graduated cylinder or bucket

· Sampling device (type needed depends upon depth to water and type of sample desired)

- Teflon bailer - Stainless steel bailer - Teflon bladder pump - Stainless steel submersible (non-oil-bearing) pump - Existing dedicated equipment - Peristaltic pump

· Sample containers

· Wastewater containers



· Field logbook

· Stopwatch

Additional equipment is required to complete measurement of field parameters (for example, pH, specific

conductance, and temperature) of the groundwater in the well. Refer to Tetra Tech SOP 061 (Field

Measurement of Dissolved Oxygen, Oxidation-Reduction Potential, pH, Specific Conductance,

Temperature, and Turbidity Using a Multi-Parameter Water Quality Meter) or individual field parameter

SOPs as appropriate.

2.0 PROCEDURE

Prior to sampling, a site-specific sampling plan should be developed. The plan should take into

consideration the site characteristics and should include:

· Specific, repeatable well measurement techniques and reference points for determining the depth to water and the depth to the bottom of the well

· Specific method of purging and selection of purging equipment

· Specific methods and equipment for measurements of field parameters

· Specific method of sample collection and the sampling equipment that will be used

· Specific parameters for which samples will be analyzed

· Order in which sample bottles will be filled, based on the analytical parameters

The following sections discuss procedures for approaching the well, establishing a sample preparation

area, making preliminary well measurements, purging the well, and collecting samples.

2.1 APPROACHING THE WELL

In general, all wells should be assumed to pose a health and safety risk until field measurements indicate

otherwise. Approach the well from the upwind side. Record well appearance and the general condition

of the protective casing, surface seal, and surrounding area in the logbook.

Once at the well, the lead person should systematically use the organic vapor detector to survey the

immediate area around the well (from the breathing zone to the top of the casing to the ground). If



elevated FID and PID meter readings are encountered, retreat to a safe area and instruct the sampling

team to either let vapors dissipate and approach the well again or put on the appropriate level of personal

protective equipment (PPE), as specified in the site-specific health and safety plan. See SOP No. 003

(Organic Vapor Air Monitoring) for additional air monitoring guidance.

Some monitoring wells have the potential to contain pressurized headspace—for example, through the

generation of gases from contaminated groundwater, due to biological processes, degradation of

contaminants, or simply based on location such as near a landfill or in areas that intersect lithological

abnormalities; or through intentional artificial means such as those associated with air sparging systems.

Injection or extraction wells may be artificially pressurized and may remain so for several days after the

system has been turned off. This presents a hazard to people opening these wells. Tetra Tech personnel

shall employ the following practices to minimize these hazards:

Wear safety glasses to protect the eyes. If site-specific observations and conditions indicate that the

wells may be pressurized, wear a full-face shield over the safety eye protection. Do not place the face or any other part of the body over the well when opening because this may

place you in a strike zone.

Open the well cover at arm’s length, then step away and allow the well to off gas and stabilize. Upon opening the well casing, the lead person should systematically survey inside the well casing, above

the well casing in the breathing zone, and in the immediate area around the well. If elevated FID or PID

meter readings in the breathing zone are encountered (see health and safety plan for action levels), retreat

and put on appropriate PPE. It is important to remember that action levels are based on readings in the

breathing zone, not within the well casing. Representative organic vapor detector readings should be

recorded in the logbook. Also look out for insects or other animals that may nest in well openings, and

refer to the health and safety plan for specific hazards.



2.2 ESTABLISHING A SAMPLE PREPARATION AREA

The sample preparation area is generally located upwind or to either side of the well. If elevated readings

are encountered using an organic vapor detector, this area should be taped off and the sample preparation

area should be located upwind of the well, where ambient conduction are measured.

2.3 MAKING PRELIMINARY WELL MEASUREMENTS

Several preliminary well measurements should be made prior to initiating sampling of the well. These

include determining water level and total well depth measurements, determining the presence of

immiscible phases, and calculating purge volumes. All preliminary measurements will be recorded in the

logbook or the Groundwater Sampling Data Sheet (included as an exhibit to this SOP) as they are

determined. SOP No. 014 (Static Water Level, Total Well Depth, and Immiscible Layer Measurement)

provides additional information concerning these preliminary measurements.

2.3.1 Water Level and Total Well Depth Measurements

Tetra Tech typically uses an electric water level indicator for water level and total well depth

measurements. This device sounds an alarm or triggers a light when the measuring probe touches the

water surface, thus closing an electrical circuit. The electric cable supporting the probe is usually

graduated to 0.01 foot and can be read at the well site directly. The distance between the static water

level and the marked or notched location at the top of the riser pipe is measured. The height of the riser

pipe above ground surface, as obtained from well location survey data, is then subtracted from the total

reading to give the depth to static water. To improve accuracy, three separate readings should be made,

and the values averaged. This helps to eliminate any errors due to kinks or bends in the cables, which

may change in length when the water level indicator is raised and lowered.

The total well depth can be measured by lowering the probe into the well until resistance is met,

indicating that the probe has reached the bottom of the well. The total well depth is then read to the 0.01-

foot fraction. The distance between the bottom of the well and the marked or notched location on the

riser pipe is measured. The height of the riser pipe above the ground surface, as obtained from well

survey data, is then subtracted from the total reading to give the depth to the bottom of the well. To

improve accuracy, three separate readings should be made, and the readings averaged.



2.3.2 Determining if Immiscible Nonaqueous-Phases Liquids are Present

If immiscible, nonaqueous-phase liquid (NAPL) are present, the following measurement activities should

be undertaken. Organic liquids are measured by lowering an interface probe slowly to the surface of the

liquid in the well. When the audible alarm sounds, record the depth. If the alarm is continuous, a floating

immiscible layer has been detected. To determine the thickness of this layer, continue lowering the probe

slowly until the alarm changes to an oscillating signal. The oscillating signal indicates that the probe has

detected an aqueous layer. Record this depth as the depth to water and determine the thickness and the

volume of the immiscible layer.

Continue lowering the probe into the well to determine if dense immiscible phases (sinkers) are present.

If the alarm signal changes from oscillating to a continuous sound, a heavier immiscible layer has been

detected; record this depth.

Continue lowering the probe to the bottom of the well and record the total depth. Calculate and record

the sinker phase volume and total water volume in the well (see equation in Section 2.3.3). If immiscible

phases are present, immediately refer to Section 2.5.3 or 2.5.4 of this SOP for sample collection

procedures.

2.3.3 Determination of Purging Volume

If the presence of immiscible phases does not need to be determined, determine the depth to water and the

total depth of the well as described in Section 2.3.1. Once these measurements have been made and

recorded, use Table 1 to calculate the total volume of water in the well. Multiply this volume by the

purging factor to determine purging volume. The minimum purging factor is typically three casing

volumes but may be superseded by site-specific program requirements, individual well yield

characteristics, or stabilization of field parameters measured during purging. Field parameters (for

example, pH, specific conductance, and temperature) should be measured prior to purging and after each

well volume. All field parameter data should be recorded in the field logbook, Groundwater Sampling

Data Sheet, or personal digital assistant (PDA). Refer to specific Tetra Tech SOP 061 as appropriate for

more detailed procedures for determining these field parameters.



The volume of water in the well is based on the following formula:

where

V = static volume of water in the well (gallons)

r = inside radius of the well (feet)

h = length of water in the well (total well depth minus depth to water) (feet)

7.48 = conversion factor (cubic feet to gallons)

Common well sizes and corresponding volumes are as follows:

1-inch well = h x 0.041 gal/ft 2-inch well = h x 0.163 gal/ft 3-inch well = h x 0.367 gal/ft 4-inch well = h x 0.652 gal/ft

2.4 PURGING THE WELL

Currently, Tetra Tech standards allow for six options for purging wells:

1. Teflon bailers

2. Stainless steel bailers

3. Teflon bladder pumps

4. Stainless steel submersible (non-oil-bearing) pumps

5. Existing dedicated equipment

6. Peristaltic pumps (these devices are for shallow wells only)

As previously stated, the minimum purging volume is typically three casing volumes. Exceptions to this

standard may be made in the case of low-yield wells. When purging low-yield wells, purge the well until

the water level is equal to the top of screen elevation (if possible). Samples should be collected no sooner

than 2 hours after purging and when sufficient groundwater volume is available.

V = πr2h x 7.48



The well should be purged until measured field parameters have stabilized. If any field parameter has not

stabilized, additional purging should be performed. To be considered stable, field parameters should

change by no more than the stabilization criteria listed on Table 1 between each well volume purged. If

the above conditions have not been met after a specified period of time, purging will be considered

complete and sampling can begin. Refer to the field sampling plan or quality assurance project plan for

specified time period. Record the final well stabilization parameters on the Groundwater Sampling Data

Sheet, and indicate if the well purging was considered complete due to stabilized parameters or exceeding

the specified period of time.

At no time should the purging rate be high enough to cause the groundwater to cascade back into the well,

as this could result in excessive aeration and potential stripping of volatile constituents.

The actual volume of purged water can be measured using several acceptable methods:

· When bailers are used, the actual volume of each bailer’s contents can be measured using a calibrated bucket.

· If a pump is used for purging, the pump rate can be determined by using a bucket of

known volume, stopwatch, and the duration of pumping time necessary to purge the known volume.

2.5 SAMPLE COLLECTION

This section first describes general groundwater sample collection procedures. This section also describes

procedures for collecting groundwater samples for volatile organic analysis (VOA) and for collecting

samples when light or heavy immiscible layers are present in a monitoring well. Samples of light and

heavy immiscible layers should be collected before the well is purged. Site-specific sampling plans may

indicate that, based on the presence of NAPL, no groundwater sample is to be collected.



2.5.1 General Groundwater Sampling Procedures

The technique used to withdraw a groundwater sample from a well should be selected based on the

parameters for which the sample will be analyzed. To ensure that the groundwater samples are

representative, it is important to avoid physically altering or chemically contaminating the sample during

collection, withdrawal, or containerization. If the samples are to be analyzed for volatile organic

compounds, it is critical that air does not become entrained in the water column.

Acceptable sampling devices for all parameters are double check valve stainless steel or Teflon bailers,

bladder pumps, low-flow positive displacement pumps, or for shallow wells, peristaltic pumps.

Additional measurements of field parameters should be performed at the time of sampling.

In some cases, it may become necessary to use dedicated equipment already in the well to collect samples.

This is particularly true of high-volume, deep wells (>150 feet) where bladder pumps are ineffective and

bailing is impractical. If existing equipment must be used, however, determine the make and model of the

pump and obtain information on component construction materials from the manufacturer or facility

representatives. If an existing pump is to be used for sampling, make sure the flow volume can be

reduced so that a reliable VOA sample can be taken. Record the specific port, tap, or valve from which

the sample is collected. If nondedicated sampling equipment is used, the least contaminated wells should

be purged and sampled first and most contaminated wells should be purged and sampled last (if past

sampling data are available to make this determination).

