Untitled - EUR-Lex

Publication No EUR 14800 of the

COMMISSION OF THE EUROPEAN COMMUNITIES

Scientific and Technical Communication Unit

Directorate-General Information Technologies and Industries, and Telecommunications Jean Monnet Building L-2920 Luxembourg

LEGAL NOTICE

Neither the Commission of the European Communities nor any person acting on behalf of the Commission is responsible for the use which might be made of the following information.

Cataloguing data can be found at the end of this publication.

Luxembourg: Office for Official Publications of the European Communities, 1992

ISBN 92-826-4968-7

© ECSC-EEC-EAEC, Brussels · Luxembourg, 1992

Printed in Belgium

Commission of the European Communities

Directorate-General for Science, Research and Development

Technical Research

The BCR programme

on applied metrology and chemical analysis

PROJECTS AND RESULTS 1988-92

BCR Community Bureau of Reference

Production and printing: POPLAR

LIST OF PROJECTS

APPLIED METROLOGY Page

Mechanical Metrology

MTR 062 Development of a six component dynamometer of 500 kN 5 MTR 071 A portable system for the testing of industrial robots 6 MTR 075 The verification of three coordinate measuring machine

evaluation algorithms 7 MTR 107 Angle gauge measurements 8 MTR 109 Development of Si02 on Si reference materials 9 MTR 118 Dynamic force calibration 10 MTR 123 Intercomparison of roudness and form measurements 11 MTR 136 Intercomparison of standards for the measurement of

low differential pressures at or near atmospheric pressure 12

MTR 138 The mathematical representation of geometric form 13 MTR 141 Evaluation of the effect of variations in the

refractive index of air upon the uncertainty of industrial interferometric length measurement 14

MTR 150 Intercomparison of flatness measuring methods and devices 15

MTR 157 Development of testing procedures for CCD cameras 16 MTR 158 Chebyshev reference software 17 MTR 159 Development of testing procedures for optical probes 18 MTR 160 Development of methods for the numerical error

correction of machine tools 19 MTR 161 Real-time position and form measurements on machine

tools and coordinate measuring machines by means of multi-function laser interferometry based on stabilized laser diodes 20

MTR 162 Multi-sensor electro-optical equipment for automated manufacturing systems 21

MTR 170 Development of a method for the characterization of roughness in 3 dimensions 22

MTR 172 An intercomparison of type examinations of non-automatic weighing instruments 23

MTR 173 Coordination of- and participation in an intercomparison of masses in the range of 1 tonne up to 5 tonnes 24

VI

MTR 174 Development of in-process measurement techniques for optical quality and position of elements in small integrated optical systems 25

MTR 176 Development of a photomask linewidth standard 26 MTR 180 Optical inspection system for the measurement of

three dimensional shapes 27 MTR 182 Combined X-ray and optical metrology for high

precision dimensional metrology 28 MTR 183 Standardless thin layer metrology using a non

destructive X-ray interference technique 29 MTR 184 STM methods for roughness and micro hardness

measurements 30 MTR 185 Characterisation and development of surfaces in the

0.1 nm range 31 MTR 187 In-line dimensional measurements of composite

workpieces produced by filament winding technology 32 MTR 188 Inspection of surface structures by conoscopic and

image processing methods 33 MTR 189 The development of a two dimensional high precision

photomask position standard 34 MTR 190 Non contact surface metrology 35 MTR 191 In-process ultra-high frequency evaluation of abrasives 36 MTR 195 The development of test and calibration procedures for

automated theodolite systems in production metrology 37

Temperature

MTR 116 Calibration of industrial platinum resistance thermometers 41

MTR 117 Nisil - Nicrosil thermocouples 42 MTR 128 Intercomparison of temperature measurements using

microcrucibles 43 MTR 133 Development of noble metal thermocouples 44 MTR 137 Intercomparison on fixed points 45 MTR 186 Measurements for the development of new reference

tables for platinum-rhodium thermocouples 46

Optical Metrology

MTR MTR MTR MTR MTR MTR

085 095 096 114 129 134

Study of the stability of silicon photodiodes 49 Luminous flux of fluorescent tubular lamps 50 Luminous flux of high pressure sodium lamps 51 Stabilized laser source for interferometry 52 Intercomparison of colour measurements 53 Intercomparison of laser power measurements 54

Vil

MTR 142 Establishment of an improved infrared spectral responsivity scale 55

MTR 165 Operation limits of intense light sources in hazardous atmospheres 56

MTR 177 Measurements of spectral transmittance and reflectance at variable angles of incidence 57

Electrical Metrology

MTR 044 Treatment, measurement and certification of nickel cylinders 61

MTR 082 Intercomparison measurements of resistances in A.C 62 MTR 092 Improvement of procedures for the testing of the

susceptibility of electronic instruments to electromagnetic radiation 63

MTR 093 Intercomparison measurements with electromagnetic field strength meters 64

MTR 094 Magnetic measurements on electrical sheet steels by means of single sheet testers 65

MTR 098 Solid state voltage transfer standards 66 MTR 099 Intercomparison of resistance standards of 1 kOhm and

10 kOhm 67 MTR 115 Calibration of capacitors and frequencies of 10 kHz to

1MHz 68 MTR 124 Intercomparison of software for evaluating high

voltage impulses and step responses 69 MTR 130 Intercomparison of thermal ac-dc current transfer

standards 70 MTR 143 Intercomparison of measurements of permanent magnets 71 MTR 181 Measurement of submicron semiconductor junction depths

and width 72

Acoustics and Ultrasonics

MTR 113 Intercomparison of ultrasonic power calibration of ultrasonic transducers from 1 to 10 MHz 75

MTR 122 Sound calibrators 76 MTR 125 The development of improved methods of sound absorption

measurement 77 MTR 127 Noise attenuation by windows (with frames) 78 MTR 132 Development of standard measurement methods for

essential properties of ultrasound therapy equipment 79

VIH

MTR 146 Intercomparison of free field calibration of microphones 80

MTR 155 Intercomparison of open-inlet/open-outlet noise measurement on fans 81

MTR 156 Calibration of sound intensity meters 82 MTR 168 Intercomparison of sound power measurements by use of

reference sound sources 83 MTR 192 Hearing protector performance in impulsive noise 84

Flow Measurements

MTR 016 Intercomparison of orifice plate discharge coefficients

MTR 108 Intercomparison of anemometer calibrations MTR 120 Intercomparison of discharge coefficients of a 600 mm

orifice plate meter MTR 121 Flow modelling for metering purposes MTR 139 Evaluation of a system for the metering of

multi-phase flows MTR 166 Intercomparison of hot water calibration test

facilities MTR 193 Installation effects on ultrasonic flow meters for

gas applications

87 88

89 90

91

92

93

Physical Properties

MTR 102 Emissivity of glass 97 MTR 105 Heat transmission through framed windows 98 MTR 106 Intercomparison of critical current measurements in

Nb3Sn superconductors 99 MTR 110 Improved energy loss coefficients for heating and

ventilating systems 100 MTR 135 Emissivity measurements at elevated temperature 101 MTR 140 Total hemispherical emissivity of coated glass 102 MTR 154 Measurements of high temperature thermal conductivity

of liquids 103 RM 268 Thermal conductivity of industrial refractories 104 RM 270 Reference material for the measurement of the

viscosity of high temperature slags 105

rx

Standardised Tests

MTR 079 Intercomparison of micro-hardness measurements MTR 103 Solderability MTR 144 Development of an abrasion test on plastic spectacle

lenses MTR 145 Intercomparison of abrasive testing for synthetic

footwear materials MTR 147 Determination of the Κ coefficient of refrigerated

trucks & containers MTR 148 Measurement of the pressure exerted by elastic medical

stockings MTR 149 Intercomparison of tensile & flexural fatigue tests

on unidirectional reinforced polymer matrix composites MTR 151 Water permeation in building materials MTR 152 Testing of the water tightness of windows MTR 153 The determination of yarn twist MTR 163 Intercomparison on the local approach to fracture MTR 164 Fire testing MTR 167 Cold bending test for roofing materials MTR 171 Timber calibration planks MTR 175 Characterization of air blast sprayers for spraying

pesticides in orchards and vineyards MTR 178 The qualification testing of heating boilers thermal

efficiency and NO, emission MTR 179 Internal pressure testing of tubes MTR 196 Fire testing of upholstered furniture RM 253 Reference material for the verification of creep

testing machines RM 269 Intercomparison of low cycle fatigue measurements

109

110

111

112

113

114

115

116

117

118

119

120

121

122

123

124

125

126

127

128

CHEMICAL ANALYSIS

Food Control

Natural toxins and microbiology

RM 226 Mycotoxin calibrants RM 328 Aflatoxin Β, in edible peanuts RMs RM 367 Deoxynivalenol (DON) in wheat and maize RM 392 Improvement in the determination of ochratoxin A in

farm animals, products and cereals

133 134 135

136

RM 276 Diarrheic shellfish poisoning (DSP) 137 RM 422 Paralytic shellfish poisoning (PSP) 138 RM 395 Ethyl carbamate in wine RMs 139 RM 301 Reference materials for microbiological testing

of food & feed 140

Polycyclic aromatic hydrocarbons (PAHs) in food 141 Determination of genotoxic compounds in processed food 142 Determination of chlorinated pesticides 143

Nitrate determination in foodstuffs 144 Heavy metals in wine RMs 145 Overall migration from plastic materials 146 Specific migration from plastic materials 147

Contaminants

RM RM RM

RM RM RM RM

204 283 285 & 266 342 407 409 410

Nutrition and nutritional labelling

Reference materials for milk fat analysis 148 Cholesterol and other sterols in edible oil and fat RMs 149 Major nutritional properties of food 150 Fruit juice analysis 151 Determination of H/D isotopic ratio at natural abundance level in wine by quantitative NMR spectrometry 152 Dietary fibre reference materials 153 Determination of common wheat in pasta 154 Identification of irradiated food 155 Improvements in analysis of vitamins in food 156 Improvements in the determination of folates in food 157 Improvements in the determination of vitamin B„ B2, and B6 158 Improvements in the determination of vitamin D 159 Development of a liver reference material for determination of vitamins 160 Development of advanced analytical methods to determine the authenticity of fruit juice 161

Other food related properties

RM 273 Water sorption isotherm reference material 162 RM 281 Reference materials for the determination of

rheological properties of flours 163 RM 300 Reference tiles for the calibration of measurement

of colour of tomato paste and similar products 164

RM RM RM RM RM

RM RM RM RM RM RM

RM RM

RM

225a 225b 239 280 284

330 333 340 341 400 401

402 406

412

XI

RM 312 Determination of polyphenolic compounds in agro-food products 165

RM 418 Application and improvements of supercritical fluid extraction (SFE) to reference measurements for food and agriculture RMs 166

RM RM RM RM RM RM

308 310 368 358 384 413

Agriculture

RM 307 Rapeseed reference materials with certified glucosinolate and sulphur contents 169 Calibrants for glucosinolate analysis of rapeseed 170 Anatoxin B! in compound animal feed 171 Aflatoxin B! in peanut meal (animal feed) 172 Determination of chlorinated pesticides in animal feed 173 Determination of amino acids in animal feed 174 Improvements in the determination of tryptophan in feed 175

Veterinary drugs in urines, tissues and feed

Stilbenes (growth hormones) in farm animals 176 Nor-testosterone in cattle urine and meat RMs 177 Sulphadimidine in pig kidney, liver and muscle RMs 178 Thyrostatics in cattle urine and meat RMs 179 Trenbolone in cattle urine and meat RMs 180 ß-Agonists in cattle and pig tissues and urine RMs 181 Chloramphenicol in meat, milk and eggs RMs 182 Zeranol in cattle urine and meat RMs 183 Oxytetracycline (OTC), dihydrostrepamycin (DSTREP) and ampicillin in calf muscle and cow milk RMs 184

RM 381 Development of a Community method for the determination of ß-agonists in animal feed 185

Other agricultural measurements

RM 309 Oil content of rapeseed 186 RM 334 Development of a method for the determination of

dry gluten in durum wheat 187 RM 338 NIR spectrometry for cereal and feed quality control 188 RM 373 Rennet whey in milk powder 189 RM 374 Improvements in Infra-Red spectroscopic analysis of

milk 190 RM 377 Determination of amylose in rice 191

RM RM RM RM RM RM RM RM RM

272 339 344 346 347 362 364 365 366

Xll

Environment

Elements and trace elements

RM RM

RM

RM

RM

RM RM RM

RM RM RM RM RM RM RM

RM

238 249

250

264

278

297 316 326

349 360 369 370 372 390 393

404

Trace elements in fish 195 Reference materials for the analysis of plants for animal feed 196 Reference materials for the analysis of the aquatic environment 197 Reference materials for the analysis of sea water and estuarine water 198 Chemical analysis to monitor damage caused by acid deposition 199 Reference materials for the analysis of freshwater 200 Human hair 201 Improvement of the state of the art in neutron activation analysis 202 Multi-element characterization in cabbage 203 Renewal of reference materials for soils 204 Reference material for the analysis of white clover 205 Reference material for the analysis of plankton 206 Reference materials for the analysis of rain water 207 Renewal of reference material for milk analysis 208 Improvement of the determination of trace elements in lichen 209 Reference material for the analysis of mercury in sea water 210

Dangerous organic compounds (PAH, PCB, dioxins, pesticides)

Chlorinated biphenyls in sewage sludge 211 Pure polychlorinated dibenzo-p-dioxins reference materials 212 Pure oxygenated-polycyclic aromatic hydrocarbons 213 Determination of chlorinated dibenzo-p-dioxins and -furanes ("dioxins") 214 Short-term mutagenicity testing 215 Determination of reference spectra of polycyclic aromatic compounds and chlorinated aromatic compounds 216 Determination of traces of PAHs in sewage sludge 217 Industrially polluted soils (coking plant soils) 218 PCBs in waste mineral oil 219 PCBs in milk powder 220 Dioxins in fly ash 221 Organo-chlorine compounds in industrial soils 222 PCBs in industrial soils 223 Modern polar pesticides in water and sediments 224 Dioxins in milk powder 225

RM RM

RM RM

RM RM


246 254

274 277

291 304

331 332 354 355 361 371 378 387 394

Xlll

RM RM RM RM

RM RM

313 315 336 345

348 351

RM 408 PAHs in industrial soil 226 RM 417 Organic and inorganic contaminants in harbour dredge 227

Element speciation

RM 311 The determination of methyl mercury species in the environment and in food 228 Alkyl-tin species in the marine environment 229 Speciation of trace metals in soil and sediment 230 Speciation of arsenic 231 Improvement of the determination of Cr in environmental matrices 232 Speciation in lead 233 Improvement of the determination of aluminium and Al-species 234

RM 385 Improvement of the determination of selenium species in environmental matrices 235

RM 405 Improvement of the determination of chromium species in environmental matrices 236

Bacterial contamination

RM 286 Reference materials for microbiological testing of water 237

RM 389 Seawater microbiology 238

Pollution

S02 in air 239 Aromatic hydrocarbons in tenax 240 Aromatic hydrocarbons in charcoal 241 Chlorinated hydrocarbons 242 Workplace air sampling 243 Improvement of the determination of fluoride and chloride in coal and fly ash 244

RM 396 Improvement of the determination of fluoride and chloride in clay 245 Aldehydes in workplace air 246 Isocyanates in workplace air 247 NO, from boilers 248

RM RM RM RM RM RM

235 265(a) 265(b) 329 335 388

RM RM RM

397 398 411

XIV

Biomedical Analysis

Electrolytes

RM RM

303 380

Hormones

RM RM RM RM RM RM

174 353 217 320 321 322

Tumour markers

RM RM RM RM

323 324 325 403

Enzymes


Other

RM RM RM RM RM RM

260 282 293 294 295 296 318 319 375

proteins

262 292 298 306 350 379

Magnesium and lithium in human serum 251 Ionised calcium in human blood, serum and plasma 252

Progesterone in human serum 253 17 ß-Oestradiol in human serum 254 Thyroxine in human serum 255 Human luteinizing hormone 256 Human follicle stimulating hormone 257 Human prolactin 258

a-Foetoprotein 259 Carcinoembryonic antigen 260 Human chorionic gonadotropin 261 Epidermal Growth Factors and Growth Factor Receptors 262

Creatine Kinase 263 Alkaline Phosphatase 264 Lactate Dehydrogenase 265 Alanine Aminotransferase 266 Prostatic Acid Phosphatase 267 Aspartate Aminotransferase 268 Pancreatic α-Amylase 269 Pancreatic Lipase 270 Monospecific antibodies to human creatine kinase Β 271

Glycated haemoglobins 272 Apolipoproteins 273 Second Reference rabbit thromboplastin 274 Thyroglobulin 275 Reference material for 14 human plasma proteins 276 Feasibility study of a preparation of purified human osteocalcin by genetic engineering 277

XV

Metabolism products

RM 376 Creatinine in human serum 278 RM 386 6 ß-Hydroxycortisol in human urine 279 RM 391 Cholesterol in human serum 280

Serological tests

RM 314 Collaborative study on Hepatitis Β vaccines 281 RM 352 Antineutrophil cytoplasmic antibodies (ANCA) 282 RM 416 Blood Grouping Reagents 283

Metals and Industrial Products

Oxygen in semiconductor silicon 287 Impurities in copper 288 Analysis of coal 289 Low oxygen in copper 290 Impurities in zinc and zinc alloys 291 Gross calorific value of natural gas 292 Titanium and titanium alloys 293 Coal bottom ash 294 Alkali leaching from pharmaceutical glass containers 295 Development of near infra red methodology for the determination of the composition of fibre blends 296 Replacement of coke CRMs 297

RM RM RM RM RM RM RM RM RM RM

RM

189 210 221 231 232 234 261 327 337 363

415

Surface Analysis

Energy and intensity calibrations for XPS and AES 301 Auger Electron Spectroscopy intensity calibrant 302 The analysis of monolayer segregants in steels 303 Silicon dioxide reference material for XPS 304 The effects of crystallinity on the quantification of Auger electron spectroscopy 305

RM 305 Intercomparison of surface analysis measurements of oxide films of aluminium 306

RM 317 Establishment of a practical background substraction algorithm for XPS and AES 307

RM 343 Second XPS intensity intercomparison 308 RM 359 Reference spectra for Auger Electron Spectroscopy 309

RM RM RM RM RM

193 287 288 290 299

APPLIED METROLOGY

Mechanical Metrology

PROJECT MTR 062

DEVELOPMENT OF A SIX COMPONENT DYNAMOMETER OF 500 kN

PROJECT DEFINITION

Based on a previous work done on a small multicomponent dynamometer (EUR 10229), a new dynamometer will be designed and built. The main requirement was for it to be suitable for the verification of hydraulic machines which have a capacity of up to 1 MN.

STATUS

In progress.

CONTRIBUTION OF THE COMMISSION

ECU 107 000

PARTICIPANT

Istituto di Metrología G. Colonnetti, I.

PROJECT MTR 071

A PORTABLE SYSTEM FOR THE TESTING OF INDUSTRIAL ROBOTS

PROJECT DEFINITION

The development and application of industrial robots is accelerating rapidly. This causes an increased need for testing, in particular in terms of movement accuracy and repeatability. The objective of the project was to produce a portable calibration system able to operate on the shop floor and cause minimum disruption of the production.

RESULTS

In a first step, feasibility studies were given to four competing proposers and were assessed by a group of experts from industries which either manufacture or utilize robots. They considered that the system to be developed should : 1. be non contacting and not require the removal of either the robot and effector

of fitting and fixtures in the working volume; 2. be capable of giving information not only upon the position of the robot and

effector to within 0.05 mm, for a 1 cubic meter working volume, but also upon its orientation to within ± Io when the robot is moving at up to 3 m/s;

3. be demonstrably free of environmental effects such as vibration and thus capable of following tool oscillations of up to 50 Hz.

A device, based upon triangulation and laser tracking by up to 4 sub-systems, was selected for development at the University of Surrey, UK. This was operational in late 1988 and was demonstrated to more then meet the specification given above. In 1989 full software for testing to the draft ISO standard for robot evaluation became available and the device was patented by the Commission of the European Communities. Any commercial user may apply to acquire a licence for the system.


ECU 436 000

PARTICIPANTS

Cranfield Ins t , of Technology Robotics and Automation Group, UK Laboratoire National d'Essais, F Physikalisch-Technische Bundesanstalt, D Universi ty of Surrey, Dept of Mechanical Engineering, UK.

PROJECT MTR 075

THE VERIFICATION OF THREE COORDINATE MEASURING MACHINE EVALUATION ALGORITHMS

PROJECT DEFINITION

Three coordinate measuring machines (3 CMMs) are used throughout industry to determine if complex parts are within the required tolerances. In general the machines operate on an automatic or semi-automatic basis in accordance with a predetermined routine. The results are then analysed by a computer using algorithms derived for specific geometrical shapes such as the straight line, plane, circle, ellipse, cylinder, cone and sphere. Since the user has no access to the evaluation programme or the algorithms employed he is forced to rely upon that the algorithms are able to cope with the problems met in practice and provide an accurate analysis. It is therefore to both the user's and the manufacturers' advantage to have available an independent means of verifying data evaluation programmes.

RESULTS

In the first phase of the project completed in 1987, data sets containing a range of deviations from ideal geometries, were produced for a range of geometrical forms. When these data sets were tested using programmes from 15 laboratories in Europe it was found that some analysis programmes were unable to interpret the information accurately. The second phase of the project was established in association with 3 CMM manufacturers. It terminated 1990. Data sets have been produced for the same basic geometries but having higher demands on the evaluation programmes. It was shown that only about 50 % of the algorithms tested obtained acceptable results. The data sets will be made available to industry. In order to maintain confidence in the result, it is necessary to keep the basis of the data sets secret. Potential users must therefore apply to PTB in Germany, via their own national metrology laboratories.


ECU 117 000

PARTICIPANTS

Hie data sets for both phases have been generated by the Physikalisch-Technische Bundesanstalt (D) prior to their distribution to JTI, DK LNE, F IHGC, I National Physical Laboratory, UK TU Eindhoven, NL, in the first phase and to National Physical Laboratory, UK IMGC, I, plus 15 further participants in the second phase.

PROJECT MTR 107

ANGLE GAUGE MEASUREMENTS

PROJECT DEFINITION

The objective of the project was to develop a simple and robust measurement device for angle measurements up to 10° with uncertainty below 1".

RESULTS

The device is terminated. It consists of two rotary tables of high accuracy and autocoüimators. It can be used to calibrate gauge blocks, autocollimators and angular laser interferometers. It can achieve an uncertainty of 0.2" (one sigma) (Publication EUR Report 11762). It was then circulated to a number of laboratories for an intercomparison to determine its performance when measuring angle gauge blocks in the range of 1" to 30". The device itself was calibrated by each participant using 5 transfer standards of nominally 1", 2", 5", 20", and 30". This calibrated instrument was then used by each participant to measure a similar set of gauges of unknown value. It was shown that the spread of the results (1 sigma) was within 0.02" and 0.07" if two outliers were not considered.

In addition, three of the participating laboratories measured the five transfer standards using their own calibration facilities. The spread of the results (1 sigma) was within 0.03" and 0.05". It was shown that the actual angle of one of the transfer standards was clearly outside the range certified by its manufacturer.

Detailed results were published in EUR Report 14058.

CONTRKJBTION OF THE COMMISSION

ECU 64 000

PARTICIPANTS

Centro Español de Metrología, E EOLAS, IRL I n s t i t u t o Portugués da Qualidade, Ρ I s t i t u t o d i Metrología G. Colonnett i , I Physikalisch-Technische Bundesanstalt, D TU Denmark, DK

PROJECT MTR 109

DEVELOPMENT OF SiO, ON Si REFERENCE MATERIALS

PROJECT DEFINITION

The objectives of the project are the development, manufacture, full characterization and testing of Si02 on Si specimens with three layer thicknesses with nominal values of 10, 50 and 120 nm, respectively. This should then, if successful, lead to the delivery of Si02 for the calibration of spectroscopic ellipsometers for the measurement of the thickness of thin films.

STATUS

In progress. The samples have been produced, characterized and analyzed for stability by IMEC. The measurements of their thickness by means of three distinct techniques, namely:

a) Single Wavelength Ellipsometry (SWE); b) Spectroscopic Ellipsometry (SE); c) Transmission Electron Microscopy (TEM);

was then intercompared at different European laboratories. The SE measurements have shown to be the most more accurate and repeatable. The measured samples have been found to be certifiable for the calibration of ellipsometers: IMEC and RSRE will be in charge of the certification phase.


ECU 110 700

PARTICIPANTS

DBP, D IMEC, Β LAMEL, I LEP, F Philips National Laboratory, NL RSRE, UK RUCA, Β Sieaens, D SOPRA, F STC Technology Ltd, UK Universidad Cooplutense, Ε

10

PROJECT MTR 118

DYNAMIC FORCE CALIBRATION

PROJECT DEFINITION

In a wide field of application industry needs to measure dynamic forces with accuracies which cannot be met at the present time because an appropriate calibration of force transducers is not yet available. In a first phase of the project it has been demonstrated that the dynamic calibration of force transducers based upon Newton's second law is, in principle, possible.

It was shown that force transducers of the same (static) class can behave considerably different when exposed to dynamic forces mainly due to their different sensitivities to transverse forces. Transverse movements of the shaker system reduce significantly the accuracy of the calibration. Spring and damping effects between parts screwed together can also influence the accuracy.

A second phase has therefore been started in which the accuracy of the calibration will be improved. This will include

the development and application of a new facility for the calibration of force transducers for frequencies up to 1000 Hz and dynamic forces up to 500 Ν using static preloads of up to 500 N. The uncertainty of the calibration facility in the said ranges will be less than 1% in amplitude and less than I o in phase; the development of a fast and low-cost calibration method for the dynamic calibration of force transducers in amplitude and phase over a frequency range of 20 - 1000 Hz based upon the comparison of simultaneously loaded force transducers; the development of facilities and improvement of interferometrical methods for the calibration of accelerometers in the frequency range of 5 Hz, or less, up- to 1600 Hz with an uncertainty of 0.1% in amplitude sensitivity and of 0.2° in the phase.

STATUS

In progress.


ECU 364 000 (phase 1) ECU 306 000 (phase 2)

PARTKJPANTS

Physikalisch-Technische Bundesanstalt, 0.

11

PROJECT MTR 123

INTERCOMPARISON OF ROUNDNESS AND FORM MEASUREMENTS

PROJECT DEFINITION

The measurements of roundnesses are amongst the most important quality control tasks undertaken by manufacturing industry. However, it is recognised that significant discrepancies in the assessment of the roundness of work pieces exist due mainly to insufficient standardisations of measurement procedures and conditions. It is the aim of the project to understand the metrological problems which lie behind the lack of standards in order to achieve a harmonisation of roundness measurements throughout the Community.

