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SUMMARY \l______ ________ /

The object of this project is to develop test methods for high-molecidar^Wei^lit'products

such as plastics and rubbers in which outdoor-exposure tests of samples together with

suitable reference samples are conducted to predict the outdoor performance of the materials

even in the regions where the climate conditions are very severe. Moreover, the object is also

to develop test methods which can provide a prediction of weatherability of materials in a

short time and to clarify the applicable range of such test methods. Finally such test methods

thus developed will be proposed as the international standards to the ISO. In fiscal 1999

investigations of weathering test methods for high molecular-weight products in Japan and

foreign countries were carried out, and developments in standardization in other countries

were surveyed by participating in the annual meeting of ISO/TC. On the other hand,

selections and preparations of specimens for the outdoor-exposure tests and exposure tests to

laboratory light sources were carried out, and then the outdoor-exposure tests have started in

three places in Japan and two places outside Japan. Also, the exposure tests to laboratory

light sources by using Xenon-arc sources were performed. Regarding reference materials, the

outdoor-exposure tests and exposure tests to laboratory light sources for four kinds of plastic

films and ten kinds of rubbers as reference specimens have been conducted.

KEYWORDS

Test methods, Outdoor-exposure tests, Exposure tests to laboratory light sources,

High molecular-weight products, Plastics, Rubbers, Reference samples,

Climate conditions, Applicable range, Standardization

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ISO TC 61 Tftxfty? SC-6 ft&i/'T, 1983 ft/N-y-ero® 32 0A65%, ISO 877 ir IS04607ISO 877-1994 Plastics-

Methods of exposure to direct weathering to weathering using glass-filtered day light, and

— 47 —

to intensified weathering by day 1 igdit using Fresnel mirrors /'/‘ffluiSti, ISO 4607ItSiLc

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iso tc 6i ro#gm*ssgteTid\ mmttDmmmm-rzmLjimt-aAyr-w.evxcoiSiJS^&^LT, r1f</jib ISO 4582-1980 Plastics-Deteraination of change in colour and variations in properties after exposure to daylight under glass, to natural weathering or laboratory light sources(7Hl$)ti$fcofc„ 4"[U, CcDfitSlx**EteefclEfisflBx.6tLfc ISO 4582- 1998 IcS-Jtfi-g-fbtfc JIS AK JIS K 7362-1999 iTSB,

iso tc 6i sc6

MrofliJS,^tDijsfclk k)®7—7(:iol 'Tif 1997 ISO 9370 Plastics-Instrumental determination of

radiant exposure in weathering tests -General guidance and basic test method A^Wi 1 RS<h LTBffSn, JIS il/C, JIS K 7363-199X

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“P1 astics-Reference specimen for weathering tests; Polyethylene film”(OST[JNIft0J^fcO, Tfi?)»Wca5-5lc, ASTM Mfc G156-97“ Standard Practice for Selecting and Characterizing Weathering Reference Materials Used to Monitor Consistency of Conditions in an Exposure Test”Srinx:A:3K#TSrlk@=#l"jot' TfiWd&fdL, NWI kWtefrtmi&fet&LkizLHy

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©Plastics; Reference specimen for Weathering test; Polyethylene film (DJIS K 7200-1986

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©Characterization of exposure test site and regional difference

(1) VAMAS Report No.30

W. D. Ketola R. M. Fischer

[mo

VAMAS TWA-12(7)mÔt^,ASTM

— 49 —

1: Description of Reference Materials and Exposures Used in Pound-Robin Tests

Reference Material and Source Exposure

Standard Describing Use

of Reference Material

Polysulfone film obtained from

Dr. A Davis, UK

UVB-313 fluorescent UV-B

lamp, 60°C

British Standard BS2782,

Part 5, Method 540C

Polystyrene plaques obtained from

Testfabrics, Inc.,(lot 2), New Jersey,

USA

water cooled xenon arc with

quartz inner and borosilicate

outer filters

U S. Society of Automotive

Engineers Standard,

SAEJ 1960

Polyethylene (Union Carbide

DFDA-1137NT) film prepared at

3M, St. Paul, Minnesota, USA

filtered open flame carbon arc

with potash lithia glass filters

Japan Industrial Stand

ard, JIS K7200

(1) ^ UVB 7>y(: 60"CT#m (2)

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Standard Practice for Selecting and Characterizing Weathering Reference Materials Used

to Monitor Consistency of Conditions in an Exposure Test

i. it mm

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Plastics - Methods of exposure to direct weathering, to weathering using glass-filtered gaylight, and to intensified weathering by daylight using Fresnel mirrors

JIS K 7363:199X(ISO 9370:1997)

Plastics - Instrumental determination of radiant exposure in weathering tests - General guidance and basic test method

JIS K 7362:199X (ISO 4582:1998)

Plastics - Determination of changes in colour and variations in properties after exposure to daylight under glass, natural weathering or laboratory light sources

JIS K 7350-1 H11 nfl: iSM1! (General guidance)JIS K 7350-2 H2SP: >7—(Xenon-arc sources)JIS K 7350-3 #3gP: (Fluorescent UV lamps)

JIS K 7350:1995 (ISO 4892:1994)

(Plastics-Methods of exposure to laboratory light sources)

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-57-

9.1) W. D. Ketola, R. M. Fischer : VAMAS Report No.30

2) ASTM G 156-97 : Standard Practice for Selecting and Characterizing Weathering

Reference Materials Used to Monitor Consistency of Conditions

In an Exposure Test

3) mm.ISO/TC61 m 47 @ t? 4 SC6/WG2 Meeting(1998.10)

4) J1S K 7200-1986 : Standard Reference Test Specimens for Calibrating a Laboratory

Light Exposure Apparatus

-58-

VAMAS

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Table 1: Description of Reference Materials and Exposures Used in Round-Robin Tests

Reference Material and Source ExposureStandard Describing Use

of Reference Material

Polysulfone film obtained fromDr. A. Davis, UK

UVB-313 fluorescent UV-B lamp, 60°C

British Standard BS2782, Part 5,Method 540C1

Polystyrene plaques obtained from Testfabrics, Inc., (lot 2), NewJersey, USA

water cooled xenon arc with quartz inner and borosilicatc outer filters

U.S. Society of Automotive Engineers Standard, SAE J19602

Polyethylene (Union CarbideDFDA-1137NT) film prepared at 3M, St Paul, Minnesota, USA

filtered open flame carbon arc with potash lithia glass filters

Japan Industrial Standard, JIS K720O 3

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-63-

Table 2: Description of Exposure Times and Characteristic Property Used for Reference MaterialsExposed in Round-Robin Tests

Reference Material Exposure PeriodsCharacteristic Property and

Method Used for MeasurementPolysulfone film 5, 15, 30, and 60

minutesabsorbance at 330 nm measured using UV-visible spectrophotometer, according to BS2782, Part 5, Method 540C

Polystyrene plaques 63, 126, 222, and 285 KJ/m2 radiant energy measured at 340 nm

change in CIE b* measured by reflectance and transmissionaccording to SAE J1960

Polyethylene film 200, 400, 600, and 800 hours

ratio of absorbance at 1715 cm'1 to absorbance at 2030 cm'1measured according to JIS K7200

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Table 3: Average Change in Absorbance at 330 nm for Polysulfone Films After Exposure to UVB-313 Fluorescent UV-B Lamps

Minutes Exposed Data Source Lab A Lab B Lab C Lab D Lab E Lab F Lab G5 minutes

(films 1, 2, and 3)Participating Labs Reference Lab

0.2080.265

0.2280.256

0.2360.260

0.2330.267

0.2300.258

0.2520.284

0.2150.230

15 minutes (films 4, 5, and 6)

Participating Labs Reference Lab

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0.4180.460

0.3970.427

0.4210.465

0.4330.502

0.4410.473

0.4520.498



0.5130.626

0.5870.702

0.5620.609

0.5860.663

0.5980.638

0.5980.657

0.5570.587



0.6450.781

0.7020.756

0.7360.775

0.7350.831

0.7730.806

0.7410.802

0.7060.734

reference lab data is the average for a single measurement on each of the three films.