General sampling procedures are as follows:

· Clean sampling equipment should not be placed directly on the ground. Use a plastic drop cloth or feed line from clean reels. Never place contaminated lines back on reels.

· Check the operation of the bailer check valve assemblies to confirm free operation.

· If the bailer cable is to be decontaminated and reused, it must be made of Teflon-coated

stainless steel.

· Lower sampling equipment slowly into the well to avoid degassing the water and damaging the equipment.

· Pump flow rates should be adjusted to eliminate intermittent or pulsed flow. The settings

should be determined during the purging operations.



· A separate sample volume should be collected to measure necessary field parameters. Samples should be collected and containerized following procedures outlined in the project-specific field sampling plan (FSP), quality assurance project plan (QAPP), and in the order of the parameters’ volatilization sensitivity. Table 2 lists the preferred collection order for common groundwater parameters.

Intermediate containers should never be used to prepare VOA samples and should be avoided for all

parameters in general. All VOA containers should be filled at a single sampling point or from a single

bailer volume. Also refer to site-specific sampling plan for other sample handling requirements that may

be unique to a site or to specific chemical constituents.

2.5.2 Collection of Volatile Organics Samples

This section discusses in detail the collection of samples for VOA using either a bailer or bladder pump.

Other pumps (such as positive displacement or peristaltic) can be used. The following factors are critical

to the collection of representative samples for VOA: ensuring that no air has become entrained in the

water column, achieving low pump flow rates (less than 100 milliliter [mL] per minute, if possible),

avoiding flow surges, and adjusting sample preservatives if they are found to cause reactions with the

sample.

2.5.2.1 Collection with Bailers

Samples for VOA should be collected from the first bailer removed from the well after purging is

complete. The most effective means requires two people. One person should retrieve the bailer from the

well and pour its contents into the appropriate number of 40-mL VOA vials held by the second person.

Each vial should be capped and inverted to check if any air bubbles are present. If a bubble exists,

unscrew the cap and add more water, or discard and repeat if vials are not pre-preserved. If bubbling

persists in a vial containing acid preservative, the sample may need to be collected without the

preservative and the laboratory notified to add preservative upon receipt. The sample should be

transferred from the bailer to the sample container in a manner that will limit the amount of agitation in

order to reduce the loss of volatile organics from the sample.



Always fill VOA vials from a single bailer volume. If the bailer is refilled, samples cannot be considered

duplicates or splits.

2.5.2.2 Collection with a Bladder Pump (Well Wizard)

To successfully perform VOA sampling with a Well Wizard bladder pump, the following steps must be

completed:

1. Following manufacturer’s directions, activate the pump. Full water flow from the discharge tubing will begin after 5 to 15 pumping cycles. These initial pumping cycles are required to purge air from the pump and discharge tubing. The discharge and recharge settings must be manually set and adjusted to pump at optimum flow rates. To activate the bladder, it is best to set the initial cycle at long discharge and recharge rates.

2. Reduce water flow rate for VOA sample collection. To reduce the water flow rate, turn

the throttle control valve (located on the left side of the Well Wizard pump control panel) counterclockwise.

3. Collect VOA sample from discharge tubing. VOA vials must be placed beneath the

discharge tubing while avoiding direct contact between the vials and the tubing. Never place tubing past the mouth of the VOA vial. The pump throttle control must be turned as necessary to maintain a trickle of water in order to obtain a meniscus in the vial.

4. Continue with non-VOA sampling. Increase pump flow rate by turning the throttle

control knob clockwise.

2.5.3 Sampling of Light Immiscible Floaters

The approach used when collecting a sample of a floating layer depends on the depth to the floating layer

and the thickness of that layer. If the thickness of the floater is 2 feet or greater, a bottom-filling valve

bailer should be used. Slowly lower the bailer until contact is made with the floater surface, and lower

the bailer to a depth less than that of the floater-water interface depth as determined by preliminary

measurements with the interface probe.

When the thickness of the floating layer is less than 2 feet and the depth to the surface of the floating

layer is less than 15 feet, a peristaltic pump can be used to extract a sample.

When the thickness of the floating layer is less than 2 feet and the depth to the surface of the floating

layer is beyond the effective “lift” of a peristaltic pump (greater than 25 feet), a bailer can be modified to

allow filling from the top only (an acceptable alternative is to use a top- loading Teflon or stainless-steel



bailer). Disassemble the bailer’s bottom check valve and insert a piece of 2-inch-diameter Teflon sheet

between the ball and ball seat. This will seal off the bottom valve. Remove the ball from the top check

valve, thus allowing the sample to enter from the top. To overcome buoyancy when the bailer is lowered

into the floater, place a length of 1-inch stainless steel pipe on the retrieval line above the bailer (this pipe

may have to be notched to allow sample entry if the pipe remains within the top of the bailer). As an

alternative, use a top-loading stainless-steel bailer. Lower the device, carefully measuring the depth to the

surface of the floating layer, until the top of the bailer is level with the top of the floating layer. Lower

the bailer an additional one-half thickness of the floating layer and collect the sample. This technique is

the most effective method of collection if the floating layer is only a few inches thick.

2.5.4 Sampling of Heavy Immiscible Sinkers

The best method for collecting a sample of a sinker is the use of a double check valve bailer. The key to

sample collection is controlled, slow lowering and raising of the bailer to and from the bottom of the well.

Sample collection methods are equivalent to those described in Section 2.5.3 above.



TABLE 1 STABILIZATION CRITERIA FOR WATER QUALITY PARAMETERS Parameter Stabilization Criterion pH ± 0.1 units Specific Conductance ± 3 percent Oxidation-Reduction Potential ± 10 millivolts Turbidity ± 10 percent (when greater than 10 nephelometric turbidity units

[NTU]) Dissolved Oxygen ± 0.3 milligrams per liter or ± 10 percent



TABLE 2 ORDER OF PREFERRED SAMPLE COLLECTION

1. VOA 2. Purgeable organic halogens (POX) 3. Total organic halogens (TOX) 4. Cyanide 5. Extractable organics 6. Purgeable organic carbon (POC) 7. Total metals 8. Dissolved metals 9. Total organic carbon (TOC) 10. Phenols 11. Sulfate and chloride 12. Nitrate and ammonia 13. Radionuclides



Tetra Tech EM Inc. EXHIBIT: GROUNDWATER Page of SAMPLING DATA SHEET Date

Well Name Screen Interval

Project

Station Elevation GND TOC

Immiscible Phases Present Yes No

Project No.

Static Water Level (from TOC)

Type

Well Location

Well Stick Up

Measured with

Sample Date

Static Elevation

PID Readings (background)

Well Depth MEAS RPTD

PID Reading (TOC)

Sampling Personnel

Feet of Water

Wells Installed by

Sample ID

Gallons/Foot

Installation Date

Duplicate ID

Casing Volume

Development Date(s)

FIELD CHEMISTRY CALIBRATIONS

Date/Time Spec. Conductance: Standard μmhos/c

Reading μmhos/cm at C

pH: pH 4.00 - _______ at _________ C

pH 7.00 - _______ at _________ C

pH 10.00 - ______ at _______ C

Slope

Dissolved Oxygen: D.O. Meter

mg/L at C

PID: Calibration Gas PPM Span Reading

PURGING

Cumulative Volume of

Water Removed (Purged)

PID/OVA Reading

Time

Discharge Rate

(mL/min)

Dissolve

d Oxygen (mg/L)

pH

Eh/ORP

(mV)

Temp. (C)

Specific Conduct. (μmhos/cm at C)

Turbidit

y (NTU)

Gallons

Casing

Vol.

Location

Value

Depth to

Water (ft)

Comments

SAMPLE PARAMETERS

Condition of well: Remarks:

SOP APPROVAL FORM

TETRA TECH EM INC.

ENVIRONMENTAL STANDARD OPERATING PROCEDURE

FIELD MEASUREMENT OF WATER TEMPERATURE

SOP NO. 011

REVISION NO. 2

Last Reviewed: November 1999

May 11, 1993

Quality Assurance Approved Date

Tetra Tech EM Inc. - Environmental SOP No. 011 Page 1 of 3Title: Field Measurement of Water Temperature Revision No. 2, May 11, 1993


1.0 BACKGROUND

Water temperature readings are used in the calculation of various forms of alkalinity, in studies of

saturation and stability with respect to calcium carbonate, in the calculation of salinity, and in general

laboratory operations. Properly measuring water temperature, therefore, is important to a wide variety of

field measurements.

1.1 PURPOSE

This standard operating procedure (SOP) establishes the requirements and procedures for measuring water

temperature in the field.

1.2 SCOPE

This SOP applies to measuring the temperature of surface water and groundwater while in the field.

1.3 DEFINITION

National Institute of Standards and Technology Certified Thermometer: A thermometer that carries

certification of its temperature-reading precision.

1.4 REFERENCE

U.S. Environmental Protection Agency. 1986. “Resource Conservation and Recovery Act (RCRA)Ground-Water Monitoring Technical Enforcement Guidance Document.” September.


The following equipment may be required for the measurement of water temperature in the field:

• Mercury-filled thermometer with metal case

• Electronic thermistor with accuracy of 0.1 EC and with an extension probe



• National Institute of Standards and Technology certified thermometer

• Sample container

• Decontamination materials

• Field logbook

2.0 PROCEDURES

Under normal conditions, temperature measurements may be made with any reliable, glass, mercury-filled

thermometer. At a minimum, the thermometer should have a scale etched on the capillary glass every 0.1

or 0.2 EC. The thermometer should have a minimal thermal capacity to permit rapid equilibration. The

thermometer should be calibrated at least annually using a precision thermometer certified by the National

Institute of Standards and Technology. Thermometers should be housed in a metal case to prevent

breakage.

In some situations, temperature measurements may be made with a digital electronic thermistor with an

accuracy of 0.1 EC. The thermistor must be maintained as described in the manufacturer’s operation and

maintenance manual. In particular, always check the energy level of the thermistor’s battery before each

use. If the standard probe is not sufficient for taking temperature readings, then an extension probe may be

used. Follow the manufacturer’s directions to ensure that unbalanced resistance in the extension probe

does not distort temperature readings.

Temperature measurements should be taken at the water source. If it is not possible to measure the

temperature at the source, collect a sample of the water to be measured and place the sample in an

intermediate container. When an intermediate container is used, fill the container with the sample and

allow the temperature of the container to equilibrate with that of the sample and record the temperature.