RESULTS

The project consisted of two intercomparisons: a) The roundness of two highly accurate transfer standards, a hemispherical glass roundness standard and a circular master was measured by national metrology institutes (NMTs). Four laboratories applying error separation techniques agreed within ± 25 nm. In some instances their 95% confidence intervals (CI) (up to 25 nm) did not overlap indicating that there are systematic errors. Laboratories without such techniques agreed within ± 50 nm the 95% CI being up to 125 nm. For these laboratories, noise caused problems when higher frequencies were not filtered. Using a hemisphere, systematic differences (10 nm) depending on the stylus direction (normal to the axis or to the surface) are apparent. b) Roundness, straightness, parallelity and cylindricity on an industrial level were measured by NMFs and industry. A cylinder with form deviations and two flats for the calibration of the transducers was circulated as well as a waviness standard. Excluding outliers, the roundness measurements were in better agreement than expected. The maximum difference between the dynamic calibrations of the transducers when using the flats was 1.3 μιη corresponding to 10%. The waviness standards are a promising alternative which should be further investigated. Filter conditons have a significant influence on the results and need to be harmonised. The measurement and calculation of profiles which are necessary to determine composed forms (parallelity, cylindricity) were not satisfactory and need to be improved.


ECU 134 000

PARTICIPANTS

The NHI's of CH, D, DK, F, I, IRL, NL, S, SF, UK and Feinprüf GmbH, D - Rank Taylor Hobson Ltd, UK - PAT Meßtechnik GmbH, D -FAG Kugelfischer Georg Schäfer GmbH, D - Hercedes Benz AG, D - Université de Liège, Β -Tampere University of Technology, SF.

12

PROJECT MTR 136

INTERCOMPARISON OF STANDARDS FOR THE MEASUREMENT OF LOW DIFFERENTIAL PRESSURES AT OR NEAR ATMOSPHERIC PRESSURE

PROJECT DEFINITION

The measurement of low differential pressure frequently forms an essential part of the measurement of the flow of gases, particularly natural gas and air. Normally, in the case of gas, precautions are taken to ensure that the differential pressure to be measured does not fall below a nominal value, such as 100 Pa. For applications in the fields of heating and ventilating engineering, aircraft instrumentation, aerodynamic research and the leak testing of enclosures for delicate instruments or hazardous materials, such an option may not exist. It is therefore necessary to be able to make measurements throughout the differential pressure range zero to 1000 Pa with a precision of ± (0.1 Pa + 0.01 % of the reading).

The initial stage will consist of constructing a transfer standard in which differential pressures will be generated. After the device has been fully characterised it will be circulated to the participating laboratories for comparison with the instruments that they usually use for calibration purposes.

STATUS

The transfer standard initially constructed for the intercomparison did not produce pressure differences which were sufficiently stable. The performance of a second one is currently being evaluated.


ECU 115 000 (estimated)

PARTICIPANTS

CETIAT, F chell Instrunents Ltd, UK Furness Controls Ltd, UK National Engineering Laboratory, UK National. Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D Technical University of Delft , NL 7 further potential participants from F, I , P, CH, S, SF.

13

PROJECT MTR 138

THE MATHEMATICAL REPRESENTATION OF GEOMETRIC FORM

PROJECT DEFINITION

The project consists in developing a mathematical theory which would enable the advantages and disadvantages of alternative mathematical representations for a specified geometry to be compared for any given orientation of the geometric form in the coordinate system of the measuring machine. This must inevitably relate uncertainty in the constants in the mathematical representation of any geometric form to the current position and orientation of the form in the coordinate system. In addition to leading to direct improvements in the uncertainties associated with data fits, it should be possible to give practical advice for the orientation of workpieces on 3 CMM when setting out to measure specific geometries. .

The following geometries have been considered in all orientations in an x-y-z coordinate system : straight line (2d) straight line (3d) flat plane circle (2d) circle (3d) sphere cylinder cone

RESULTS

The theory developed describes how the above geometric elements can reliably be represented in terms of sets of algebraic parameters. For any element, it enables to determine whether a possible parametrisation is good or not and gives a quantitative measure for the "degree of goodness".

Two sets of parametrisations are recommended. The first set applies to full elements, i.e. elements that are to be derived from measurements distributed throughout the feature. The second applies to partial elements derived from measurements over a relatively small portion of a feature. The parametrisation recommended is optimal or near-optimal in terms of the above measure. Considerations have been given to the relationship between recommended parametrisation and algorithms used to determine numerical values of geometric element parameters. In addition, ways are recommended on how to algebraically represent the distance of a point from each of the main geometric elements, the formulae being given in terms of the recommended parameters. A detailed description can be found in EUR Report 13517.


ECU 40 000

PARTICIPANT

National Physical Laboratory/ UK

14

PROJECT MTR 141

EVALUATION OF THE EFFECT OF VARIATIONS IN THE REFRACTIVE INDEX OF AIR UPON THE UNCERTAINTY OF INDUSTRIAL

INTERFEROMETRIC LENGTH MEASUREMENT

PROJECT DEFINITION

When measuring distance using laser interferometers it is necessary to take into account the refractive index of the air through which the beam passes. This is in turn a function of the composition of the air and thus errors may become significant when measurements are made in polluted environments if corrections are not made. To this end compensation devices are commercially available but the limit of their effectiveness is unclear in comparison to the measurement accuracy of 1 part in 107now sought by a number of key industries (e.g. electronics). Work by PTB under typical industrial conditions demonstrated that refractive indices determined with commercial compensation devices could differ by up to 1 part in 106from those measured with the PTB air refractometer. It is the aim of the project to determine reasons for these differences.

RESULTS

A portable measurement package composed of a refractometer and instrumentation for the measurement of air temperature, pressure, relative humidity and C02 content has been built and calibrated. It enables to determine the refractive index of air directly or by calculation using the environmental measurements and correction equations, both methods having a relative uncertainty of less than 10"7 . The package has been circulated to 15 locations of 6 industrial companies. At each place, samples of air have been taken for subsequent chemical analysis. It has been shown that the index directly measured by the package and the calculated one differ by only about 10"" if a modified Edlen equation is used and corrections are applied for the levels of C02 which exceeded that assumed by Edlen. Commercial compensation devices used by industry gave a measuring accuracy of >5*10 ~7 whilst in-house compensators achieved about 1*10 "7. This is considered to be due to the greater stability of the sensors in the latter instruments and the employment of a more exact determination of humidity. If humidity is not measured but assumed to be 50 % errors of the order of 2*10 '7 can be expected. The best accuracies were achieved by refractometers which, however, need also regular calibration. Generally, the only significant air contaminant measured was C 0 2 , the uncertainty due to hydrocarbon contamination being only of the order of 3*10 "'. The results are published in EUR report 13517.


ECU 125 000,

PARTICIPANTS

National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D.

15

PROJECT MTR 150

INTERCOMPARISON OF FLATNESS MEASURING METHODS AND DEVICES

PROJECT DEFINITION

Flatness is a basic geometrical quality; since a plane is a simple element of the Cartesian system used in dimensional metrology, incorrect flatness measurements give rise to other related errors in form shape and, of course, even length. In the intercomparison, the participants were requested to measure at PTB a single granite table of 1 m χ 2 m with their own equipment and their own procedure.

RESULTS

The comparison measurements were all carried out in a temperature and humidity controlled laboratory; the granite table had an intentional flatness error of about 10 μιη to be determined. All participants contacted 104 points in a 100 mm χ 100 mm grid. In the majority of cases the measurement results agreed to about 0.5 μπι to 1.0 μπι. On the contrary, the flatness deviation values determined by the different participants according to ISO DIS 8512 turned out to differ up to even a few μπα. A software intercomparison has been proposed as a means to explain these differences as a further step to harmonising the measuring methods.



PARTICIPANTS

Metrology laboratories fro« DK, SF, F, GR, I , NL, UK EDA, F Huiler Wedel, D PTB, 0 Rank Taylor Hobson, UK Hyler, CH

16

PROJECT MTR 157

DEVELOPMENT OF TESTING PROCEDURES FOR CCD CAMERAS

PROJECT DEFINITION

Charged couple devices (CCDs) are used to convert optical images into electrical signals. Cameras constructed from them· can be used in the analyses of the images for metrological or recognition purposes. They have the advantages of being contactless, fast and flexible in operation but as yet no standardized test methods exist for the determination of their performance characteristics. In particular, for metrological purposes, there is a need to develop methods for the assessment of the errors associated with a camera so that these can be compensated for and the accuracies of the instruments enhanced at low cost. At an early stage of the project, a list of parameters and test methods to be investigated will be discussed and agreed with representatives of industry. The work will cover the development of methods for the full assessment of the performance of both the optical and electrical elements of CCD cameras. Effects of changing environmental conditions (such as temperature) will be studied as well as the capability of CCD cameras to measure moving objects.

STATUS

In progress.


ECU 153 700

PARTICIPANTS

Coordinator : Laboratoire National d'Essais, F Consiglio Nazionale deLle Richerche, Centro di Studio per La Televisione, I.

17

PROJECT MTR 158

CHEBYSHEV REFERENCE SOFTWARE

PROJECT DEFINITION

Coordinate measuring machines are the heart of the metrological control system flexible manufacturing units. For their operation they rely upon computer software to convert the point by point information gathered by scanning the object into a 3 dimensional representation of the article being measured. This software is generally based upon a mathematical method called 'least mean square statistics". However, for many production purposes where tolerances have to be observed, the use of a different mathematical approach based upon "Chebyshev statistics" is more appropriate. Experience obtained in a current BCR project on the comparison of least mean squares software has shown that much of that currently available is inadequate and non-validated. The purpose of the present project is to develop reference algorithms and software based on the Chebyshev principle against which the software of 3-coordinate measuring machines can be validated. Finally the algorithms and their documentation will be made available to European industry via the metrology laboratories of the Member States thereby assisting it to maintain its world leadership in the field of coordinate measurement technology. After a careful study of available literature, algorithms will be developed for various basic geometrical forms such as lines, circles, spheres, cylinders and cones or parts thereof. They will be validated using a variety of data sets representing the form under consideration distorted by known amounts. Meetings with representatives of the European coordinate measuring machine industry will be held in the course and at the end of the project to assess the suitability and acceptability of the approach proposed and algorithms developed.

STATUS

In progress.


ECU 645 800

PARTICIPANTS

Coordinator : National Physical Laboratory, UK Centrun voor Uiskunde en Informatica, NL Physikalisch-Technische Bundesanstalt, D.

18

PROJECT MTR 159

DEVELOPMENT OF TESTING PROCEDURES FOR OPTICAL PROBES

PROJECT DEFINITION

Three coordinate measuring machines measure the geometry of objects by scanning their surface either mechanically or optically. Optical systems ("optical probes") are increasingly used by industry as they are capable of high scanning speeds when measuring a broad spectrum of objects in a contactless manner. Although they are already widely used there exist neither standardized nor generally acknowledged testing and calibration procedures for them. Thus specification of probes of different manufacturers cannot be compared directly. Probes working on three different optical principles will be investigated and their essential characteristics identified. This will include both kinematic and dynamic behaviour. As a result of the initial investigations, draft recommendations for testing procedures will be discussed with industrial representatives. Computer simulation of the probes will be developed which when used with appropriate experimental measurements will allow the overall error associated with each type of probe to be broken down into its constituent parts. Overall it is the aim of the project to establish unified testing procedures for optical probes and methods for the correction of their errors suitable as a basis for standardisation.

STATUS

In progress.


ECU 574 900

PARTICIPANTS

Coordinator : Physikalisch-Technische Bundesanstalt, D RWTH Aachen, Laboratorium für Werkzeugmaschinen und Betr iebslehre, D Universi ty of Zaragoza, Escuela Técnica Superior de Ingenieros Indust r ia les, E.

19

PROJECT MTR 160

DEVELOPMENT OF METHODS FOR THE NUMERICAL ERROR CORRECTION OF MACHINE TOOLS

PROJECT DEFINITION

Inaccuracies in the use of machine tools are mainly caused by errors of form geometry, changes of the geometry due to finite stiffness and, most important, changes of the geometry due to thermal effects. The aim of this project is the on-line improvement of the geometrical accuracies of machine tools by the adaptation and extension of the correction methods used in the field of coordinate measuring machines. Although establishing general principles, the project will mainly deal with a five axis milling machine for which an error model describing these errors will be developed and its effectiveness demonstrated. A bibliographical study on currently available error models, methods of temperature corrections and methods of parameter extraction from measurements of work pieces will facilitate the establishment of concepts for an error model which will take into account the finite stiffness of the machine as well as the influence of a given temperature distribution on the geometry. The error model will be based upon a combined analytical and empirical approach. In order to develop and verify the concepts and model, measurements of objects will be made on the milling machine and on a 3-coordinate measuring machine. Important aspects of the project will be the implementation of the hardware and software needed to demonstrate the feasibility of on-line error compensation on this machine and the assessment of the actual improvement of the accuracy brought about by the project.

STATUS

In progress.


ECU 588 000

PARTICIPANTS

Coordinator : Eindhoven University of Technology, Metrology Laboratory, NL Fa. MAHO Ag, Pfronten, D NV Phi l ips Gloeilampen Fabrieken, NL Physikalisch-Technische Bundesanstalt, D.

20

PROJECT MTR 161

REAL-TIME POSITION AND FORM MEASUREMENTS ON MACHINE TOOLS AND COORDINATE MEASURING MACHINES BY MEANS

OF MULTI-FUNCTION LASER INTERFEROMETRY BASED ON STABILIZED LASER DIODES

PROJECT DEFINITION

For flexible manufacturing units to be cost effective they must operate on the principle of minimum waste by getting the product right the first time. In order for them to do so it will be necessary to transfer those reference standards currently realized in the laboratory to real-time operation in the manufacturing units. The purpose of this project is to demonstrate the feasibility of doing this in the case of length and angle measurement. Although the project will require significant improvements in existing measuring techniques, it is their combination and application in the industrial environment which will constitute the major step forward in the field.

STATUS

In progress.


ECU 1 303 000

PARTICIPANTS

Coordinator : Cart Zeiss, 0 Physikalisch-Technische Bundesanstalt, D The Technical Universi ty of Denmark, DK I n s t i t u t e fo r Product Development,, DK.

21

PROJECT MTR 162

MULTI-SENSOR ELECTRO-OPTICAL EQUIPMENT FOR AUTOMATED MANUFACTURING SYSTEMS

PROJECT DEFINITION

Automated manufacturing processes need high-accuracy and high-resolution systems and devices for dimensional analysis, particularly for the high-speed measurements of absolute distances and profiles. Although electro-optical systems and techniques could provide reliable and fast methods systems which have been built based upon these principles are very limited in the industrial environment and do not meet the specifications required by industry.

The aim of the project is therefore to investigate various approaches to absolute distance meters and profile meters based upon electro-optical methods paying due attention to industrial needs. The feasibility of the system in an industrial environment will be demonstrated.

STATUS

In progress.


ECU 743 400

PARTICIPANTS

Coordinator : Université degli Studi di Brescia, Departimento di Autonazione Industríale, Χ Centro Inforaazioni Studi Esperienze, Mi Laño, I Universität Stuttgart, Institut für Technische Optik, 0.

22

PROJECT MTR 170

DEVELOPMENT OF A METHOD FOR THE CHARACTERISATION OF ROUGHNESS IN 3 DIMENSIONS

PROJECT DEFINITION

The assessment of engineering surfaces plays an important role in the manufacturing industry. National and international standards, e.g. ISO, DIN, BS, ANSI, exist for a range of 2 dimensional surface roughness measurement and are used extensively in industry today. However, much of the current research work and industrial reasoning recognises the fact that all surfaces interact 3-dimensionally and that a 2-dimensional characterisation of surface roughness does not reflect it real properties. It is becoming increasingly obvious that a full understanding between surface topography and functional performance can only be realised if a 3-d approach to surface characterisation is used.

The intention of this project is therefore to develop a method for the characterisation of roughness in 3 dimensions based upon both optical and mechanical measurement techniques. The project will be carried out in close connection with industry. A survey of industrial and research institutes will establish the background of the 3-dimensional characterisation of the roughness of engineered and functional surfaces. A detailed investigation of measurement and data analysis techniques will follow and the relationship between manufacture, characterisation and function of surfaces will be established using selected example surfaces. Before finalising recommendations the results will be disseminated and discussed with European industries.

STATUS

In progress.


ECU 519 100

PARTICIPANTS

Ecole Centrale de Lyon, F Exxon Chemicals L td , UK Lucas Industry, UK Perthen-Feinprüf GmbH, D Somicronic, F Universi ty of Birmingham, UK (coordinator) Uhitestone Business Communications, UK

23

PROJECT MTR 172

AN INTERCOMPARISON OF TYPE EXAMINATIONS OF NON-AUTOMATIC WEIGHING INSTRUMENTS

PROJECT DEFINITION

Different types of weighing instruments adapted to specific applications, are widely used in industry and trade. The Directive 90/384 EEC of the Council on non-automatic weighing instruments defines essential requirements for the performance of weighing instruments rather than giving technical solutions. As type approval procedures will have to ensure that instruments conform to the Directive, CEN/CENELEC will be given a mandate from the Commission to produce a harmonised European standard based on the OIML Recommendation R 76. However, experience with the OIML recommendations has shown that problems exist in their application in a uniform manner leading to disputes over the type approvals granted by the different type approval authorities.

The aim of the project is to compare the results of type approval procedures carried out in the Member States and EFTA States and thereby quantify and understand the problems involved. To this end three different types of instruments will be circulated to the National Metrology Institutes.

STATUS

In progress.


ECU 390 000

PARTICIPANTS

National Metrology Institutes from : B, DK, D, E, f, I, IRL, NL, UK, A, CH, ICL, N, S, SF.

24

PROJECT MTR 173

COORDINATION OF AND PARTICIPATION IN AN INTERCOMPARISON OF MASSES IN THE RANGE OF 1 TONNE UP TO 5 TONNES

PROJECT DEFINITION

The most accurate force standards are based on machines operating on the deadweight principle. They make use of well known masses which bring about accurate forces under the influence of the local gravity. In order to calibrate the masses used in their deadweight machines the National Standards Laboratories of the Community have developed various facilities. They need to be compared on a regular basis in order to ensure consistency of measurements of masses and forces throughout the Community and to achieve mutual confidence on the standards of the Member States. However, no intercomparison of masses above 1 tonne has ever been undertaken between the National Standards Laboratories.

The aim of the project is therefore to undertake an intercomparison of mass standards in the range of 1 - 5 tonnes in order to show the level of agreement between the European mass standards in that range and to determine reasons for differences. 5 masses of nominally 1000 kg will be circulated to the participants.

STATUS

The project will start in 1992.


ECU 50 000

PARTICIPANTS

DANTEST, DK Laboratoire National. d'Essais, F National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D Raute Precis ion, SF

25

PROJECT MTR 174

DEVELOPMENT OF IN-PROCESS MEASUREMENT TECHNIQUES FOR OPTICAL QUALITY AND POSITION OF ELEMENTS IN SMALL

INTEGRATED OPTICAL SYSTEMS

PROJECT DEFINITION

The objectives of the project are:

the development of in-process test techniques for the surface quality of small optical components with nanometer accuracy;

the mutual positioning of these components with sub-micron accuracy in a system to operate within the production environment.

The components that will be considered are: lenses and reflectors with aspherical, rotationally symmetric surfaces, moulds for producing aspherical lenses, and relief holograms both in reflection and in transmission. Combination of aspherical surfaces and relief holograms will also be studied.

STATUS

The work is in progress.


ECU 858 230

PARTICIPANTS

Coordinator: Nederlandse Philips Bedrijven, NL Universität Stuttgart, Institut für Technische Optik, D

26

PROJECT MTR 176

DEVELOPMENT OF A PHOTOMASK LINEWIDTH STANDARD

PROJECT DEFINITION

The objective of the project is to produce a photomask linewidth calibration standard covering the dimensional range 0.20 (im up to 50 urn, with a 95% confidence level uncertainty in the calibration of lines of at least ± 0.02 urn in the 0.2 μτη up to 10 um range, and of at least ± 0.05 μιη in the 10 um to 50 urn range. The standard, to be fabricated in high density chromium (optical density greater than 2.5 at 450 nm) on a fused quartz plate coated with a conducting layer, is to be suitable for use in both optical and electron beam systems. Initially, ten artefacts will be manufactured, three of these being calibrated and retained by the Commission, the National Physical Laboratory (NPL) and the Physikalisch-Technische Bundesanstalt (PTB).

STATUS



ECU 1 241 873

PARTICIPANTS

Compugraphics In ternat iona l L td, UK Dupont Photomask L t d , F National Microelectronics Research Center, IRL National Physical Laboratory, UK (coordinator) Physikalisch-Technische Bundesanstalt, D Rutherford and Appleton Laboratories, UK

27

PROJECT MTR 180

OPTICAL INSPECTION SYSTEM FOR THE MEASUREMENT OF THREE DIMENSIONAL SHAPES

PROJECT DEFINITION

The integration of high precision 3D-shape measurements of workpieces into a "computer integrated manufacturing" (CIM) production line wül be of increasing importance within the next few years. Although various potentially well-suited optical measuring techniques have been developed they suffer considerable constraints with regard to the range of measurement, the measuring time, the flexibility with respect to different workpieces and their overall cost. These problems which have prevented the economic introduction of such systems into a CIM environment can in principle be solved by the use of a modular, computer-aided system architecture. In order to obtain the utmost versatility as a key to low cost solutions both software and hardware will have a modular system structure and the measuring techniques will provide both comprehensive topographic 3-D shape information and the required resolution, measuring range and dynamics.

The objective of the project is to determine the feasibility of a modular, computer-aided 3D-shape inspection system within a CIM environment, thereby taking into account the application of the inspection system in industry together with the industrial requirements and specifications.

The inspection system shall make use of optical topographic measuring techniques. Two classes of workpieces to be measured shall be considered, mainly made from metal, ceramics and plastics: objects with diameters of up to 100 mm to be measured with an accuracy between 0.5 urn and 2 μπι and objects with diameters of up to 1000 mm to be measured with an accuracy between 2 μπι and 100 μπι.

In order to determine which optical techniques are most suitable for such an inspection system a literature study and a theoretical analysis of techniques based upon the moiré principles, diffraction pattern techniques, opto-mechanical scanning and sampling techniques will be carried out in the first part of the project (6 months). This shall be followed by an experimental study (6 months) to clarify possible remaining questions.

STATUS

In progress.


ECU 49 600 for the theoretical part ECU 73 000 for the experimental part (estimated)

PARTICIPANTS

Fraunhofer Institute for Information and Data Processing, Karslruhe, D (Coordinator) TN0 Institute of Applied Physics, Delft, NL

28

PROJECT MTR 182

COMBINED X-RAY AND OPTICAL METROLOGY FOR HIGH PRECISION DIMENSIONAL METROLOGY

PROJECT DEFINITION

The purpose of the project is to develop an instrument for the measurement of lineai displacements with ultra high precision, i.e. ± 1 0 pm measurement uncertainty foi displacements up to 10 μΐη, and ±100 pm for displacements up to 1 mm. The instrument will use a combination of x-ray and optical interferometry and operate in two distinct modes, depending on the magnitude of the displacement. In particular

i) for displacements up to 10 μτη, a scanning monolithic x-ray interferometei (SMXRI) will directly measure the full distance, the optical interferometer (ΟΓ, operating in combination solely to increase the measuring speed by elirninarin{ the requirement to individually count all the x-ray fringes;

ii) for displacements greater than 10 μιη the OI shall measure the displacement o: an optical mirror mounted on a precision translation stage, with the SMXRI usee to interpolate the fringe count at the beginning and at the end of th< measurement.

The design of the instrument will also allow the measurement of tilts with nrac sensitivity, thus making it applicable to:

the calibration of precision displacement transducers, the dimensional metrology of semiconductor masks and wafers, the investigation of the fringe interpolation errors of high accuracy lase interferometers.

STATUS



ECU 1 028 048

PARTICIPANTS

Istituto Metrología G. Colonnetti, I National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D, (Coordinator)

29

PROJECT MTR 183

STANDARDLESS THIN LAYER METROLOGY USING A NON DESTRUCTIVE X-RAY INTERFERENCE TECHNIQUE

PROJECT DEFINITION

The objective of this project is to develop a non destructive technique - NAMK (Nanometer Metrology using Interference of X-Rays) - for the assessment of the composition and thickness in the 1 to 300 nm range of single and multi layers of crystalline, polycrystalline and amorphous materials. The efficiency of NAMK will be investigated in a wide range of applications. As a result different films with very well controlled thicknesses and composition will be fabricated and proposed as reference standards for metrological applications.

STATUS



ECU 595 120

PARTICIPANTS

Centre National, de la Recherche Scientifique, F Laboratoire d'Electronique Philips, F, (Coordinator) Nederlandse Philips Bedrijven P.O. I&E, NL Societa Ital iana Vetro, I

30

PROJECT MTR 184

STM METHODS FOR ROUGHNESS AND MICRO HARDNESS MEASUREMENTS

PROJECT DEFINITION

Vickers micro hardness measurements according to ISO standards are used extensivelj as a testing method in microelectronics fabrication and thin layer technology using indentations with diagonal lengths shorter than 2 μτη. Currently the primar} measurement standards are based on optical methods and have an intrinsic uncertaintj of about 0.5 μπι. The objective of this project is to apply the scanning tunnelling microscope (STM) technique to produce a new more precise method for the measurement of roughness in the range 1 nm < R, < 0.5 μπα and the determinatior of micro-hardness. The project, in which advanced image processing algorithms will also be developed tc improve the quality of the indentation image, is expected to lead to the construction oi an operating two stage prototype instrument and the associated software. Thii prototype will be tested individually by each partner. Comparison measurements wil be undertaken to link the STM measurements to the conventional ones, to investígate whether the existing written standards can be transferred to the STM technique or new ones have to be considered.