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Figure 2: Absorbance change at 330 nm for polysulfone films exposed to UVB-313 fluorescent lampsfor five minutes

Table 4: Components of Variance Analysis of Round-Robin Data for 330 nm Absorbance Change of Polysulfone Films

Data Analyzed Source of Variability Variance Percent of total variability330 nm absorbance Laboratory 0.0006change reported by Lab x time 0.0002participating labs total lab 0.0008 80%

Operator 0.0000Operator x lab 0.0000

total operator 0.0000 0%Film 0.0002 20%

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Film 0.0002 22%Total 0.0009 100%

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Table 5: Results for ASTM E 691 Analysis of Round-Robin Data for 330 nm Absorbance Change of Polysulfone Films Exposed to UVB-313 Fluorescent Lamps

Repeatability ReproducibilityMinutes Grand Standard Difference Standard Difference

Data Analyzed Exposed Mean Deviation 2-sigma limit Deviation 2-sigma limitparticipating lab 5 0.239 0.008 0.022 0.016 0.045data for all films 15 0.422 0.012 0.034 0.025 0.070

30 0.567 0.014 0.039 0.033 0.09260 0.720 0.016 0.045 0.043 0.120

participating lab 5 0.232 0.003 0.008 0.016 0.045data for films 15 0.427 0.006 0.017 0.026 0.073exposed in 30 0.576 0.002 0.006 0.033 0.092center of holder 60 0.724 0.007 0.020 0.047 0.132

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Table 6A: Mean CIE db* Measured by Reflectance for Polystyrene Plaques Exposed in Water Cooled Xenon Arcs According to SAE J1960

Radiant exposure (KJ/m2, 340 nm) Source of data Lab A Lab B Lab C Lab D Lab E Lab F Lab G Lab H

63 participating lab NM 2.23 2.53 2.65 1.03 2.43 2.51 2.2563 reference lab 2.20 2.47 2.68 2.56 2.49 2.44 2.33 2.16126 participating lab NM 3.64 4.31 4.40 2.44 3.98 4.24 NM126 reference lab 3.68 6.98 4.32 4.23 3.98 3.90 3.88 NM222 participating lab NM 5.87 6.94 6.05 4.80 6.54 NM 6.06222 reference lab 5.81 6.47 4.11 5.78 6.35 6.36 NM 6.74285 participating lab NM 7.45 8.70 8.36 6.16 7.95 8.09 7.98285 reference lab 7.19 8.04 9.07 7.78 7.91 7.83 7.45 7.68

10

— 68 —

Table 6B: Mean CIE db* Measured by Transmission for Polystyrene Plaques Exposed in Water Cooled Xenon Arcs According to SAE J1960

Radiant exposure (KJ/m2, 340 nm) Source of data Lab A Lab B Lab C Lab D Lab E Lab F Lab G Lab H

63 participating lab 1.02 1.14 1.25 1.19 0.91 1.42 1.16 NM63 reference lab 1.06 1.19 1.35 1.21 1.19 1.15 1.17 1.10126 participating lab 1.78 2.18 2.03 2.00 1.82 2.52 2.30 NM126 reference lab 1.79 1.94 2.16 2.01 1.90 1.88 1.99 NM222 participating lab 2.93 3.53 3.31 2.82 3.56 4.14 NM NM222 reference lab 3.06 3.29 3.67 2.83 3.15 3.22 NM 3.02285 participating lab 3.68 4.51 4.49 4.01 4.49 5.00 4.71 NM285 reference lab 3.84 4.13 4.78 3.96 4.04 3.98 3.90 3.99

Note: NM means that the participating lab did not make this measurement or that the correct radiant exposure was not used.

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8.00 -

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Figure 3: Average db* (reflection) reported by participating laboratories with upper and lower 95% prediction limits determined from MINITAB™ regression analysis

Table 7: Repeatability and Reproducibility Results for Polystyrene db* from Analysis of Round-Robin Data According to ASTM E 691

REPEATABILITY REPRODUCIBILITYMeasurement radiant exposure Grand mean standard difference standard difference

geometry (KJ/m2 at 340 nm) db* for all labs deviation 2-sigma limit deviation 2-sigma limitreflectance 63 2.43 0.05 0.14 0.28 0.78

126 4.11 0.07 0.20 0.44 1.23222 6.29 0.12 0.34 0.53 1.48285 8.09 0.09 0.25 0.52 1.46

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Table 8A: Components of Variance Analysis for Polystyrene db* (Reflectance) After Xenon Arc Round-Robin Exposures

participating lab data reference lab dataradiant exposure source of % of total source of % of total

(KJ/m2 at 340 nm) variability variance variance variability variance variance63 Lab 0.027 93% Lab 0.031 98%

Plaque 0.002 7% Plaque 0.001 2%Operator 0.000 0% Total 0.032 100%

Total 0.029 100%126 Lab 0.094 97% Lab 0.042 73%


Total 0.097 100%222 Lab 0.183 91% Lab 0.220 98%


Total 0.202 100%285 Lab 0.172 95% Lab 0.318 97%


Total 0.180 100%

-72 —

Table 8B: Components of Variance Analysis for Polystyrene db*

participating lab data reference lab dataradiant exposure source of % of total source of % of total

(KJ/m2 at 340 nm) variability variance variance variability variance variance63 Lab 0.026 84% Lab 0.007 88%


Total 0.031 100%126 Lab 0.060 95% Lab 0.032 97%


Total 0.063 100%222 Lab 0.221 98% Lab 0.069 97%


Total 0.224 100%285 Lab 0.103 91% Lab 0.089 97%


Total 0.113 100%

Table 9: Effect of plaque position on CIE b* and db* measured by transmissionCEE b* (D65, 10° observer) db* relative to file

Plaque position file plaque A plaque B plaque A plaque Bat port of integrating sphere 0.61 2.19 3.01 1.58 2.40midway between integrating sphere and detector 0.52 2.50 3.28 1.98 2.76at detector port 0.50 2.61 3.33 2.11 2.83

% difference between highest and lowest value -18% 19% 11% 34% 18%

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! figure 4: Exposure position of polyethylene films in specimen drum of carbon arc device

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— 75

Table 10: Mean carbonyl index for polyethylene films exposed in filtered open flame carbon arc devices

Mean Carbonyl Index(ratio of absorbance at 1715 cm'1 to absorbance at 2030 cm'1)

Exposure time Data Source Lab A Lab B Lab C Lab D Lab G Lab H200 hours Operator A 2.27 0.95 1.36 1.65 0.44 1.69

films Operator B NM NM 0.87 1.57 NM 1.561, 2, and 3 Reference Lab 1.32 1.47 1.47 2.12 0.63 2.57

Ref. Lab peak to peak 1.05 1.14 1.11 1.56 0.53 1.81400 hours Operator A 4.92 4.50 7.71 6.61 2.02 6.54






Ref. Lab peak to peak 18.34 32.24 34.77 12.93 18.58 23.97NM - not measured

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Figure 5: Carbonyl ratio for polyethylene film exposed for 400 hours in carbon arc device. Ratio is ratio of absorbance at 1715 cm~l to absorbance at 2030 cm-* (peak ratio data is for the actual peaks at 1713 cm’l and 2020 cm-*)

Table 11: Summary of ASTM E 691 analysis for 1715/2030 cm'l carbonyl index of polyethylene filmsafter 200, 400, and 600 hour exposures in filtered open flame carbon arc devices

hours exposed data analyzed grand meanrepeatability

standard deviationreproducibility

standard deviation200 hours participating lab, operator A 1.39 0.31 0.69

films participating lab, operator B 1.49 0.15 0.741, 2, and 3 reference lab 1.60 0.35 0.79

reference lab without film 1 1.64 0.22 0.94400 hours participating lab, operator A 5.38 1.14 2.32






reference lab without film 10 37.36 1.70 19.10

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Mfotefr^fzZ tlztz&oTable 12: Components of Variance Analysis for 1715/2030 cm-* Carbonyl Ratio Data Results from additional analysis of polyethylene films exposed in filtered carbon-arc devices:

hours exposed

participating lab data operator A reference lab data

Variable variance % of total variance variance % of total variance200 hours Lab 0.36 71% 0.39 68%films 1, 2, and 3 Film 0.15 29% 0.19 32%

total 0.31 100% 0.58 100%400 hours, Lab 3.45 64% 5.44 45%films 4, 5, and 6 Film 1.96 36% 6.60 55%



total 281.21 100% 222.39 100%

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Table 13: Results from 11 consecutive measurements of caibonyl index by one operator on film H9

Statistical parameter

carbonyl index based on ratio of absorbance at 1715 cm*1 to

absorbance at 2030 cm*1carbonyl index based on ratio of peak

absorbances at 1713 cm*1 and 2020 cm"1Mean 27.21 19.91Maximum 27.90 20.30Minimum 25.27 18.91Standard deviation 0.97 0.42Coefficient of Variance 3.6% *2.1%95% confidence interval 25.27-29.16 18.07-21.14