Dispose of the sample and collect a new sample. Place the new sample in an intermediate container and

repeat the process just described.

Take temperature readings using the thermometer or probe while it is immersed in water long enough to

allow complete equilibration. Depending on the type of thermometer, immerse it to mark or immerse

totally. Report results to the nearest 0.1 or 1.0 EC, depending on the project specifications.



Record measurements in the field logbook. After taking the measurements, decontaminate the thermometer

or probe.

SOP APPROVAL FORM

TETRA TECH EM INC.


FIELD MEASUREMENT of pH

SOP NO. 012

REVISION NO. 3


May 18, 1993


Tetra Tech EM Inc. - Environmental SOP No. 012 Page 1 of 6Title: Field Measurement of pH Revision No. 3, May 18, 1993


1.0 BACKGROUND

Determining pH is critical for predicting and interpreting the reactions and migration of dissolved chemical

constituents in groundwater or surface water. The pH of groundwater or surface water must be determined

when a sample is collected in the field.

1.1 PURPOSE

This standard operating procedure (SOP) establishes the requirements and procedures for measuring the

pH of water samples in the field.

1.2 SCOPE

This SOP applies to the use of pH meters in the field.

1.3 DEFINITIONS

pH Electrode: An electrode that measures the hydrogen ion potential of a solution by comparing it to a

standard solution with a known hydrogen ion potential. A thin glass membrane functions as a cation

exchange surface. When the electric potential of the interior of the glass membrane is compared to the

electric potential of a standard solution kept isolated from the environment, a quantitative determination of

the change in the internal solution’s electric potential, induced by the external solution, can be made.

Nernst Potential: Nernst Potential is the voltage observed when the glass membrane separates the external

solution from the internal solution. Nernst Potential varies depending on the hydrogen ion potential

between the external and internal solutions and, therefore, correlates with the pH of the solution. Because

the hydrogen ion content of the internal solution is constant, the changes in Nernst Potential are due to the

changes in the external solution.

Buffer Solution: A buffer solution is capable of maintaining the relative concentrations of acids and bases

by neutralizing, within limits, added acids or bases. It has a known pH for a specific temperature range.



1.4 REFERENCES

None


The pH meters used by personnel in the field should have temperature and slope adjustments and a

repeatability of plus or minus 0.01 standard pH unit. Meters used for pH field measurement should be of

rugged construction. A foam-lined carrying case is convenient both for transport and for use as a work

table. Battery-operated meters with easily replaceable or rechargeable batteries are required. Also, a spare

pH electrode should be available in the field. Both the spare and working electrodes should be immersed in

a pH 4 or pH 7 buffer solution when not in use.

The following are recommended for field measurement of pH:

• pH meter with repeatability of ±0.01 standard pH unit

• Buffer solutions of pH 4, 7, and 10

• pH electrode (probe)

• Electrode filling solution

• Electrode holder

• Calibrated thermometer

• Deionized water and wash bottle

• Disposable beakers

• Logbook or field sheets

2.0 PROCEDURES

Meter calibration and field measurement procedures are outlined in the following subsections.



2.1 CALIBRATION

Commercially prepared buffer solutions should be used for calibration. Solutions traceable to the National

Institute of Standards and Technology can be purchased inexpensively from any major laboratory supply

company. These solutions are certified with an accuracy of plus or minus 0.01 pH unit at a specific

temperature, usually 25 EC. Theoretically, buffer solutions are stable indefinitely. However, they are

susceptible to contamination, and old, partially full bottles should be replaced.

Because various terms are used to describe the pH meter calibration process, providing a detailed set of

instructions for each type of instrument is not practical. Always refer to the manufacturer’s instructions

when using a particular instrument. The general procedure below can be used to calibrate any pH meter.

1. Calibrate the meter with two buffer solutions to determine if the electrodes are in workingorder. The slope cannot be adjusted with a one-point calibration.

2. To calibrate the meter, use one buffer solution with a pH greater than and one buffersolution with a pH less than the anticipated pH of the sample. For example, for ananticipated pH of 6, calibrate with pH 4 and pH 7 buffers; for an anticipated pH of 8,calibrate with pH 7 and pH 10 buffers.

3. Ensure that the buffers are at the same temperature as the sample (within 2 EC). Pouraliquots into small containers; never put the electrode into the buffer storage bottles.

4. Adjust the instrument to read the pH 7 buffer accurately. Adjust the temperaturecompensator according to the manufacturer’s instructions. Be sure to rinse the probe withdeionized water after taking the calibration measurement.

5. Adjust the instrument to read the pH of the second buffer accurately. If it is not possibleto adjust the instrument to read the pH of buffer solutions accurately, check for a defectiveelectrode or contaminated buffer solution. Be sure to rinse the probe with deionized waterafter taking the calibration measurement.

6. The meter must be calibrated before the start of each work day. Check the calibrationperiodically and recalibrate if necessary.



2.2 FIELD MEASUREMENT

Do not filter field samples prior to analysis. When measuring the pH of groundwater samples, use a

submersible pump or bladder pump to obtain the sample to minimize the release of gas from the sample.

The procedure below should be used for field measurement of pH.

1. Calibrate the instrument and set the temperature compensation in accordance with themanufacturer’s instructions.

2. Collect the sample to be measured in a prerinsed jar or beaker or a flow-through cell.

3. Measure the temperature of the sample to the nearest 0.1 EC.

4. Set the temperature compensation on the pH meter to the temperature of the sample,following the manufacturer’s instructions.

5. Rinse the probe with deionized water.

6. Immerse the probe in the sample. Record the pH value indicated. If the sample is beingpumped through a closed container, wait for the temperature and pH to stabilize. Stopsample flow to eliminate streaming potential. Record the pH value indicated.

7. Record measurements in a logbook, on field sheets, or as specified in the project workplan.

3.0 POTENTIAL PROBLEMS

Temperature, atmospheric contamination, and ionic strength are factors that may affect pH measurements.

Each of these three factors is discussed below. Color, turbidity, and colloids will not affect pH

measurements.

Temperature: As indicated in Table 1, pH is affected by temperature. To prevent this from causing

incorrect pH readings, the temperature compensator on the pH meter must be set to the temperature of the

sample. Also, the meter must be calibrated at approximately this same temperature. The temperatures of

the buffer and the unknown liquid should both be recorded at the time of measurement. Ideally, their

temperatures should be within 2 EC of each other.



Atmospheric Contamination: Atmospheric contamination can be a significant problem when sampling the

pH of groundwater. When the sample is exposed to air, dissolved oxygen and carbon dioxide can change a

sample’s pH. To ensure that this problem does not affect the pH measurement, a groundwater sample

should ideally be pumped through a closed container in which pH and temperature probes are immersed.

The measurements should not be recorded until both temperature and pH have stabilized. The sampling

pump should be stopped before recording the data because a streaming potential will affect the

measurement in a flowing sample.

Ionic Strength: Because of the potential for errors due to ionic strength, pH measurement should always

be accompanied by a measurement of specific conductance.

In general terms, pH is a measure of hydrogen ion activity. Normally, water samples are assumed to be

ideal solutions in which other ions do not affect hydrogen ion activity. However, if the ionic strength is too

high, this assumption does not hold true. Some site investigations include sampling of waste ponds or other

highly contaminated water that has very high ionic strength. Because buffer solutions used in the field are

not made with a similarly high concentration of dissolved ions, pH measurement of highly contaminated

water will be inaccurate. Similarly, pH measurement of samples with very low ionic strength will be

inaccurate because the low ionic strength of the sample approaches the level of resistance in the glass

electrode. To reduce this problem, samples with very low ionic strength should be stirred for a few seconds

before taking a reading. Even then, several minutes may be required for the reading to stabilize.

High sodium concentration also may produce errors in pH measurement because of the high ionic strength

of these solutions. To measure the pH of such solutions, a special electrode is needed. Such an electrode

can be purchased from any of several electrode manufacturers.



TABLE 1

pH OF BUFFER SOLUTIONS AS A FUNCTION OF TEMPERATURE

Standard

Buffer Solution pH

4.0 7.0 10.0

Temperature (EC)

0 4.01 7.13 10.34

5 3.99 7.10 10.26

10 4.00 7.07 10.19

15 3.99 7.05 10.12

20 4.00 7.02 10.06

25 4.00 7.00 10.00

30 4.01 6.99 9.94

SOP APPROVAL FORM

TETRA TECH EM INC.


FIELD MEASUREMENT OF SPECIFIC CONDUCTANCE

SOP NO. 013

REVISION NO. 2


May 18, 1993


Tetra Tech EM Inc. - Environmental SOP No. 013 Page 1 of 6Title: Field Measurement of Specific Conductance Revision No. 2, May 18, 1993


1.0 BACKGROUND

Specific conductance is a widely used parameter for evaluating groundwater and surface water quality. It is

a simple indicator of change within a system and provides useful information to laboratory personnel

performing other measurements on a water sample.

1.1 PURPOSE

Specific conductance should be determined at the time the sample is collected. This standard operating

procedure (SOP) establishes the requirements and procedures for measuring the specific conductance of

groundwater or surface water in the field.

1.2 SCOPE

This SOP applies to the use of specific conductance meters in the field.

1.3 DEFINITION

Specific Conductance - Specific conductance is the reciprocal of electrical resistivity. The values of

electrical resistivity and specific conductance depend on the number of ions in a solution. Pure water has

100 percent resistivity and no specific conductance. As ions are added to a solution, resistivity drops and

specific conductance increases.

1.4 REFERENCES

U.S. Environmental Protection Agency. 1996. “Test Methods for Evaluating Solid Waste, Volume 1C:Laboratory Manual Physical/Chemical Methods, SW-846.”

American Society for Testing and Materials Annual Book of Standards. “Standard Test Methods forElectrical Conductivity and Resistivity of Water, Method D-1125.”

U.S. Geological Survey. 1977. National Handbook of Recommended Methods for Water DataAcquisition.




Specific conductance meters should measure temperature, have a temperature compensator, and read

directly in micromhos per centimeter (Fmhos/cm), corrected to 25 EC. For field measurements, a probe-

type unit is preferred over a pipet-type unit. Specific conductance meters should have a foam-lined carrying

case and should be battery-operated with easily rechargeable or replaceable batteries. A relative accuracy

of plus or minus 3 percent is adequate.

The following are required for calibrating a specific conductance meter and for the field measurement of

specific conductance:

• A probe-type specific conductance meter meeting the requirements given above

• Deionized water and wash bottle

• Disposable beakers

• Reagent-grade potassium chloride (KCl) or a commercially-prepared, standard 0.01 molar(M) KCl solution

• Sampling containers

• Sampling equipment

• 1-liter mixing container

• Calibrated thermometer

• Field logbook

2.0 PROCEDURES

Meter calibration and field measurement procedures are outlined in the following subsections.