STATUS



ECU 538 927

PARTICIPANTS

Danish I n s t i t u t e of Fundamental Hetrology, DK, (Coordinator) I r i s h National Science and Technology Agency, IRL I s t i t u t o d i Metrología G. CoLonnetti, I Of f i c ine Gal i leo Spa, I Physikalisch-Technische Bundesanstalt, D

31

PROJECT MTR 185

CHARACTERISATION AND DEVELOPMENT OF SURFACES IN THE 0.1 nm RANGE

PROJECT DEFINITION

Surfaces with roughnesses in the 0.1 nm range are increasingly required by the optical, laser, x-ray, precision bearing engineering and semiconductor industries. Nevertheless, neither the metrology nor the appropriate calibration techniques and reference artifacts for the quantitative characterisation of such super smooth surfaces exist. The objective of this project is to improve the international comparability of the roughness values of super smooth surfaces of dielectric materials, such as glass or fused silica, by the production and certification of a set of reference artifacts in the range of surface roughnesses from rms values of 0.05 nm to 0.5 nm. These references will be characterised and calibrated with respect to their surface spatial wavelength in the range from 1 0 " ^ to 10"Ίη. To this end, the partners in the project will jointly develop new appropriate manufacturing processes and improve a set of existing measurement techniques including:

atomic force microscopy (AFM); a high resolution diamond stylus profilometer; a high resolution interference microscope; different scattering measurements systems;

to the extent necessary for the certification of the reference samples. The project will also investigate the problems of packing, transportation and storage under clean conditions of the reference samples.

STATUS



ECU 1 416 131

PARTICIPANTS

Compagnie de Saint-Gobaín, F Cork Regional Technical College, IRL Deutsche Forschungsanstalt für Luft und Raumfahrt, D, (Coordinator) Fogale Manoteen, F Rank Taylor Hobson Ltd, UK Rollei Fototechnic GmbH & Co, D

32

PROJECT MTR 187

IN-LINE DIMENSIONAL MEASUREMENTS OF COMPOSITE WORKPIECES PRODUCED BY FILAMENT WINDING TECHNOLOGY

PROJECT DEFINITION

Dimensional measurements on workpieces made of composite materials are currentl] being performed after the production process, leading to high scrap rates and manpowei costs. In order to increase the reliability and effectiveness of the production processe they need to be fully automated, in particular those using the filament windinj technology. Progress, however, has been hindered by the lack of knowledge o appropriate metrological methods to accurately measure the size of composit« workpieces during the manufacturing process.

In a first part of the project physical properties of the pre-cured and cured advancec composites will be determined that might be used for dimensional measurements o composite workpieces made of glass reinforced polyester, carbon/epoxy, kevlar/epoxy This will include the viscoelastic creep behaviour to determine the dimensional stabilit; of the materials under stress/strain and temperature variation; the DC electrica resistivity and the AC electrical resistivity in the range of 20 Hz to 10 Hz; the relativi permittivity; the permeability; and the acoustic impedance. Measuring instruments wil then be designed and constructed for in-process dimensional measurements of composite workpieces of the above range of materials; the instruments should achieve thi following specification during the normal production process:

thickness measurements in the range of 1 to 30 mm, accuracy 0.1 mm (on pre-cured and post-cured workpieces) length measurements in the range of 0.5 to 50 m, accuracy 2 mm; roundnes measurements in the range of 0.5 to 3 m, accuracy 1 mm (on post-cured workpieces)

The project is limited to the metrological aspects of the development of the instruments Work directly related to the control and automation of the production process i excluded.

STATUS

In progress.


ECU 584 000

PARTICIPANTS

Brunei. University, The Brunei Centre for Manufacturing, UK TVR - Tecnologie Vetroresina S.p.A., I, (Coordinator)

33

PROJECT MTR 188

INSPECTION OF SURFACE STRUCTURES BY CONOSCOPIC AND IMAGE PROCESSING METHODS

PROJECT DEFINITION

Up to now the post-process assessment of surface microstructure has frequently been carried out by means of visual inspection and comparison.

The aim of the project is to develop a system based on holographic methods and image processing including digital and/or neural computing methods which is capable of automatically inspecting, analysing and classifying surfaces in bores of diameters down to 60 mm in a machine workshop environment. The feasibility of the system will be demonstrated by applying the method to analyse and classify honed surfaces as they are produced in cylinder bores for combustion engines.

The complete system will consist of a holographic sensor which basically consists of a bi-refringent crystal and which will be integrated into a special microscope. The system will include all the software for the assessment of the surface finish according to standardised requirements for roughness profile test methods (e.g. DIN specifications) and all the necessary components, control systems and software to automatically determine the surface structure, its analysis and classification according to standardised criteria as laid down in the Goetze HON-Atlas.

STATUS

In progress.


ECU 493 300

PARTICIPANTS

Le Conoscope, F Pat Meßtechnik GmbH, D, (Coordinator)

34

PROJECT MTR 189

THE DEVELOPMENT OF A TWO DIMENSIONAL HIGH PRECISION PHOTOMASK POSITION STANDARD

PROJECT DEFINITION

Optical lithography in integrated circuit fabrication presently consists of about 21 successive mask steps. Up to now no calibrated two dimensional photomask positioi standard (2DPPS) traceable to the SI unit of length exists; metrological institutes cai supply only one dimensional line scale calibrated with sufficient accuracy. A two dimensional standard mask is a necessary tool to examine the dimensione tolerances of successive production steps, in order to ensure the quality of instrument (e.g. pattern generators, wafer measuring machines, wafer steppers, mask measurin machines) and to avoid commercial disputes. The aim of the project is to produce for industrial calibration purposes a 7" calibrât» 2DPPS accurate and certified to 50 nm, thus meeting the requirements of lithograph for the 0.3 μπι geometries (64 Mbit DRAM, 80 nm overlay accuracy). This standard wi! later be made available as a calibration reference to the semiconductor and equipmen industry. The project will also investigate the instrumentation and the substrat requirements necessary to achieve a future 10" calibrated 2DPPS.

STATUS



ECU 1 106 000

PARTICIPANTS

Conpugraphics Internat ional L t d , UK National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D, (Coordinator)

35

PROJECT MTR 190

NON CONTACT SURFACE METROLOGY

PROJECT DEFINITION

In many industrial sectors assurance of functional surface quality is critically hampered by the inadequacies of current surface metrology techniques. New technology is required for full micro topographic surface analysis and for high-speed, in-process and immediate post-process, measurement of surface quality measures such as roughness, waviness, repeat or isolated geometrical features. Only in this way will it be possible to meet the increasingly stringent quality requirements and support the move towards high speed automated manufacturing. It is the aim of the project to investigate optical phenomena which could potentially be used for analysis and measurement of engineering surfaces, and developing them to provide for improved measurement procedures and practices.

The techniques investigated are phase contrast methods, infrared scattering, shearing interferometry, projected fringes, scanning differential heterodyne interferometry, scanning confocal microscopy and high speed laser scanning.

To determine the performance and limitations of the above techniques, a wide range of test surfaces will be used, representing engineering components, machine components, domestic products, flat and structural glass products.

The measurement results obtained using the above techniques will be compared with conventional techniques (such as contact or optical stylus). The techniques will be related to requirements for measurements in product design and development as well as for in-process and post-process manufacturing quality control.

Finally, surface parameters will be identified which can be determined by each individual technique to the required accuracy and the influences of error sources on the accuracy will quantitatively be determined.

STATUS

In progress.


ECU 1 116 400

PARTICIPANTS

SIRA Ltd (UK), Coordinator SKF Engineering and Research Centre B.V., S Nederlandse Philips Bedrijven Β.V., NL Institutet för Optisk Forskning, S Universität Stuttgart, Institut für Technische Optik, 0.

36

PROJECT MTR 191

IN-PROCESS ULTRA-HIGH FREQUENCY EVALUATION OF ABRASIVES

PROJECT DEFINITION

Grinding is a very complex process of increasing potential in material removal rate and surface finish quality which requires real-time in-process monitoring of grinding and dressing operations, diagnosis of process states and the use of sensor based expert control system. As a first step towards a fully integrated process monitoring, diagnostic and control system for grinding and dressing operations it is the aim of the project to develop the appropriate metrology and to find correlations of signal patterns with process states. This will include the development of ultra-high frequency capacitive and piezoelectric sensors with a bandwidth of up to at least 1 MHz and the development of a high speed signal analysis network for signal conditioning and data processing based upon neural techniques (bandwidth of at least 10 MHz).

STATUS

In progress.


ECU 600 000

PARTICIPANTS

Armines, F FogaLe Nanotech, F Fritz Studer AG, CH, (Coordinator) IUF-ETH Zürich, CH Walter Oittel GmbH Luftgerätebau, D

37

PROJECT MTR 195

THE DEVELOPMENT OF TEST AND CALIBRATION PROCEDURES FOR AUTOMATED THEODOLITE SYSTEMS IN PRODUCTION METROLOGY

PROJECT DEFINITION

Coordinate measuring systems based upon computer controlled automated theodolites have a large number of potential applications in production industries such as those concerned with automobiles, shipbuilding, large machine, aircraft and spacecraft, etc. Although these systems are cost effective, flexible in use and sufficiently accurate, they have not yet been widely accepted by industry. This is mainly due to the fact that no instrument-independent guidelines or standards exist which would enable the user to quickly and reliably determine or verify the measurement accuracy of their system.

Calibration and test methods which are cheap, easy and fast to handle shall therefore be developed in the project. They will be based upon calibrated reference objects. The work will include the determination of the influence of a variety of different targets on the measurement accuracy and the development of appropriate correction procedures where they are required. The uncertainty of automated theodolite intersection systems will be described by the superposition of its individual error components. At a final stage of the project draft guidelines will be established for the calibration, acceptance testing and periodic inspection of automated theodolite systems. The measurement distances covered by the project will be up to 25 m.

STATUS

In progress.


ECU 482 000

PARTICIPANTS

LEICA Heerbrugg AG, CH PhysikaLisch-Technische Bundesanstalt, D, (Coordinator)

Temperature

41

PROJECT MTR 116

CALIBRATION OF INDUSTRIAL PLATINUM RESISTANCE THERMOMETERS

PROJECT DEFINITION

Industrial platinum resistance thermometers (IPRTs) can be used to accurately measure temperature if they are carefully selected and individually calibrated. The individual calibration of a thermometer involves the fitting of an interpolation curve to a limited number of calibration points so as to be able to describe accurately the variation in the electrical resistance of the thermometer as a function of temperature.

In order to establish a suitable calibration procedure, this project selected two groups of six IPRTs. The IPRTs in one group were calibrated in the temperature range 0 °C to 630 °C and those in the other group were calibrated in the temperature range 0 °C to 850 °C.

RESULTS

A number of platinum resistance thermometers were obtained from seven European suppliers. They were first tested for stability and a number of them failed. It was possible however to select six thermometers for each temperature range that were sufficiently stable. Excessive instability and hysteresis were found with the calibrations above 630 °C which also affected the accuracy of the calibrations at lower temperatures. In the temperature range 0°C to 630°C a quadratic curve was shown to be an adequate means to interpolate between the calibration points. Using a fourth order interpolation procedure with the most stable thermometers, it was possible to measure temperature to within ± 50 mK in the temperature range 0 °C to 630 °C. As an extension to the exercise, six of the thermometers are currently being calibrated in the temperature range -200 °C to 0 °C.


ECU 68 035

PARTICIPANTS

Istituto di Metrología G. Colonnetti, I National Physical Laboratory, UK Institut National de Métrologie,, F

42

PROJECT MTR 117

NISIL - NICROSIL THERMOCOUPLES

PROJECT DEFINITION

Type Κ (rdckd-chromiiim/nickel-aluniinium) thermocouples are widely used in industry for measuring temperature in the range 200°C to 1000°C but drift by more than 5°C in the range 300°C to 500°C due to metallurgical ordering and disordering (the hysteresis effect). Nickel-cliromium-silicon/nickel-silicon-magnesium thermocouples (known as Nicrosil/Nisil or Type N) were developed in order to overcome this problem, although they have not yet been widely adopted. Both Type Κ and Type Ν thermocouples, when used in their mineral insulated form with stainless steel or Inconel sheaths, can show large calibration drifts above 1000°C due to contamination from the sheaths.

Recently, Type Ν thermocouples have been developed which are sheathed in alloys similar in composition to Nicrosil and should have lower calibration drifts above 1000°C due to contamination. The project was aimed at investigating the high temperature stability of such thermocouples from two different sources under continuous exposure to progressively higher temperatures and conditions of temperature cycling. Measurements were also made with Inconel-sheathed Type Κ thermocouples for comparison purposes.

RESULTS

The measurements established the limits of temperature exposure to which mineral insulated metal sheathed thermocouples can be subjected without failing or drifting unacceptably : upto 1300°C for Type Ν thermocouples sheathed in Nicrosil related alloys or upto 1200°C for Type Κ Inconel sheathed thermocouples.


ECU 19 000

PARTICIPANT

National Physical Laboratory, UK

43

PROJECT MTR 128

INTERCOMPARISON OF TEMPERATURE MEASUREMENTS USING MICROCRUCIBLES

PROJECT DEFINITION

Generally thermocouples are calibrated by comparison with a standard thermocouple or with a fixed point cell, both methods being long and expensive; by the wire bridge method, which is limited to the Pd and Au points and has sources of uncertainties.

The purpose of the project was to assess the validity of a new in-situ method for calibrating thermocouples based on the realisation of the fixed points with microcrucibles. Calibrations of type S thermocouples using silver microcrucibles were compared with calibrations using large classical cells in five national laboratories.

RESULTS

The results confirm that microcrucibles can be used to accurately calibrate thermocouples. Discrepancies between results were spread over a range of 0.17°C and were consistent with the estimated uncertainties in the measurements.


ECU 59 000

PARTICIPANTS

INN, F INGC, I NPL, UK VSL, NL Dansk Technologisk Institut, DK

44

PROJECT MTR 133

DEVELOPMENT OF NOBLE METAL THERMOCOUPLES

PROJECT DEFINITION

Temperatures between 1000°C and 1600°C are measured in industry by means of platinum-rhodium thermocouples whenever accuracy is required since Chromel Alumel thermocouples used in the lower temperature range are not sufficiently stable. Pyrometers cannot provide accurate measurements unless the emissivity of the surface is very accurately known. Noble metal thermocouples themselves need periodic recalibration because there are a number of damage mechanisms that can cause drifting.

The aim of this project was to evaluate the stability and repeatability of platinum-gold thermocouples that recent work outside Europe has indicated might be useful as new transfer standards between the primary metrology laboratories and the industry calibration laboratories. They appear to be more stable and more accurate and therefore would both facilitate the task of industry laboratories and reduce the work of primary metrology laboratories.

RESULTS

The reproducibility of the measurements with the platinum-gold thermocouples was not significantly better than would be expected with platinum-rhodium thermocouples with differences between the laboratories ranging from 2μν (0.1°C) to 20μν (1°C) depending upon the origin of the thermocouples. However the long term stability of platinum-gold thermocouples is still expected to be better than platinum-rhodium ones.


ECU 50 000

PARTICIPANTS

IHGC, I NPL, UK INK, F VSL, NL

45

PROJECT MTR 137

INTERCOMPARISON ON FDŒD POINTS

PROJECT DEFINITION

The practical temperature scale is realised in the range up to 1600°C by means of the fixed melting points of pure metals.

Different design and construction of the cells, sources of supply and handling of the metals, procedure and equipment used to reach equilibrium, can cause discrepancies in diese values.

The project involves the intercomparison of the Zn and Sn points in a first phase followed by the intercomparison of Al and Ag points in a second phase.

STATUS

Most of the laboratories have completed their measurements on the Zn and Sn cells, and the circulation of the Al and Ag cells has begun.

CONTRIBUTION OP THE COMMISSION

ECU 165 000

PARTICIPANTS

IMGC, I PTB, 0 VSL, NL NPL, UK Instituto Portuguese da Qualidade, Ρ Centro Español de Metrología, Ε Dansk Teknologisk, DK

Statens Provningsanstalt, S Swiss Federal Office of Metrology, CH

46

PROJECT MTR 186

MEASUREMENTS FOR THE DEVELOPMENT OF NEW REFERENCE TABLES FOR PLATINUM-RHODIUM THERMOCOUPLES

PROJECT DEFINITION

New standard reference tables for thermocouples are necessary as a result of the introduction of the new international temperature scale, ITS-90, which interpolates between fixed points by means of a standard platinum resistance thermometer instead of thermocouples. Unfortunately, in the case of S, R, and Β thermocouples, they cannot be produced by a mathematical transformation of existing data because of anomalies which arise at discontinuities in the thermal EMF versus temperature t-90 characteristic.

New measurements were therefore undertaken in four laboratories to calibrate a number of platinum rhodium/platinum thermocouples with reference to the new international temperature scale, ITS-90. The thermocouples were calibrated at fixed points and also compared with high temperature standard platinum resistance thermometers that were calibrated in agreement with ITS-90.

RESULTS

Reference functions, describing the EMF characteristics of the different types of thermocouples investigated in the project in terms of the new international temperature scale ITS-90, were obtained on the basis of the measurements. A fourth order polynomial function was found to give a good fit in the range 630° to 1064°C for the measurements whose reproducibilities were generally + 1 μν. The results of the project are being used to revise the international reference tables for thermocouples (IEC 584-1).


ECU 42 767

PARTICIPANTS

Nederlands Meetinstituut, Van Swinden Laboratorium, NL National Physical Laboratory, UK Ν Istituto di Metrología G. Colonnetti, V

Optical Metrology

49

PROJECT MTR 085

STUDY OF THE STABILITY OF SILICON PHOTODIODES

PROJECT DEFINITION

Silicon photodiodes have replaced other types of photodetectors such as photocells in a wide range of optical radiation measurements. They possess many qualities which make them ideally suited for many applications (high quantum efficiency over a wide range of wavelength from 200 run to over 1000 nm), uniform response over their sensitive area and very good linearity. For accurate work there remain difficulties regarding stability. As the demand for calibration of photodiodes as transfer standards is increasing considerably, it was the objective of this project to share the work of evaluating in well-defined conditions the stability of a number of the best photodiodes from various manufacturers.

RESULTS

Devices manufactured by 5 different companies (Centronic, UK, model OSD100-S - AEG, D, model BPW35 - UDT, USA, model PIN-10DP/SB-EG & G, USA model UV444BQ -Hamamatsu, Japan, model S1227-101OBQ) have been tested over a period of five years. All these photodiodes met the following criteria :

photovoltaic (unbiased) type spectral response ranging from 200 to 1000 nm commercial availability with active area of 100 mm2

The data base consisted of 4000 results, obtained by the 4 participating laboratories testing 100 devices, 10 times each. The Centronic and Hamamatsu devices have been identified as extremely stable (change in response 1%), and well suited to act as transfer standards.


ECU 142 000

PARTICIPANTS

Institut National de Métrologie, F Istituto Elettrotecnica Nazionale Galileo Ferraris, I National Physical Laboratory, D Physikalisch-Technische Bundesanstalt, D

50

PROJECT MTR 095

LUMINOUS FLUX OF FLUORESCENT TUBULAR LAMPS

PROJECT DEFINITION

Because of the size and shape of these lamps, the luminous flux is more difficult to measure than for spherical lamps. Four types of tubular lamps with lengths ranging from 60 cm to 1.50 m are circulated together with incandescent lamps which serve as reference.

RESULTS

Excellent agreement (about 1%) was obtained by the two laboratories which use the goniophotometer for the measurement of the luminous flux.

Even though the results of some laboratories appeared to be affected by systematic errors related to spectral distribution, length of the tube and distortions in the power supply, they were consistent with the stated uncertainties, and in no case differed by more than 5%. The results of the intercomparison should lead to the revision of the instrumentation and the procedures used in order to reduce disagreement. The intercomparison has, on the whole, managed to provide traceability to the photometric standards maintained at BIPM, IEN, NPL and PTB.


ECU 179 000

PARTICIPANTS

B r i t i s h Standards I n s t i t u t e , UK General E lec t r i c Company/Hirst Research Centre, UK 1s t i tu to Elet t rotecnico Nazionale Gali leo Ferrar is , I Laboratoire Central d ' E l e c t r i c i t é , Β Lysteknisk Laboratorium, DK National Physical Laboratory, UK Nederlandse P h i l i p s Bedrijven B.V., NL Osram GnbH, D Phi l ips Gloei lampenfabrieken, NL Physikalisch-Technische Bundesanstalt, D Thorn Eni L ight ing L t d , UK

51

PROJECT MTR 096

LUMINOUS FLUX OF HIGH PRESSURE SODIUM LAMPS

PROJECT DEFINITION

The project is very similar to the project on high pressure mercury lamps. This had shown discrepancies between the participants and because of the commercial importance of sodium lamps it was considered important to verify that the luminous flux can be measured correctly. Each participant was requested to carry out the measurements on four high pressure sodium lamps and four incandescent lamps.

RESULTS

A standard deviation of 0.64% was observed between eight of the laboratories involved. This result can be considered satisfactory in view of the poor stability and variations frequently found among production lamps. The work carried out should enable the other laboratories to identify errors in their measurements and correct them in the future.


ECU 110 000

PARTICIPANTS

British Standards Institute, UK Constructions Electriques Schreder, Β General Electric Company/Discharge Lanp Development Laboratory, UK General Electric Conpany/Hirst Research Centre, UK Instituto di Optica, Ε Istituto Elettrotecnico Nazionale Galileo Ferraris, I Keuring van Elektrotechnische Materialen, NL Laboratoire Central d 'Electr icité, Β Laboratoire Central des Industries Electriques, F Lysteknisk Laboratoriua, DK National Physical Laboratory, UK Nederlandse Philips Bedrijven B.V., NL Osraa GnbH, D Physikalisch-Technische Bundesanstalt, D Thorn Eai Lighting Ltd, UK

52

PROJECT MTR 114

STABILIZED LASER SOURCE FOR INTERFEROMETRY

PROJECT DEFINITION

Multiple wavelength interferometry is a technique used in mechanical metrology laboratories throughout the world for the absolute measurement of length of gauge blocks and length bars. Current instruments use cadmium and mercury gas discharge lamps to provide the measurement wavelengths. They present the disadvantage however of low intensity which limits the performance of this kind of calibration both in terms of speed and maximum length capability. The objective of the project is to develop a compact laser source, based on available He Ne lasers, stabilized at 543 nm and possibly at 594 or 612 ran.

RESULTS

The project studied the stabilization of newly available green and yellow helium-neon lasers. The stabilization was tested on lasers from three manufacturers. In each case, the adjustment must be slightly different and the lasers must be calibrated individually. The results are nevertheless very satisfactory as in the worst case observed, there is a drift of only 3.108 for 1000 hours operation. The stabilized two-colour laser is already used by the firm TESA on an equipment designed for the automatic calibration of gauge blocks in metrology laboratories.


ECU 107 000

PARTICIPANTS


53

PROJECT MTR 129

INTERCOMPARISON OF COLOUR MEASUREMENTS

PROJECT DEFINITION

Most consumer goods have a colour the definition of which is included in the commercial specifications. Examples are abundant and include paint, textiles, paper, plastic and food products etc. The tightness of specification is in great part due to the fact that the eye is a very good detector and is capable of recognizing very small colour differences. While the eye can detect differences as low as 1 CIELAB unit in extreme cases, the lowest uncertainty that can be achieved in the best absolute measurements is not smaller than 0.2 to 0.4 of a unit. There are two types of instruments:

colorimeters - which are adequate for colour difference, but not accurate for colour specification; spectrophotometers - which provide accurate measurements for colour specifications, together with good colour difference measurements.

In this intercomparison the participants measured the colour of 14 ceramic standards produced by British Ceramic Research ltd, known to be stable and uniform and widely used throughout the world for many years, using an opal glass with a matt surface as a reference white standard to compare against. The measurements have been carried out in the three different geometries recommended by CIE and used almost universally in industry:

a) specular included, b) specular excluded, c) 0/45° radiance factor.

RESULTS

Systematic errors as high as ± 0.5 % have been found, the differences observed in geometry (c) being somewhat better. Of particular concern are the differences in the spectral reflectance values of ± 0.4% for the white tile in geometry (b) and of + / -0.25% for the black tile in geometry (a), as these are not better than what might be expected from commercial spectrophotometers. All the measured values have been converted to absolute values traceable to the absolute scale of diffuse reflectance kept at PTB (Germany).


ECU 36 000

PARTICIPANTS

BAM, D ETCA, F Instituto de Optica "Daza de Valdes", E National Physical Laboratory, UK

54

PROJECT MTR 134

INTERCOMPARISON OF LASER POWER MEASUREMENTS

PROJECT DEFINITION

The measurements of the intercomparison consisted in the calibration at two primary metrological laboratories of two transfer standards (Tl and T2), supplied by LNE, under the following conditions :

1) standard T l , at 1 W with Ar+, and Nd:YAG and COj, lasers 2) standard T2, at 20 W with Nd:YAG and C0 2 lasers, at 80 W with C0 2 lasers and

at 300 W with C0 2 lasers.

Each measurement has been carried out three times on different days to check for repeatability.

RESULTS

The results normalized on common conditions are given in the table, Y being the beam diameter and S the detector sensitivity.

Laser rated φ power W mm

LNE S 6(S)

μΥ/W %

PTB S 6(S)

μΥ/W %

Deviation %

Tl radiometer

Ar YAG

co2

2 2 2

2.9 5.0 3.5

333.8 0.5% 333.0 0.7% 314.0 0.5%

334.0 332.5 330.8

0.3% 0.2% 1.0%

0.1% -0.1% 5.4%

T2 radiometer, T(water) = 14.5 °C

YAG co2

co2

co2

20 20 70

300

10 10 10 10

267.2 1.0% 255.8 1.3% 257.7 1.4% 261.4 1.2%

268.3 264.1 266.1 274.9

0.5% 0.8% 0.9% 1.0%

0.4% 3.2% 3.3% 5.2%

The Ar and Nd:YAG results are satisfactory, as they lie well within the uncertainty intervals. The discrepancy at the C0 2 laser line is more difficult to understand and can be due to transverse beam profile effects.


ECU 34 313

PARTICIPANTS

Laboratoire National d'Essais, F Physikalisch-Technische Bundesanstalt, D

55

PROJECT MTR 142

ESTABLISHMENT OF AN IMPROVED INFRARED SPECTRAL RESPONSTVTTY SCALE

PROJECT DEFINITION

Before this project the calibration of IR detectors could be carried out at NPL between 1 and 3 μιη with an uncertainty of 3 %. This L· based on the use of a cryogenic radiometer. At high wavelengths up to 20 μιη, the uncertainty is estimated to be up to 20 % which is much too high.

The project consisted in establishing another absolute calibration point at 10.6 μπι (corresponding to the C0 2 laser).

RESULTS

An absolute spectral responsivity scale has been established at two wavelengths, 1.3 and 10.5 μιη, using laser radiation, with an uncertainty of less than ± 2.5 % over the spectral range 1 μιη to 20 urn.