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Table 14: Repeatability Standard Deviation and 95% Repeatability Limits for Reference Materials Evaluated in ASTM/VAMAS TWA 12 Round-robin

Reference material and measured property exposure period

repeatabilitystandarddeviation

95% repeatability limits

polysulfone film 5 minutes 0.003 ±0.006(absorbance change at 330 nm for film 15 minutes 0.006 ±0.012exposed in center of fluorescent 30 minutes 0.002 ±0.004UV device running UVB 313 lamps) 60 minutes 0.007 ±0.014polystyrene plaque 63 KJ/m^ at 340 nm 0.05 ±0.10(db* measured by reflectance) 126 KJ/m2 at 340 nm 0.07 ±0.14

222 KJ/m2 at 340 nm 0.12 ±0.24285 KJ/m^ at 340 nm 0.09 ±0.18

polystyrene plaque 63 KJ/m^ at 340 nm 0.07 ±0.14(db* measured by transmission) 126 KJ/m2 at 340 nm 0.06 ±0.12

222 KJ/m^ at 340 nm 0.17 ±0.34285 KJ/m2 at 340 nm 0.09 ±0.18

polyethylene film 200 hours 0.15 ±0.30(carbonyl index for films exposed at 400 hours 0.34 ±0.68bottom and center position in holder) 600 hours 4.17 ±8.34

800 hours 0.87 ±1.74

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Table 15: Grand mean, reproducibility standard deviation and 95% reproducibility limits for polysulfoneand polystyrene reference materials evaluated in ASTM/VAMAS TWA12 round-robin

Reference material and measured property exposure period

grandmean

reproducibilit y standard deviation

95%reproducibility

limitspolysulfone film 5 minutes 0.232 0.016 ±0.032(absorbance change at 330 run for film 15 minutes 0.427 0.026 ±0.052exposed in center of fluorescent 30 minutes 0.576 0.033 ± 0.066UV device running UVB 313 lamps) 60 minutes 0.724 0.047 ±0.094polystyrene plaque 63 KJ/m2at340 nm 2.43 0.28 ±0.56(db* measured by reflectance) 126 KJ/m2 at 340 run 4.11 0.44 ±0.88

222 KJ/m2 at 340 nm 6.29 0.53 ±1.06285 KJ/m2 at 340 nm 8.09 '0.52 ± 1.04

polystyrene plaque 63 KJ/m2 at 340 nm 1.18 0.18 ±0.36(db* measured by transmission) 126 KJ/m2 at 340 nm 2.14 0.28 ±0.56

222 KJ/m2 at 340 nm 3.47 0.50 ±1.00285 KJ/m2 at 340 nm 4.53 0.34 ±0.68

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Table 16: DE data for 24 fabrics and 4 reference materials exposed in IFAI round-robin study. All materials were exposed in water cooled xenon arc device operated according to SAE J1885.

Sample Lab A Lab B Lab C Lab E Lab F Lab G Lab H Lab J Lab K Ave.standarddeviation

1 6.34 6.22 7.18 7.78 6.33 6.38 7.16 7.39 6.48 6.81 0.572 5.97 6.08 6.47 6.99 6.01 5.34 6.49 6.94 4.79 6.12 0.723 7.25 7.76 7.92 8.93 7.29 7.19 8.06 8.07 6.54 7.67 0.694 8.38 11.99 11.89 12.80 9.41 8.89 11.07 10.79 6.41 10.18 2.065 7.75 10.94 11.08 11.87 8.80 8.42 11.26 8.49 5.19 9.31 2.166 11.65 16.89 15.04 18.87 13.90 14.06 16.44 17.80 11.23 15.10 2.647 3.62 4.71 4.41 5.27 4.52 3.40 5.08 5.99 6.26 4.81 0.968 4.25 5.38 5.42 6.66 5.70 5.61 5.44 7.42 3.91 5.53 1.079 9.78 10.04 11.92 11.96 10.88 10.31 11.52 10.86 8.74 10.67 1.0610 8.00 7.16 8.11 8.51 7.58 8.42 8.50 9.68 9.28 8.36 0.7811 7.15 6.65 7.21 7.17 6.30 6.62 7.47 8.14 6.85 7.06 0.5412 10.04 10.52 11.12 10.97 9.38 9.63 11.22 12.90 11.80 10.84 1.1013 3.94 2.73 4.26 4.20 2.55 3.74 4.81 5.67 4.46 4.04 0.9714 0.82 1.13 0.90 1.11 1.05 0.93 0.92 0.76 1.23 0.98 0.1615 1.26 0.76 0.91 0.71 0.64 0.68 0.69 0.82 0.73 0.80 0.1916 1.00 1.28 0.82 1.02 0.75 1.69 0.50 0.68 0.56 0.92 0.3817 0.86 1.37 1.78 1.59 2.86 1.03 0.59 1.74 0.83 1.41 0.6918 1.45 1.81 0.95 1.50 1.08 0.73 0.99 1.16 1.10 1.20 0.3319 1.26 2.80 2.23 2.37 1.46 1.33 1.96 1.60 1.34 1.82 0.5520 1.46 2.37 1.98 2.00 1.72 1.55 1.81 1.82 1.55 1.81 0.2821 5.27 12.83 12.23 13.87 11.28 11.85 12.74 13.74 13.93 11.97 2.6822 6.58 2.92 8.79 6.24 5.41 5.99 7.21 10.05 11.18 7.15 2.5223 3.54 2.53 2.59 4.10 3.93 3.81 4.58 4.83 4.86 3.86 0.8724 1.11 1.17 1.24 2.02 1.55 1.47 1.68 2.01 2.08 1.59 0.38

L2 (37.6 KJ) 10.98 9.47 10.52 10.79 9.84 11.07 10.40 10.76 9.84 10.41 0.57L4 (113 KJ) 6.62 5.79 6.46 6.81 6.39 6.77 6.66 6.48 7.50 6.61 0.45L6 (225 KJ) 3.58 3.69 3.81 3.81 3.36 3.86 4.01 3.86 3.68 3.74 0.19

pSTY db* (113 KJ) 4.37 5.00 5.26 5.64 4.33 4.64 4.98 4.09 3.70 4.67 0.61pSTY db* (225 KJ) 8.26 9.70 10.03 10.16 8.64 8.57 9.42 7.65 7.20 8.85 1.05

— 84 —

Table 17: Laboratories from IFAI round-robin showing best and worst agreement for blue wool and polystyrene reference materials.

reference lab pair with smallest lab pair with largestmaterial between lab difference between lab difference

L2 blue wool lab F (dE = 9.64) and lab K (dE = 9.84) lab B (dE = 9.47) and lab G (dE = 11.07)L4 blue wool lab C (dE = 6.46) and lab J (dE = 6.48) lab B (dE = 5.79) and lab K (dE = 7.50)L6 blue wool lab B (dE = 3.69) and lab K (dE = 3.68) lab F (dE = 3.36) and lab H (dE = 4.01)polystyrene (113 KJ) lab F (db* = 4.33) and lab A (db* = 4.37) lab K (db* ~ 3.70) and lab E (db* = 5.64)

Table 18: Comparison of test fabric results in labs that showed excellent agreement in results for reference materials

ReferenceMaterial

laboratories with best agreement^

IFAI round-robin delta E for Fabric #11, Fabric #5, and Fabric #13 after radiant exposure of 451 KJ/m^ at 340 nm

Fabric #11 Fabric #5 Fabric #13L2 blue wool Lab F = Lab K Lab F Lab K Lab F Lab K Lab F

6.30 6.85 &80 5.JP 2.55 4.45L4 blue wool Lab C = Lab G Lab C Lab G Lab C Lab G Lab C W,G

7.21 6.62 JJ.A9 &42 4.25 3.74L6 blue wool Lab B = Lab K Lab B Lab K LabB Lab K Lab B Lab K

6.65 6.85 10.94 5.19 2 75 4.45polystyrene, 113 KJ Lab F = Lab A Lab F Lab A Lab F Lab A Lab F Lab A

6.30 7.15 &<M 7.75 2.55 3.P4A If the delta E data for the fabrics was within 10%, the laboratory results wereconsidered to be equal. Data in italics indicate that the delta E results for the test fabric were not equal, even though the labs produced equal results for the reference material.