K 'C1 % C2

106 x C3

2.1 METER CALIBRATION

Reagent-grade KCl is the universal standard for calibrating specific conductance equipment. The electrodes

are calibrated by reading the specific conductance of standard KCl solutions. A concentration of 0.01 M

KCl should be used because its specific conductance is closest to that of most natural samples.

The measuring circuit of the specific conductance meter is calibrated either by the manufacturer or with a

calibrating resistor. The manufacturer’s instructions for the particular instrument should be followed for

calibrating the specific conductance meter.

Individual manufacturers may use slightly different terminology, but the following general procedure will

always apply:

1. Prepare a 0.01 M KCl solution by dissolving 0.745 gram of pure, dry KCl in 1 liter ofdeionized water. The base conductivity for the prepared solution is 1,408.1 Fmhos/cm at25 EC; if the deionized water has any conductance, it must be corrected to 25 EC andadded to the value of the solution. Alternatively, commercially prepared solutions can beused.

2. Measure the temperatures of the 0.01 M KCl solution and the deionized water used for thedilution. They should be at the same temperature (±0.2 EC).

3. Using Table 1, determine the expected specific conductance of the 0.01M KCl solution atthe temperature measured.

4. Measure the specific conductance of the 0.01M KCl solution and of the deionized water.

5. Use the following equation to check the cell constant specified by the manufacturer:

whereK = the cell constantC1 = the specific conductance of the deionized waterC2 = the specific conductance of the 0.01 M KCl solutionC3 = the expected specific conductance from the Table 1

6. A measured cell constant different from that specified by the manufacturer generallyindicates that the electrodes are dirty. If this is the case, replace the electrode with a clean



spare or clean and replatinize the electrode in accordance with instructions in themanufacturer’s manual or in the American Society for Testing and MaterialsMethod D-1125, Section 8.3.

7. After verifying that the cell constant is acceptable, measure the specific conductance ofsamples in accordance with to the procedure given in Section 2.2.

2.2 FIELD MEASUREMENT

Do not filter samples before analysis. To minimize gas releases from groundwater samples, a submersible

pump or bladder pump should be used to obtain samples.

The following procedure should be used for field measurement of specific conductance:

1. Calibrate the instrument and check the cell constant in accordance with the manufacturer’sinstructions and the procedure provided in Section 2.1.

2. Collect the sample in a prerinsed jar or beaker or a flow-through cell.

3. Rinse the specific conductance meter probe with deionized water.

4. Using a thermometer or the specific conductance meter itself, measure and record thetemperature of the sample in EC.

5. Immerse the specific conductance meter probe in the sample. Record the reading inFmhos/cm.

6. Record measurements in the field logbook or as specified in the project work plan.

3.0 POTENTIAL PROBLEMS

Principal problem areas for specific conductance measurement are the temperature effect, determination of

the cell constant, and allowance for very high ionic strengths. A change in temperature of 10 EC can cause

a 20 percent change in the measured specific conductance. Reported data should note whether temperature

correction has been applied. Some instruments perform temperature correction automatically, but this, too,

should be noted for the reported data. All data should be corrected to 25 EC.



Field personnel must be aware that a significant change in the cell constant indicates that the electrodes

require cleaning or replacement. The constant should be checked at each calibration, as described in

Section 2.1.

Specific conductance varies directly with ion concentrations up to a specific conductance of about

5,000 Fmhos/cm. Samples collected at most sites seldom have a specific conductance greater than

5,000 Fmhos/cm. Readings above this level should not be considered accurate. However, such

readings can still provide useful information about the relative levels of conductance and should be noted.



TABLE 1

RELATIONSHIP OF TEMPERATURE AND SPECIFIC CONDUCTANCEFOR 0.01 M POTASSIUM CHLORIDE SOLUTION

Temperature(EC)

Expected Specific Conductance

of 0.01 M KCl Solution(Fmhos/cm)

15 1,141.5

16 1,167.5

17 1,193.6

18 1,219.9

19 1,246.4

20 1,273.0

21 1,299.7

22 1,326.6

23 1,353.6

24 1,380.8

25 1,408.1

26 1,436.5

27 1,463.2

28 1,490.9

29 1,518.7

30 1,546.7

SOP APPROVAL FORM TETRA TECH EM INC. ENVIRONMENTAL STANDARD OPERATING PROCEDURE RECORDING OF NOTES IN FIELD LOGBOOK SOP NO. 024 REVISION NO. 1 May 18, 1993 Last Reviewed: December 2008

December 5, 2008 Quality Assurance Approved Date

Tetra Tech EM Inc. – Environmental SOP No. 024 Page 1 of 6Title: Recording of Notes in Field Logbook Revision No. 1, May 18, 1993

Last Reviewed: December 2008

1.0 BACKGROUND

The field logbook should contain detailed records of all the field activities, interviews of people, and

observations of conditions at a site. Entries should be described in as much detail as possible so that

personnel can accurately reconstruct, after the fact, activities and events during their performance of field

assignments. Field logbooks are considered accountable documents in enforcement proceedings and may

be subject to review. Therefore, the entries in the logbook must be accurate and detailed; and they must

reflect the importance of the field events.

1.1 PURPOSE

The purpose of this standard operating procedure (SOP) is to provide guidance to ensure that logbook

documentation for any field activity is correct, complete, and adequate. Logbooks are used for

identifying, locating, labeling, and tracking samples. A logbook should document any deviations from

the project approach, work plans, quality assurance project plans, health and safety plans, sampling plans,

and any changes in project personnel. They also serve as documentation of any photographs taken during

the course of the project. In addition, the data recorded in the logbook may assist in the interpretation of

analytical results. A complete and accurate logbook also aids in maintaining good quality control.

Quality control is enhanced by proper documentation of all observations, activities, and decisions.

1.2 SCOPE

This SOP establishes the general requirements and procedures for recording notes in the field logbook.

1.3 DEFINITIONS

None

1.4 REFERENCES

Compton, R.R. 1985. Geology in the Field. John Wiley and Sons. New York, N.Y.




The following items are required for field notation:

• Field logbooks

• Ballpoint pens with permanent ink

• 6-inch ruler (optional)

Field logbooks should be bound (sewn) with water-resistant and acid-proof covers; they should have

preprinted lines and wide columns. They should be approximately 7 1/2 by 4 1/2 inches or 8 1/2 by 11

inches in size. Loose-leaf sheets are not acceptable for field notes. If notes are written on loose paper,

they must be transcribed as soon as possible into a regular field logbook by the same person who recorded

the notes.

Logbooks can be obtained from an individual’s office supply room or directly from outside suppliers.

Logbooks must meet the requirements specified in this SOP and should include preprinted pages that are

consecutively numbered. If the numbers must be written by hand, the numbers should be circled so that

they are not confused with data.

2.0 PROCEDURES

The following subsections provide general guidelines and formatting requirements for field logbooks, and

detailed procedures for completing field logbooks.

2.1 GENERAL GUIDELINES

• A separate field logbook must be maintained for each project. If a site consists of multiple subsites, designate a separate logbook for each subsite. For special tasks, such as periodic well water-level measurements, data from multiple subsites may be entered into one logbook that contains only one type of information.

• All logbooks must be bound and contain consecutively numbered pages.

• No pages can be removed from the logbook for any purpose.



• All field activities, meetings, photographs, and names of personnel must be recorded in the site logbook.

• Each logbook pertaining to a site or subsite should be assigned a serial number based on the date the logbook is issued to the project manager. The first issued logbook should be assigned number 1, the next issued logbook assigned number 2, and so on. The project manager is to maintain a record of all logbooks issued under the project.

• All information must be entered with a ballpoint pen with waterproof ink. Do not use pens with “wet ink,” because the ink may wash out if the paper gets wet. Pencils are not permissible for field notes because information can be erased. The entries should be written dark enough so that the logbook can be easily photocopied.

• Do not enter information in the logbook that is not related to the project. The language used in the logbook should be factual and objective.

• Begin a new page for each day’s notes.

• Write notes on every line of the logbook. If a subject changes and an additional blank space is necessary to make the new subject title stand out, skip one line before beginning the new subject. Do not skip any pages or parts of pages unless a day’s activity ends in the middle of a page.

• Draw a diagonal line on any blank spaces of four lines or more to prevent unauthorized entries.

2.2 LOGBOOK FORMAT

The layout and organization of each field logbook should be consistent with other field logbooks.

Guidelines for the cover, spine, and internal pagination are discussed below.

2.2.1 FORMAT OF FIELD LOGBOOK COVER AND SPINE

Write the following information in clear capital letters on the front cover of each logbook using a

Sharpie® or similar type permanent ink marker:

• Logbook identification number

• The serial number of the logbook (assigned by the project manager)

• Name of the site, city, and state

• Name of subsite if applicable

• Type of activity



• Beginning and ending dates of activities entered into the logbook

• “Tetra Tech EM Inc.” City and State

• “REWARD IF FOUND”

Some of the information listed above, such as the list of activities and ending dates, should be entered

after the entire logbook has been filled or after decision that the remaining blank pages in the logbook will

not be filled.

The spine of the logbook should contain an abbreviated version of the information on the cover: for

example, “1, Col. Ave., Hastings, 5/88 - 8/88.”

2.2.2 First Page of the Field Logbook

Spaces are usually provided on the inside front cover (or the opening page in some logbooks), for the

company name (“Tetra Tech EM Inc.”), address, contact name, and telephone number. If preprinted

spaces for this information are not provided in the logbook, write the information on the first available

page.

2.3 ENTERING INFORMATION IN THE LOGBOOK

Enter the following information at the beginning of each day or whenever warranted during the course of

a day:

• Date

• Starting time

• Specific location

• General weather conditions and approximate temperature

• Names of personnel present at the site. Note the affiliation(s) and designation(s) of all personnel

• Equipment calibration and equipment models used.

• Changes in instructions or activities at the site

• Levels of personal protective clothing and equipment



• A general title of the first task undertaken (for example, well installation at MW-11, decon at borehole BH-11, groundwater sampling at MW-11)

• Approximate scale for all diagrams. If this can’t be done, write “not to scale” on the diagram. Indicate the north direction on all maps and cross-sections. Label features on each diagram.

• Corrections, if necessary, necessarily including a single line through the entry being corrected. Initial and date any corrections made in the logbook.

• After last entry on each page, initials of the person recording notes. No information is to be entered in the area following these initials.

• At the end of the day, signature of the person recording notes and date at the bottom of the last page. Indicate the end of the work day by writing “Left site at (time).” A diagonal line must be drawn across any remaining blank space at the bottom of this last page.