STATUS

In progress.


ECU 85 000

PARTICIPANTS


56

PROJECT MTR 165

OPERATION LIMITS OF INTENSE LIGHT SOURCES IN HAZARDOUS ATMOSPHERES

PROJECT DEFINITION

The objective of the work is to investigate the conditions in which optical instruments using intense light sources (such as lasers) can operate safely in hazardous atmospheres (containing vapours of combustible products or suspended combustible particles). The influence of the following parameters is going to be experimentally addressed:

the nature of the light (coherence, intensity, wavelength, spectral width and modulation);

the characteristics of the illuminated particles (size, chemical and physical nature, means of presentation to the light beam);

the nature of the gaseous environment, with the aim of classifying the optical hazard of the atmosphere in terms analogous to the electrical case, and of investigating thoroughly the minimum ignition energy, the auto ignition temperature and the burning velocity.

A small fraction of the work is devoted to theoretical mechanistic investigations of the initiation phase of explosions.

STATUS



ECU 390 340

PARTICIPANTS

Centre d'Etudes et Recherche de Charbonnage de France, F Imperial College, UK Physikalisch-Technische Bundesanstalt, 0 SIRA Communications Ltd , UK, (Coordinator) Si ra Safety Services, UK Universi ty of Leeds, UK

57

PROJECT MTR 177

MEASUREMENTS OF SPECTRAL TRANSMITTANCE AND REFLECTANCE AT VARIABLE ANGLES OF INCIDENCE

PROJECT DEFINITION

Available spectrophotometers allow the measurement of the spectral transmittance CT) and reflectance (R) of optical components only at normal incidence. From these data it is possible to obtain a rough estimate of the daylight and solar parameters of the glazing materials used for building and car windscreens. However the realistic computation of natural lighting inside structures requires the measurements of Τ and R at different angles of incidence, to account for the fact that the angle of the sun is a function of hour, date and latitude. As a prerequisite to the development of an improved method for determining the angular dependence of Τ and R, this project will be carried out along two parallel activities:

a) an intercomparison of the features of the existing instruments modified to perform such measurements on a limited scale,

b) a preliminary feasibility study to demonstrate that a new proposed technique is capable of meeting the prescribed requirements.

STATUS



ECU 23 500 and ECU 16 200 for the feasibility study.

PARTICIPANTS

Interconparison : Centre Scient i f ique et Technique du Batiaent, F Flachglas AG, D Glaverbel, Β I n s t i t u t National du Verre, Β Oxford Polytechnic, UK, (Coordinator) PilJcington, UK Saint Gobaiη Recherche, F Società I ta l i ana Vetro, I Stazione Sperimentale del Vetro, I Technical Research Centre, SF TNO, NL Uppsala Univers i ty , S

Feas ib i l i t y study : I s t i t u t o Nazionale d i Ot t i ca , I

Electrical Metrology

61

PROJECT MTR 044

TREATMENT, MEASUREMENT AND CERTIFICATION OF NICKEL CYLINDERS

PROJECT DEFINITION

In this project a set of nickel cylinders has been produced, treated by annealing at 450°C for one hour in vacuum to make them magnetically soft, and their magnetic saturation polarization certified for the calibration of magnetic measurement apparatus.

RESULTS

The work has been terminated. 45 certified reference samples were produced and are available upon request.

Their characteristics are as follows:

Material Density Dimensions Cross sectional area

nickel of purity 99.98 % 8.9 g/cm3 + / - 0.01 g/cm3

about 10 mm in diameter and 10 mm in length 3.157 cm2 + / - 0.001 cm2

Temperature coefficient at 25°C: -4.4 10 ̂ T/K

The certification of the magnetic saturation polarization is based on a detailed comparison of measurements with the Laboratoire d'Electronique de Grenoble which has shown excellent agreement (3 parts in 104).


ECU 19 212

PARTICIPANTS

Physikalisch-Technische Bundesanstalt, D

62

PROJECT MTR 082

INTERCOMPARISON MEASUREMENTS OF RESISTANCES IN A.C.

PROJECT DEFINITION

Calibration of resistances is a very important activity for industry laboratories and metrology laboratories. Primary metrology laboratories are estimated to carry out some 10.000 calibrations per year over all in the Community. The value of the resistance in a.c. is influenced by the frequency and this results in increased causes of inaccuracy at high frequency. The intercomparison involves resistors 0.1 i!, 1 Ω, 10 Ω, 100 Ω, 1 kn, 10 kQ, 100 kQ and 1 ΜΩ with coaxial UHF connectors. Measurements are to be done at frequencies ranging from 120 Hz to 10 kHz.

RESULTS

Resistors of nominal values, 1 Ω, 10 Ω, 100 Ω, 11(Ω, 10 kΩ, 100 kn and 1 ΜΩ have been calibrated at 120 Hz, 400 Hz, 15922 Hz and 10000 Hz. The uncertainties observed have been of the order of 1 ns in the time constant and of a few parts in 10"6 in the time constant.


ECU 31 000

PARTICIPANTS

1 s t i t u t o Elettrotecnico NazionaLe Gali leo Ferrar is , I Laboratoire Central des Industr ies Electr iques, F National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D Van Swinden Laboratorium/Dienst van het IJkwezen, NL

63

PROJECT MTR 092

IMPROVEMENT OF PROCEDURES FOR THE TESTING OF THE SUSCEPTIBILITY OF ELECTRONIC INSTRUMENTS

TO ELECTROMAGNETIC RADIATION

PROJECT DEFINITION

The introduction of electronic systems and microprocessors in measuring instruments that were initially mechanical in nature (balances, flow meters, etc) and in many other forms of instrumentation has introduced new problems of reliability. The electronic part can produce parasitic signals or wrong signals under the effect of electrical perturbations conducted in the mains (voltage peaks or voltage interruptions) or even more so under the influence of electromagnetic radiation (such as produced by antennae of portable radio transmitters, radar, etc) or by high frequency instrumentation in the vicinity. The specifications for military applications are well defined but they are hardly applicable for commercial instruments because they would make them uneconomical. The task of the project consisted in investigating the main parameters of the testing procedure for commercial instruments in an anechoic test chamber. The investigation covers the range of 80 MHz to 1 GHz. The final product of the project should be a detailed description of a test procedure, with appropriate instrumentation and calibration procedure.

RESULTS

Both a vector (IFS type EFS1) and an isotropic sensor (made by Holladay Instr.) have been used to monitor the level of the radiated EM field. The conclusions of the project are that, in the case of a shielded room without absorbers, the measured field strength depends greatly on the type of sensor, with readings differing by as much as a factor 4. Indeed, at constant antenna power in the 80 - 200 MHz range, the vector and the isotropic sensor have been found to display across the room variations at 28 and 17 dB respectively. However, these variations due to standing waves can be strongly reduced (to ±3 dB over the full volume, and to ± 1 dB over the test area) by the presence of absorbers. In this case the results have been found to be essentially independent of the field sensor used.


ECU 59 500

PARTICIPANTS

Elektronikcentralen, DK

64

PROJECT MTR 093

INTERCOMPARISON MEASUREMENTS WITH ELECTROMAGNETIC FIELD STRENGTH METERS

PROJECT DEFINITION

Many existing international electromagnetic (EM) compatibility regulations that refer to a variety of different fields, ranging from legal metrology to environment and safety, impose requirements on susceptibility and electromagnetic field strength in the rf range. The reliability of the associated measurements is at present not satisfactory since the EM field sensors are not all based on the same physical principle. As a consequence, in response to the same field, the reading of two meters may differ, even when they are correctly used. Calibration laboratories have set-ups where the EM field can be calculated and when confirmed by measurement. However, at different test stations, instrument calibration is performed using non homogeneous techniques, in a variety of conditions and procedures. The present intercomparison is a first step towards the harmonisation of testing procedures. Three probes will be circulated :

a magnetic probe (RMCO 6507) an electric isotropic probe (EMCO 7130) an isotropic probe manufactured by Aeritalia.

The measurement will be performed at linear polarization field levels of 1, 3 and 10 V/m, and .5, 1, 3, 10, 27, 100, 300, 500, 1000 MHz.

STATUS

In progress.


ECU 153 000

PARTICIPANTS

AeritaLia, I Area Brown Boves, CH British Aerospace, UK Elektronikcentralen, DK Laboratoire Central des Industries Electriques, F National Physical Laboratory, UK Philips, NL Physikalisch-Technische Bundesanstalt, D Radio Frequency Technologies Ltd, IRL Technical Research Centre, SF Van Swinden Laboratorium, NL

65

PROJECT MTR 094

MAGNETIC MEASUREMENTS ON ELECTRICAL SHEET STEELS BY MEANS OF SINGLE SHEET TESTERS

PROJECT DEFINITION

The production of electric steel sheet of various qualities is not far from IM tonnes. The prices vary considerably with the power losses in the material. For that reason an intercomparison was organised in the previous BCR programme. It had shown that the accuracy required by the commercial classifications are hardly achievable by the best laboratories. The measurements were done by the usual Espstein frame method. This method is time consuming and therefore expensive. The IEC has proposed a new method called the Single Sheet tester which is capable of accommodating sheets of 500 χ 500 mm. Most producers and some metrology laboratories are already equipped for this kind of measurement. The project was designed for measurements to be done on six different materials available in sheet of two or three thicknesses.

RESULTS

The participating laboratories measured for 7 sheets of grain oriented material and 13 sheets of non-oriented material the specific power Loss (Ps), the specific apparent power (Pa), and the relative magnetic permeability (Pr). In the case of Ps for oriented sheets, 3 laboratories agreed to within ± 1 % , 4 to within 3% and on sheets 4-6,5 laboratories agreed to within 3%; while for non-oriented sheets, 4 laboratories agreed to within ± 1%, except for sheet 17 which was particularly wavy and, in some cases, at higher field (1.5 T). In the case of Pa for oriented sheets, 4 laboratories agreed to within 1% for many measurements and to within ± 5 % for the majority of the remainder, while for non-oriented sheets, 5 laboratories agreed to within ± 1 % at J = l and 1.3 T, and within ± 5% at different values of J with the exception of sheet 17. All measured values of Pr have always been found to agree within ± 1% at any value of J.


ECU 69 000

PARTICIPANTS

B r i t i s h Steel Corporation, UK CockeriLL Sambre SA, Β I s t i t u t o Electrotécnico Nazionale Gal i leo Ferrar is , I National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D Stahlwerke Bochun Akt iengesel lschaft , D

66

PROJECT MTR 098

SOLID STATE VOLTAGE TRANSFER STANDARDS

PROJECT DEFINITION

The primary volt is derived at present from Josephson Junctions and maintained in the metrology laboratories with Weston Cells. The transfer of the volt e.g. to industrial calibration laboratories is done by means of digital voltmeters which provide an accuracy of about 10 ppm. Recent solid state voltage standards using Zener diodes appeared to be able to transfer and maintain the volt with an accuracy of the order of 1 ppm or better over one year. The objective of the project was to investigate how such a solid state standard would behave when transported from one metrology laboratory to another for an intercomparison. Three instruments are being circulated amongst the metrology laboratories for calibration at 1 V and at 10 V.

RESULTS

For intercomparison measurements three sources of two different types have been circulated: 1. Fluke model 732 with the output of 10 V, 1.018 V and 1 V. 2. Cropico VSIO, with the output of 10 V. 3. Cropico ECSI, with the output of 1.018 V and 1 V. The laboratories agreed in their measurements to within ± 1 χ 10*. The long term stability analysis performed by the pilot laboratory (PTB) over a longer period (5 years) has shown for all sources a linear drift with time of a few parts in 10"6.


ECU 51 400

PARTICIPANTS

Physikalisch-Technische Bundesanstalt, D National Physical Laboratory, UK Ministère des Affaires Economiques/Service de la Métrologie, Β Laboratoire Central des Industries Electriques, F Van Swinden Laboratorium/Dienst van het IJkwezen, NL Ist i tuto Elettrotecnico Nazionale GaLileo Ferraris, I Institute for Industrial Research and Standards, IRL Elektronik Centralen, DK

67

PROJECT MTR 099

INTERCOMPARISON OF RESISTANCE STANDARDS OF 1 kOHM AND 10 kOHM

PROJECT DEFINITION

The calibration of resistors is one of the most frequently requested and the tendency is for it to increase. The signals produced by measuring instruments are processed through resistors before display or treatment in computers. The resistors must in particular be of very high stability and generate very little noise. For telecommunications and also space, the tolerances are of the order of 10"4 to 5.10'5 and there temperature coefficients must be as low as 1 ppm/°C or better. Aircraft computers for example must be able to operate at temperatures ranging from -50 to +40 °C which would cause large resistance variations if resistors were not of very high quality. The resistors for the intercomparison were selected in the range corresponding to the major industrial needs.

RESULTS

The set of four resistors intercompared consisted of: 1. 10 kn resistor, manufactured by ESI, supplied by PTB. 2. 10 kn resistor, manufactured by ESI, supplied by NPL. 3. Two distinct 1 kn resistors manufactured by Tinsley, supplied by NPL. The linear fit to all data shows an overall standard error of 2 ppm twice the greatest uncertainty given by each participating laboratory.


ECU 37 000

PARTICIPANTS

National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D Laboratoire Central des Industries Electriques, F Istituto ELettrotecnico Nazionale Galileo Ferraris, I Ministère des Affaires Economiques/Service de la Métrologie, Β EOLAS, IRL Elektronikcentralen, DK

68

PROJECT MTR 115

CALIBRATION OF CAPACITORS AT FREQUENCIES OF 10 kHZ TO 1 MHz

PROJECT DEFINITION

The market of capacitors represents more than 3.10' ECU in Europe. For electronic equipment the characteristics of these capacitors must be determined at frequencies up to 1 MHz. The accuracy requirements are beyond the capabilities of the best metrology laboratories. The project therefore was given the objective of developing a method of calibration for capacitors of 1 pF to 1 uF at 100 kHz and at 1 MHz. When the calibration method is optimized, high quality capacitors will be calibrated to serve as transfer standards for other metrology laboratories.

RESULTS

The study consisted in the characterization at radio frequency of capacitors, both of the two-terminal and of the four-terminal pair connection mode. Two different domains have been experimentally investigated:

capacitors ranging from 1 pF to 1 uF at frequencies from 1 to 100 kHz both for capacitance and loss factors capacitors ranging from 1 pF to 1 nF at frequencies up to 1 MHz for both capacitance and loss factor.

A detail model of equivalent circuit was investigated. The study confirmed that 4-tp modelling is intrinsically better than 2-tp at all frequencies. However, the experts agreed that this last model remains sufficiently accurate for most practical purposes. The higher uncertainties were found at low frequencies and remained within 10"4.


ECU 81 000

PARTICIPANT

Laboratoire Central des Industries Electriques, F

69

PROJECT MTR 124

INTERCOMPARISON OF SOFTWARE FOR EVALUATING HIGH VOLTAGE IMPULSES AND STEP RESPONSES

PROJECT DEFINITION

In the last few years computer controlled digital recorders have almost completely replaced analog oscilloscopes in high voltage (hv) test laboratories, as they enable automated hv testing and record processing. However, as yet, no generally accepted software or algorithm exists for the data processing of hv impulses and of the step responses of hv dividers. The objective of the intercomparison is to gather a sound and updated body of information for the establishment of a future standardized software in hv impulse tests. A set of data files on several typical hv impulses and step responses, both synthetic and actually measured, will be sent to each participating laboratory to compute with its individual software the prescribed parameters.

STATUS



ECU 10 000

PARTICIPANTS

10 laboratories from different Member states plus Finland, Sweden and Switzerland.

70

PROJECT MTR 130

INTERCOMPARISON OF THERMAL AC-DC CURRENT TRANSFER STANDARDS

PROJECT DEFINITION

The voltage and current units in a.c. are related to d.c. units by means of thermal converters. In the past BCR programme an intercomparison was made of the calibration of high frequency voltage by means of ac-dc thermal converters. This involved seven metrology laboratories in the Member States. The main reason for this is the considerable requirements of industry for a wide variety of applications where instruments of very high accuracy are used (current sources, multimeters, etc). A large number of industry laboratories are also accredited for carrying out such measurements. The field of electric current was not covered by this intercomparison and it is felt by the metrology laboratories of the Member States that there is a need to ensure that there is sufficient agreement among themselves. This is of particular importance for the future to facilitate mutual acceptance of calibration laboratories. The project consists of an intercomparison of the calibrations of thermal ac-dc current transfer devices for currents ranging from 10 mA to 20 A. The measurements are done on a set of five single junction thermal converters with appropriate shunts for the différent current ranges. Each device is to be calibrated at 10 or 20 Hz, 1 kHz, 20 kHz, 50 kHz and 100 kHz. In the case of 20 A the maximum frequency is limited to 5 kHz.

RESULTS

The project established a very good agreement among the participating metrology laboratories in the two 10 mA to 20 A and 10 Hz to 100 kHz ranges: at low current level (10 mA and 100 mA) the standard deviation was found between 15 to 30 10"6, than it was observed to progressive degrees to 100 10* over the full ranges of currents to 20 A and above.



PARTICIPANTS

Elektronik Centralen, DK ΙΕΝ,Ι Laboratoire Central des Industries Electriques, F Physikalisch-Technische Bundesanstalt, D VSL, NU

71

PROJECT MTR 143

INTERCOMPARISON OF MEASUREMENTS OF PERMANENTMAGNETS

PROJECT DEFINITION

The intercomparison covers the determination of : remnant induction Br; coercivities H^ and He,; maximum energy product (ΗΒ)„„.

NdFeB and AlNiCOe have been selected because of their properties and technological importance. Two classes of measuring techniques will be used by the participants. The first and most widely used employs a closed circuit apparatus, in which cylindrical samples are placed in between the poles of an electromagnet. In the second, approximately 3 mm diameter spheres will be held in the field of an open circuit apparatus, such as vibrating magnetometers. This latter intercomparison will be limited to NdFeB, because, in this configuration, the high remanence and low coercivity of AlNiCOe make it difficult to correct for demagnetizing effects. As accurate calibration is an essential pre-requisite for the success of the intercomparison, reference samples will be distributed to all participants.

RESULTS

Besides AINiCO and NdFeB specimens, Ni reference specimens were also circulated for calibration purposes. The results of the audits are complex, but in general it can be said that the agreement obtained has been quite good within the two separate groups (cylinders and spheres). The correlation between the results of the two separate methods turned out to be unsatisfactory in so far as the small spherical specimens had changed their properties as a results of the preparation process.


ECU 40 000

PARTICIPANTS

Physikalisch-Technische Bundesanstalt, D (Coordinator) Centro Magneti Permanenti S.p.A., I Instituto de Ciencia de Materiales de Aragon, Zaragoza, Ε Krupp Uidia GmbH, D Hagnet-Physik Dr. Steingroever GmbH, D Philips Components, NL Physikalisch-Technische Bundesanstalt, D Sieaens AG, D Swift Levick Hagnets Ltd, UK Thyssen Edelstahlwerke AG, 0 Universidad Ingeniera Técnica Industrial, E Ugimag Recosa AG, CH

Industrie Ossidi Sinterizzati S.p.A., I s t i t . Haspec, Parnta, I Laboratoire d'Electrotech Grenoble, F National Physical Laboratory, UK Philips Components, UK Rheinisch-Westfälische T.H. Aachen, D Sunderland Polytechnic/Magnet Centre, Technical University of Denmark, DK University of Dublin, IRL Universidade Porto, Ρ Vakuumschmelze GmbH, D

72

PROJECT MTR 181

MEASUREMENT OF SUBMICRON SEMICONDUCTOR JUNCTION DEPTHS AND WIDTH

PROJECT DEFINITION

The quantitative determination of junction depths and lateral outdiffusion lengths as well as the measurement of carrier concentration form an essential part in the control of semiconductor processing. In this project the spreading resistance technique (SRP) for the determination on Si structures of:

junction depths, lateral spreading with outdiffusion lengths carrier concentrations,

will be extended in resolution down to the nanometre range and improved in view of its possible standardisation.

STATUS



ECU 465 350

PARTICIPANTS

Interuniversitair HicroeLectronica Centrum, B, (Coordinator) Katholieke Universiteit Leuven, Β Seaiconductor Assessment Services, UK

Acoustics and Ultrasonics

75

PROJECT MTR 113

INTERCOMPARISON OF ULTRASONIC POWER CALIBRATION OF ULTRASONIC TRANSDUCERS FROM 1 TO 10 MHz

PROJECT DEFINITION

The objective of the intercomparison is to compare the ultrasonic power calibration of a number of standard transducers in primary laboratories.

STATUS

In view of potential measurement difficulties, it was agreed that the intercomparison should initially be restricted to calibrations of only one of the transducers, namely the 4 MHz one. The results of this initial phase demonstrated that at least one laboratory had to further develop its equipment in order to eliminate possible sources of error. This having been done, the intercomparison is now continuing with the 1, 2, 5 and 10 MHz transducers.


ECU 65 000

PARTICIPANTS

Physikalisch-Technische Bundesanstalt, D Toegepast Natuurwetenschappelijk Onderzoek TNO, NL National Physical Laboratory, UK

76

PROJECT MTR 122

SOUND CALIBRATORS

PROJECT DEFINITION

A sound calibrator is a portable device which produces a known sinusoidal sound pressure of a specified level and frequency. Sound calibrators are used extensively in routine technical measurements for a quick verification or recalibration of microphones used in the field. There are however, in this kind of calibration, sources of errors which are suspected but not well investigated. They originate from the ambient conditions, mainly ambient temperature and pressure. The main errors probably come from the coupling between the calibrators and the microphones. The objective of the project was to investigate how accurately microphones are calibrated by well characterized sound calibrators. Measurements were made with one precision and two ordinary sound calibrators, using seven standard and non-standard microphones.

RESULTS

The range of differences in the measured sound pressure levels was 0.09 dB for the precision sound calibrator and 0.35 dB for the ordinary sound calibrators. It was concluded that some of the discrepancies in the results were due to the coupling between the calibrators and the microphones.


ECU 183 000

PARTICIPANTS

Laboratoire National d'Essais, F Van Swinden Laboratorium, NL National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D Universi ty of Copenhagen, DK I s t i t u t o d i Acoustica, E I n s t i t u t National de Métrologie, F

77

PROJECT MTR 125

THE DEVELOPMENT OF IMPROVED METHODS OF SOUND ABSORPTION MEASUREMENT

PROJECT DEFINrnON

Many materials used for the construction and furnishing of buildings are required to have sound absorption properties aimed at preventing either echo phenomena or sound transmission to other parts of the building. Methods have therefore been developed to measure sound absorption in the laboratory. However, in many cases the value obtained is dependent upon the design of the measuring room. Moreover, values of greater than 1, which are theoretically impossible since they imply that more sound is absorbed than is incident, are frequently obtained.

The aim of the project is to develop a series of artefacts whose sound absorption characteristics are known both theoretically and experimentally. Techniques will then be developed to characterize measuring rooms and thus enable comparable sound absorption values to be obtained in different laboratories.

STATUS

Flat reference absorbers have been developed for which it is possible to determine both theoretically and experimentally the "true" sound absorption coefficients. Work is continuing to investigate the sound absorption coefficients that are actually measured with these reference absorbers in different reverberant rooms.


ECU 159 000

PARTICIPANTS

Initial Investigation, Fraunhofer Institut für Bauphysik, D

78

PROJECT MTR 127

NOISE ATTENUATION BY WINDOWS CWITH FRAMES)

PROJECT DEFINITION

This intercomparison dealt with laboratory measurements of the sound insulation of double-glazed framed windows. It followed a previous intercomparison of measurements on window panes without frames. The aim of the present project was to determine the measurement precision associated with a measurement procedure better defined than the one in the present ISO Standard 140/3.

Measurements were carried out on two windows that had different kinds of glazing. The measurement guidelines given to the participating laboratories referred to the ISO standard and additionally described in detail the two noise source positions and the window mounting conditions.

RESULTS

Using prescribed noise source positions and window mounting conditions, the reproducibility was found to be different for the two windows that were tested. Large values were obtained for the window with 6-16-6 double glazing, particularly at frequencies corresponding to strong resonances of the system, with single number reproducibilities of 3.3 dB for Rw and 4.5 dB for R traffic. For the other window with 44R-6-8 double glazing, the single number reproducibilities were 1.7 dB for Rw and 2.5 dB for R traffic.


ECU 142 000

PARTICIPANTS

Centre Scientifique & Technique de La Construction,. Β PTB, D University of Salford, UK Acoustical Investigation & Research Organisation Ltd, UK TNO, NL Technical. Universiteit Eindhoven, NL Instituto de Acústica, E Universiteit Leuven, Β Saint-Gobain V i t rage, F CSTB, F Flachglas AG, 0 Fraunhofer I n s t i t u t fü r Bauphysik, D Univ. of Oenmark, DK Centre expérimental de Recherches et d'Etudes du Bâtiment et des Travaux Publ ics, F Laboratorio Nacional de Engenharia C i v i l , Ρ Laboratorio de la Dirección General Para la Vivien da y Arquitectura Min is ter io de Obras Publicas, Ε

79

PROJECT MTR 132

DEVELOPMENT OF STANDARD MEASUREMENT METHODS FOR ESSENTIAL PROPERTIES OF ULTRASOUND THERAPY EQUIPMENT

PROJECT DEFINITION

The measurement methods in the new proposed IEC standard on the testing and calibration of ultrasound therapy equipment are based on the use of hydrophones to map the ultrasonic fields in planes perpendicular to the direction of the ultrasonic beam at different distances from the transducer face. A definition of beam cross-sectional area (BCA) will be used but there is a need to test the validity of the definition over a wide range of transducers and for ones functioning correctly and incorrectly. It is also proposed to develop simplified measurement techniques and to obtain relevant information on the ultrasound field produced by the transducer. Beam non-uniformity and hot spots (high ultrasonic energy spots within the total field) should also be investigated.

RESULTS

Rapid measurement procedures for the BCSAj (Beam Cross Sectional Area) and BCSAQ have been developed and tested. A factor for converting the BCSA„ to the ERA (Effective Radiating Area) has been theoretically determined. Validation measurements for the BNR (Beam Non-uniformity Ratio) have been carried out. The overall uncertainties are 5-8% for all measurements using raster scans (95% confidence level). Validation measurements at NPL and TNO generally showed very close agreement. The measurement methods developed in the project will be introduced into the proposed revision of the IEC standard on the testing and calibration of therapeutic equipment.