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Table 19: Rank order of 24 fabrics tested in IFAI round-robin study based on delta E. Fabric with largest delta E is assigned rank of 24, while fabric with smallest delta E is assigned a rank of 1.

Sample Lab A Lab B Lab C Lab E Lab F Lab G Lab H Lab J Lab K average1 10 10 11 9 9 10 11 12 9 112 11 11 12 11 11 13 12 13 14 123 7 7 9 7 8 8 8 10 8 84 4 3 4 3 4 5 6 5 10 55 6 4 6 5 6 6 4 8 12 66 1 1 1 1 1 1 1 1 3 17 15 13 14 14 14 16 14 14 11 148 13 12 13 12 12 12 13 11 16 139 3 6 3 4 3 3 3 4 6 410 5 8 8 8 7 6 7 7 5 711 8 9 10 10 10 9 9 9 7 1012 2 5 5 6 5 4 5 3 2 313 14 16 15 15 17 15 15 15 15 1514 24 23 23 22 22 22 21 23 20 2215 19 24 22 24 24 24 22 22 23 2416 22 21 24 23 23 17 24 24 24 2317 23 20 19 20 16 21 23 19 22 2018 18 19 21 21 21 23 20 21 21 2119 19 15 17 17 20 20 17 20 19 1720 17 18 18 19 18 18 18 18 18 1821 12 2 2 2 2 2 2 2 1 222 9 14 7 13 13 11 10 6 4 923 16 17 16 16 15 14 16 16 13 1624 21 22 20 18 19 19 19 17 17 19

R, to average for all labs 0.92 0.97 0.99 0.98 0.97 0.97 0.99 0.98 0.93 1.00

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Table 20: Rank comparisons of “test fabrics” to fabric #13 that has been arbitrarily selected as a control material known to give acceptable performance. Numbers in bold italics are “errors” where the ranking of the fabric is either higher or lower than the fabric 13 “control”.

Sample Lab A Lab B Lab C Lab E Lab F Lab G Lab H Lab J Lab K average6 1 1 1 1 1 1 1 1 3 1

21 12 2 2 2 2 2 2 2 1 212 2 5 5 6 5 4 5 3 2 39 3 6 3 4 3 3 3 4 6 44 4 3 4 3 4 5 6 5 10 55 6 4 6 5 6 6 4 8 12 610 5 8 8 8 7 6 7 7 5 73 7 7 9 7 8 8 8 10 8 822 9 14 7 13 13 11 10 6 4 911 8 9 10 10 10 9 9 9 7 101 10 10 11 9 9 10 11 12 9 112 11 11 12 11 11 13 12 13 14 128 13 12 13 12 12 12 13 11 16 137 15 13 14 14 14 16 14 14 11 14

; \13 14 16 15 15 17 15 . IS": 15 * 15 V* 1523 16 17 16 16 15 14 16 16 13 1619 19 15 17 17 20 20 17 20 19 1720 17 18 18 19 18 18 18 18 18 1824 21 22 20 18 19 19 19 17 17 1917 23 20 19 20 16 21 23 19 22 2018 18 19 21 21 21 23 20 21 21 2114 24 23 23 22 22 22 21 23 20 2216 22 21 24 23 23 17 24 24 24 2315 19 24 22 24 24 24 22 22 23 24

Table 21: Summary of ranking errors assuming that various fabrics from the IFAI round-robin are used as the control of known performance

control materialaverage delta E

of control materialnumber of

ranking errorspercenterrors comments

fabric #13 4.04 8 3.9%fabric #2 6.12 7 3.4%fabric #10 8.36 9 4.3% 4 errors in Lab Kfabric #9 10.67 10 4.8%

fabric #21 11.97 12 5.8% 10 errors in Lab A

Table 22: Analysis of rank errors from IFAI round-robin study of 24 fabrics as a function of delta E difference between the pairs being compared.

Delta E difference between ranked pairs

number of pair comparisons

number of ranking errors

percent error rate

0-1 390 100 25.6%1-2 248 23 9.3%2-3 253 7 2.8%3-4 255 4 1.6%4-5 270 5 1.8%5-6 249 1 0.4%

— 88 —

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TABLE 1 Layout of experiment comparing new lot of a reference material with an original lot that has already been characterized

by conducting a round-robin study according to section 5.7

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one *1 a, D1,X2 a2 D12X3 a3 D13

xn an D1„

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Ar = A]7|s / Aj030

Ar : absorbance ratio (Carbonyl Index)

Aim : absorbance at 1715 cm"1 [log (I0/I)j

AjQ30 : absorbance at 2030 cm'1 [log (I„/I)]

I0 : transmittance by base line method for each wave number

I : transmittance by each wave number

Wave number (cm• ’>)

noma! polyethylene

reference polyethylene

Fig. 1 IR spectrum of polyethylene film Fig.2 Calculating method of Carbonyl Index

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UDC 678:620.115: 620.193.6: 53.089. 6: 535. 23

JAPANESE INDUSTRIAL STANDARD j l S

Standard Reference Test Specimens for K 7200-1986Calibrating a Laboratory Light

Exposure Apparatus1. Scope

This Japanese Industrial Standard specifies the standard reference test specimens, hereinafter referred to as the "standard test specimen", for calibrating the irradiation energy(2) from a laboratory light exposure (weather resistance) apparatus(x).

Notes (1) The laboratory light exposure (weather resistance) apparatus to which the standard test specimen is applied shall be as follows:

(a) The apparatus specified in JIS B 7751(b) The apparatus specified in JIS B 7752(c) The apparatus specified in JIS B 7753(d) The apparatus specified in JIS B 7754

(2) The irradiation energy means the energy of light irradiated on a unit area of the standard test specimen.

Remarks 1. The standard test specimen shall be the one, manufactured under a specified condition, whose characteristic value is rated by means of the light exposure (weather resistance) tester installed in a public or quasi-public organization.

2. The example of how to use the standard test specimen is shown in the Appendix.

3. In this standard the units and numerical values given in { } are in accordance with the conventional unit system and appended for reference only.

Applicable Standards:

JIS B 7751-Glass-Enclosed Carbon-Arc Type Apparatus for Artificial Light Exposure Tests

JIS B 7752-Light-and-Water-Exposure Apparatus (Enclosed Carbon-Arc Type)

JIS B 7753-Light-and-Water-Exposure Apparatus (Open-Flame Sunshine Carbon-Arc Type)

JIS B 7754-Light-Exposure and Light-and-Water-Exposure Apparatus (Xenon-Arc Lamp Type)

JIS K 0115-General Rules for Absorptiometric AnalysisJIS K 0117-General Rules for Infrared Absorption Photometric AnalysisJIS K 6900-Glossary of Terms Used in Plastic IndustryJIS Z 8722-Methods of Measurement for Colour of Reflecting or Transmitting

ObjectsReference Standards:

JIS K 0501-General Rule for Chemical Standard MaterialsJIS Z 8203-SI Units and the Use of their Multiples and of Certain other Units

— 112

3K 7200-1986

(4) Cut and polish to make the size specified.

(5) Condition in a dark place at 23 ± 2°c of temperature and 50 ± 5 % of relative humidity for not less than 30 days.

4.2.2 SR-LS-PE SR-LS-PE shall be prepared according to the following procedures by using a compression molding method.

(1) After 5-min kneading the material of 4.1.2 between two rolls whose surfaces are heated at 150 to 170°C , cut into small pieces of individually 0.4 to 0.5 g.

(2) After pre-heating in a compression molding machine for heating whose surface is heated at 160 to 180^0, for 90 sec. , compress the material for 40 sec, and cool in a compression molding machinefor cooling whose surface temperature is 30 to 40°C, for 120 sec, which is followed by forming a press sheet of 50 mm x 40 mm x 0.2 mm. Furthermore, repeat this operation once again, and prepare the press sheet of thickness specified in Table 2.

(3) Cut it in the size specified.

5. Dimensions of Standard Test Specimen

The dimension of standard test specimen shall be as shown in Table 2.

Table 2. Dimensions of Standard Test SpecimenUnit: mm

Symbol Length Width Thickness

SR-LS-PMMA 50 ± 1 30 ± 1 3.0 ±0.1

SR-LS-PE 38 ± 2 35 ± 1 0.20 ±0.02

6. Quality of Standard Test Specimen Prior to Irradiation

The quality of the standard test specimen prior to irradiation shall be as follows:

(1) SR-LS-PMMA The dispersion in a lot shall be not more than 0.03 in the range (maximum value - minimum value) among the peak values of the transmittance measured in the vicinity of 420 nm.