The following information should be recorded in the logbook after taking a photograph:

• Time, date, location, direction, and, if appropriate, weather conditions

• Description of the subject photographed and the reason for taking the picture

• Sequential number of the photograph and the film roll number or disposable camera used (if applicable)

• Name of the photographer.

The following information should be entered into the logbook when collecting samples:

• Location description

• Name(s) of sampler(s)

• Collection time

• Designation of sample as a grab or composite sample

• Type of sample (water, sediment, soil gas, etc.)

• On-site measurement data (pH, temperature, specific conductivity)

• Field observations (odors, colors, weather, etc.)

• Preliminary sample description

• Type of preservative used

• Instrument readings.



If pre-printed field data forms are available (forms such as the micropurge field data collection form),

data should be entered on these pre-printed forms rather than into field logbooks. Note in the logbook

that the field data are recorded on separate forms.

2.4 PRECAUTIONS

Custody of field logbooks must be maintained at all times. Field personnel must keep the logbooks in a

secure place (locked car, trailer, or field office) when the logbook is not in personal possession.

Logbooks are official project documents and must be treated as such.

SOP APPROVAL FORM

TETRA TECH EM INC.


FIELD MEASUREMENT OF GROUNDWATER INDICATOR PARAMETERS

SOP NO. 061

REVISION NO. 2

Last Reviewed: July 2009

July 2009 Quality Assurance Approved

Date

Tetra Tech EM Inc. - Environmental SOP No. 061 Page 1 of 9 Title: Field Measurement of Groundwater Revision No. 2, July 2009 Indicator Parameters Last Reviewed: July 2009

1.0 BACKGROUND

Various water quality monitoring systems can be used for determining groundwater indicator parameters

in the field. Commonly measured field indicator parameters include pH, specific conductance,

temperature, oxidation-reduction potential (ORP), dissolved oxygen (DO) and turbidity. Groundwater

field measurements are typically collected in conjunction with groundwater sampling or monitoring well

development (see SOPs 010, 015, and 021).

Various types of water quality systems exist including down-hole systems and flow through cells. Tetra

Tech used several common water quality meters including various types of In-Situ, YSI, Hydac, and

Horiba meters (see Figure 1 at the end of this SOP). The sampling team should select the type of meter or

monitoring system based on site-specific conditions including data collection needs, the types of wells

being sampled, and the sampling procedures used. Multiple parameter systems should be used when

multiple field parameters are to be measured.

1.1 PURPOSE

This standard operating procedure (SOP) establishes the general requirements and procedures for using

various water quality monitoring systems for determining groundwater pH, specific conductance,

temperature, ORP, DO and turbidity in the field.

1.2 SCOPE

This SOP applies to general procedures for calibrating and operating water quality monitoring systems in

the field. The project work plan or field sampling plan should identify the types of systems to be used

and the actual project-specific field parameters to be measured. For each type of water quality system,

the manufacturer’s manual should be consulted for specific operating instructions.


1.3 DEFINITIONS

Single Parameter System: A meter or monitoring system consisting of a single probe designed to

measure a single indicator parameter.

Multiple Parameter System: A meter or monitoring system consisting of multiple probes capable of

measuring multiple indicator parameters.

Open Container Measurements: Field measurements performed in an open container such as a cup, a

jar, or a bucket where an air/water interface exists.

Flow-Through Chamber or Cell: A plastic cell or chamber connected to the sample pump discharge

tubing so that a continuous flow of water passes across the probes. Additional tubing is used to route

water from the flow-through cell to a waste container or final discharge point.

Down-Hole Monitoring System: A meter or monitoring system where probes are submerged by

inserting them into the well. The probes are attached to the meter (located at the well head or ground

surface) by one or more cables.

pH: A measure of the acidity or alkalinity of a solution. The pH scale ranges from 0 to 14 with strongly

acidic solutions at the low end, strongly basic solutions at the high end, and “pure” or neutral water at 7.

Field measurements of pH are recorded in standard units.

Specific Conductance: The ability of a solution to conduct electricity; a measure of the solution’s ionic

activity and content. The higher the concentration of ionic (dissolved) constituents, the higher the

conductivity. Conductivity of the same water changes substantially with temperature. Specific

conductivity is generally found to be a good measure of the concentration of total dissolved solids (TDS)

and salinity. Conductivity is measured by placing two electrodes (with opposite electrical charge) in the

water. For a known electrical current, the voltage drop across the electrodes reveals the solution’s

resistance. Since the resistance of aqueous solution changes with temperature (resistance drops with

increasing temperature), the resistance is corrected to the resistance of the solution at 25 ºC. Field

measurements are recorded in units of microsiemens per centimeters (µS/cm).


Temperature: The degree of hotness or coldness of the solution being measured. Field measurements

are typically recorded in degrees Celsius (°C).

ORP: ORP, or redox potential, is the tendency of a chemical species to acquire electrons and be reduced.

In aqueous solutions, the reduction potential is the tendency of the solution to either gain or lose

electrons when new chemical species are introduced. A solution with a higher (more positive) reduction

potential than the new species will have a tendency to gain electrons from the new species (to be reduced

by oxidizing the new species) and a solution with a lower (more negative) reduction potential will have a

tendency to lose electrons to the new species (to be oxidized by reducing the new species). Just as the

transfer of hydrogen ions between chemical species determines the pH of an aqueous solution, the transfer

of electrons between chemical species determines the reduction potential of an aqueous solution. Like

pH, the reduction potential represents an intensity factor. It does not characterize the capacity of the

system for oxidation or reduction, in much the same way that pH does not characterize the buffering

capacity. Field measurements are typically recorded in millivolts (mV).

DO: Dissolved oxygen (or oxygen saturation) is a relative measure of the amount of oxygen dissolved or

carried in a given medium. In aquatic environments, dissolved oxygen is a relative measure of the

amount of oxygen (O2) dissolved in the water. Field measurements are typically recorded in milligrams

per liter (mg/L).

Turbidity: Turbidity is the cloudiness or haziness of a fluid caused by individual particles (suspended

solids). Fluids can contain suspended solid matter consisting of particles of many different sizes. While

some suspended material will be large enough and heavy enough to settle rapidly to the bottom of the

container if a liquid sample is left to stand, very small particles will settle only very slowly or not at all if

the sample is regularly agitated or the particles are colloidal. These small solid particles cause the liquid

to appear turbid. Field measurements are typically recorded in Nephelometric Turbidity Units (NTU).

1.4 REFERENCE

Essential Handbook of Ground-Water Sampling by Gillian Nielsen, 2007.

Tetra Tech EM Inc. July 2009. SOPs 010, 015, and 021



The following items are typically required to measure groundwater pH, specific conductance,

temperature, ORP, DO, and turbidity using this SOP:

• Single or multiple parameter water quality measuring system

• Specific conductance calibration solutions

• Buffer solutions of pH 4, 7, and 10 for pH calibration

• Distilled or deionized water

• Rinse bottle

• 50-milliliter (mL) sample cups or beakers

• Sample tubing and connectors (specific to each type of system)

• Waste container to collect purge water

• Logbook or field data sheets

2.0 PROCEDURES

The procedures outlined in this SOP are general and may apply to various types of water quality

monitoring systems to measure groundwater pH, specific conductance, temperature, ORP, DO and

turbidity in the field. General procedures for testing and calibrating the monitoring systems are presented

first, followed by procedures for using the instruments and making field measurements. Each particular

monitoring system should be identified in the project work plan or field sampling plan and should be

operated in accordance with the manufacturer’s instruction manual.


2.1 TESTING AND CALIBRATION PROCEDURES

Each field meter or monitoring system should be calibrated according to manufacturer’s specifications.

In general, equipment should be thoroughly cleaned then calibrated and tested before the start-up of

sampling at each site. Equipment should be calibrated and tested using manufacturer provided solutions

and standards. Care should be taken to rinse the probes between testing and calibration to prevent cross

contaminating solutions. Solutions should be poured from the manufacturer’s container into another

container to prevent compromising the entire solution provided by the manufacturer. Calibration and

testing of field equipment should be documented each time it is performed in field logbooks (or field data

sheets, if applicable). If testing and calibration measurements are out of tolerance, the instrument must be

serviced or repaired.

2.2 FIELD MEASUREMENT PROCEDURES

Each field meter or monitoring system should be operated according to manufacturer’s specifications.

The actual field procedures will vary depending on the type of monitoring system being used (open

container systems, flow-through cell systems, or down-hole systems) and the types of field parameters

being measured. In addition, most systems include a data logging option. A description of open

container, flow-through cell, and down-hole measurement processes are discussed below, followed by a

general procedural summary and a summary of common errors associated with field measurements of

indicator parameters.

2.2.1 Open Container Measurements

Open container measurements consist of collecting groundwater and placing it in a cup or container for

field measurements using a hand held system. This method of field measurements is commonly used

when bailing wells, but can also be used when pumping wells. Prior to field measurements, the

equipment must be cleaned and calibrated following manufacturer’s specifications. Field measurements

should then be made at the frequency and for the indicator parameters specified in the project work plan

or field sampling plan. To make open container field measurements, samplers collect groundwater from

the well and place in a cup or container large enough to adequately submerge the probe or probes, as

specified in the manufacturer’s operations manual. For open containers, measurements should be taken in

the following order: temperature, specific conductance, pH, and turbidity. Open container systems are

not recommended for low-flow sampling as flow-through systems are more appropriate. The probes and


cup or container should be thoroughly rinsed after each field measurement and between sampling

locations.

2.2.2 Flow-Through Cell Measurements

Flow-through cell systems consist of measuring groundwater parameters as a continuous flow of water

passes across the probes through a cell or chamber, and is primarily used when pumping wells and using

low-flow sampling procedures. Prior to field measurements, the equipment must be cleaned and

calibrated following manufacturer’s specifications. Field measurements should then be made at the

frequency and for the indicator parameters specified in the project work plan or field sampling plan.

The flow-through cell or chamber is placed “in line” between the discharge tubing of the pump and the

container used to collect purged water. The outlet from the pump must be connected to the sample

chamber input. The sample chamber outlet must then be connected or routed to a waste container (or to

another designated discharge point). Tubing, fittings, and adaptors are generally required and may be

provided by the manufacturer. Pump discharge tubing and chamber inlets and outlets are typically 1/2 or

3/8 inch diameter.

After the cell or chamber is connected to the pump discharge tubing and waste collection container, the

sensors should be inserted into the sensor mounting plate in their respective ports. Any unused sensor

ports must have plugs installed to close off the sample chamber. The probe cables are then connected to

the meter following manufacturer’s specifications.

With the system connected, the sampler should turn on the pump according to the manufacturer’s

instructions and then turn on the water quality monitor. Before recording any values, the sample chamber

should be full, all air should be voided, and all of the displayed values should be stable. The probes and

sample chamber should be thoroughly rinsed between sampling locations.