ECU 70 000

PARTICIPANTS

National Physical Laboratory, UK Physikalisch-Technische Bundesanstalt, D TNO, NL

80

PROJECT MTR 146

INTERCOMPARISON OF FREE FIELD CALIBRATION OF MICROPHONES

PROJECT DEFINITION

Microphones are calibrated by the reciprocity technique, where a set of 3 microphone is used 2 by 2, one acting as transmitter and the other as receiver. By 3 measuremeni it is possible to find the sensitivity of each microphone expressed as the outpt voltage/sound pressure on the microphone diaphragm.

Reciprocity calibration can be performed either with a coupler or in a free fie] situation. Until now most work has been concentrated on pressure calibration wit couplers. However practical measurements, in particular field measurements related 1 legislation, require free-field calibrations of microphones, sound level meters, etc.

Two previous BCR intercomparisons dealt with the pressure calibration with couple of 1/2" and 1" microphones and had an important influence on the revision of the IS standards. The objective of the present intercomparison is to measure the free-fid sensitivities of six standard 1/2" and 1" microphones and resolve the reasons for ar differences that are observed between laboratories.

STATUS

In progress.


ECU 179 000

PARTICIPANTS

DTH, OK Physikalisch-Technische Bundesanstalt, D National Physical Laboratory, UK Laboratoire National d'Essais, F VSL, NL

81

PROJECT MTR 155

INTERCOMPARISON OF OPEN-INLET/OPEN-OUTLET NOISE MEASUREMENT ON FANS

PROJECT DEFINITION

The BCR intercomparison MTR 077 "In-duct noise measurements on fans" terminated in 1988. A natural follow-up of this project is to extend it to other installation situations such as free-inlet/free-outlet, free-inlet/ducted-outlet and ducted-inlet/free-outlet. As no specific internationally agreed standard exists, it is expected that the project will have major influence on standardization. Two test fans will be circulated between the participants, one a belt driven centrifugal fan and the other an axial fan with close-coupled motor mounted in the airflow. The fans will be mounted in test rigs assembled from a standard set of ducting to be circulated with the fans. This will ensure identical installation conditions for every measurement. The two fans are the same as have been used in the earlier intercomparison together with, as far as possible, the ducting used earlier. This will enable direct comparison with results from the earlier intercomparison concerning measurement of sound power inside ducts. Each of the participating laboratories will use its own noise measurement instrumentation to determine the noise levels of the fans both in-duct and at the open inlet or outlet.

STATUS

The two fans are currently being circulated.



PARTICIPANTS

National Engineering Laboratory, UK Woods of Colchester, UK CETIAT, F Soler Y Palau, E UCL, Β Deutsche Forschungs und Versuchsanstalt für Luft und Raumfahrt, D Novenco, DK

82

PROJECT MTR 156

CALIBRATION OF SOUND INTENSITY METERS

PROJECT DEFINITION

The number of measurements of sound power from machines is going to increase after the adoption of the directive on machines. Use of sound intensity techniques requires the calibration of sound intensisty meters although the methods are not at present well established.

The project is therefore structured to establish methods of calibrating sound intensity probes; to establish methods of determining the directionality of sound intensity probes; to establish simplified methods of verifying the calibration of sound intensity probes; to establish methods of determining the lowest measurable intensity.

The methods developed in the project will be incorporated in the IEC standard on "instruments for the measurement of sound intensity".

STATUS

Started in 1990.


ECU 188 000

PARTICIPANTS

National Physical Laboratory, UK ßrüel and Kjaer, DK CETIH, F DTH, DK Physikalisch-Technische Bundesanstalt, D

83

PROJECT MTR 168

INTERCOMPARISON OF SOUND POWER MEASUREMENTS BY USE OF REFERENCE SOUND SOURCES

PROJECT DEFINITION

Several Community Directives require measurement of the sound power emitted by machines such as household appliances, those used in the work place and those used by the construction industry. Such measurements have to be made in accordance with many different national and international standards all of which basically reflect the requirements of the ISO 3740 series and ISO 9295. These latter standards are rated at different precision levels and the measurements made are not always in agreement with the required uncertainty limits for a particular class of machine.

Ihe first phase of the project is for laboratories, PTB and Briiel and Kjaer, to investigate the different techniques available for the calibration of reference sound sources and agree calibrations for 4 selected sources. The second phase is an intercomparison of the calibration of sound power reference source involving the 6 - 8 different laboratories in Europe capable of such measurements. Finally, having agreed the calibration of the reference sources, they will be used in an intercomparison of sound power measurements by the substitution method in accordance with the draft revision of the ISO 3740 series.

STATUS

Phase 1 of the project has been completed. Calibrations of reference sound sources in reverberation rooms show systematic differences when different microphone arrangements are used, and it is concluded that more precise results are obtained with fixed microphone positions than with rotating microphone arrays. In the case of free-field measurements, it is concluded that a scanning microphone array (spiral path method) should be used instead of fixed microphone positions.


ECU 85 000

PARTICIPANTS

PTB, D BrQel and Kjaer, OK KUL Leuven, Β HEL, UK Staatliches HateriaLprüfungsamt, D BAM Berlin, 0 Lydtecknisk Inst i tut , DK TPD TNO-TH, NL

84

PROJECT MTR 192

HEARING PROTECTOR PERFORMANCE IN IMPULSIVE NOISE

PROJECT DEFINITION

The directive on the protection of workers from the risks related to exposure to noise at work (86/188/EEC) requires that workers should be provided with hearing protectors if the noise exposure is greater than 90 dB (A) or, in the case of impulsive noise, the maximum sound pressure level is greater than 200 Pascal.

The current standard, ISO 4869, determines the noise attenuation of a hearing protector as a function of frequency by measuring the human threshold of hearing with and without the hearing protector : the difference between the two thresholds is defined as the attenuation of the hearing protector. This method present two major problems. Firstly, it cannot be used with non-linear or amplitude-sensitive hearing protectors which provide increasing attenuation with increasing noise level so as to allow speech communication whilst at the same time attenuating hazardous noise. Secondly, irrespective of the linearity of the hearing protector, it is not possible to determine the attenuated maximum sound pressure level in the case of impulsive noise.

The answer to these problems lies in the use of acoustic measurements in the ear under the hearing protector when using realistic noises. Initially, hearing protector characterization methods will be developed that use test subjects, but ultimately it is intended to extend them to head simulators in order to be able to conduct tests that would otherwise expose subjects to potentially hazardous noises.

STATUS

Two initial studies are currently under way to investigate the feasibility of making appropriate measurements at a safe location in the ear under the hearing protector and to establish a suitable set of standard impulsive noise sources for laboratory tests.


ECU 50 000 (initial studies)

PARTICIPANTS

Berufsgenossenschaftliches Institut für Arbeitssicherheit, D Health and Safety Executive, UK Institut Franco-Allemand de Recherche de Saint-Louis, F Institut National de Recherche et de Sécurité, F Karolinska Institutet, Department of Technical AudioLogy, S Nederlands Instituut voor Preventieve Gezondsheidszorg, NL Physikalisch-Technische Bundesanstalt, D Schweizerische Unfall Versicherungsanstalt, CH Technical University of Oenmark, The Acoustics Laboratory, DK TN0 Institute for Perception, NL University of Salford, Department of Applied Acoustics, UK

Flow Measurements

87

PROJECT MTR 0 1 6

INTERCOMPARISON OF ORIFICE PLATE DISCHARGE COEFFICIENTS

PROJECT DEFINITION

Orifice plate meters are widely used for the metering of natural gas, hydrocarbons, industrial products, water etc with an uncertainty under ideal conditions of 0.7 to 1.0%. In order to obtain this uncertainty meters must be designed and used in accordance with the provisions of ISO 5167 which is based on experimental data obtained in the 1930's. With the increase in energy prices in 1978 it was decided to determine a new data base with a view to revising ISO 5167. To this end parallel programmes of work were started in Europe and the United States.

RESULTS

The European programme concentrated on determining the discharge coefficients of a 100 mm and a 250 mm orifice plate meters under ideal flow conditions when fitted with 6 orifice plates with ß ratios in the range 0.2 to 0.75. The fluids used were natural gas, air and water. In addition the effects of different pipe work installation geometries on the discharge coefficients were determined. The US programme, led by the American Petroleum Institute, determined the discharge coefficients of different meters with the same plate ß ratio as the European programme but for pipe diameters ranging from 50 to 375 mm. In this case the fluids used were oil and water and only ideal flow conditions were employed. An equation, with an overall uncertainty of ± 0.5%, developed as part of the European project has been accepted with a minor modification as the basis for the American Petroleum Institute's new standard and should form the basis of the next revision of the ISO standard. The project was terminated by the establishment of a data base available in both written and floppy disc formats.


ECU 681 000

PARTICIPANTS

British Gas, UK CEAT, F DeLft Hydraulics Laboratory, NL Gasunie, NL Gaz de France, F NEL, UK PTB, D Ruhrgas, D

PROJECT MTR 108

INTERCOMPARISON OF ANEMOMETER CALIBRATIONS

PROJECT DEFINITION

Anemometers are instruments used to measure air and gas velocities in applications ranging from wind tunnel experiments to determine air pollution, smoke extensions and potential wind conditions around buildings, to the assessment of conformance to national and industrial regulations in mines, clean rooms, spray booths, etc. They need therefore to be accurate to better than 10%. Above 2.5 - 3 m/s this is no problem since pitot tubes can be used for their calibration. Below this figure calibration is much more difficult, so much so that a recent survey showed that less than 20% of instruments are accurate to within better than 10% whilst some 40% had errors of over 20%. It is against this background that an intercomparison of anemometer calibration facilities was launched.

RESULTS

Two anemometers, one of the hot wire type and the other based upon a pulsed thermistor, have been circulated to 12 laboratories for calibration in the range 0 - 2.5 m/s at temperatures of 15 - 25° C. Due to faults, repairs and recalibration of the anemometers the termination of the project was delayed. The results are being evaluated.


ECU 105 000

PARTICIPANTS

British Maritime Technology, UK BSRIA, UK Centre d'Etudes et de Recherches de Toulouse, F CETIAT, F Dantec Electronik, DK DTI, OK Hochschule für Technik und Wirtschaft, Gießen, D Laboratorio Oficial J.M. Madariaga, E Politécnico di Torino, I The Technical Research Centre of Finland, SF TNO, NL Ui lheln Larabrecht GmbH, D.

89

PROJECT MTR 120

INTERCOMPARISON OF DISCHARGE COEFFICIENTS OF A 600 MM ORIFICE PLATE METER

PROJECT DEFINITION

Project MTR 016 describes programmes of measurements in Europe and the USA aimed at determining the discharge coefficients of orifice plate meters used for the metering of natural gas, hydrocarbons, water and industrial products. As a result of this work a new empirical equation relating flow rate to the differential pressure across an orifice plate meter has been developed and is currently being incorporated in national and international standards. However, the measurements were performed on meters whose diameters were in the range 50 - 250 mm, which means that there has been no check upon the validity of the equation for the meters of 600 mm and above used for the fiscal metering of natural gas and oil. This is the purpose of this project.

RESULTS

The programme has been completed and the data used to finalise the discharge coefficient equation developed under project MTR 016.


ECU 440 000

PARTICIPANTS

British Gas, UK Delft Hydraulics Laboratory, NL Gasunie, NL NEL, UK

90

PROJECT MTR 121

FLOW MODELLING FOR METERING PURPOSES

PROJECT DEFINITION

Two flow rigs, one for water and one for air, were circulated in an intercomparison of laser doppler and hot wire anemometry measurements. Complex systematic differences in results were observed for not only the two types of measuring system but also between instruments of different design based on the same principle. Additionally, the inability to measure sufficiently close to the wall led to unacceptable differences between the integrated flow and that measured by an accompanying flow meter.

RESULTS

Using the measured inlet flow profiles and the geometries of the flow rigs, an intercomparison of flow computations was made using different computer codes for the same two down stream planes measured in the experimental programme. The results showed considerable dispersion particularly in the turbulence parameters. Even when two models used nominally identical computer codes there were significant differences in results because of grid size effects, especially near the walls. Moreover, the integrated flow varied by up to 18 %.

A comparison of the theoretical and experimental results suggested that on average the former differed from the latter by about 4 %. It is therefore unlikely that current flow computations can be used to limit the need for experimentation.


ECU 494 000

PARTICIPANTS

CranfieLd Inst, of Technology, UK Delft Hydraulic, NL 1ST Lisbon, Ρ NEL, UK ONERA, F Technical University Eindhoven, NL TH Aachen, D Univ. Ancona, I Univ. Bremen, D Univ. College Dublin, IRL Univ. of Surrey, UK Univ. Thessaloniki, GR

91

PROJECT MTR 139

EVALUATION OF A SYSTEM FOR THE METERING OF MULTI-PHASE FLOWS

PROJECT DEFINITION

There are a number of attempts being made to use unproven methods to measure multiphase flow in particular for the oil industry (oil + water, oil + gas, etc).

The project consists of developing equipment for multiphase flow metering, based on the separation of the fluids, and using existing technology.

While the hardware development will be essentially paid by industry, the Commission will support the calibration in the laboratory, after the feasibility stage is terminated.

STATUS

Difficulties have been encountered in achieving the required accuracy. The design of the equipment had therefore to be changed significantly before the calibration phase covered by the Commission project could start.

The project should now finish at the end of 1992.


ECU 160 700

PARTICIPANTS

NEL, UK

92

PROJECT MTR 166

INTERCOMPARISON OF HOT WATER CALIBRATION TEST FAdLITIES

PROJECT DEFINITION

The project consists in circulating 3 transfer standards packages of different diameters in the commonly met range 15 to 150 mm. Each package will comprise two meters in series in order to have a built in check on stability. In general one meter will be of the turbine type and the other a heat meter, probably of the electromagnetic type in order to minimize flow disturbance.

The packages will be circulated to the participating laboratories who will calibrate them at fixed temperature in the range 20 - 70 °C and at designated flow rates across their entire range. The procedure to be adopted is defined in detailed guidelines produced by the pilot laboratory, the Jutland Technological Institute.

STATUS

The meter packages have been manufactured to the required standard and tested by approximately half the participating laboratories. The project should be finished at the end of 1993.



PARTICIPANTS

CETIAT, F Finnish District Heat Ass., SF IHGC, I Inspection Générale de La Métrologie, Β Instituto Superior Técnico, Ρ Jysk TeknoLogisk, DK National Engineering Lab., UK Nederlands Meetinstituut, NL PTB, D Swiss FederaL Office HetroLogy, CH

In addition further participation is expected from Dantec (DK) and at least one additional Finnish test centre.

93

PROJECT MTR 193

INSTALLATION EFFECTS ON ULTRASONIC FLOW METERS FOR GAS APPLICATIONS

PROJECT DEFINITION

Ultrasonic gas meters have been developed to a stage where they can be considered as alternatives to orifice plate and turbine meters for fiscal metering, particularly for large gas transmission lines applications. However, their use is not covered by the existing directives on gas flow and there are no recognised standards for their installation and operation.

The purpose of the present study is to investigate the effects of upstream disturbances on the accuracy of 150 mm and 300 mm ultrasonic gas meters with a view to developing appropriate written standards.

STATUS

In progress.


ECU 220 000

PARTICIPANTS

BP International, UK British Gas pic, UK Daniel Industries, UK Departeent of Energy, UK Gaz de France, F Nederlandse Aardolie B.V., NL NNI, NL N.V. Gasunie, NL PTB, D Ruhrgas AG, 0 SIM, F

Physical Properties

97

PROJECT MTR 102

EMISSIVnY OF GLASS

PROJECT DEFINITION

The heat transmission through double glazed windows is for a large extent determined by the heat barrier created by the gap between the two sheets of glass. The gap must be small enough to avoid convection, the filling gas should have rninimum thermal conductivity. When these conditions are satisfied there remains the need to minimize radiation. The amount of heat radiated by a surface is proportional to its emissivity. The emissivity of normal glass is close to one (0.9) and to reduce it one applies reflecting coatings on the glass. New coatings are still being developed although this technique has already a very wide application. The determination of the emissivity can be done by spectrophotometry or by means of radiometry. Measurements are difficult and of relatively high uncertainty. The objective of the project was therefore to study a simplified method (based on the use of reference materials) and with an uncertainty not higher than a few per cent.

RESULTS

A new procedure has been developed and tested which allows the evaluation of the total normal and hemispherical emissivity of the surface of solids in the temperature range between 50 °C and 100 °C, in a considerably shorter interval than with conventional procedures. The receiver system has been calibrated in such a way that no comparison measurements must be carried out between sample and blackbody; this calibration can be checked and controlled with reference samples. The uncertainty is of 0.02 for the total normal emissivity and of 0.03 for the total hemispherical emissivity. Suggestions are given to extend the useful temperature range.


ECU 64 700

PARTICIPANT

Physikalisch-Technische Bundesanstalt, D

98

PROJECT MTR 105

HEAT TRANSMISSION THROUGH FRAMED WINDOWS

PROJECT DEFINITION

The results of a previous intercomparison in which measurements of heat transmission were made on two different sized double-glazed window units (without frames) showed rather large discrepancies between the different laboratories. In this latest intercomparison, seven double-glazed reference panel units and seven double-glazed framed windows were circulated and measurements were made under commonly agreed and very detailed specified conditions. The reference panels had a rigid foam insulation material between the panes because a particular problem in the previous intercomparison had been the variation in the thickness of the airgap between the panes. Each participating laboratory made measurements on one panel unit and one window using a guarded hot box apparatus.

RESULTS

The standard deviation about the mean of the standardised U-values was about 5 % for the reference panels and about 7 % for the windows. Excluding outliers where reasons for discrepancies could be postulated, the range of the standardised U-values was 2.03 to 2.29 W/m2K for the reference panels and 2.46 to 2.84 W/m2K for the windows.


ECU 58 000

PARTICIPANTS

Forschungsinstitut für Uärmeschutz, D Fraunhofer Institut für Bauphysik, D Centre Expérimental de Recherches et d'Etudes du Bâtiment et des Travaux Publics, F Centre Scientifique et Technique du Bâtiment, F Institut für Fenstertechnik, D British Board of Agreement, UK Pilkington Brothers, UK Istituto Centrale per I'lndustrializazione della Tecnología Edilizia, I National Physical Laboratory, UK Toegepast Natuurwetenschappelijk Onderzoek, NL Centre Scientifique et Technique de La Construction, Β

99

PROJECT MTR 106

INTERCOMPARISON OF CRITICAL CURRENT MEASUREMENTS IN NbjSn SUPERCONDUCTORS

PROJECT DEFINITION

The current carrying capability of superconductors is limited by the strength, of the applied magnetic field. An intercomparison of critical current determinations in a Nb3Sn superconductor was undertaken between laboratories within the Community. Subsequently a second intercomparison involving laboratories in Europe, Japan and the USA was arranged as part of the Versailles Project on Advanced Materials and Standards (VAMAS). As the wires have to be heat treated to form the superconducting Nb3Sn phase, the intercomparisons were structured in order to identify differences arising from both the heat treatment and the critical current measurements.

RESULTS European intprrnmparison Completed in 1986, this intercomparison showed an agreement on critical current measurements to within 6 % irrespective of whether the specimens were heat treated individually by the participants or centrally in a single batch. The major source of differences was identified as induced strain effects, the magnitude of which depended upon the details of the mandrel upon which the specimen was wound and the method of fixing it in place. VAMAS intercomparison 22 laboratories from Europe, USA and Japan made measurements on 3 wires of different construction and hence current carrying capacity. The results reflected the same trends as found in the European intercomparison. The between laboratory standard deviation increased from 6 % to 12 % as the current carrying capacity of the wire decreased from approximately 550 to 400 A. The induced strain in the different experimental set-ups was again approximately equivalent to the observed scatter in the critical current data. A second round using a single wire on identical mandrels and more precisely defined test procedures reduced the scatter in the data from 8.3 to 2.2% at a field strength of 12 Tesla.


ECU 32 400

PARTICIPANTS

European laboratories : CEA Sac lay, F Clarendoa Lab., UK CNRS, F ENEA, I IHGC, I INFN, I Kerforschungszentrum Karlsruhe, D Rutherford Appleton Lab, UK SCK/CEN, 8 Siemens AG, D Twente University of Technology, NL Universiteit Nijmegen, NL VacuumschmeLze GmbH, D

100

PROJECT MTR 110

IMPROVED ENERGY LOSS COEFFICIENTS FOR HEATING AND VENTILATING SYSTEMS

PROJECT DEFINITION

In order to design an efficient air heating or ventilation system it is necessary to know accurate values of the mechanical energy losses associated with the various ducting and other components of the system and how they vary with installation conditions. The currently tabulated values are often of unknown quality, contradictory and devoid of essential information, such as Reynolds number and installation effect dependencies. The net result is that designers of ventilation systems for commercial, residential and industrial building, mines, etc. have to incorporate large factors of safety to ensure their systems work. This in turn leads to not only larger than necessary system components but, more importantly in the long term, higher running costs since the system may be operating under far from optimum conditions. A project has therefore been undertaken to produce new traceable mechanical energy loss data for ducting components.

RESULTS

A procedure for the determination of energy loss coefficients was developed and tested via an intercomparison involving 4 laboratories. For values in the range 0.31 to 0.72 the laboratories agreed to within one standard deviation of 2 to 7 %. Further improvements were then made to the procedure and the energy loss coefficients for the entire range of circular ducts configurations used by industry were determined for normal span flow rates (Reynolds numbers) encountered in practice.

Using the approximately 1100 combinations a data base has been produced in both written and micro-computer based form. This will be available to the industry at the end of 1992.


Preliminary studies : ECU 114 500 Main project : ECU 591 000

PARTICIPANTS

CETIAT, F NEL, UK SUD, D Uni. Catholique de Louvain, Β Univ. Hannhein, D

101

PROJECT MTR 135

EMTSSIVTTY MEASUREMENTS AT ELEVATED TEMPERATURE

PROJECT DEFINITION

The heat emitted by radiation depends essentially on the emissivity of the surface of the material; polished metals have a very low emissivity and therefore emit little radiation, black surfaces have a high emissivity. Emissivity is thus fundamental in all temperature measurements by optical means since the amount of radiation recorded by a pyrometer can only be converted into temperature through the Planck law if one knows the emissivity of the surface. This is a major problem that makes it almost impossible to measure accurately temperature by optical means if the material surface is non-uniform.

The project involves the comparison of spectral emissivity measurements at 500°C on a black-body with those taken normal to the surfaces of low and medium emissivity materials (platinum, stainless steel and silicon carbide or graphite) at 3 wavelengths (2.26, 3.79 and 5.06 μπι). Instead of using a black-body reference, one laboratory (IMGC) used an integrating sphere reflectometer and an infrared thermometer.

RESULTS

In a first phase that did not involve IMGC, the agreement between the laboratories was not good, and the normal spectral emissivity values obtained by the different laboratories varied by more than 0.2 in some cases. The agreement was improved when the results from 2 laboratories were corrected as a result of re-calibrations of their commercial black-body cavities against an NPL standard.

In a second phase, involving only IMGC and NPL, very good agreement was obtained, even though the techniques used by the two laboratories were very different. All the normal spectral emissivity values agreed to within 0.02 and there appeared to be no systematic differences.


ECU 61 000

PARTICIPANTS

NPL, UK Etablissement Technique Central de l'Arnenent, F Ecole Centrale des Arts et Métiers, F IMGC, I

102

PROJECT MTR 140

TOTAL HEMISPHERICAL EMISSIVITY OF COATED GLASS

PROJECT DEFINITION

As it is not possible in the present state of the art to determine the total emissivity in a practical way in routine laboratories, the problem of importance for industry is to know the correlation between hemispherical emissivity and normal emissivity. Industry actually determines normal emissivity by integrating spectral reflectivity measurements (in the infrared) by means of a spectrophotometer. The project will start with a rather basic step in which the few laboratories which are able to make measurements at a wide angle from normal will compare results. In particular PTB does total emissivity measurement. NPL does absolute infrared spectral reflectivity measurement and should provide an interesting verification as both approaches should ultimately provide the same result.

RESULTS

Three types of coated flat glass, with normal emissivities of 0.14, 0.32 and 0.62, were analyzed by measuring: a) thermal radiation using broadband detectors (PTB, TNO and OU), b) spectral reflectance between 5 and 55 μπι (NPL, SG). In spite of the different measuring procedures the agreement between single angular values for all three coatings was within .015 (NPL and PTB) and within 0.041 (all participants). The agreement between the three laboratories who measured up to 80° (NPL, TNO, OU) was within .028. After correcting for the initial differences between samples, the mean modulus of difference (averaged over all angles for each type of coating) was within .007 (NPL and PTB) and within .014 (all participants). The significant extension of the angular range achieved with respect to previously published studies (from 70 to 85°) allows a more accurate characterization of industrial architectural coatings, and can be used by the glass industry to improve the standards on thermal insulation.


ECU 50 000

PARTICIPANTS

National. Physical. Laboratory, UK Open University, UK Physikalisch-Technische Bundesanstalt, 0 Stazione Sperimentale del Vetro, I TNO, NL

103

PROJECT MTR 154

MEASUREMENTS OF HIGH TEMPERATURE THERMAL CONDUCTIVITY OF LIQUIDS

PROJECT DEFINITION

A comparative study of the advantages and problems associated with the different available techniques for the determination of the thermal conductivity of melts at temperatures up to 1500 °C was undertaken. This showed that all existing techniques were incapable of achieving the precision required by the steel, non-ferrous, glass and other industries.

A new non-interactive technique based on the measurement of thermal dissipation into a reusable sensor implanted into the container wall was however considered viable in terms of the requirement. A feasibility study has therefore been launched to validate the approach.

STATUS

Although the project is still in progress, the new sensor has been shown to be both stable and to have a sufficiently high signal to enable the high temperature thermal conductivity of the liquid to be determined. When perfected the performance of this sensor will be compared with that of conventional techniques.


ECU 115 500

PARTICIPANTS

University of Lisbon (Coordinator), Ρ Imperial College, UK National Physical Laboratory, UK

104

PROJECT RM 268

THERMAL CONDUCTIVITY OF INDUSTRIAL REFRACTORIES

PROJECT DEFINITION

The project originated from industrial requirements for better characterisation of refractories. Results from ASTM methods and from methods preferred in Europe were said to differ by up to 30 %. This made it impossible to design correctly furnaces for metallurgy and other applications. A new practical method had been studied by a group of laboratories from industry and was being proposed for ISO standardisation. The purpose of the project was to connect the results of that method to results from the accurate method of hot guarded plate. In addition, the work was intended to produce the reference materials necessary to maintain that correlation. The project will cover several types of refractories.

STATUS

The first material being studied is a porous calcium silicate. Work is still in progress.