(2) SR-LS-PE The ratio of absorbances (Ams/A2e30) measured at 1715 cm- i and 2030 cm- 1 shall be not more than 0.05.

7. Method to Decide the Characterisitcs of Standard

7.1 Organization for Deciding Characteristics The official organizations for deciding characteristics shall be five at least, such as national or public research organization, public inspection organization, or other quasi-organization.

7.2 Sampling Draw at random standard test specimens enough quantity of pieces for tests so as to let them represent the lot.

7.3 Number of Standard Test Specimens The number of the standard test specimens shall be not less than 3 pieces per one tester.

— 113-

2. Definitions

2K 7200-1986

The definitions of main terms used in this standard shall be in accordance with JIS K 6900.

3. Classification The classification of standard test specimens shall be as shown in Table 1.

Table 1. Classification of Standard Test Specimens

Class Symbol Features

Coloredpolymethylmethacrylatestandardtestspecimen

SR-LS-PMMAThis test specimen can be used for finding relatively the irradiation energy from the color fading of dyestuff caused by light irradiation, and in the range of 10 to 40 hours of irradiation time.In case of spraying, this cannot be used.

Polyethylenefilmstandardtestspecimen

SR-LS-PEThis specimen can be used for finding relatively the irradiation energy from the amount of carbonyl group formed owing to oxidation reaction by light irradiation, and in the range of 40 to 200 h of irradiation time.

Composition‘Material and Preparation

4.1 Composition and Material

4.1.1 Composition of Colored Poly methyl Methacrylate Standard Test Specimen (Hereinafter Referred to as SR-LS-PMMA) SR-LS-PMMA shall be composed of mainly methyl methacrylate monomer, 0. 0020 ± 0. 00005 % by mass of solvent yellow 33 (color index 47000) as dyestuff, 0. 010 ± 0. 0005 % by mass of 2-(2*-hydroxy- 5*-methyl-phenyl) benzotriazol as ultraviolet ray absorbent, 0.010 ± 0.0005 % by mass of azobis-isobutyronitrille as initiator, and 0. 35 ±0.05 % by mass of stearic acid as parting agent.

4.1.2 Material of Polyethylene Film Standard Test Specimen (Hereinafter Referred to as SR-LS-PE) The material of SR-LS-PE shall be the high- density polyethylene containing trans-type vinylene group (wave number 965 cm- *) , whose ratio of absorbances at 965 cm-1 to 2030 cm~ 1 is 1. 0 to 1.3, whose melt flow rate is 0. 2 to 0. 4 g per 10 min, and whose density is 950 to 956 kg /m 3 ( 0. 950 to 0. 965 g /cm 3) .

4.2 Preparation Method

4.2. 1 SR-LS-PMMA SR-LS-PMMA is prepared according to the following procedures by using a casting method.

(1) Pour the mixture having the composition such as 4.1.1. into two polished tempered sheet glasses set in parallel so as to get the thickness specified in Table 2.

(2) Polymerize the mixture at 80°C for 8 h. Next let it harden at 120°C for 1 h, and remove the sheet glasses.

(3) Carry out masking for the protection of its surface.

— 114 —

4K 7200-1986

7.4 Operating Condition of Light Exposure (Weather Resistance) Tester The operating condition of light exposure (weather resistance) tester shall be as shown in Table 3.

Table 3. Operating Condition of Light Exposure (Weather Resistance) Tester

Items

Enclosed carbon- arc type light- exposure tester

Enclosedcarbon-arc typelight-and-water-exposuretester

Open-framesunshinecarbon-arctype light-and-water-exposuretester

Xenon-arc lamp type light-exposure and light - and-water exposure tester

Discharge current (A) 15 to 17 15 to 17 58 to 62 -

Discharge voltage (V) 125 to 145 125 to 145 48 to 52 -

Temperature at black panel (°C) 63 ± 3 63 ± 3 63 ± 3 63 ± 3

Humidity in a tester (% RH) 50 ± 5 50 ± 5 50 ± 5 50 ±5

Using time of a glove or filter

Use a new one.

0 h for 2 sheets500 h for 2 sheets1000 h for 2 sheets1500 h for 2 sheets

Use a new one.

Condition of rotating frame for sample

Fill up the frame for sample by using such as white board to eliminate a blank space.

Spraying No spraying.

7.5 Method and Location of Attaching Standard Test Specimen

7.5.1 In the Case of SR-LS-PMMA In the case of SR-LS-PMMA, attach the standard test specimen shown in [Fig. 1 (a)] to the auxiliary holder shown in [Fig. 1 (b)], and then attach the auxiliary holder to the sample holder shown in Fig. 2.

7.5.2 In the Case of SR-LS-PE In the case of SR-LS-PE, attach the mount holding the^standard test specimen shown in [ Fig. 1 (c)] to the auxiliary holder shown in [Fig. 1 (d)], and then attach the auxiliary holder to the sample holder shown in Fig. 2.

115 —

5K 7200-1986

Fig. 1. An Example of Attaching Standard Test Specimento Auxiliary Holder Unit: mm

(a) Dimension of SR-LS-PMMA (b) Auxiliary Holder forSR-LS-PMMA(Material: Aluminum plate of

1 mm thickness)

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(c) Dimensions of SR-LS-PE and a Mount(Material of a mount: plastic)

(d) Auxiliary Holder with a Mount for SR-LS-PE (Material: Aluminum plate of

1 mm thickness)

Standard test

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4

-116-

6K 7200-1986

Fig. 2. Attaching Location of Auxiliary Holder on Sample HolderUnit: mm

In the case of an enclosed carbon-arc In the case of an enclosed carbon- type and open-flame sunshine carbon- arc type and xenon-arc lamp arc type light-and-water-exposure type light-exposure tester,tester.

Sample holder

auxiliary holder

Standard test specimen

Sample holder

auxiliary holder

Standard test specimen

7.6 Irradiation Time Irradiation time shall be as follows:

(1) In the case of SR-LS-PMMA, it shall be 20 h.

(2) In the case of SR-LS-PE, it shall be 60 h.

— 117 —

7.7 Measuring Standard Test Specimen by a Spectrophotometer7.7.1 Measuring of SR-LS-PMMA

7K 7200-1986

(1) Measuring Principle of SR-LS-PMMA The absorption spectra of SR-LS-PMMA change as shown in Fig. 3 by the irradiation of light. Concerning the absorption in the vicinity of 420 nm, the peak position of an absorption does not change but only the absorbance changes. There is a correlation between the absorbance and irradiation time (irradiation energy) , and the comparison of irradiation energy can be carried out relatively by using this correlation.

Fig. 3. Absorption Spectra of SR-LS-PMMA (Example)

Irradiation for 40 h

Irradiation for 20 h

Irradiation for 10 hNo irradiation yet

Wavelength (nm)

(2) Measuring Apparatus The spectrophotometer specified in JIS K 0115 shall be used as a measuring apparatus. Instead, the spectrophotometer specifies in JIS Z 8722 may be used too.

(3) Measuring Method Measure the transmittance or absorbance at the peak near 420 nm within 5 nm of the wave length width before and after the irradiation during specified time. 4

(4) Calculating Method The changing ratio of absorbances shall be calculated according to following formula (1):

A -logd/r.) -log (i/Tt) Ac~ log (i/r.) X100 (1)

where Acr0

r,

log (1/To)

log (1/7,)

changing ratio of absorbance (%) transmittance before irradiation transmittance after /-hour irradiation absorbance before irradiation absorbance after / - hour irradiation

— 118 —

8K 7200-1986

(5) Changing Ratio of Absorbance and Irradiation Time The relation between the changing ratio of absorbance and irradiation time shall be shown in Fig. 4.

Fig. 4. Relation between Changing Ratio of Absorbance and Irradiation Time (Example)

a o

Irradiation time (h)

7.7.2 Measuring Method of SR-LS-PE 1

(1) Measuring Principle of SR-LS-PE When the light having an energy more than the bond energy in molecular chain is irradiated into a polyethylene molecule, a cleavage takes place, and owing to the oxidation reaction with the oxygen in air, carbonyl group is produced. As shown in the infrared absorption spectra of SR-LS-PE of Fig. 5, the number of carbonyl groups increases with the lapse of irradiation time (irradiation energy). Because there is a correlation between the number of carbonyl groups and irradiation time (irradiation energy), the irradiation energy can be compared correlatively by making use of this relation.