2.2.3 Down-Hole Measurements

Down-hole measurement systems consist of inserting the probes (or a multi-parameter sensor housing)

inside a well to obtain field measurements, and is primarily used when pumping wells. Prior to field

measurements, the equipment must be cleaned and calibrated following manufacturer’s specifications.


Field measurements should then be made at the frequency and for the indicator parameters specified in

the project work plan or field sampling plan.

The probes or sensor are attached to a hand held meter or control unit by a cable and lowered inside the

well to be sampled. Limiting factors when using down-hole systems include probe or sensor diameters

and available cable lengths. The probes should be thoroughly decontaminated between sampling

locations...

2.2.4 General Procedures for Field Measurements of Indicator Parameters

The following section discusses general procedures that typically apply to making field measurements of

indicator parameters using various types of field instruments. Each particular type of meter or monitoring

system should be identified in the project work plan or field sampling plan and should be operated in

accordance with the manufacturer’s instruction manual.

1. Inspect the instrument and batteries prior to the field effort.

2. Check the integrity of the buffer solutions used for field calibration since frequent replacement is necessary as a result of degradation upon exposure to the atmosphere.

3. If applicable, make sure all electrolyte solutions within the electrode(s) are at proper levels and no air bubbles are present within the electrode(s).

4. Calibrate the meter and electrode(s) on a daily use basis (or as recommended) following manufacturer's instructions and record data in field logbook or on field data sheets.

5. Immerse the electrode(s) in the sample. Stabilization may take several seconds to several minutes. If the parameter values continues to drift, the sample temperature may not be stable, a physical reaction (e.g., degassing) may be occurring in the sample, or the meter or electrode may be malfunctioning. The failure of the measurements to stabilize should be clearly noted in the logbook or field data sheet. For DO, provide for sufficient flow past the membrane by gently stirring the sample. Probes without stirrers placed in wells (down-hole measurements) may be gently moved up and down to achieve the required mixing.

6. Read and record the value of each parameter being measured making sure units of measure are clearly recorded.

7. Rinse the electrode(s) with deionized water.

8. Store the electrode(s) in accordance with manufacturer’s instructions


2.2.5 Common Errors or Problems Associated With Field Measurements

The project work plan or field sampling plan should clearly identify the types of parameters to be

measured, the measurement frequency, and “stabilization” requirements. It is essential to ensure that the

type of monitoring system selected is compatible with the monitoring well sampling or development

methods to be utilized. Some common errors to avoid are identified below:

• No, or incorrect equipment calibration

• Incorrect or expired calibration standards

• Poor equipment maintenance

• Inadequate training or unfamiliarity with equipment

• No record of units of measure and “+” or “-“ values for ORP

• Too much time taken to measure temperature sensitive parameters

• DO and ORP measured in closed systems (flow-through cell or down-hole) instead of closed cell systems


FIGURE 1 THE HORIBA U-10 WATER QUALITY MONITORING SYSTEM

THE IN-SITU TROLL 9500 LOW-FLOW SYSTEM THE YSI HAND HELD 556 METER

Horiba U-10

In-Situ Troll

YSI 556


Appendix B. Lab Reports

January 09, 2015Date:STAT Analysis Corporation

Project: Pecatonica TMDL, Freeport, ILClient: Tetra Tech EM Inc.

Work Order: 14120344Work Order Sample Summary

Lab Sample ID Client Sample ID Collection DateTag Number Date Received

Revision 1

14120344-001A WC01 - 121114 12/11/2014 9:14:00 AM 12/11/201414120344-001B WC01 - 121114 12/11/2014 9:14:00 AM 12/11/201414120344-002A WC01 - 121114-D 12/11/2014 9:14:00 AM 12/11/201414120344-003A SB02 - 121114 12/11/2014 11:28:00 AM 12/11/201414120344-004A SB03 - 121114 12/11/2014 12:15:00 PM 12/11/201414120344-005A SB01 - 121114 12/11/2014 1:56:00 PM 12/11/201414120344-006A SB01 - 121114-D 12/11/2014 1:56:00 PM 12/11/2014

Page 2 of 14

January 09, 2015Date:STAT Analysis Corporation

Project: Pecatonica TMDL, Freeport, ILCLIENT: Tetra Tech EM Inc.

Work Order: 14120344CASE NARRATIVE

Revision 1

Phosphate results for samples SB01 - 121114 (14120344-005A) and SB01 - 121114-D (14120344-006A) were initially reported as Phosphate as PO4. The report contains Phosphate results expressed as Phosphorus (as P).

Total Kjedahl Nitrogen analysis was subcontracted to First Environmental Laboratories, Naperville, IL NELAP 100292.

Page 3 of 14


Work Order: 14120344

Date Printed: January 09, 2015

STAT Analysis Corporation2242 West Harrison St., Suite 200, Chicago, IL 60612-3766Tel: (312) 733-0551 Fax: (312) 733-2386 [email protected]

Date Reported: January 09, 2015

Accreditations:IEPA ELAP 100445;ORELAP IL300001;AIHA-LAP, LLC 101160;NVLAP LabCode 101202-0

ANALYTICAL RESULTS

Revision 1

Client Sample ID:WC01 - 121114Lab ID: 14120344-001 Collection Date: 12/11/2014 9:14:00 AM

Matrix: Water

Analyses Result Qualifier Units Date AnalyzedRL DF

Phosphorus (as P) SM4500P,B,E Analyst: YZPrep Date: 12/16/2014Phosphorus (as P) * 12/16/20140.050 mg/L 10.10

Total Suspended Solids E160.2 Analyst: RWPrep Date: 12/12/2014Total Suspended Solids * 12/12/20147.5 mg/L 1ND

Client Sample ID:WC01 - 121114-DLab ID: 14120344-002 Collection Date: 12/11/2014 9:14:00 AM

Matrix: Water


Total Suspended Solids E160.2 Analyst: RWPrep Date: 12/12/2014Total Suspended Solids * 12/12/20147.5 mg/L 1ND

Client Sample ID:SB02 - 121114Lab ID: 14120344-003 Collection Date: 12/11/2014 11:28:00 AM

Matrix: Water


Total Kjeldahl Nitrogen M4500-NORG Analyst: SUBPrep Date:Total Kjeldahl Nitrogen * 12/18/20141.0 mg/L 1ND

Nitrate and Nitrite M4500-NO3F Analyst: YZPrep Date: 12/13/2014Nitrogen, Nitrate-Nitrite 12/13/20140.20 mg/L 19.5

Ammonia as Nitrogen E350.1 Analyst: YZPrep Date: 12/16/2014Nitrogen, Ammonia (As N) * 12/16/20140.050 mg/L 10.071

Qualifiers: J - Analyte detected below quantitation limitsB - Analyte detected in the associated Method Blank

S - Spike Recovery outside accepted recovery limitsR - RPD outside accepted recovery limits

ND - Not Detected at the Reporting Limit

E - Value above quantitation range* - Non-accredited parameter H - Holding time exceededHT - Sample received past holding time

RL - Reporting / Quantitation Limit for the analysis

Page 4 of 14







ANALYTICAL RESULTS

Revision 1

Client Sample ID:SB03 - 121114Lab ID: 14120344-004 Collection Date: 12/11/2014 12:15:00 PM

Matrix: Water



Nitrate and Nitrite M4500-NO3F Analyst: YZPrep Date: 12/13/2014Nitrogen, Nitrate-Nitrite 12/13/20140.20 mg/L 114


Client Sample ID:SB01 - 121114Lab ID: 14120344-005 Collection Date: 12/11/2014 1:56:00 PM

Matrix: Water





Phosphorus (as P) SM4500P,B,E Analyst: YZPrep Date: 1/8/2015Phosphorus (as P) * 1/8/20150.062 mg/L 1.250.16






Page 5 of 14







ANALYTICAL RESULTS

Revision 1

Client Sample ID:SB01 - 121114-DLab ID: 14120344-006 Collection Date: 12/11/2014 1:56:00 PM

Matrix: Water











Page 6 of 14

Project: Pecatonica TMDL, Freeport, IL

CLIENT: Tetra Tech EM Inc.Work Order: 14120344

ANALYTICAL QC SUMMARY REPORT

BatchID: 81514Wet Chemistry

QC SUMMARY

PREP SUMMARY

Sample ID:NH4MBW1 121614

TestNo:E350.1

Analysis Date:12/16/2014

Prep Date:12/16/2014

Analyte Result SPK valueSPK

Ref Val % RECRPD

Ref Val %RPDLow Limit

High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:LACHAT_141216E

SeqNo:2870200MBLK

SampType:

Nitrogen, Ammonia (As N) *0.050ND

Sample ID:NH4LCSW1 121614

TestNo:E350.1




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2870201LCS

SampType:

Nitrogen, Ammonia (As N) 2.5 87.6 80 120 *0.050 0 0 02.191

Sample ID:14120344-005AMS

TestNo:E350.1




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB01 - 121114


SeqNo:2870203MS

SampType:

Nitrogen, Ammonia (As N) 2.5 89.2 75 125 *0.050 0.1247 0 02.354

Sample ID:14120344-005AMSD

TestNo:E350.1




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB01 - 121114


SeqNo:2870204MSD

SampType:

Nitrogen, Ammonia (As N) 2.5 87.4 75 125 20 *0.050 0.1247 2.354 1.832.311

Sample ID Matrix pH SampAmt Sol Added Sol Recov Fin Vol factor PrepStart PrepEnd12/16/201412/16/20141.000NH4MBW1 121614 50 500 0

12/16/201412/16/20141.000NH4LCSW1 121614 50 500 012/16/201412/16/20141.00014120344-003A 50 500 0Water

12/16/201412/16/20141.00014120344-004A 50 500 0Water

12/16/201412/16/20141.00014120344-005A 50 500 0Water

12/16/201412/16/20141.00014120344-005AMS 50 500 0Water

12/16/201412/16/20141.00014120344-005AMSD 50 500 0Water

12/16/201412/16/20141.00014120344-006A 50 500 0Water

12/16/201412/16/20141.000IDOC1 50 500 0

12/16/201412/16/20141.000IDOC2 50 500 0

12/16/201412/16/20141.000IDOC3 50 500 0

12/16/201412/16/20141.000IDOC4 50 500 0

Qualifiers: J - Analyte detected below quantitation limits

B - Analyte detected in the associated Method BlankS - Spike Recovery outside accepted recovery limits