ECU 115 050

PARTICIPANTS

Forschungsinstitut der Feuerfest-Industrie, D Hoogovens Groep Β.v., NL KernforschungsanLage JÜLichr D Didier Uerke AG, D Netzsch Geratebau GmbH, D British Ceramic Research Ltd, UK Morgan Materials Technology Ltd, UK GR Stein Refractories Ltd, UK National Physical Laboratory, UK Laboratoires de Réfractaires et Minerais, F Société Française de Céramique, F Studiecentrum voor Kernenergie, NL Universität Stuttgart, D Société Lorraine de Laminage Continu, F Commissariat à l'Energie Atomique, F Isover Saint-Gobain, F Forschungsinstitut für Uarmeschutz E.V. München, 0

105

PROJECT RM 2 7 0

REFERENCE MATERIAL FOR THE MEASUREMENT OF THE VISCOSITY OF HIGH TEMPERATURE SLAGS

PROJECT DEFINITION

It is important to know the viscosities of slags at high temperatures since it is one of the factors which controls their flow and heat transfer characteristics in steelmaking for continuous casting, etc.

RESULTS

After a great deal of experimentation a reference material based upon LijO, Alj03 and Si02 was produced with a viscosity in the range 1 - 1 0 Pa.s at temperatures between 1500 and 1100°C. A subsequent intercomparison, involving the use of graphite and molybdenum crucibles and bobs fabricated from platinum, showed the material to be chemically stable up to 1500°C. However, there was a wide dispersion (ca ± 50 %) in the results with the temperature for a particular viscosity varying by as much as 100°C for a viscosity of 1 Pa.s and 60°C for 5 Pa.s. In general the results for rotating crucible studies were lower than those obtained with rotating cylinder methods and those obtained with graphite contact materials were higher than those obtained when using molybdenum. A second intercomparison has now been completed and the results indicated that : (i) the overall scatter was reduced from ± 50 to ± 40 % by using a more

rigorous protocol for measurements; (ii) there was good agreement (ca ± 50 %) between the results obtained in

the four laboratories which used viscometers with molybdenum components;

(iii) there was good agreements between these results and those obtained in a viscometer using platinum components.

It was concluded that principal source of scatter was the small changes in chemical composition of the SRM resulting from its reaction with graphite components. This proposition was confirmed by the results of the chemical analysis of the post-measurement samples.


ECU 60 700

PARTICIPANTS

BUI i ton Research, NL British Gas London Research, UK CIREP, F CNRS, F Haake Hess-Technik GmbH, D Hoesch Stahl AG, D Hoogovens Ijnuiden, NL I^>erial College of Science and Technology, UK Hetallurgica GabH, D NPL, UK PTB, D

Standardised Tests

109

PROJECT MTR 079

INTERCOMPARISON OF MICRO-HARDNESS MEASUREMENTS

PROJECT DEFINITION

Hardness measurements are a comparatively quick and simple method of checking upon the quality of a material since the resistance to indentation is related to strength. As a result a number of hardness scales have been developed based upon the dimensions of the indentations made when diamonds or balls are pressed into the material under known loads. For small components, thin coatings, brittle materials or where the part may not be destroyed and the presence of a macro-indentation would be deleterious, so called micro-hardness techniques are applied upon the same principles but using much smaller indenters and loads (200 g). The purpose of the project was to determine the level of agreement on Vickers - micro - hardness measurements between the laboratories of the Community Member States and to examine the metrological problems.

RESULTS

The project was terminated 1990. Steel, copper and brass micro-hardness blocks were circulated to the participating laboratories. Measurements made by the pilot laboratory at the beginning and the end of the intercomparison showed that the hardnesses of the blocks were stable with time. The laboratories were requested to measure the diagonals of a series of indentations made by the pilot laboratory under undisclosed conditions and to make their own hardness determinations under specified conditions. The measurements of four laboratories of the lengths of identical indentations were in good agreement (discrepancies of the order of tenths of a micron) whilst one laboratory showed a systematic discrepancy over the whole range of lenghts. The reason may be that the line standard was not properly applied or the zero adjustment was faulty. One of the four laboratories made its own indentations using a sputtered indenter which had significant influence on its results. The remaining three laboratories were in good agreement (deviations in general less than 2 %.HV).


ECU 25 000

PARTICIPANTS

Bundesanstalt für Materialprüfung, D Dantest, DK IMGC, I NPA NRU, D Technische Universität Berlin, D.

110

PROJECT MTR 103

SOLDERABnJTY

PROJECT DEFINITION

Worldwide over 1012 soldered joints are made annually in the production of electronics for the consumer, industrial and military markets. About 1/3 of these are made within the Community. With increasing manufacturing automation the cost of identifying and replacing a defective component on a circuit board is often many times that of the actual component. It is thus cost-effective for manufacturers to apply goods-inwards acceptance checks on, say, 0.1 % of a component batch. Currently for solderability this is done visually on component's leads dipped into a pot of molten solder. Such qualitative tests lead to disputes. Attempts have therefore been made to develop so called wetting balances. The project aims to understand the effects of instrumental variables on the results obtained and to develop reference surfaces which will define a solderability scale reproducible to within 5 %.

RESULTS

Tests with wetting balances from the three European manufacturers showed the importance of the thermal mass of the sample holder, the solder bath size and exposed surface area and the timings used when performing solderability determinations. By minor modifications to the instruments results agreeing to better than ± 10 % were obtained in one laboratory. An intercomparison was then performed between the three manufacturers using copper specimens, pre-treatment kits, solder and flux provided by the coordinating laboratory. When using benzotriazole passivation and the instrumental modifications suggested, the laboratories were able to achieve the overall goal of a repeatability on any part of the solderability curve to within ± 8 %, a reproducibility of the mean of ± 5 % and a reproducibility of a single measurement of ± 15 % or 0.3 sec. By comparison the participants found some difficulty in using the sulphurization technique given in the AFNOR standard NF C90-551. Although they were in general able to achieve a similar repeatability as obtained with BTA the between laboratory reproducibility was inferior. Work is continuing to develop an improved reference surfaces which define a complete solderability scale.


ECU 91 400

PARTICIPANTS

6EC Research, UK National Physical Laboratory, UK AEG Telefunken, D Netronelec, F STC Technology, UK S6S-Thonson, I Sienens, D nu l t icore Solders L td , UK Radiometer A/S, DK Nederlands Phi l ips Bedri jven, NL

I l l

PROJECT MTR 144

DEVELOPMENT OF AN ABRASION TEST ON PLASTIC SPECTACLE LENSES

PROJECT DEFINITION

About 45% of all ophthalmic lenses are made from plastic materials (CR39 or polycarbonate) and this percentage is growing all over the world. The reason for this is the convenient combination of properties such as optical homogeneity, low mass, low fragility, etc.. The optical quality of plastic lenses is comparable with that of glass lenses, however the low abrasion resistance of their surface is a disturbing factor, and great efforts are being made to harden the surfaces by appropriate coatings. The abrasion process is very complex and difficult to be reproduced by a simple procedure: before this project no test method existed suitable to the needs of the developing engineer. Europe is a producer of high quality lenses, the Far East fabricating lower quality but cheaper products. The European industry through its professional organization (EUROM) agreed to support financially the development of a test method to consistently measure and characterize this commercially very important quality factor.

RESULTS

A test method has been developed that matches the complex abrasive effects induced by actual everyday use. The work carried out included

the development of a special cleaning system, of an optical system for the measurement of scattered light and of a suitable abrasive mixture easy to be standardized; a field test; the controlled abrasion and inspection of a great number of different lenses by different manufacturers.

A draft of a standard based on the results of the work has been proposed to CEN/TC 170/WG 2.


ECU 70 000

PARTICIPANTS

EUROH - European federation of precision aechanicat and optical industries Institut für Augenoptik, AaLen, D.

112

PROJECT MTR 145

INTERCOMPARISON OF ABRASIVE TESTING FOR SYNTHETIC FOOTWEAR MATERIALS

PROJECT DEFINITION

It has been known for some time that tests done on polyurethane sole materials had accepted products in Greece which were later refused in Germany. Similarly Italian shoes were refused in Germany and England. Finally, examples exist of shoes from the Far East being imported into the Netherlands, which appear to be less demanding on testing, and then refused in the UK and in France.

The intercomparison was to cover the following properties

apparent density tensile strength and elongation at rupture flexing life tear strength abrasion

The tests were made on each of three qualities of foam polyether and of polyurethane of three densities.

RESULTS

The determination of the apparent density shows no problem. For tensile strength and tear strength, the results were spread in a range of ± 30%. After the specimens were treated by hydrolysis, the dispersion of results was sometimes much higher. For the flexing life tests and the abrasion tests, the dispersion of results was higher. The major observation from this intercomparison is that a number of laboratories did not follow the test conditions requested in the standardised method they were applying. It was also observed that the testing procedure e.g. for flexing life and abrasion, was not sufficiently described in the existing standardised methods.


ECU 26 000

PARTICIPANTS

Prüf- und Forschungsinstitut für die Schuhherstellung, D Inescop, E Centre Technique Cuir, F SATRA House, UK Hellenic Leather Center S.A., GR CIHAC (Vigevano), I TNO, NL Centro Tecnológico do Calcado, Ρ

113

PROJECT MTR 147

DETERMINATION OF THE Κ COEFFICIENT OF REFRIGERATED TRUCKS & CONTAINERS

PROJECT DEFINITION

The testing of refrigerated trucks and containers is done according to recommendations of ATP (Agreement on the Transport of Perishable Goods) which was taken under the umbrella of the Economic Committee for Europe (UN). Not all testing stations recognize each other and this is of course a source of difficulties. The major testing stations of Europe agreed that this situation could be improved by an intercomparison. A container was circulated to each station and the tests were witnessed by an expert of Lloyds Register who made his own report on the measurements. Each station produced a report. The observer collected all reports and produced a synthesis report. The tests were done by adjusting the power of a heat source inside a container to maintain a constant temperature difference between the inside wall and the outside wall. The outside is cooled with cold air. The Κ coefficient is the power divided by the container surface and the temperature difference.

RESULTS

The results have shown that some outlying results were caused by inappropriate calibration of the thermocouples or by neglecting the power losses in the cables. They also showed that it was desirable to select a rather low internal air circulation and a temperature differential of 30K. The intercomparison also provided the basis for the participants to adopt new specifications for the tests so that the level of uncertainty would not be higher than 5 %, while at present differences can be as high as 10 %. It of course also provides increased confidence in the capabilities of the different participants.


ECU 37 000

PARTICIPANTS

Cenagref, FR TUV Bayern, D Sprenger Instituut, NL ITV de Madrid, E CENAGREF, FR V. Politécnica Hadrid, E Refrigerate Vehicle Test Station, UK Rijksdienst voor het Uegverkeer, NL CNR Istituto perla Técnica del Freddo, I TUV, D Lloyd's Register of Shipping, UK

114

PROJECT MTR 146

MEASUREMENT OF THE PRESSURE EXERTED BY ELASTIC MEDICAL STOCKINGS

PROJECT DEFINITION

In the various European countries the pressure exerted on the leg by elastic stockings is measured according to different test methods and procedures. Studies had shown significant discrepancies among those methods. The aim of this intercomparison was not to promote, nor to criticise any of the methods used at different national test institutes, but rather to ensure a common statement of results. To this end two series of parallel tests were conducted, one employing the normal conditions used in each institute, and one with normalised preconditioning of the specimen. In order to ensure that the broadest area of products were examined, the specimens to be tested were prepared in three different Member States (UK, F, D) and belonged to three different compression classes, each defined as customary in its country of manufacturing.

RESULTS

The project clearly showed that the different test methods were effectively measuring slightly different properties. Although the results from some methods more or less agreed it was clear that a single method was required if medical practioners were to be able to compare the pressure exerted by different stockings. All participants therefore met and evaluated each others methods in a single laboratory over a period of two days.

Whilst the fully automated Hohenstein method clearly gave the best repeatability its cost was considered to make it unsuitable for widespread use in an industry characterized by small producers. Finally the experts agreed that the French method based upon the use of a commonly available tensile testing should be recommended for standardization as a reference method.


ECU 55 900

PARTICIPANTS

ITF Lyon, F CentexbeL, Β Hatra, UK Hohenstein, D Dept. CLin. Majadahonda, E TNO, NL

115

PROJECT MTR 149

INTERCOMPARISON OF TENSILE & FLEXURAL FATIGUE TESTS ON UNIDIRECTIONAL REINFORCED POLYMER MATRIX COMPOSITES

PROJECT DEFINITION

Fibre reinforced polymer matrix composites, originally developed for aeronautic purposes, have a unique combination of high strength, stiffness, lightness and corrosion resistance. Today they are also used structurally in a wide range of industries, most notably boat, ship and offshore construction, transport and chemical engineering. As international trade in them develops it has become apparent that test procedures developed locally upon the basis of particular applications are insufficient. Initiatives are therefore in hand to produce written test standards agree but these are being inhibited by the lack of knowledge of the effects of test variables upon results. The situation is further complicated by the fact that, unlike conventional materials, fibre composites do not exhibit a well defined failure. Indeed they may fail locally by matrix cracking, debonding or fibre fracture during the first phase of a test but since the fault does not propagate or further deformation takes place elsewhere, the part may still be serviceable. The project is therefore to investigate the effects of tensile and flexural test variables on the measured properties of a range of common unidirectional reinforced polymer matrix composites and to establish reproducible failure criteria.

STATUS

Homogeneous batches of glass, carbon and aramid fibre reinforced polymer matrix composites have been purchased and distributed to intercomparison participants for tensile and flexural testing according to well defined guidelines. Participants are also determining the effects of systematically varying individual test parameters such as specimen design, strain rate etc.


ECU 23 000 for materials.

PARTICIPANTS

The project is being run as part of the VAHAS in i t ia t ive by the National. Physical Laboratory, UK and the University of Conpiegne, F. I t is open to participation from a l l Member States and laboratories in the USA, Canada and Japan.

116

PROJECT MTR 151

WATER PERMEATION IN BUILDING MATERIALS

PROJECT DEFINITION

One of the major causes of damage to buildings is the ingress of water or humidity. This project therefore examined the method for determining the water permeation in low-density building materials such as extruded polystyrene and agglomerated (vermiculite) particle board, that are commonly used for thermal insulation. All the laboratories used the same basic gravimetric technique in which the sample is sealed into the mouth of an impermeable "cup", containing either desiccant or a salt solution, which is then placed in an environmental chamber. A constant vapour pressure difference is maintained across the sample and the water vapour permeability of the material is calculated from the steady decrease, or increase, in the weight of the cup.

RESULTS

Excluding outliers, for which explanations could be postulated, the range of the measured water vapour permeabilities remained very large ( ± 1 5 % for the polystyrene and ± 20 % for the particle board) despite the fact that the test conditions were rigidly defined. An improvement of the situation would appear to necessitate modifications to the currently used design of the apparatus.


ECU 70 000

PARTICIPANTS

Hin is t , de Obras Publicas y Urbanismo, E TNO - IBBC, NL Centre Scient. & Techn. du Bâtiment, F Univ. of Strathclyde, UK Centre Expérin. de rech, et d'études du Bât.S Trav. Publ ics, F Techn. Univ. of Denmark, OK K.U.L., Leuven, Β Laboratorio Nacional de Engenheria Civil, Ρ Staatliches Material Prufungsamt, 0 MTCB/CSTC, Β Forsschungsinstit. für Uärmeschitz e.V., München, D E0LAS, I University of Lund, S

117

PROJECT MTR 152

TESTING OF THE WATER TIGHTNESS OF WINDOWS

PROJECT DEFINITION

Windows are tested for mechanical resistance, air tightness and water tightness.

There is a CEN standard which described three methods. The preferred method is only

used in two countries. In Germany, the laboratory of Rosenheim which had initially developed the method has now abandoned it because the stability of the nozzles is apparently creating too many problems. The other CEN methods are not used as described. In France, in particular, the water spray is not directed perpendicular to the window because too many windows are considered to be bad, but it is inclined 45° downwards. The project will consist of an intercomparison in which two windows of different design will be tested for water tightness by the participants.

STATUS

In progress.



PARTICIPANTS

Min. de Obras Publicas y Urbanismo, ES Building Research Establishment, UK Centre Technique du Bois et de L'ameublement, FR Centre Scient, et Techn. de la Construction, Β Inst, für Fenstertechnik e.V., D EOLAS, IRL Danish Building Research I n s t i t u t e , DK TNO - IB8C, NL Laboratorio Nacional de Engenharia C i v i l , Ρ ETEN, GR

118

PROJECT MTR 153

THE DETERMINATION OF YARN TWIST

PROJECT DEFINITION

The amount of twist imparted to a yarn during the spinning process determines not only the strength, size etc of the yarn but also its appearance. Thus if the twist in nominally identical yarns varies from bobbin to bobbin when the yarn is woven the eye sees the difference and the material is considered faulty. For this reason both the spinning and weaving sides of the textile industry place great emphasis on the determination of the twist in a yarn by including tolerances in contract conditions. With regard to written standards it appears that for ring spun yarns there are adequate national and international (ISO) standards. In the case of yarns produced by the so-called open end spinning process (DE) however, there is no approved method. There is therefore a need for prestandardization work in the case of OE yarns to allow a twist measurement method acceptable to all to be agreed. The participants will test three types of yam by the so called twist untwist method and will then compare results.

RESULTS

ITF Mulhouse has fabricated and tested 18 batches of threads, including : 1 3 materials (VIS/CO 67%/33%; PES/CO 67%/33%; PES 100%) 2 2 titles (20 tex and 50 tex) 3 3 twist coefficients (115, 125, 135). The results of the tests indicate important differences in the measured twist values from the actual ones: a 40-45% for VIS/CO, using the simple twist/untwist method; b 10-15% for VIS/CO, 15-30% for PES, 20-30% for PES/CO, using the method

with double counter try (NF G 07 - 09). It was concluded from this preliminary work that no method is as yet sufficiently developed to be proposed as a standard and thus the intercomparison will not be carried out.


ECU 39 500

PARTICIPANTS

Inst, für Textile und Verfahrenstsechnik, D Dansk BekLaednings og Textil Institut, DK Centre de Recherches Textiles de Mulhouse, F Laborat. de Ensayos e Investigaciones Textiles del Acondicionamiento Terrasense LEITAT, E Ministerio de Comercio e Turismo, Ρ Vezelinstituut TNO, NL Laborat. Central du Minist, des Affaires Economiques, Β Instituto dos Texteis, Ρ Ε.Ν.S.Ι.T.M., F International Institute for Cotton, UK Instituto "0. Rivetti" del CNR, I

119

PROJECT MTR 163

INTERCOMPARISON ON THE LOCAL APPROACH TO FRACTURE

PROJECT DEFINITION

Approximately 30 laboratories will participate in an intercomparison which consists of two parts, one experimental and the other computational. In the experimental part each laboratory will perform 6 tests at 100 °C and 9 tests at -196 °C on each of 2 materials to determine their ductile and cleavage fracture characteristics using a defined specimen geometry and test procedure. In essence the test consists of the accurate and continuous measurement of the minimum section of the specimen during deformation. In the computational part of the exercise the laboratories will use the same computer codes to treat a set of data provided by the coordinating laboratory. In this way it will be possible to identify the origins of the major difference in the results submitted by the participants.

STATUS

The theoretical and experimental parts of the intercomparison were completed in Spring 1992 showing a very large measure of agreement. The report will be available in Autumn 1992.



PARTICIPANTS

Fraoetoee/Franasoft/Unirec, F UTC/Aerospatiale Coinpiègne, F CEA Sac Lay, F IRSID St-Gereain-en-Laye, F E.D.F. Höret s/Loing, F EcoLe des Mines/Centre des Matériaux, F CEN/SCK, Β Rolls-Royce g Associated Ltd, UK ECN/Delft University Petten/Delft, NL «PA Stuttgart, D Franhoffer Institut, OK Sieaens/KUU, D BAH Berlin, 0 ENEL Hilan, I Inasaet San Sebastien, E Sinei Trondheim, Ν SP/National Testing Institute, S

120

PROJECT MTR 164

FIRE TESTING

PROJECT DEFINITION

The first part of the project investigated calibration methods for transducers measuring radiant heat flux. At SP calibrations were performed using a black-body cavity as a radiation source. At FRS calibrations were performed against a secondary standard radiant heat flux meter that was traceable to an absolute method of measuring radiant heat flux based on the temperature rise of a copper block as a function of time.

The second part of the project investigated the use of plate thermometers to measure the temperature to which construction products are subjected during fire resistance tests in furnaces of various designs. Plate thermometers have a much larger surface area than ordinary thermocouples and it had been suggested that they would ensure that furnaces of different designs would expose specimens to identical heating conditions. Two tests were carried out in four laboratories. In the first test the furnaces temperature was controlled using ordinary ISO standard thermocouples and in the second with plate thermometers.

RESULTS

Calibrations of radiant heat flux meters using the methods used by SP and FRS produced systematic differences of upto 8 %. The reasons for these differences are not clear and are still being discussed.

The differences in temperature between the different fire resistance furnaces were considerably less when the furnaces were controlled by plate thermometers instead of thermocouples. After 45 minutes, for example, the differences were less than 10°C instead of more than 100°C.


ECU 64 000

PARTICIPANTS

Statens Provensanstalt, S Fire Research Station, UK Bundesanstalt für Materialforschung und Prüfung, D Centre Scientifique et Technique du Bâtiment, F Centro Studi ed Esperienze, I Loss Prevention Counci L, UK

121

PROJECT MTR 167

COLD BENDING TEST FOR ROOFING MATERIALS

PROJECT DEFINITION

The major performance characteristics required from roofing materials are dimensional stability, resistance to flow, tensile strength, flexibility at low temperatures. While there is reasonable agreement among testing laboratories for the three first properties, different methods were still in use for the cold bending test leading to discrepancies of ± 6 °C between laboratories for a test at about 20 °C. The task of the contractor was to improve the method initially developed by himself, to make it more reliable.

RESULTS

The tests on at least 10 different materials have shown that the speed of deformation was not very critical, that the diameters of the mandrel on which specimens are bent should not be too small C30 mm is preferred) and that results are more consistent when they cylinders of the bending device are spring-loaded. A limited round robin involving three laboratories indicated that the differences between laboratories could be reduced to about ± 3 CC -with the improved method. The final report was offered to CEN for the preparation of the standard.


ECU 46 000

PARTICIPANTS

BDA Keurings-en Certificeringsinstituut BV, NL Bundesanstalt für MateriaLforschung und- prüfung, 0 Centre Scientifique et Technique du Bätinent, F

122

PROJECT MTR 171

TIMBER CALIBRATrON PLANKS

PROJECT DEFINITION

Timber is an important construction material frequently used in the whole of Europe. Whilst it is an environment-friendly material its basic problem is the variation in its mechanical properties. Each individual piece of timber must therefore be graded in order to ensure that it can be used safely in construction. Timber can be graded by visually looking at defects and applying certain criteria. Automatic grading is much more effective saving time, money and resources, the potential annual saving for Europe being estimated at 0.5 - 1.5 billion ECU. The majority of timber stress grading machines test the timber by measuring the stiffness at small increments along the length Cbending type). This being a dynamic process it became increasingly obvious that the calibration of grading machines must be done dynamically in order to correctly describe their performances. Although about 150 bending type machines are already being used appropriate calibration procedures and planks do not yet exist. The aim of the project is therefore to develop appropriate calibration procedures and calibration planks which would permit all parties involved to operate to the same level of acceptance. Based on the findings of the project certified planks could be made available to all interested parties.

STATUS

In progress.


ECU 274 000

PARTICIPANTS

Building Research Establishment, UK Centre Technique de l'Industrie du Bois, Β EOLAS, IRL Ludwig-Haximilians Un ivers i tä t , D The Swedish I n s t i t u t e for Wood Technology Research, S The TechnicaL Research Centre of Finland, SF.

123

PROJECT MTR 175

CHARACTERIZATION OF AIR BLAST SPRAYERS FOR SPRAYING PESTICIDES IN ORCHARDS AND VINEYARDS

PROJECT DEFINITION

The performance of air blast sprayers used to treat orchard crops, vines and hops is presently the cause of considerable concern because of the risk of environmental contamination in the application of pesticides. In this project the methods of characterization of such sprayers will be intercompared at six different European institutes. The study is expected to provide manufacturers and government agencies with a consistent body of sound experimental evidence to allow the definition of a method for the specification of sprayers performance that will be later submitted to international standardization committees.

STATUS



ECU 97 900

PARTICIPANTS

AFRC Engineering Chemical Application Group, UK Biologische Bundesanstalt für Land und Forstwirstchaft Fachgruppe für Anwendungstechnik, D Centre National du Machinisme Agricole du Génie Rural des Eaux et des Forêts, F Estación de Mecánica Agrícola, E Istituto di Meccanica Agraria, I Instituut voor Mechanisatie Arbeid en Gebouwen, NL.

124

PROJECT MTR 178

THE QUALIFICATION TESTING OF HEATING BOILERS THERMAL EFFICIENCY & NO, EMISSION

PROJECT DEFINITION

The 1990 directive on gas appliances obliges Member States to

accept for any given design of boiler the efficiency rating on a scale with 2 % intervals as determined by a notified laboratory from another Member State; ensure that boilers conform to the provisions of the future directive on minimum energy requirements currently being drafted by DG XVII.

To this end CEN has a mandate from the Commission to produce standards specifying the efficiency and emission requirements for central heating boilers and the methods to be used for demonstrating conformance to these requirements. Intercomparisons have shown that the proposed test methods lead to unacceptable differences between the results of different laboratories when determining both thermal efficiencies and NO, emission values. The purpose of the project is to determine the origin of these differences.

STATUS

Started 1991, in progress.


ECU 7 1 5 0

PARTICIPANTS

Association Royale des Gaziers Belges, Β British Gas, UK CETIAT, F Danish Gas Technology Centre, DK DTI, DK Gaswfirme Institut, D Gaz de France, F Italgas, I Merogaz, Β Swedish National. Testing & Research Insitute, S TÜV Rheinland, D Universi té de Liège, Β VEG-Gasinstituut, NL.

125

PROJECT MTR 179

INTERNAL PRESSURE TESTING OF TUBES

PROJECT DEFINITION

In the power generation, nuclear, chemical and petrochemical industries plants designed upon the basis of uniaxial creep data are thought to be inadequate because

of the many assumptions made in the prediction of component behaviour and hence lifetime from uniaxial specimen data; the anisotropy of materials' properties; design related discontinuities (e.g. welds, changes in section) cannot be incorporated in uniaxial tests differences in surface to volume ratios between uniaxial specimens and real components.