Fig. 5. Infrared Absorption Spectra of SR-LS-PE (Example)

2030 cm"

Wave number (cm- i)

— 119 —

9K 7200-1986

(2) Measuring Apparatus The infrared spectrophotometer specified in JIS K 0117 shall be used as a measuring apparatus.

(3) Measuring Method Measure the infrared absorption spectra after irradiation, in the range of from 2200 cm-1 to 1600 cm-1. In this case, use for the scanning speed the same as for a quantitative analysis.

(4) Calculating Method After finding the absorbance of methylene group at 2030 cm-1, and of carbonyl group at near 1715 cm-1 on the infrared absorption spectrum after irradiation, calculate the ratioof absorbances for carbonyl group according to the following formula (2):

where

Ar=

Ar:Ami :

A.2030 :

4:

I:

AmiAioiO (2)

ratio of absorbanceabsorbance at 1715 cm-1 [log( Jo/I )]absorbance at 2030 cm-1 [log( 4// )]transmittance measured by base-line method at individual wave number (Refer to Fig. 5).transmittance at the peak of individual wave number (Refer to Fig. 5)

Remark: The utilization of absorbance at 2030 cm-i as an internal standard has an effect to correct the error between infrared spectrophotometers.

(5) Absorbance Ratio and Irradiation Time The relation between theabsorbance ratio and the irradiation time shall be as shown in Fig. 6.

Fig. 6. Relation between Absorbance Ratio and Irradiation Time (Example)

0 20 40 SO 80 WO 120 140 ISO 180 200Irradiation time (h)

-120-

10K 7200-1986

7.8 Characteristic Value of Standard Test Specimen In order to arrange the characteristic values to be marked on a standard test specimen, calculate the total average value, standard deviation, and confidence limits at 95 % of the results measured at five organizations at least out of the organizations specified in 7.1.

8. Marking

The marking items concerning the standard test specimen shall be as follows, and the marking may be carried out on a record card.

(1) Class of standard test specimen

(2) Name of the organization deciding characteristic values

(3) Names of measuring organization and used spectrophotometer

(4) Characteristic values (kind of tester, total average value, standard deviation, and confidence limits at 95 %)

(5) Lot number of manufacturing

(6) Name of supplier

(7) Verifying organization and date of verification

(8) Storing method and available period

(9) Other necessary information

121 —

11K 7200-1986

Appendix Utilization of Standard Test Specimen

1. Utilization for Calibration of Irradiation Energy from a Light Exposure(Weather Resistance) Tester

In order to calibrate the irradiation energy from a light exposure (weather resistance) tester, the following utilization will be adopted as an example.

(1) When irradiating a standard test specimen under the condition specified in 7. Method to Decide the Characteristics described in the standard body, if the changing ratio of measured absorbance (in the case of SR-LS-PMMA) or the ratio of absorbances (in the case of SR-LS-PE) falls in the limit of characteristic value represented on the standard test specimen, the tester may be considered to be operated normally.

(2) In case of falling out of the limit of characteristic values represented on the standard test specimen, following items of the tester (x) referred to shall be inspected and adjusted.

(a) Discharge current and discharge voltage

(b) Remaining length of the carbon

(c) Adjusting condition of a black panel thermometer, machine inside temperature and humidity

(d) Existence of unusualness of a glove

(e) Using time of a glove or filter

Note (x) Refer to Note (x) of the Standard body 1.

(3) After adjusting, irradiate the standard test specimen again, and confirm that the values are set in the limit of characteristics.

(4) When the test results carried out repeatedly under the normal operating condition are out of the range of characteristics, following method can be adopted in the case of SR-LS-PE in order to get the coefficientof irradiation condition of the tester referred to. If the linear relation between the irradiation time and the ratio of absorbances (Ar) is confirmed after the irradiation for 30, 60, 90, and 120 h by using the tester referred to, the following value can be used for the caribration as the factor for irradiation condition of the tester.

Ar of standard test specimen by theFactor of the _ tester referred to_________________tester referred to Ar of standard test specimen rated

previously

- 122 —

12.K 7200-1986

2. Method for Utilization of Irradiation or Exposure Together with the Sample

When carrying out the test for material or products by means of a light exposure (weather resistance) tester or outdoor exposure test, a standard test specimen is irradiated or exposed together with the sample, and the following methods such as relatively comparing of irradiation energy or recording as a reference value according to the result of test, is available.

(1) In the case of Using SR-LS-PE

(a) Testing by a Light Exposure (Weather Resistance) Tester

Irradiate a standard test specimen together with a sample at 63 ± 3°C of a black panel temperature for 40 to 200 h. Next, after replacing by a new standard test specimen, irradiate it together with the sample. Repeat this irradiation until finishing the irradiation to the sample. Measure the absorbance ratio of respective standard test specimens. The total of the absorbance ratios of each standard test specimen until finishing the sample irradiation, shall be regarded as the index of condition under which the sample is irradiated.The comparison, however, between the light exposure (weather resistance) testers having respectively different light source, is impossible. The reason is that the changing condition of absorbance ratio is different according to the kind of light source.

(b) In the Case of Exposure Together with Sample at Outside ExposureTest Expose a standard test specimen together with a sample forone month, and, after replacing by a new standard test specimen, continue to expose together with the sample. Repeat this exposure until finishing the exposure of the sample. Measure the absorbance ratio of respective standard test specimen. The total of the absorbance ratios of each standard test specimen until finishing the sample irradiation shall be regarded as the index of condition under which the sample is irradiated.

(2) In the Case of Using SR-LS-PMMA to a Light Exposure (WeatherResisting) Tester When the relation between irradiation time andthe changing ratio (Ac ) of absorbance has been obtained previously, a standard test specimen is usable to the test by a light exposure tester by using 10 to 40 h unit similarly to (1)(a). This, however, cannot be used for the test employing spraying.

— 123 —

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0 NS—6(S —2) ■ SP(S —2)

— 206 —

NS - 6SP<D*[S - 4]

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M

— 207

11.1.

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-209 —

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0° 22.19 13.69 25.61 25.89 25.99 25.08

— 210 —

1.1.3-7 flm cfctf&ftftftfliai:

ma301~310(nm)

(KJ/rrf*nm)

311~32(Xnm)

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(KJ/rrf*nm)

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(KJ/nrf*nm)

Oct-99 126.0285 716.9656 1370.387 1658.67 1755.738 1910.465 2258.516 2366.792 2343.274 3001.245Nov-99 63.32066 438.7975 922.0561 1154.977 1230.681 1345.209 1596.423 1684.807 1678.949 2158.07Dec-99 40.76232 322.7019 734.5034 952.6602 1025.372 1125.536 1338.436 1417.707 1416.96 1825.851Jan-00 37.97569 301.5624 681.5636 877.2361 939.9564 1028.035 1219.25 1288.027 1284.859 1654.012Feb-00 61.07936 460.7682 1046.381 1344.969 1443.878 1585.779 1885.992 1990.018 1977.446 2528.977Mar-00 120.5674 760.8515 1553.026 1903.164 2027.791 2219.004 2635.472 2772.027 2750.533 3524.071

211-

Oct-99Nov-99Dec-99Jan-00

301-310(nm) 311-320(nm) 321-330(nm) 331-340(nm) 341-350(nm) (KJ/nf *nm) (KJ/nrf*nm) (KJ/rrf*nm) (KJ/rrf*nm) (KJ/nrf*nm)

126.029 716.966 1370.387 1658.670 1755.73863.321 438.797 922.056 1154.977 1230.68140.762 322.702 734.503 952.660 1025.37237.976 301.562 681.564 877.236 939.956

351-360(nm) 361-370(nm) 371-380(nm) 381-390(nm) 391-400(nm) (KJ/rrf*nm) (KJ/rrf*nm) (KJ/rrf*nm) (KJ/rrf*nm) (KJ/rrf*nm)

1910.465 2258.516 2366.792 2343.274 3001.2451345.209 1596.423 1684.807 1678.949 2158.0701125.536 1338.436 1417.707 1416.960 1825.8511028.035 1219.250 1288.027 1284.859 1654.012

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11.2

1) #48[E]IS0/TC61

2) ISO TC/61 MEETING Williamsburg, USA 27 September—2 October 1999

IS0/TC61 SC6 N736 Brief Minutes of the 21st meeting of ISO TC/61 SC6

Plastics — Aging, Chemical and Environmental Resistance

3) S471UISO/TC45

— 213 —

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— 217 —

ISO TC/61 MEETING 27 September - 2 October 1999

WILLIAMSBURG, USA

ISO/TC 61 SC6 N736

Brief Minutes of the 21st meeting of ISO TC/61 SC6 Plastics — Aging, Chemical and Environmental Resistance

Thursday, 30 September 1999, Williamsburg, USA

Attendance:Country Delegate Alternate Observer

BelgiumCanadaFrance

Roland DewittMario PerronAlain Ravet

Germany Jorg Boxhammer Peter Trubiroha (SC Convenor)

F.P. Berg (SC secretary)

JapanKoreaNetherlandsSwedenUnitedKingdom

Yashushi Watanabe Joon-Hyung Kim Huub OmlooElvy LarssonDuncan Gardiner

Y. Takane

United States Warren Ketola A. Lecompte (translator)

1. Opening of the Meeting.

Chairman Trubiroha opened the meeting at 14:00 and welcomed the delegates. Mr. Trubiroha announced that a consecutive translation is available for all who requested.