R - RPD outside accepted recovery limits


* - Non Accredited Parameter H/HT - Holding Time Exceeded

E - Value above quantitation range

Page 9 of 14




BatchID: R105623Wet Chemistry

Sample ID:N2N3MBW1 121314

TestNo:M4500-NO3F




Ref Val % REC RPD Ref Val %RPD

Low Limit

High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:LACHAT_141213A

SeqNo:2867869MBLK

SampType:

Nitrogen, Nitrate-Nitrite 0.20ND

Sample ID:N2N3LCSW1 121314

TestNo:M4500-NO3F




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2867870LCS

SampType:

Nitrogen, Nitrate-Nitrite 10 107 80 1200.20 0 0 010.67


TestNo:M4500-NO3F




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB01 - 121114


SeqNo:2867872MS

SampType:

Nitrogen, Nitrate-Nitrite 10 88.2 75 1250.20 10.77 0 019.59


TestNo:M4500-NO3F




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB01 - 121114


SeqNo:2867877MSD

SampType:

Nitrogen, Nitrate-Nitrite 10 95.1 75 125 200.40 10.77 19.59 3.4720.28







Page 10 of 14





Sample ID:TPMBW1 121614

TestNo:SM4500P,B,E





Low Limit

High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_141216B

SeqNo:2870160MBLK

SampType:

Phosphorus (as P) *0.050ND

Sample ID:TPLCSW1 121614

TestNo:SM4500P,B,E




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_141216B

SeqNo:2870161LCS

SampType:

Phosphorus (as P) 0.5 101 80 120 *0.050 0 0 00.5073

Sample ID:14120344-001BMS

TestNo:SM4500P,B,E




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

WC01 - 121114

Run ID:SPEC_141216B

SeqNo:2870163MS

SampType:

Phosphorus (as P) 0.5 88.9 75 125 *0.050 0.1035 0 00.548

Sample ID:14120344-001BMSD

TestNo:SM4500P,B,E




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

WC01 - 121114

Run ID:SPEC_141216B

SeqNo:2870164MSD

SampType:

Phosphorus (as P) 0.5 84.1 75 125 20 *0.050 0.1035 0.548 4.480.524







Page 11 of 14






TestNo:SM4500P,B,E


Prep Date:1/8/2015



Low Limit

High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_150108C

SeqNo:2883532MBLK

SampType:



TestNo:SM4500P,B,E


Prep Date:1/8/2015


Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_150108C

SeqNo:2883533LCS

SampType:

Phosphorus (as P) 0.5 101 80 120 *0.050 0 0 00.5073


TestNo:SM4500P,B,E


Prep Date:1/8/2015


Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB01 - 121114

Run ID:SPEC_150108C

SeqNo:2883535MS

SampType:

Phosphorus (as P) 0.5 77.8 75 125 *0.050 0.1586 0 00.5477


TestNo:SM4500P,B,E


Prep Date:1/8/2015


Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB01 - 121114

Run ID:SPEC_150108C

SeqNo:2883536MSD

SampType:

Phosphorus (as P) 0.5 75.3 75 125 20 *0.050 0.1586 0.5477 2.350.535







Page 12 of 14





Sample ID:TSSMBK 12/11/14

TestNo:E160.2





Low Limit

High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:BALANCE_141211A

SeqNo:2866885MBLK

SampType:

Total Suspended Solids *7.5ND

Sample ID:TSSLCS 12/11/14

TestNo:E160.2




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2866886LCS

SampType:

Total Suspended Solids 1000 94.6 80 120 *7.5 0 0 0946

Sample ID:14120315-012ADUP

TestNo:E160.2




Ref Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2866889DUP

SampType:

Total Suspended Solids 0 0 0 0 20 *7.5 0 0 0ND







Page 13 of 14

1 of 14

April 07, 2015Date:STAT Analysis Corporation

Project: 103IS3456, Pecatonica TMDL, Stephenson Co., ILClient: Tetra Tech EM Inc.



Revision 0

15030703-001A WC-01-032415 3/24/2015 9:18:00 AM 3/24/201515030703-001B WC-01-032415 3/24/2015 9:18:00 AM 3/24/201515030703-002A SB-01-032415 3/24/2015 1:26:00 PM 3/24/201515030703-003A SB-02-032415 3/24/2015 11:20:00 AM 3/24/201515030703-004A SB-03-032415 3/24/2015 11:50:00 AM 3/24/2015

2 of 14


Project: 103IS3456, Pecatonica TMDL, Stephenson Co., ILCLIENT: Tetra Tech EM Inc.


Revision 0


3 of 14

Project: 103IS3456, Pecatonica TMDL, Stephenson Co., IL

Client Sample ID: WC-01-032415

Collection Date: 3/24/2015 9:18:00 AM

Matrix: Water

Analyses Result Qualifier Units Date AnalyzedRL

Client: Tetra Tech EM Inc.


DF

Lab ID: 15030703-001

Date Printed: April 07, 2015


Date Reported: April 07, 2015


ANALYTICAL RESULTS

Revision 0


Total Suspended Solids E160.2 Analyst: PBGPrep Date: 3/27/2015Total Suspended Solids * 3/27/20157.5 mg/L 110

Qualifiers: J - Analyte detected below quanititation limitsB - Analyte detected in the associated Method Blank



E - Value above quantitation range* - Non-accredited parameterHT - Sample received past holding time

H - Holding time exceeded


4 of 14


Client Sample ID: SB-01-032415

Collection Date: 3/24/2015 1:26:00 PM

Matrix: Water




DF

Lab ID: 15030703-002





ANALYTICAL RESULTS

Revision 0











5 of 14




Matrix: Water




DF

Lab ID: 15030703-003





ANALYTICAL RESULTS

Revision 0

Total Kjeldahl Nitrogen M4500-NORG Analyst: SUBPrep Date:Total Kjeldahl Nitrogen * 4/1/20151.0 mg/L 11.0









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Matrix: Water




DF

Lab ID: 15030703-004





ANALYTICAL RESULTS

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QC SUMMARY

PREP SUMMARY


TestNo:E350.1


Prep Date:3/27/2015

Analyte Result SPK valueSPK Ref

Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:LACHAT_150327B

SeqNo:2933638MBLK

SampType:



TestNo:E350.1


Prep Date:3/27/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2933640LCS

SampType:

Nitrogen, Ammonia (As N) 2.5 101 80 120 *0.050 0 0 02.526


TestNo:E350.1


Prep Date:3/27/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-02-032415


SeqNo:2933642MS

SampType:

Nitrogen, Ammonia (As N) 2.5 103 75 125 *0.050 0.1711 0 02.735


TestNo:E350.1


Prep Date:3/27/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-02-032415


SeqNo:2933643MSD

SampType:

Nitrogen, Ammonia (As N) 2.5 106 75 125 20 *0.050 0.1711 2.735 3.072.82


3/27/20153/27/20151.000NH4LCSW1 032715 50 500 0

3/27/20153/27/20151.00015030703-002A 50 500 0Water

3/27/20153/27/20151.00015030703-003A 50 500 0Water

3/27/20153/27/20151.00015030703-004A 50 500 0Water

3/27/20153/27/20151.00015030703-003AMS 50 500 0Water

3/27/20153/27/20151.00015030703-003AMSD 50 500 0Water







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Sample ID:N2N3MW1 032615

TestNo:M4500-NO3F


Prep Date:3/26/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:LACHAT_150326C

SeqNo:2933479MBLK

SampType:



TestNo:M4500-NO3F


Prep Date:3/26/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2933480LCS

SampType:

Nitrogen, Nitrate-Nitrite 10 95.8 80 1200.20 0 0 09.581


TestNo:M4500-NO3F


Prep Date:3/26/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-02-032415


SeqNo:2933482MS

SampType:

Nitrogen, Nitrate-Nitrite 50 103 75 1251.0 9.582 0 060.9


TestNo:M4500-NO3F


Prep Date:3/26/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-02-032415


SeqNo:2933483MSD

SampType:








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TestNo:E160.2


Prep Date:3/27/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:BALANCE_150327B

SeqNo:2934229MBLK

SampType:



TestNo:E160.2


Prep Date:3/27/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2934230LCS

SampType:

Total Suspended Solids 1000 99.5 80 120 *7.5 0 0 0995


TestNo:E160.2


Prep Date:3/27/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

WC-01-032415


SeqNo:2934232DUP

SampType:

Total Suspended Solids 0 0 0 0 20 *7.5 0 10 10.59







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TestNo:SM4500P,B,E


Prep Date:3/30/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_150330B

SeqNo:2935079MBLK

SampType:



TestNo:SM4500P,B,E


Prep Date:3/30/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_150330B

SeqNo:2935080LCS

SampType:

Phosphorus (as P) 0.5 101 80 120 *0.050 0 0 00.5073


TestNo:SM4500P,B,E


Prep Date:3/30/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-032415

Run ID:SPEC_150330B

SeqNo:2935084MS

SampType:

Phosphorus (as P) 0.5 84.6 75 125 *0.050 0.1247 0 00.5477


TestNo:SM4500P,B,E


Prep Date:3/30/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-032415

Run ID:SPEC_150330B

SeqNo:2935086MSD

SampType:

Phosphorus (as P) 0.5 82.9 75 125 20 *0.050 0.1247 0.5477 1.560.5392







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Project: 103IS3456, Pecatonica TMDLClient: Tetra Tech EM Inc.



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15040582-001A WC-01-041715 4/17/2015 8:24:00 AM 4/17/201515040582-001B WC-01-041715 4/17/2015 8:24:00 AM 4/17/201515040582-002A WC-01-041715-D 4/17/2015 8:24:00 AM 4/17/201515040582-003A SB-02-041715 4/17/2015 9:47:00 AM 4/17/201515040582-004A SB-03-041715 4/17/2015 10:12:00 AM 4/17/201515040582-005A SB-01-041715 4/17/2015 11:02:00 AMMS/MSD 4/17/201515040582-005B SB-01-041715 4/17/2015 11:02:00 AM 4/17/201515040582-006A SB-01-041715-D 4/17/2015 11:02:00 AM 4/17/201515040582-007A SB-04-041715 4/17/2015 11:37:00 AM 4/17/2015

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Project: 103IS3456, Pecatonica TMDLCLIENT: Tetra Tech EM Inc.