By using component testing designers can reduce plant capital costs and preventative maintenance whilst at the same time improving heat transfer efficiencies.

The purpose of the project is to examine the effect of variables on the test method in order that recommendations for a standardised test can be made.

STATUS

In progress.


ECU 240 000

PARTICIPANTS

AEA Dounreay, UK Babcock, UK CEA Cararache, F ERA Techno Cogy, UK Interatoa, D JRC Petten. KFA Jülich, D MPA Stuttgart, D Coordinator: National. Engineering Laboratory, UK Powergen, UK Stein Industrie, F TNO, NL Université Besançon, F VTT Technical. Research Centre, SF

126

PROJECT MTR 196

FIRE TESTING OF UPHOLSTERED FURNITURE

PROJECT DEFINITION

A draft directive on the fire behaviour of upholstered furniture is currently being prepared, the aim of which is to reduce the fire hazards of upholstered furniture in the home and in public places. There is little disagreement over the test methods to be used for the First Essential Requirement which will require that furniture should not ignite in the first place when exposed to typical ignition sources such as a cigarette or burning match. The problem lies with the Second Essential Requirement of the draft Directive which is concerned with what happens after the furniture has started to bum. The text in the draft Directive says that the heat, smoke and toxic gases produced should not endanger the lives or the well-being of exposed people during a period long enough for them to be able to escape. The project will establish test methods to implement the Second Essential Requirement by evaluating the post-ignition fire behaviour of upholstered furniture on a sound scientific basis without discriminating against any particular products.

STATUS

In progress.


ECU 1 500 000 (estimated)

PARTICIPANTS

Major fire testing laboratories from all Member States are expected to participate.

127

PROJECT RM 253

REFERENCE MATERIAL FOR THE VERIFICATION OF CREEP TESTING MACHINES

PROJECT DEFINITION

Creep is the continuous plastic deformation of a material under stress, generally at high temperatures, which will eventually lead to a component or structure becoming so weakened that it is unable to support the applied load. In view of the slowness of the process creep testing is expensive. It is therefore important that the test assembly be shown to be functioning correctly and is not, for example, misaligned so that the specimen experiences bending as well as tensile forces. Initially this may be done by considering each of the component parts of the assembly in turn. Eventually, however, it will be necessary to demonstrate that the entire assembly is functioning correctly and gives reproducible results. This may be accomplished by use of a reference material with a well documented behaviour over a relatively short time period.

STATUS

A number of materials were examined before a nickel based solid solution allow was found which gave a highly reproducible creep curve of sufficient length within a time of 500 hours at 600 to 700°C. A special melt of this alloy was prepared and its homogeneity checked. Following an intercomparison of creep measurements the material was certified at the beginning of 1990, the parameters being the time taken to accumulate strains of 2 and 4 % together with the minimum creep rate at 400 hours, calculated from the best fit straight line between 350 and 450 hours of testing. In addition the material was examined for use as a reference material for high temperature tensile testing but the presence of serrated yielding in the range 400 - 600°C made it unsuitable.


ECU 103 600

PARTICIPANTS

British Steel, UK Siemens AG, 0 Haterialprüfungsanstalt, 0 Metaalinstituut, NL Central Electricity Research Lab, UK BAH, D CEN Sac lay, F NPL, UK Centre Recherches Métallurgiques, Β Technische Hoschschule, D Electricité de France, F Trinity College, IRL

128

PROJECT RM 269

INTERCOMPARISON OF LOW CYCLE FATIGUE MEASUREMENTS

PROJECT DEFINITION

Structures and parts are normally designed so that their in-service deformation is solely elastic and at such a level as to not induce fatigue failure. However, for advanced applications such as gas turbines, electric power plants and nuclear reactors, it becomes impossible to avoid repeatedly stressing parts beyond their elastic limit during critical phases of operation such as start up and shut down. As a result fatigue lives for materials are reduced from many millions of cycles in the elastic range to thousands in the plastic range. Low cycle fatigue tests which should simulate in-service plastic stressing are not standardized. The purpose of the project is to provide a clear understanding of the effects of test parameters in order that the standardization process may proceed upon a sound basis.

STATUS

Four materials, 2 strain softening, 1 strain hardening and 1 strain stable were purchased and, following homogeneity testing, were distributed to the participants. Each of these made measurements in accordance with a well defined set of guidelines using their normal design of specimen and types of extensometers plus a range of failure criteria. The results of the intercomparison show that the differences between laboratories are frequently greater than a factor of 10 whilst the variations within any given laboratory are significantly less. Although the scatter depends of a variety of parameters it appears that the use of ridged specimens leads to much reduced lifetime. Excluding the results of such specimens, the scatter remains unacceptable for reasons which were not resolved by the intercomparison. However, subsequent research suggests that even small amounts of specimen misalignment could account for it. Experiments are therefore being undertaken to confirm this.


ECU 344 600

PARTICIPANTS

University of Bristol, UK UNIREC, F UKAEA, UK Rolls-Royce Ltd, UK Brown Boveri g Co, D BAH, D Metaalinstituut TNO, NL JRC Petten CEAT, F CISE Spa, I ERA Technology Ltd, UK Electricité de France, F NPL, UK CRM, Β CEGB, UK Institute of Materials Science, TH Darastadt 0

In addition the inclusion of this project in the VAHAS initiative has resulted in measurements in 12 laboratories in Japan.

CHEMICAL ANALYSIS

Food Control

133

PROJECT RM 226

MYCOTOXIN CALIBRANTS

PROJECT DEFINITION

Mycotoxins are the general class of toxic compounds produced by fungi and occur widely in food and other agricultural products.

Reliable determination of these compounds depends upon the availability of calibrants of proven identity and certified composition. Although for many of the more important compounds, suitable calibrants are available there are a number which present difficulties.

The objective is to provide calibrant solutions of those mycotoxins for which there is a broad European need and which are not available at an acceptable level of reliability elsewhere. The work will focus on aflatoxin M„ ochratoxin-A and fumonisin FI?! and FB2.

STATUS

Initial stability studies have been successfully completed for the ochratoxin-A solution. The preparation of a batch of ampouled fumonisin solutions is in progress. The preparation of a batch of aflatoxin M¡ in chloroform is finished by the RTVM Bilthoven NL. Certification of the aflatoxin M, solution involving 5 laboratories will be started in 1992.


ECU 150 000 (Estimated)

PARTICIPANTS

Istituto Tossine e Micotossine da Parassiti Vegetali, Ban', I Leatherhead Food R.A., Surrey, UK -Ministry of Agriculture, Food and Fisheries (HAFF) Food Science Laboratory, Norwich, UK RHM Research, High Wycombe, UK Rijksinstituut voor Volksgezondheid en Milieu Hygiene (RIVM) Bilthoven, NL Royal Veterinay & Agricultural University, Institute of Hygiene & Microbiology, Copenhagen, DK.

134

PROJECT RM 328

AFLATOXINB, IN EDIBLE PEANUTS RMs

PROJECT DEFINITION

Aflatoxins are potent carcinogens and may occur as a consequence of fungal attack in certain food. There is therefore extensive monitoring by food control laboratories and by the food industry to ensure that vulnerable products such as peanuts and figs satisfy national requirements. Most Member States impose limits of either 5 μg/kg of anatoxin B! or 10 Mg/kg of total aflatoxin (B,+B2+G1+G2). Immunological assays are increasingly used for rapid screening and commercial kits require validation by means of reference materials. The objective of the project was to provide appropriate CRMs.

RESULTS

Two peanut butter RMs were certified for their individual and total aflatoxin contents. The certified contents are as follows :

RM

N°

385

401

Aflatoxin content in jig/kg

B,

7.0 + 0.8

< 0.2

B2

1.1 ± 0.2

< 0.1

G,

1.7 + 0.3

< 0.1

G2

0.3 ± 0.1

< 0.1

Total

10.1 ± 0.9

< 0.1

Certification measurements were made by 9 laboratories using a variety of extraction and clean-up procedures with HPLC as the final step.

The project is terminated: report EUR 13 901 (1991).


ECU 40 899

PARTICIPANTS

Istituto Supen'ore di Sanità, Roma, I Keuringsdienst van Waren, Rotterdam, UK Laboratoire Central de la Repression des Fraudes, Massy, F. Laboratory of the Government Chemist, Teddington, UK Leatherhead Food Research Association, Leatherhead, UK MAFF Food Science Laboratory, Norwich, UK Rijksinstituut voor Volksgezondheid en Milieuhygiene (RIVM), Bilthoven, NL Royal Veterinary and Agricultural University, Copenhagen, DK TNO-CIVO Institutes, Zeist, NL

135

PROJECT RM 367

DEOXYNIVALENOL (DON) IN WHEAT AND MAIZE

PROJECT DEFINITION

DON is a fungal toxin particularly associated with cereals. In extreme cases, DON in mouldy grain has caused serious human illness. The presence of DON in grain may lead to feed-refusal by farm animals. Contamination by DON is of concern for crops grown in areas whose climates favour mould formation, notably, north-America and northern Europe. Discrepancies of two orders of magnitude in the results of laboratories have been recorded in recent international studies. The objective of the project was to improve the reliability of the methods and to provide blank and contaminated maize and wheat RMs.

RESULTS

Four preliminary intercomparisons of methods have been made to reduce the major sources of errors. A pair of wheat and a pair of maize reference materials have been prepared. They consist of naturally contaminated samples having low levels close to the recommended (voluntary) action limits, and samples having low levels to provide a means of checking analytical background and recovery efficiency. Certification measurements were made by 8 laboratories using a variety of extraction and clean-up procedures with HPLC as the final step. The certified values are as follow :

RM

377

378

379

396

Sample

maize flour "low level"

maize flour 'high level'

wheat flour "high level"

wheat flour "low level"

DON content mg/g

< 0.05

0.43 ± 0.04

0.67 ± 0.02

< 0.05

The project is terminated (EUR report in preparation).

CONTRIBUTIONOF THE COMMISSION

ECU 103 431

PARTICIPANTS

Bayerische Landesanstalt für Tierzucht, Grub/Poing, 0 - CIV0-TN0, Zeist, NL - Istituto Tossine et Hicotossine da Parassiti Vegetali, Bari, I - Keuringsdienst van Uaren voor het Gebied Rotterdam, Rotterdam, NL - HAFF, Norwich, UK - RIKILT, Uageningen, NL - RIVH, Bilthoven, NL - RHH Research Ltd., Bucks, UK - Royal Veterinary and Agricultural University, Copenhagen, OK - Unilever Research, Bedfordshire, UK - Universität Hünchen, Hünchen, D.

136

PROJECT RM 392

IMPROVEMENT IN THE DETERMINATION OF OCHRATOXIN-A IN FARM ANIMALS, PRODUCTS AND CEREALS

PROJECT DEFINITION

Ochratoxin A (OA), a mycotoxin, is a suspect kidney carcinogen and has been shown to have teratogenic activity. Its occurrence as a consequence of fungal attack in foods from plant origin such as cereals and beans is well known and widely reported in the scientific literature. The presence of OA in edible animal tissues and particularly in pig kidneys, as a result of consumption of contaminated feed has been demonstrated in Denmark and Sweden. Recently, individual Member States have begun to set up tolerance limits. A guideline for cereals exists in France and in the UK an industrial limit for cereals is used. The objective of the project is to improve the reliability of the methods to determine OA and to provide "blank" and naturally contaminated wheat and lyophilised pig kidney RMs.

STATUS

A pair of wheat reference materials have been prepared. They consist of naturally contaminated samples containing the toxin at levels close to the recommended (voluntary) action limits, and samples having low levels to provide a means of checking analytical background and recovery efficiency.

An intercomparison study with about 30 European laboratories was carried out. The results show that the major difficulties arise from the clean-up step of the method used and consequently, the 2nd intercomparison will concentrate on this aspect of the procedure.



PARTICIPANTS

Bayerische Landesanstalt für Tierzucht, Grub/Poing, D Bundesanstalt für Fleischforschung, Kulmbach, D Bundesgesundheitsamt, Berlin, D Centro de Investigación y Control de Calidad ( C I . C C ) , Madrid, E Centro Nacional de Alimentación y Nutrición, Madrid, E Danish Heat Research Institute, Roskilde, DK Department of Microbiology, Royal Dental College, Copenhagen, DK Institut für Med. Mikrobiologie, U-München, D Istituto Superiore di Sanità, Roma, I Ist i tuto Toss i ne e M i co toss i ne da Parasit!" Vegetal i, CNR, Bari, I Keuringsdienst van Uaren voor het Gebied, Rotterdam, NL Laboratoire Hunicipal de Bordeaux, Bordeaux, F Laboratorio Nacional de Engenharia e Tecnología Industrial, Lisboa, Ρ Laboratory of the Government Chemist, Middlesex, UK Leatherhead Food Research Association, Surrey, UK Le Laboratoire de La Répression des Fraudes de Rennes, Rennes, F Ministry of Agriculture, Food and Fisheries (MAFF), Food Science Laboratory, Norwich, UK RHH Research Ltd., Bucks, UK Rhone Poulenc Diagnostics, Glasgow, UK Rijksinstituut vor Volksgezondheid en Milieu Hygiene (RIVM), Bilthoven, NL Rijkskwaliteïtinstituut voor Land- en Tuinbouwprodukten (RIKILT), Wageningen, NL Royal Veterinary and Agricultural University, Institute of Hygiene and Microbiology, Copenhagen, DK State Laboratory, Dublin, IRL TN0, Biotechnology and Chemistry Institute, Zeist, NL Unilever Research, Bedfordshire, UK Universidad Complutense, Madrid, E.

137

PROJECT RM 276

DIARRHEIC SHELLFISH POISONING (DSP)

PROJECT DEFINITION

DSP toxins are produced by marine algae and are accumulated by shellfish, particularly by mussels. More than five different DSP toxins have been identified so far, but two of them are predominant in Europe (okadaic acid and DTX-1). The consumption of DSP contaminated mussels can cause gastrointestinal disorder. DSP toxins are also considered to be potent tumour promoters. Contamination of shellfish by DSP occurs regularly in Europe and most Community Countries operate DSP monitoring schemes on imports of shellfish and at production sites. The European Community (DG VI - Agricultural Services) is preparing a Directive (COM (89) 645 final) which will establish limits of DSP toxins in shellfish. The method for DSP determination is normally the non-specific mouse/rat bioassay and, to a lesser extent, chemical analysis by HPLC. Development of chemical methods is being hampered by the interference of organic acids with the determination of DSP toxins and by the lack of pure toxins. The aim is to provide samples of individual toxins, to develop a candidate official method and to raise the reliability of the determination by European laboratories.

STATUS

Significant quantities of okadaic acid have been produced from cultures of algae. Chromatographic methods for routine monitoring and absolute identification of DSP toxins are being developed. Solutions of okadaic acid, contaminated mussels and mussel extracts for intercomparisons are being prepared. An intercomparison involving some 20 laboratories to assess performance of HPLC methods will be completed in 1992.



PARTICIPANTS

Agricultural University, Copenhagen, DK CNEVA, Paris, F Fisheries Research Center, Dublin, IRL IEO, Vigo, E IFREHER, Hantes, F INS, Lisboa, Ρ Institut für Veterinärmedizin des Bundesgesundheitsamtes, Berlin, D ISS, Roma, I Ludwig MaximiUians Universität, München, D HAFF, Burnham on Crough, UK Ministerio de Sanidad, Majadahonda, Ε RIKILT, Uagengingen, NL RIV0, Ijmuiden, NL Staatliches Veterinäruntersuchungsamt für Fische, Cuxhaven-F, D ULB, Bruxelles, Β Universidad de Santiago, Lugo, Ε Universidad de Vigo, Ε Universität Hohenheim, Stuttgart, 0 University of Göteborg, S.

138

PROJECT RM 422

PARALYTIC SHELLFISH POISONING (PSP)

PROJECT DEFINITION

PSP toxins are produced by marine algae and are accumulated by shellfish. They are of particular concern in mussels. Eighteen different P^P toxins have been identified. Contamination of shellfish by PSP occurs regularly in Europe and in extreme cases can be fatal. Most Community Countries operate PSP monitoring schemes on imports of shellfish and at production sites. The European Community (DG VI - Agricultural Services) is preparing a Directive (COM (89) 645 final) which will establish limits of PSP toxins in shellfish. The method for PSP determination is normally the mouse bioassay and, to a lesser extent, chemical analysis by HPLC. Development of chemical methods is being hampered by the lack of pure toxins. Apart from the undesirability of animal testing, biological methods do not permit identification of the individual toxins and generally have low reproducibility. They are also unsuitable for studies to ascertain the effect of external factors (eg. Temperature, light, N03, etc.) on growth and toxin production of algae. The objectives of the project are to improve chemical methods of analysis and to develop reference calibrants and mussel RMs.

STATUS

Individual PSP toxins are being extracted and fractionated from contaminated mussels and methods for routine monitoring and absolute identification of PSP toxins are being developed. Solutions of PSP toxins, contaminated mussels and mussel extracts for intercomparisons are being prepared. An intercomparison involving some 15 laboratories to assess performance of HPLC methods will be completed in May 1992.



PARTICIPANTS

Agricultural University, Copenhagen, DK CNEVA, Paris, F Fisheries Research Center, Dublin, IRL IE0, Vigo, E IFREMER, Nantes, F INS, Lisboa, Ρ ISS, Roma, I IVB, Berlin, 0 Ludwig Haximillians Universität, Hünchen, 0 HAFF, Essex, UK Ministerio de Sanidad, Hajadahonda, Ε RIKILT, uageningen, NL RIVO, I¡muiden, NL SVF, Cuxhaven-F, 0 ULB, Bruxelles, Β Universidad de Santiago, Lugo, Ε Universidade de Vigo, Ε Universität Hohenheim, Stuttgart, 0 University of Göteborg, S.

139

PROJECT RM 395

ETHYL CARBAMATE IN WINE RMs

PROJECT DEFINITION

Ethyl carbamate (EtC) is a carcinogenic substance, present in all fermentation media containing ethanol. The United States and Canada have established a limit of 30 μ%/\ in wine, which is also recommended by The European Communities and the Organisation Internationale du Vin et de la Vigne (OTV). This limit may be lowered in the near future and will required improvement of methodology, a problem of concern for the OIV and the Communities. Ethyl carbamate is usually determined by Gas Chromatography (GC). There are differences between the various methods used which arise from the varying sample preparation procedures and detection systems (FID, NP, MS, etc.). The objective of the project is to improve the accuracy and the level of agreement between European laboratories and to prepare reference materials.

STATUS

The first intercomparison in which 25 laboratories determined EtC in four samples of white and red wines will be completed in 1992.



PARTICIPANTS

Bayerische Landesanstalt Für ueinbau und Gartenbau, Veitshöchheim, D Chivas Brothers Ltd., Renfrewshire, UK CIVC, Epernay, F Danish Technological Institute, Aarhus, DK Federal Office of Public Health, Bern, CH Institut du Vin, Paris, F Institut Cátala de la Vinya i del Vi, Penedés, Ε. Instituto Sperimentale per l'Enologia, Asti, I Instituto do Vinho do Porto, Ρ ISPRA, Joint Research Centre, Conmission Laboratorio Arbitral, Madrid, Ε LNETI, Oueluz, Ρ HAFF, Norwich, UK Hax von Pettenkoffer Institut-BGA, Berlin, 0 Ministerie van Economische Zaken, Brussel, Β Ministry of Agriculture, Athens, GR Pent lands Scotch Uhisky Research Ltd., Edinburgh, UK Pernod Ricard, Creteil, F State Laboratory, Dublin, IRL Station Vinicole du Β.Ν.I.e., Cognac, F TNO-CIVO, Zeist, NL United Distillers International, Clackmannanshire, UK Universidad de Cordoba, Cordoba, E Université de Bordeaux, Talence, F

140

PROJECT RM 301

REFERENCE MATERIALS FOR MICROBIOLOGICAL TESTING OF FOOD AND FEED

PROJECT DEFINITION

The total number of food samples examined in the European Community can be estimated as being 107 per year. False analytical results can have huge economical and public health consequences. Economical consequences of false-positive results may vary from unnecessary delay in the distribution of food, to unnecessary destruction of wholesome foods or to a damage of good reputation of food manufacturers. Public health consequences due to the distribution of contaminated food occur in case of false negative results. On the basis of inter-laboratory studies it is estimated that 5% or even more of all determinations may produce more or less deviating results. Hence the need for RMs. General requirements for reference materials from microbiological studies are:

the colony-forming units (cfu) should be homogeneously spread over the material and should be stable for a sufficient time. the microflora species present should be representative for those encountered in practice (e.g. presence of competitive flora).

All these criteria were first met in 1985 when sub lethally stressed cfu's of Salmonella were protected in spray dried milk. Further stability studies are being carried out. A similar study has been started for Listeria monocytogenes. If this kind of preservations is demonstrated to be of sufficient stability, the work will be extended to other species such as: Enterobacteriaceae, Escherichia coli, Coliforms, Staphylococcus aureus, Clostridium perfringens, Bacillus cereus, Shigella, Campylobacter jejuni, Yersinia enterocolitica and Vibrio parahaemolyticus. The work further consists of analytical feasibility studies in laboratories in the Member States and will soon lead to certification of spray dried milk capsules containing Salmonella.

STATUS

The work began in 1987. Three intercomparisons have been concluded for Salmonella and two for Listeria. The certification of the first Salmonella capsules can be envisaged in 1992.



PARTICIPANTS

34 laboratories from the 12 Member States.

Pilot laboratory: Dr Α. Havelaar, RIVM (NL)

141

PROJECT RM 204

POLYCYCUC AROMATIC HYDROCARBONS (PAHs) IN FOOD

PROJECT DEFINITION

PAHs are a broad class of environmental contaminants which arise mainly through incomplete combustion processes (in auto-exhaust, fossil-fuel power-generators, etc.). As many PAHs are potent mutagens or carcinogens, their presence in foods is carefully monitored. Their high genotoxic activity requires that the compounds are determined at low levels (fig/kg) which poses considerable analytical difficulty. The food industry has set a maximum permissible limit for benz (a) pyrene in refined edible oil of 1 /ig/kg. The objective is to improve the accuracy of the determination through intercomparisons and to prepare CRMs.

STATUS

Four intercomparisons have been carried out at progressively lower PAH levels. Initially only calibration and instrumental aspects were considered. In the second study, five representative PAHs in a highly contaminated coconut oil (benz (a) pyrene content of around 40 /xg/kg) and green kale were analysed. Serious discrepancies were observed. In the next study, participants analysed a coconut oil which had been prepared by the coordinating laboratory who added known amounts of 5 compounds (benz (a) pyrene content of 13 £¿g/kg) to an almost blank oil.

Considerable improvement was observed and biased methods were identified. The fourth study involved a typical semi-refined food oil with a benz (a) pyrene content of around 4 ¿ig/kg and showed that certification of a reference material at this level is now possible. Coconut oil reference materials will be prepared and certified during 1992.



PARTICIPANTS

Biochemisches Institut für Umweltcarcinogene, Ahrensburg, D Bundesanstalt für Materialprüfung, Berlin, 0 Bundesanstalt für Fleischforschung, Kulmbach, D CIVO/TNO, Zeist, NL Conservatoire National des Arts et Hétiers,Paris, F Food Inspection Service, Groningen, NL Institut des Corps Gras, Pessac, F Keuringsdienst van Uaren voor the Gebied, Amsterdam, NL Ministry of Agriculture, Food and Fisheries CHAFF), Norwich, UK Rijksinstituut voor Volksgezondheid en Milieuhygiene, Bilthoven, NL Rijkskwaliteitsinstituut voor Land- en Tuinbouwprodukten CRIKILT), Wageningen, NL Torry Research Station, Aberdeen, UK Unilever Research, Bedfordshire, UK Uni lever Research, Vlaardingen, NL Unimills, Hamburg, 0 Union Deutsche Lebensmittelwerke GmbH, Hamburg, D Université di Perugia, Perugia, I.

142

PROJECT RM 283

DETERMINATION OF GENOTOXIC COMPOUNDS IN PROCESSED FOOD

PROJECT DEFINITION

Concern about long term exposure to carcinogenic substances which may be present at trace levels in the human diet has greatly increased in the last decade. This has resulted in the development of government regulations, quality control and improvement of industrial food processing. The presence of genotoxic compounds such as heterocyclic amines has been demonstrated in foodstuffs submitted to excessive heating, however, toxicologists are not yet able to agree on maximum exposure levels that can be tolerated by humans. The objective of the project is to support collaborative studies aimed at evaluating the best methods of determination of a series of genotoxic compounds in food matrices. Reference materials will also be prepared, if necessary.

STATUS

A first intercomparison addressed the instrumental determination of three-imidazoquinolines (IQ, Me-IQ, Me-IQx) in ethanol and showed that whereas the HPLC method worked well, GLC was unsatisfactory. Good correlation was obtained for the mutagenicity tests (Ames test) and showed a very high mutagenic activity for these compounds. A second intercomparison on the determination of the same compounds in specially prepared meat extract is in progress and will be terminated end of 1992.



PARTICIPANTS

Biochemische Institut für Umweltcarcinogens, Alsemberg, D British Industrial Biological Research Association, Carshalton, UK Conservatoire National des Arts et Métiers, Paris, F CPC, Thayngen, CH. Institut für Biochemie, Karlsruhe, D Istituto Mario Negri, Milano, I Istituto di Igiene, Genoa, I Ministry of Agriculture, Fisheries & Food, Norwich, UK National Food Agency, Soeborg, DK NESTEC, Lausanne, CH Rijksinstituut voor Milieu en Hygiene, Bilthoven, NL Universität Uürzburg, D

Université Catholique de Louvain, Bruxelles, Β University of Surrey, Guilford, UK

143

PROJECTS RM 285 and RM 266

DETERMINATION OF CHLORINATED PESTICIDES

PROJECT DEFINITION

Although chlorinated pesticides (e.g. HCB, HCH, the drins, DDT, etc.) are not being used nor produced anymore in the Community, they are still present in soils because of their high stability and may, therefore, be present in certain crops. In other countries these products are still being used, which makes it necessary to determine chlorinated pesticides in food and animal feed imported from such countries. A preliminary intercomparison has shown that results of different laboratories disagree widely. Hence the need for collaborative trials with the aim of improving the state of the art which could lead to certification exercises. Matrices for which certification is foreseen are: milk powder, pork fat and animal feed. A typical pesticide determination of two parts: (i) extraction and clean-up of the extract, and (ii) separation, identification and quantification. Two milk powder samples were certified: a spiked one and one with natural (low), endogenous levels. The spiked material will mainly allow the user to verify the performance of part (ii) of the determination, because endogenous pesticides are chemically bound to fats, eel walls, etc. which renders the extraction and clean-up of samples with endogenous levels more troublesome in terms of quantitative recovery. The other materials such as pork fat, foreseen to be certified next will not be issued in the form os spiked materials. Hence the necessity to feed selected pigs with a pesticide enriched diet, before taking their fat.