2. Roll Call

Chairman Trubiroha called the role and circulated an attendance list. Ten (10) P members were represented. No “O” members were present. A copy of the mailing list (N730) was circulated and members were asked to make any appropriate corrections.

-218-

ISO/TC 61/SC6 N736Brief minutes for meeting No.21, 30 September 1999, Williamsburg

Page 2

3. Adoption of the Agenda

The agenda (N715) was adopted with the addition of items 12.1, discussion of revision of ISO 472, and 7.2., appointment of a convenor for WG3. Mr. Trubiroha indicated that the correct document for the report of status of work (agenda item 6) was N729 instead of N713.

4. Appointment of the Drafting Committee

Mr. Ketola volunteered to write the English minutes. The French minutes will be written and distributed after the meeting.

5. Approval of Minutes from 1998 meeting in Whistler Canada

The brief minutes (N698) and the Meeting Summary (N700) for the 20th meeting held in Whistler were approved as published.

6. Report of the Secretary on Status of Work

Mr. Berg reviewed the status report for Subcommittee 6 work items (N729) and advised those in attendance that the reports from the working groups will show that significant progress was made on a number of items. An updated report on status of work reflecting progress made at this meeting will be distributed late in 1999 or early 2000.

ISO TMB has distributed a list of projects where progress has been delayed. For SC6, item 589, WD 16019 has not progressed for over 60 months. ISO requires that the document be at a DIS (or equivalent) stage by 84 months. It is likely that this item will be dropped from the official work program. Progress to gather data and information necessary to prepare drafts for consideration by the WG/SC is being made , but it is likely that a new work item will have to be taken for this project. Significant progress has been made on other projects that are behind the target schedule from ISO.

7. Reports of the Working Group Convenors

7.1 WG2 ‘Exposure to Light’, Dr. J. Boxhammer, Germany

WG2 met on Tuesday, 28 September. Nine countries (14 delegates, observers, and alternates) were represented. Dr. Boxhammer submitted his report (N733).

Item 265B, CD 15542 (former DTR 9763), Solar radiation and its measurement for determining outdoor exposure levels ISO Central Secretariat deleted this item from the official work program. No progress was made during the year. Mr. Ketola will contact Mr. Zerlaut, former project leader about preparation of an updated report or draft standard.

-219-


Page 3

Item 589, WD 16019, New Work Proposal on use of black panel and black standard thermometers. Temperature measurements for the second phase of the study are complete but data analysis is still underway. A report of the results from the second phase be completed by the end of 1999 and the black panels will be sent to Japan for the third phase of the experiment (outdoor exposures). The target date for preparation of a working draft of the report is September 2000.

Item 631, ISO CD 15314: Plastics - Method for marine exposures ofplastics.Mr. Ketola tabled a draft including all comments from the CD ballot. The WG unanimously recommended that the revised draft should be advanced to DIS.

Item 633, Type IDTR, Weathering Tests for Photodegradable Plastics Mr. Ketola presented a summary of voting results and comments to the WG. The WG felt that negative votes were mostly caused by confusion about whether the draft was a DTR or a CD. The working group unanimously agreed that a revised draft to address negative comments should be submitted for vote as a Technical Specification.

Five year reviews Results from the five year review are reported in ISO TC/61 SC6 N726.

ISO 877 (1994) The working group unanimously recommended that this standard should be reconfirmed for another five years. The project leader was asked to prepare a proposal to divide the standard into separate standards covering conventional and solar concentrating exposure.

ISO 4892-2 (1994); ISO 4892-3 (1994); ISO 4892-4 (1994)

Germany and the USA presented technical justification for their votes on disapproval for reconfirmation. Based on this information, the working group unanimously recommended that all three parts should be revised. Project leaders are:

Revision of ISO 4892-2 Boxhammer/DERevision of ISO 4892-3 Brennan/USARevision of ISO 4892-4 Watanabe/Japan

An ad hoc group consisting of USA, Germany, UK, and Japan will prepare a revision for part 2 as a model for for the revision of parts 3 and 4. Target dates are end of 1999 for preparation of the revised part 2 , and end of June 2000 for the draft revisions of parts 3 and 4. These documents will be circulated within SC6 for comments.

Reference material for use in weathering tests A draft document is in preparation but not complete. Mr. Trubiroha will distribute a completed draft to

220-

ISO/TC 61/SC6N736Brief minutes for meeting No.21, 30 September 1999, Williamsburg

Page 4

Mr. Ketola (USA) and Mr. Watanabe (Japan) by the end of the year. The objective of this project is preparation of a Technical Specification (TS).

Future work There were no new items of future work.

Mr. Gardiner (UK) asked what could be done to take a more proactive role in advising other ISO committees about the use of weathering standards that are the responsibility of WG2. The WG indicated that continued liaison and personal support to these committees remains the best way to help other committees.

There was unanimous approval of SC6 members in attendance to accept all WG2 recommendations for advancing these documents.

7.2 WG3, ‘Various Exposures’, Mr. Trubiroha, Germany

WG3 met on Monday, 27 September with eight countries (11 delegates, alternates, and observers) present. Mr. Trubiroha (acting concenvor) submitted his report (N734).

SC9 has accepted transfer of ISO 182, parts 2, 3, and 4 (projects 28B, 28C, 28D, and 28E) from SC6. These standards are now part of the work program of SC9/WG20.

Based on results from five year review, WG3 unanimously recommended that ISO 4611 (1987) be reconfirmed for another five years.

Dr. Carlile (Italy) has retired, and Italy did not nominate a replacement for him, creating an opening for convenorship of WG3. Mr. Trubiroha, SC6 Convenor, requested that Dr. Igancy Jakubowicz (Sweden) has agreed to be considered for the convenorship of WG3.

There was unanimous approval of SC6 members in attendance on the appointment of Dr. Jakubowicz as WG3 convenor, and to accept all WG3 recommendations made at this meeting for advancing their documents.

7.3 WG7 — Basic Standards, W. Ketola, USA

WG7 met on Monday, 27 September with six countries (10 delegates, alternates, and observers) present. Mr. Ketola submitted his report (N735).

Project 16D, ISO FDIS 62 Plastics — Determination of Water Absorption The revised ISO 62 was published on 1 Februrary 1999. Mr. Trubiroha, project leader, reported that a round-robin involving three materials (1 mm and 2 mm thick PMMA, and 1 mm thick PC) and sixteen participants has started. So far, daa has been received from 10 participants. Analysis of all round-robin data will be complete in early 2000.

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Project 195A, ISO 2578, Plastics — Determination of Time-Temperature Limits After Prolonged Exposure to Heat. At the last meeting, revision of ISO 2578 was approved based on the USA negative vote for reconfirmation. Because the concerns of the USA are being addressed in an IEC working group (SC15E/WG1) no work was done on preparation of a revised ISO 2578. The IEC working group is conducting a round-robin for both TI (thermal index) and RTI (relative thermal index). The working group recommended that ISO 2578 be reconfirmed for another five years. Future revisions can be based on results from the IEC working group.

Project 706, ISO CD 16869, Plastics - Assessment of the efficacy offungistatic compounds in plastic formulations. The CD ballot closed on 15 April 1999. There were 16 approvals and 1 disapproval (USA). Comments from the USA were incorporated into a revised draft that was submitted as a DIS on 4 August 1999.