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Project: 103IS3456, Pecatonica TMDL

Client Sample ID: WC-01-041715


Matrix: Water




DF

Lab ID: 15040582-001





ANALYTICAL RESULTS

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Total Suspended Solids E160.2 Analyst: PBGPrep Date: 4/20/2015Total Suspended Solids * 4/20/20157.5 mg/L 1ND







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Client Sample ID: WC-01-041715-D


Matrix: Water




DF

Lab ID: 15040582-002





ANALYTICAL RESULTS

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Total Suspended Solids E160.2 Analyst: PBGPrep Date: 4/20/2015Total Suspended Solids * 4/20/20157.5 mg/L 1ND







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Matrix: Water




DF

Lab ID: 15040582-003





ANALYTICAL RESULTS

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Matrix: Water




DF

Lab ID: 15040582-004





ANALYTICAL RESULTS

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Matrix: Water




DF

Lab ID: 15040582-005





ANALYTICAL RESULTS

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Client Sample ID: SB-01-041715-D


Matrix: Water




DF

Lab ID: 15040582-006





ANALYTICAL RESULTS

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Matrix: Water




DF

Lab ID: 15040582-007





ANALYTICAL RESULTS

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QC SUMMARY

PREP BATCH SUMMARY


TestNo:E350.1


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2957244MBLK

SampType:



TestNo:E350.1


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2957225LCS

SampType:

Nitrogen, Ammonia (As N) 2.5 103 80 120 *0.050 0 0 02.564


TestNo:E350.1


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-041715


SeqNo:2957227MS

SampType:

Nitrogen, Ammonia (As N) 2.5 96.9 75 125 *0.050 0.255 0 02.678


TestNo:E350.1


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-041715


SeqNo:2957228MSD

SampType:

Nitrogen, Ammonia (As N) 2.5 99.4 75 125 20 *0.050 0.255 2.678 2.272.739


4/24/20154/24/20151.000NH4LCSW1 042415 50 500 0

4/24/20154/24/20151.00015040582-003A 50 500 0Water

4/24/20154/24/20151.00015040582-004A 50 500 0Water

4/24/20154/24/20151.00015040582-005A 50 500 0Water

4/24/20154/24/20151.00015040582-005AMS 50 500 0Water

4/24/20154/24/20151.00015040582-005AMSD 50 500 0Water

4/24/20154/24/20151.16015040582-006A 50 580 0Water

4/24/20154/24/20151.00015040582-007A 50 500 0Water

4/24/20154/24/20151.00015040604-009A 50 500 0Aqueous







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QC SUMMARY

ANALYTICAL RUN SUMMARY

Sample ID:N2N3MBW1 042015

TestNo:M4500-NO3F


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2952752MBLK

SampType:



TestNo:M4500-NO3F


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2952753LCS

SampType:

Nitrogen, Nitrate-Nitrite 10 103 80 1200.20 0 0 010.26


TestNo:M4500-NO3F


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-041715


SeqNo:2952756MS

SampType:

Nitrogen, Nitrate-Nitrite 10 99.1 75 1250.20 9.276 0 019.19


TestNo:M4500-NO3F


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-041715


SeqNo:2952757MSD

SampType:


SeqNo Sample ID Type Test Code Batch DF Date Analyzed

ICVICV 1 04/20/2015 10:192952749 N2N3_W R108761

ICBICB 1 04/20/2015 10:212952750 N2N3_W R108761

SAMP10 PPM NO2 1 04/20/2015 10:232952751 NO2_WW R108761

MBLKN2N3MBW1 042015 1 04/20/2015 10:252952752 N2N3_W R108761

LCSN2N3LCSW1 042015 1 04/20/2015 10:272952753 N2N3_W R108761

SAMP15040582-005A 1 04/20/2015 10:292952755 N2N3_W R108761

MS15040582-005AMS 1 04/20/2015 10:312952756 N2N3_W R108761

MSD15040582-005AMSD 1 04/20/2015 10:332952757 N2N3_W R108761

SAMP15040582-003A 1 04/20/2015 10:362952758 N2N3_W R108761

SAMP15040582-004A 1 04/20/2015 10:382952759 N2N3_W R108761

SAMP15040582-006A 1 04/20/2015 10:402952760 N2N3_W R108761

SAMP15040582-007A 1 04/20/2015 10:422952761 N2N3_W R108761

CCVCCV 1 04/20/2015 10:442952762 N2N3_W R108761

CCBCCB 1 04/20/2015 10:462952763 N2N3_W R108761







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QC SUMMARY



TestNo:SM4500P,B,E


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_150424A

SeqNo:2957102MBLK

SampType:



TestNo:SM4500P,B,E


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:SPEC_150424A

SeqNo:2957103LCS

SampType:

Phosphorus (as P) 0.5 101 80 120 *0.050 0 0 00.5073


TestNo:SM4500P,B,E


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-041715

Run ID:SPEC_150424A

SeqNo:2957105MS

SampType:

Phosphorus (as P) 0.5 103 75 125 *0.050 0.07797 0 00.5923


TestNo:SM4500P,B,E


Prep Date:4/24/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

SB-01-041715

Run ID:SPEC_150424A

SeqNo:2957106MSD

SampType:

Phosphorus (as P) 0.5 101 75 125 20 *0.050 0.07797 0.5923 1.810.5817


ICVICV 1 04/24/20152957100 P_TW_SM4500 R108895

ICBICB 1 04/24/20152957101 P_TW_SM4500 R108895

MBLKTPMBW1 042415 1 04/24/20152957102 P_TW_SM4500 R108895

LCSTPLCSW1 042415 1 04/24/20152957103 P_TW_SM4500 R108895

SAMP15040582-005A 1 04/24/20152957104 P_TW_SM4500 R108895

MS15040582-005AMS 1 04/24/20152957105 P_TW_SM4500 R108895

MSD15040582-005AMSD 1 04/24/20152957106 P_TW_SM4500 R108895

SAMP15040582-001B 1 04/24/20152957107 P_TW_SM4500 R108895

SAMP15040582-006A 1 04/24/20152957108 P_TW_SM4500 R108895

CCVCCV 1 04/24/20152957109 P_TW_SM4500 R108895

CCBCCB 1 04/24/20152957110 P_TW_SM4500 R108895







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QC SUMMARY



TestNo:E160.2


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ

Run ID:BALANCE_150420F

SeqNo:2954210MBLK

SampType:



TestNo:E160.2


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2954211LCS

SampType:

Total Suspended Solids 1000 95.6 80 120 *7.5 0 0 0955.5


TestNo:E160.2


Prep Date:4/20/2015


Val % RECRPD


High Limit

RPDLimit Qual

Units:mg/L

PQL

Customer ID:

ZZZZZ


SeqNo:2954214DUP

SampType:

Total Suspended Solids 0 0 0 0 20 *7.5 0 0 0ND


MBLKTSSMBK 4/21/15 1 04/20/20152954210 TSS_W R108806

LCSTSSLCS 4/21/15 1 04/20/20152954211 TSS_W R108806

SAMP15040542-011A 1 04/20/20152954212 TSS_W R108806

SAMP15040542-012A 1 04/20/20152954213 TSS_W R108806

DUP15040542-012ADUP 1 04/20/20152954214 TSS_W R108806

SAMP15040582-001A 1 04/20/20152954215 TSS_W R108806

SAMP15040582-002A 1 04/20/20152954216 TSS_W R108806

SAMP15040639-001B 1 04/21/20152954217 TSS_W R108806

SAMP15040604-006A 1 04/21/20152954238 TSS_W R108806







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1

DATA VERIFICATION SUMMARY

This section is a brief verification of the results of the analytical chemistry test performed on surface

water samples collected from the Lower Pecatonica River in Stephenson County, Illinois, in three

sampling events, in December 2014, March 2015, and April 2015. Tetra Tech collected the samples as

part of a study to establish total maximum daily load (TMDL) values for the Pecatonica watershed. The

samples were hand-delivered to STAT Analysis Corporation (STAT) in Chicago, Illinois, who identified

each batch of samples as a work order. The TKN analyses were subcontracted to First Environmental

Laboratories, Inc., of Naperville, Illinois, and the results included with STAT’s results. Table 1 lists the

methods used in the analyses. The three methods referenced for each parameter are comparable to one

another.

Table 1. Laboratory methods

Parameter Method Stated in QAPP Method used by

lab Method indicated in IEPA data submittal template

Total suspended solids

SM 2540 D-1997 EPA 160.2 160.2_M

Total phosphorus SM 4500P B,E-1999 SM 4500-P B,E 4500-P-E

Nitrogen, ammonia SM 4500-NH3 C-1997 EPA 350.1 350.1

Nitrogen, nitrate-nitrite

SM 4500NO3 F-2000 SM 4500-NO3 F 4500-NO3(F)

Total Kjeldahl nitrogen

EPA 351.2 v2.0 1993 EPA 351.2 351.2

The following sections discuss the results of each work order, with emphasis on irregularities that would

affect data usability. A final section provides an overall summary of the results of this data verification.

1.0 Work Order No. 14120344

Work order No. 14120344 includes four samples and two field duplicate samples collected on 11

December. There were no problems with sample preservation and holding times, blanks, laboratory

control sample (LCS) results, and laboratory duplicate results.

Most field duplicate results were practically identical. The field duplicate sample from SB01-121114

yielded approximately 4 times the phosphorus concentration as the primary sample. The results were

submitted individually to IEPA for the primary sample and the field duplicate, and the reported results are

not qualified.

Most matrix spike/matrix spike duplicate (MS/MSD) results were within their quality control (QC) limits.

The TKN MS/MSD analyses yielded recoveries of about 80 percent, below the laboratory’s QC limits of

90 to 110 percent. However, the MS and MSD recoveries were within the acceptable range set forth in the

2

QAPP (75-125%). The MS and MSDs reported by the lab were considered acceptable and were not

qualified.


Work Order No. 15030703 includes four samples collected on 24 March. There were no problems with

sample preservation and holding times, blanks, LCS results, and laboratory duplicate results.

Most matrix spike/matrix spike duplicate (MS/MSD) results were within their quality control (QC) limits.

The TKN MS/MSD analyses yielded recoveries just over 80 percent, below the laboratory’s QC limits of

90 to 110 percent. However, the MS and MSD recoveries were within the acceptable range set forth in the

QAPP (75-125%). The MS and MSDs reported by the lab were considered acceptable and were not

qualified.


Work Order No. 15040582 includes five samples and two field duplicate samples collected on 17 April.

There were no problems with sample preservation and holding times, blanks, LCS results, and laboratory

duplicate results.

Most field duplicate results were practically identical, but the field duplicate sample from SB01-041715

yielded about twice the phosphorus concentration as the primary sample. The results were submitted

individually to IEPA for the primary sample and the field duplicate, and the reported results are not

qualified.

Most matrix spike/matrix spike duplicate (MS/MSD) results were well within their quality control (QC)

limits. The TKN MS/MSD analyses yielded recoveries just over 80 percent, below the laboratory’s QC

limits of 90 to 110 percent. However, the MS and MSD recoveries were within the acceptable range set

forth in the QAPP (75-125%). The MS and MSDs reported by the lab were considered acceptable and

were not qualified.

4.0 Overall Evaluation

There were no results rejected; all results may be used for any purposes.

Illinois River (Peoria Area)

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