Five year reviews

During 1999, five year reviews were conducted on ISO 176, ISO 177, ISO 183, ISO 483, and ISO 4577. Results from the five-year review ballot are summarized in SC6 N728. Based on the five year review ballot, the working group made the following recommendations :

ISO 176:1988 Plastics - Determination of loss of plasticizers - Activated carbon method

Revise to add precision statement (W. Ketola project leader)

ISO 177:1988 Plastics - Determination of migration of plasticizers

Reconfirm

ISO 183: 1976 Plastics - Qualitative evaluation of the bleeding of colourants

Revise based on disapprovals from the USA and Netherlands (H. Omloo project leader)

ISO 483:1988 Plastics - Small enclosures for conditioning and testing using aqueous solutions to maintain humidity at constant value

Based on a negative from Germany, revise (fast track ballot) to harmonize the tolerance for % RH with the requirements of ISO 291 and section5.1.1.1 of ISO 483

222-

ISO/TC 61/SC6 N736Brief minutes for meeting No.21,30 September 1999, Williamsburg

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ISO 4577, Plastics - Propylene and propylene copolymers, determination of thermal oxidative stability in air - oven method

Reconfirm and transfer to ISO TC/61 SC9/WG6.

The subcommittee unanimously accepted all recommendations of WG7 for advancement of their standards.

8. Liaison Reports

A liaison report from the ASTM G3 Committee on Weathering and Durability was distributed as document N724. Dr. Boxhammer gave an oral report on the work of ISO/TC45/SC2. A written summary of this report will be distributed as document N732. Dr. Kockott, liaison to ISO/TC35/SC9/WG26, has retired. Dr. Boxhammer reported at this WG is working on a revision of ISO 2810 (outdoor weathering of paints and coatings) and a new standard for image analysis of changes caused by weathering. ISO/TC35/SC9/WG26 is also working on a revision of ISO 11341 (xenon arc exposures of paints and coatings). The basis for this revision is the same as for the revision of ISO 4892-2. Efforts to keep these standards as similar as possible will be made. Mr. Riedl will replace Dr. Kockott as liaison officer to ISO/TC35/SC9/WG26. A summary of liaison reports is found at the end of these minutes.

9. Items on which no progress has been made

Refer to Mr. Berg’s report in item 6.

10. Items for Future Work

At the 1998 meeting, Mr. Trubiroha asked that SC6 members to provide input to a joint ISO/IEC TAG on Metrology regarding how metrology impacts SC6 standards. No SC6 members provided input and Mr. Trubiroha has informed ISO TAG 4 that there is no interest in this project from SC6.

11. Requirements for 1999 Meeting

Mr. Trubiroha announced that the 2000 meeting will be hosted by France from 23 through 30 September at Futuroscope of Poitiers. The following are the meeting requirements for 2000.

SC6 Convenors 0.5 hour, 09:00 on MondayWG2 4 blocks on TuesdayWG3 2 blocks on Monday AM (beginning at 09:30)WG7 2 blocks on Monday PMSC6 2 blocks on Thursday PM

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12. Any other business.

Mr. Berg distributed a list of terms that will be sent to SCI for consideration in the revision of ISO 472. SC6 members must provide information on additional terms for inclusion in the ISO 472 revision to Mr. Berg before the end of April 2000, so he can prepare the complete SC6 response to SCI by 15 May.

13. Approval of resolutions.

No resolutions were brought up for SC action.

14. Closing of the meeting.

Chairman Trubiroha thanked the delegates and closed the meeting at 15:08 hr.

Respectfully submitted,

Warren Ketola

Liaison Reports to SC6,1999

Committee Liaison OfficerStatus or SC6 document number for written report

ISO TC/35 SC9 WG 26 A. Riedl Dr. Boxhammer provided an oral summary‘Performance tests’ (2000) at this meeting (see item 8)ISO TC/45 SC2 ‘Rubber and rubber products — physical and degradation tests’

J. Boxhammer Written report distributed as ISO TC/61 SC6 N732

ISO TC/180 ‘Solar Energy’

W. Ketola No report

CEN TC/254/ WG10 ‘Flexible roof coverings, weathering’

P. Trubiroha Mr. Trubiroha provided an oral summary at this meeting. No activity during the year outside of the preparation of a German translation of a standard describing weathering tests for flexible roof coverings. Publication of this standard is scheduled for late 1999 or early 2000.

ASTM G3 Committee ‘Weathering and Durability’

W. Ketola Written report distributed as ISO TC/61 SC6 N724

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DOC SC6/WG2 N 733

Brief Minutes of the meeting of ISO/TC61/SC6/WG2 „Light Exposure"

Held on 28th September, 1999, Williamsburg USA

Present:

Name Country (status) Box no.M. Perron Canada (0) 20X. J. Ling China (D) 261Ch. Gancet France (D) 135A. Ravet France (D) 97F. Berg Germany (Sec SC6) 120P. Trubiroha Germany (D) 133J. Boxhammer Germany (Convenor) 168F. Bemardi Italy (D) 226Y. Watanabe Japan (D) 61Y. Takane Japan (0) 60Y-W.Kim Korea (D) 169D. Gardiner United Kingdom (D) 40W. Ketola United States (D) 17P. Brennan United States (A) 35

1. Opening of the meeting

The meeting was opened at 9.00 a.m..

2. Roll Call of Delegates

The roll call of delegates was conducted and the mailing list was circulated for corrections.

3. Draft Agenda (doc. ISO/TC61/SC6 N722)

The draft agenda was adopted.

4. Approval of minutes (doc. ISO/TC61/SC6 N696)

The brief minutes of the Whistler meeting were approved as published.

5. Status of work (doc. ISO/TC61/SC6 N723)

The status of work was presented. Active items are on the agenda.

6. Item #265B-CD 15542

No official work was done during the last year. Mr. Ketola will contact Mr. Zerlaut for getting information on the status of this project.

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7. Item#589-WD 16019

Mr. Ketola informed the WG on the „Phase II“-measurements carried out in USA. The measurements are completed but the data have still to be evaluated until the end of 1999. The measuring elements will then be sent to Japan for conducting „Phase III“- measurements.

A working draft is expected for September 2000. Due to the very long preparation stage (longer than 7 Years) this WI will probably automatically deleted. The question how to proceed will be clarified with the CS.

8. Item # 631 - CD 15314

A redrafted CD including all comments was tabled and discussed by the PL Mr. Ketola. The WG unanimously agreed to recommend the document to SC6 for advancement to DIS.

9. Item # 633 - Preparation of DTRtype 1

The summary of voting results containing four negatives was presented by the PL. The WG felt that the negative votes were mostly caused by the fact that the paper was circulated as a CD even though a TS was intended. Taking the comments from the ISO CS into account a revised document will be prepared reflecting the comments received. The WG unanimously agreed to proceed the redrafted document for vote as a Technical Specification.

10. Five year reviews

The results of systematic review were given in doc. ISO/TC61/SC6 N726. Based on the results the following decisions were unanimously made by the WG.

ISO 877 (1994)

The standard will be reconfirmed.

The PL was asked to prepare a proposal how to divide the standard in two parts (conventional and accelerated outdoor exposure) and reflecting the comments made by Japan until the next meeting in France.

ISO 4892-2 (1994); ISO 4892-3 (1994); ISO 4892-4 (1994)

Germany and USA explained the technical reasons for disapproval of part 2. The WG unanimously decided for revision of part 2 (PL: Boxhammer/DE) based on these informations. The parts 3 (PL: Brennan/US) and 4 (PL: Watanabe/Japan) shall be revised too taking the restructered part 2 as a model. The documents will be redrafted by an ad hoc group with USA, Germany, UK and Japan. The target dates are as follows: Preparation of part 2 (as a model) until the end of 1999, parts 3 and 4 until the end of June 2000. The documents will then be circulated in SC6 for comments. Discussion and decision for CD vote follows at the next meeting in France.

— 226 —

11. Reference materials for use in weathering tests

A draft document was not yet available but Mr. Trubiroha will send a structered paper to Mr. Ketola and Mr. Watanabe by the end of the year. The objective of this work is a TS.

12. Future work

There were no new items.

13. Requirements concerning a future meeting

For the 2000 meeting four blocks will be needed on Tuesday.

14. Any other business

Mr. Gardiner distributed a note and raised the question how the WG could take a more proactive role in advising other committees (e.g. in ISO or CEN) who propose to apply weathering standards to specific materials or products. There was no answer beyond the existing liaison activities and personal support given by individual experts on request.

The SC6-Secretary informed that SC6 and ist WG's are asked to give information about new terms to be incorporated in the new (4th) edition of ISO 472.

The meeting was closed at 12:40 p.m..

— 227 —

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12 ^ 3 n - OSTI.GOV

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