RESULTS

Two milk powder samples, one of endogenous and low level, the other spiked to contents of 20-50 ng/g dry mass were certified (RM 285), EUR Report 12319, 1989. Endogenous OCPs in pork fat has been certified in 1991 (RM 266), EUR Report 14063, 1992.


ECU 400 000

PARTICIPANTS

An Foras Taluntais, Carlow, IRL - Boter- en Kaascontrolest, Leeuwarden, NL - Chemisches Untersuchungsamt, Münster, D - CIV0-TN0, Zeist, NL - Ist. Sup. Sanita, Roma, I - Keuringsdienst ν. Haren, Amsterdam, NL -Keuringsdienst ν. Uaren, Utrecht, NL - Laboratoire Municipal et Régonial, Rouen, F - Laboratory of the Government Chemist, London, UK - L.A.R.A., Toulouse, F - Landesanstalt für Lebensmittelchemie, Berlin, D -Milchwirtschaftliche Untersuchungs- und Versuchsanstalt, Kempten, D - Ministère de l'Agriculture, Paris, F - National Food Institut, Soeborg, DK- Nestle, Vevey, CH - Rijkszuivelstation, Melle, Β - Rikilt, Wageningen, NL - RIVM, Bilthoven, NL - Shell Res. Ltd., sittingbourne, UK

144

PROJECT RM 342

NITRATE DETERMINATION IN FOODSTUFFS

PROJECT DEFINITION

The level of nitrate in food is increasingly controlled because of possible risk to human health and especially to children. There is controversy over the possible relationship between nitrate and formation of carcinogenic nitrosamines. For baby food, the legal limit in several Member States is 50 mg/kg, by comparison, the EC legal limit for fresh water is 40 mg/kg. Nitrate level can reach 3 to 4 g/kg in fresh vegetable. The objective of the project is to improve methodology through intercomparison and to prepare CRMs if necessary.

STATUS

A first intercomparison on orange juice materials (blank and spiked) and beet root juice involving HPLC techniques, cadmium reduction methods and enzymatic kits is terminated. The results have shown that the differences between methods are not significant, the relative coefficient of variation being less than 10%. A reference material consisting of freeze dried lettuce powder will be prepared.



PARTICIPANTS

Bundesforschungsanstalt, Geisenheim/Rhei'ngau, D Consellaria de Sanidad, Dirección General Consumo, Valencia, E Deutsche Granini, Bielefeld, D Eden-Waren GmbH, Bad Soden, D

ERA, Perugia, I Greenlab APO, Fori», I Institut d'Hygiène et d'Epidémiologie, Brussels, Β Institute of Horticultural Research, Warwick, UK

Istituto Superi ore di Sanità, Roma, I Laboratoire Central de la Repression des Fraudes, Massy, F Laboratoires Associés de Recherches Agricoles, LARA, Toulouse, F Laboratorium voor Bromatologie, Rijksuniversiteit van Gent, Β Laboratory of the Government Chemist, Teddington, UK

Landesuntersuchungsamt für Gesundheitswesen Nordbayern, Uürzburg, D Merck, Darmstadt, D National Food Agency, Soeborg, DK Bayerische Hauptversuchanstalt für Landwirtschaft, Freising, D Research Center for Horticulture, Arslev, DK Servicio Vasco de Salud-Osakidetza, Osasun Zuzendaria, Bilbao, Ε Station Fédérale de Recherches en Chimie Agricole et sur l'Hygiène de l'Environnement, Liebefeld, CH Stazione Sperimentale per l'lndustria délie Conserve Alimentan', Parma, I The National Food Center, TEAGASC, Dublin, 1RL TN0/C1V0, Zeist, NL Universidad Complutense, Faculdad de Farmacia, Madrid, E

145

PROJECT RM 407

HEAVY METALS IN WINE RMs

PROJECT DEFINITION

Traces of toxic elements such as Pb, Cd, As, Al and Hg are commonly present in wines and spirits. The Organisation International du Vin et de la Vigne (OIV) and most developed countries have established maximum levels for lead and cadmium in wine (around 300 and 100 /xg/I respectively). These limits are likely to be lowered in the near future. It is important for economic and health reasons that the concentration of metals are determined accurately. The problem of the analysis of heavy metals in wines is currently being investigated by the OIV and many oenological laboratories. The Commission's Directorate for Agriculture (DG VI) requires methods that allow reliable determination of Pb in European wines so that they can solve trade disputes, particularly with the United States which is considering reducing the Pb concentration from 300 to 150 μgΛ. The aim of the project is to improve the methodology for the analysis of toxic elements in wine, in particular for Pb and Cd, to increase the level of agreement between European laboratories and to prepare reference materials.

STATUS

An intercomparison of methods (AAS, IDMS, GFAAS, ICP, Polarography, etc.) for the analysis of Pb between approximately 20 laboratories was completed in November 1991 and showed a high level of agreement between specialized laboratories. Further studies on Pb and Cd are planned and consideration will be given to the problems of As, Al and Hg analysis.



PARTICIPANTS

Bundesgesundheitsamt - B.C.A. - Max-von-Pettenkofer-Institut, Berlin, 0 - Centre Nacional de la Recherche Scientifique, Vernaison, F - Chemisches Untersuchungsamt Speyer, D - E C Ν, Petten, NL -Gesellschaft für Strahlen- und Umweltforschung, Neuherberg, D - Institut de l'Environnement, Ispra, I -Institut d'Hygiène et d'Epidémiologie, Bruxelles, Β - Institut du Vin, Lykovrissi Attikis, GR -Instituto da vinha e do Vinho, Lisboa, Ρ - Instituto do Vinho do Porto, Ρ - Kernforschungsanlage Jülich GmbH, Jülich, D - Laboratoire de la concurrence, consommation et répression des fraudes, Illkirch Grassenstaden, F - Laboratoire de la Répression des Fraudes, Montpellier, F - Laboratoire de la Répression des Fraudes, Talence, F - Laboratorio Agrario del Norte, Dpto de Productos Agrarios, Santander, Ε - Laboratorio Analisi e Recerca dell'1st i tuto Agrario di San Michèle, I -Landesuntersuchungsamt für das Gesundheitswesen Nordbayern, Würzburg, D - HAFF - Food Safety Directorate - Food Science Laboratory, Norwich, UK - Ministerio de Agricultura, Madrid, E - National Food Agency of Denmark, Soborg, DK - Tickle & Reynolds, Exeter, UK - TNO Biotechnology t Chemistry Institute, Zeist, NL - Ufficio Repressione Frodi di Genova, I - Uff icio Repressione Frodi di Asti, I - Universidad de Santiago de Compostela, E - Université de Montpellier, F - University of Gent, Β.

146

PROJECT RM 409

OVERALL MIGRATION FROM PLASTIC MATERIALS

PROJECT DEFINITION

The Commission is in the process of completing the Community law in the sector of plastic materials as laid down in the Framework Directive (89/109/EEC) relative to materials and articles intended to come into contact with foodstuffs. According to Directive 90/128/EEC plastic materials and articles to come into contact with foodstuffs shall not transfer their constituents (overall migration) to foodstuffs in quantities exceeding 10 mg per dm2 of surface area of material or article. This limit is 60 mg per kg of foodstuff for plastic containers, articles that can be filled and articles whose surface area is difficult to determine. According to the rules laid down in Directives 82/711/EEC, 85/572/EEC and 90/128/EEC, CEN has nearly completed methods for the measurement of overall migration in the three aqueous food simulants. A method for the measurement of overall migration in olive oil is in an advanced stage of preparation. The practical application of the latter method is particularly difficult. The Programme has been requested by the responsible Commission services (DG III) and CEN to establish samples of plastics with certified overall migration characteristics to allow laboratories to demonstrate the reliability of their measurements.

STATUS

A candidate material for testing overall migration in aqueous simulants has been identified. A first intercomparison between 23 laboratories on the measurement of overall migration from polyamide into 3 % acetic acid and into 15 % ethanol and on the quantification of olive oil in solution has shown that certification of the property can be achieved. A batch of polyamide reference material has been prepared and certification measurements should be completed in 1992. A search is in progress for suitable materials for intercomparisons on the measurement of overall migration in olive oil.



PARTICIPANTS

ADRIA, Quimper, F - BPI, Ghent, Β - Bundsamt fur Gesunheits-Uesen, CH - CICC, Madrid, Ε - CL, Sttutgart, D - CSI Ricerca Applicata Montedison, Milano, I - Food Inspection Service, Utrecht, NL - Fraunhofer Institut, Munich, 0 - I.P.O., Lisboa, Ρ - ICI Ui Iton Centre, Cleveland, UK - INS, Lisboa, Ρ - Instituto Carlos IM, Majadahonda, Ε - ISS, Roma, I - Kantonales Laboraforum, CH. - Laboratoire National D'Essais, F - Laboratoire Cantonal de Chimie, CH - LGC, Leatherhead, UK - MAFF, Norwich, UK - NATEC, Hamburg, D -NFA, Soborg, DK - Packforsk, Kista, S - Pira Int., Surrey, UK - Technical Research Centre of Finland, Espoo, SF - TNO -CIVO, Zeist, NL - Universidade do Porto, Porto, P.

147

PROJECT RM 410

SPECIFIC MIGRATION FROM PLASTIC MATERIALS

PROJECT DEFINITION

The Commission is in the process of completing the Community law in the sector of plastic materials as laid down in the Framework Directive (89/109/EEC) relating to materials and articles intended to come into contact with foodstuffs. According to Directive 90/128/EEC a number of monomers and starting substances can be used for the preparation of plastic materials. The maximum quantity of these monomers and starting substances that can be released from the plastics materials into foodstuffs (SML), or may be present in the material as residual (QM), is established in the above Directive. Verification of compliance with the migration limits shall be carried out in accordance with Directives 82/711/EEC, 85/572/EEC and 128/90/EEC, which concern the basic rules for testing migration, the list of simulants to be used for testing migration and establish the specific migration limits respectively. According to the above Directives, CEN is about to complete methods for the measurement of migration of several monomers. However, methods for the determination of more than 40 monomers are urgently needed, and many more will be required when additives are considered under Directive 90/128/EEC. The objective of the project is to develop the basic methodology for determination of monomers with emphasis on multi-methods. These methods will be drafted as CEN norms, CEN taking responsibility for their validation. The project includes preparation of a handbook of analytical data.

STATUS

The preparation of a handbook of spectral and physico-chemical data of monomers has been undertaken in conjunction with a bank of monomers and starting substances by the Food Science Laboratory, MAFF, Norwich, U.K.. Priorities for method development have been established in collaboration with other organisations and support to basic method development by Community laboratories is being arranged,



PARTICIPANTS

Fraunhofer Institut, Hunich, D -Packforsk, Kista, S ICI Uilton Materials Research Center, Cleveland, UK ISS, Rome, I MAFF, Norwich, UK Pira International, Surrey, UK TN0-CIV0, Zeist, NL University of Santiago de Compostela, ES

Other participants to be identified for method testing.

148

PROJECT RM 225 (a)

REFERENCE MATERIALS FOR MUX FAT ANALYSIS (butyric acid and fatty acid profile)

PROJECT DEFINITION

Butter fat is more complex than the common animal and vegetable oils and fats and, generally, its analysis is carried out in specialised dairy laboratories. Gas chromatographic (GC) determination of the fatty acid profile via their methyl esters is complicated by the wide range of volatility of the components (C4:0, butyric acid up to C18 and, in trace amounts, higher acids). In addition butyric acid, a fatty acid virtually unique to butter fat, is an important quality indicator and, because the natural range is relatively low (typically 3.2 to 4.0% absolute), the mean value of 3.6% is often taken as the presumptive value for estimating the amount of butter in mixtures of fat e.g. in chocolate confectionary for tax purposes.

RESULTS

A batch of milk-fat containing added anti-oxidant was ampouled under nitrogen and the stability of the fatty acids demonstrated in a 3 year study. The butyric acid content was certified after a preliminary study of methods. Certification was based on Community employed GLC methods (via underivatised butyric acid and via methyl esters) and, by HPLC and GC-MS methods which had been specially developed for this work. A mixture of tributyrin and beef-fat was used to validate the methods used in the study. The fatty acid profile was determined by 6 laboratories which were experienced with milk-fat analysis. Certified values are given for 9 of the major components and indicative values for a further 21 fatty acids. The project is terminated (provisional report available).


ECU 130 000

PARTICIPANTS

Bundesanstalt für Hi Ichforschung, Kiel, 0

Faculté des Sciences Agronomiques de l'Etat, Getnbloux, Β Hannah Research Institute, Scotland, UK

Instituto del Frio, Madrid, Ε

Istituto Sperimentale Lattiero Caseario, Milano, 1

Laboratory of the Government Chemist (LGC), Middlesex, UK

Leatherhead Food RA, Surrey, UK

Mi Ichwirtschaftliche Untersuchungs- und Versuchsantalt, Kempten, D

Ministry of Agriculture, Fisheries and Food (MAFF), London, UK

National Food Institute, Soborg, DK

MZO, Ba Ede, NL

RIKILT, Wageningen, NL

Université di Milano, Milano, 1.

149

PROJECT RM 225 (b)

CHOLESTEROL AND OTHER STEROLS IN EDIBLE OIL AND FAT RMs

PROJECT DEFINITION

Concern over the relationship between cholesterol in the diet and the risk of heart disease continues and there is a move towards low cholesterol diets. Cholesterol is one of the components included in the Communities proposed Directive on Food labelling.

The reliable determination of cholesterol at low levels (1 mg/100 g) has become increasingly important to confirm claims of cholesterol free or reduced oils and fats. There is also interest in other sterols, both for health purposes and as a means of identifying the origin of oils.

RESULTS

A series of intercomparisons has shown that one of the major sources of errors in cholesterol analysis by GLC is incomplete extraction following saponification. The various GLC methods applied by the participants gave very good recoveries of cholesterol added after saponification of a vegetable oil. A quantitative extraction method has been developed and validated in a study using radio labelled cholesterol and its oléate. A GC-MS method using stable labelled cholesterol has also been developed. Certification measurements of three existing RMs (vegetable oil RM 162, animal fat RM 163 and milk-fat RM 164) involving 9 laboratories are finished.

The major and minor sterol components of RM 162 (a blend of soya and maize oil) have been identified in a study involving 2 independent laboratories using GC-MS. The project is terminated (EUR report in preparation).


ECU 38 880

PARTICIPANTS

Faculté des Sciences Agronomiques, Gembloux, Β Institut des Corps Gras, Pessac, F tstituto Sperimentale Lattiero, Milano, I Laboratory of the Government Chemist (LGC), Middlesex, UK Leatherhead Food R.A., Surrey, UK Hilchwirtschaftliche Untersuchungs- und Versuchsanstalt, Kempten, D Ministerie van Economische Zaken, Brussel, Β RIKILT, Uageningen, NL Université degli Studi di Milano, Milano, I.

150

PROJECT RM 239

MAJOR NUTRITIONAL PROPERTIES OF FOOD

PROJECT DEFINITION

The main nutritional properties of a food are defined by its major organic components; total protein, total fat, carbohydrate (starch and sugars) and dietary fibre. Knowledge of the contents of major elements such as Ca, Κ, Ρ and Na is also important. Accurate determination of these components has become more important because of the greater demand for reliable food labelling (Directives 79/112/EEC and 90/496/EEC) and, the implications for intra-community trade in food products. Although routinely determined in industry and for nutritional purposes, collaborative studies have shown that even the most experienced laboratories can make significant errors.

RESULTS

A preliminary intercomparison of methods identified many of the methodological weaknesses. 5 reference materials (full cream milk powder, wholemeal and rye flour, haricot beans and lyophilised pork muscle) have been prepared and shown to be homogeneous and stable and have been certified with respect to total Ν protein, ash, total fat, dietary fibre by the AOAC method, lactose and for Ca, Κ, Na, Mg, Cl and P. Indicative values for starch, free sugars and dietary fibre by the Englyst method were also established. Indicative values for several important vitamins are proposed (see project 341). The project is terminated (provisional reports are available).


ECU 289 000

PARTICIPANTS

AFRC Institute of Food Research, Bristol, UK - Agricultural Research Center of Finland, Jokioinen, SF -Agricultural University, Uageningen, NL - Bundesforschunganstalt für Getreide und Kartoffelverarbeitung, Detmold, D - Bundesforschungsantalt für Ernährung, Stuttgart, D - Centro Nacional de Alimentación, Madrid, Ε - CIVO/TNO, AJ Zeist, NL - CNRS, Vernaison, F - Eastern Health Board, Dublin, IRL - Gesselschaft für Strahlen und Uweltforschung, Neuherberg, D. - INRA, Poligny, F -ITCF, Paris, F - Keuringsdienst van Waren, Maastricht, NL - Laboratory of the Government Chemist,

Middlesex, UK - Leather-head Food RA, Surrey, UK - LNT1, Lisboa, PT - Milk Marketing Board, Surrey, UK -Ministère des Affaires Economiques, Bruxelles, Β - National Food Agency, Soborg, DK - National Food Administration, Uppsala, SE - Netherlands Controlling Authority for milk and milk products. An Leusden, NL - NIZO, Ba Ede, NL - Plasmon Dietetic) Alimentan' Spa, Milano, I - Rijkszuivelstation, Melle, Β -RIKILT, Wageningen, NL - RISO National Laboratory, Roskilde, DK - RIVM, Bilthoven, NL - Statens Mejeriforsog, Hillerod, DK - Unilever Research, Bedforshire, UK - Université ambiéntale, Venezia, I.

151

PROJECT RM 280

FRUIT JUICE ANALYSIS

PROJECT DEFINITION

A number of physical and chemical measurements are used for controlling the commercial quality of fruit juice and related products. Definition and specification of fruit juice are subject to EEC Directives (75/726/EEC as amended). Some aspects which are not covered by Directives are subject to national regulations which, unfortunately, tend to differ. This situation adds further trade difficulties to those which arise from differences in the results of measurements even when standardized methods are used, e.g. nitrate determination. For these reasons, the Fruit Juice Trade Associations have requested that the BCR program organizes intercomparisons of methods at Community level and develops, if necessary, appropriate reference materials. Results of the work may be used by the CEN (European Committee for Standardization) which is currently issuing norms in this field.

STATUS

The project progressed by steps involving three intercomparisons covering major inorganic elements, major organic compounds and amino acids. The production of a freeze dried orange juice reference material has been shown to be feasible and the production of a final batch will be completed in 1992.



PARTICIPANTS

CIV0 Institutes TNO, Zeist, NL - Coca Cola, Essen 0 - Deutsche Granini, Bielefeld, D - Di Giorgio International, Turnhout, Β - Eckes, Nieder-Olm, D - Eurocitrus, Oosterhout, NL - Gattefosse, Saint-Priest, F - Industrial Research Laboratory for Fruit and Vegetable Industry, Arsley, DK - Institut für Lebensmitteltechnologie, TU Berlin, D - Institut für Ueinchemie und Getränkeforschung, Geisenheim, D -Institut für Anorganische Chemie, Universität Regensburg, Regensburg, D - Istituto Nazionale della

Nutrizione, Roma, I - Joker, Häcon, F - Laboratoire de la Consommation et de la Répression des Fraudes, Rennes, F - Laboratoires Associés de Recherches Agricoles, Toulouse, F. - Laboratorio G. Safina, Palermo, I - Laboratorium voor Bromatologie, Rijksuniversiteit Gent, Β - Laboratory of the Government Chemist, London, UK - Landesuntersuchungsamt für das Gesundheitswesen Nordbayern, Uürzburg, D - Looza, Borgloon, Β - Marie Brizard & Roger International, Bordeaux, F - Pernod Ricard, Créteil, Fr - Plasmon Dietetici, Milano, I - Reggio Calabria, I - Station d'Oenologie et de Technologie Végétale, Narborme, F - Station Oenologique de l'Hérault, Montpellier, F - Stazione Sperimentale Essenze e Derivati Agrumari, Stazione Sperimentale per l'Industria del le Conserve Alimentan, Parma, I.

152

PROJECT RM 284

DETERMINATION OF H/D ISOTOPIC RATIO AT NATURAL ABUNDANCE LEVEL IN WINE BY QUANTITATIVE NMR SPECTROMETRY

PROJECT DEFINITION

The use of Nuclear Magnetic Resonance (NMR) to detect the fraudulent addition of sugar and water to grapes during wine making, to increase the alcoholic strength of wine is well established. The deuterium isotope redistribution from sugar to ethanol during fermentation is characterized by the H/D NMR but the method requires a set of reference ethanols of known H/D ratio at natural abundance levels for the calibration and alignment of NMR spectrometers. The objective of the project is to prepare three ethanol reference materials from different phytobiological origins:

ethanol from sugar beet, a Calvin type plant which normally has a low deuterium content; ethanol from grape having a medium deuterium content; ethanol from maize, a Hatch-Slack type plant with high deuterium content.

RESULTS

The certification of the H/D ratio of three ethanols (sugar, grape and maize) is completed. The certified reference ethanol will be available during 1992. A reference Tetramethyl urea (TMU) sample for use as an internal standard is also available in 500 and 1 000 ml quantities for official SNIF-NMR measurements of wine and must. The project is terminated (EUR report in preparation).


ECU 150 000

PARTICIPANTS

Eurofins, Nantes, F. Istituto de Enología, Asti, 1 Laboratory of Government Chemist, London, UK University of Copenhagen, DK University of Brussels, Université Libre de Bruxettes, Β University of Hantes, F University of Regensburg, D University of Antwerp, Β University of Frankfurt, D University of Amsterdam, Hi University of Montpellier, F University of Leiden, ML University of Dublin, IRL University of Marburg, D University of Strasbourg, D

153

PROJECT RM 330

DIETARY FIBRE REFERENCE MATERIALS

PROJECT DEFINITION

Dietary fibre represents that part of the carbohydrate in'food which is not digested in the small intestine. A widely accepted working definition of dietary fibre is the sum of lignin and polysaccharides. Intense interest in dietary fibre has arisen from claims of its benefit in control of bowel function, reduced risk of intestinal cancer, reduced plasma cholesterol and glucose levels and from the movement towards the consumption of more fibre and less fat. Controversy over the choice of methods comes from difficulty in relating specific fibre components to their physiological function and the conflicting requirements for robust and convenient analytical procedures for routine analysis. For food labelling purposes there is an urgent need for the Community to adopt a single method for dietary fibre to allow comparability of values. Essentially, the choice lies between the AOAC procedure, widely used in continental Europe the Englyst method which has been recommended by the UK and the Uppsala method used in the Scandinavian countries. The objective is to produce a range of reference materials in which dietary fibre and its components are characterised by the most commonly used procedures to allow quality control in food industry and the public control laboratories.

STATUS

Wholemeal and rye flour and haricot bean reference materials have been certified for major dietary components including dietary fibre by the AOAC method in project 239. This project will address more complex foods especially cereal and vegetable type ones. The first phase will consist of a detailed method study which started in 1991.



PARTICIPANTS

AFRC Institute of Food Research, Norwich, UK - AFRC, Bristol, UK - Agricultural University, Wageningen, NL - Agricultural Research Center of Finland, Jokioinen, SF - Bundesforschungsanstalt für Getreide- und Kartoffelverarbeitung, Detmold, D - Bundesforschungsanstalt für Ernährung, Stuttgart, 0 - Centro Nacional de Alimentación y Nutrición, Madrid, E - CETS, Institut Quimie de Sarria, Barcelona, E - Danish Research Service for Plant and Soil Science, Arslev, DK - Dunn Clinical Nutrition Centre, Cambridge, UK - Eastern Health Board, Dublin, IRL - INRA, IPV, Montpellier, F - Instituto de la Grasa y sus Derivados, Sevilla, E - Istituto Nacionale de la Nutritione, Roma, I - ITGF, Paris, F - Keuringsdienst van Waren, Maastricht, NL - Leatherhead Food RA, Surrey, UK - LGC, Middlesex, UK - LNETI, Lisboa, Ρ -Merck, Darmstadt, D - Ministère des Affaires Economiques, Bruxelles, Β - Ministry of Agriculture, Fisheries and Food, London, UK - National Food Administration, Uppsala, S - National Food Agency, Soborg, DK - Nestle Research Dept, Vevey, CH - Nutrexpa, Barcelona, E - RHM Research & Engineering Ltd, Bucks, UK - RIKILT, Wageningen, NL - TNO-CIVO, Zeist, NL - Unilever Research, Bedfordshire, UK -Universidad Complutense de Madrid, Facultad de Farmacia, Madrid, E - Universita Ambientale, Venezia, I. - Universität des Saarlandes, Saarbrücken, D - University for Prevention of Cardiovascularic Disease, Bruxelles, Β.

154

PROJECT RM 333

DETERMINATION OF COMMON WHEAT IN PASTA

PROJECT DEFINITION

Pasta manufacturers in the EEC are required by law to use Durum wheat semolina flour when they manufacture dry pasta products labelled 100 % Durum. The incorporation of common wheat varieties in pasta product semolina constitutes an adulteration in the Internal Market and a fraud when export refunds are claimed on Durum wheat basis. Wheat traders, pasta manufacturers and official food control laboratories need to have accurate and reliable methods which can identify any possible adulteration of their wheat and wheat semolina stocks or of the pasta products including "couscous" put on the internal and international market. The high temperature and drying conditions used in pasta process denature the specific wheat proteins and make impossible to use the classical electrophoresis methods to determine the composition of the wheat semolina mixture.

After consultation of legislative authorities and the Union of Organisation of Manufacturers of Pasta Products (UNAFPA), a project aiming at the development of raw analytical methods was initiated.

STATUS

The results obtained after two years are as follows:

1) Extraction, electrophoretic fractionations and densitometric scanning of 1 D-ω -gliadins, (Common wheat proteins) were studied and tested on industrial pasta produced at 60°, 78°/92° and 100 °C. The method will be validated in 1992 in an intercomparison working group of 10-12 laboratories.

2) HPLC/immunological detection was investigated for γ-gliadins and the application of the method was demonstrated for pasta dried at 60°, 78792 °C at level as low as 3-4%. However, the application of the method to pasta samples dried at 100 °C was not possible below 15% adulteration. Further research is needed to optimize extraction of γ-gliadins.

3) Determination of specific albumins. The method allows to detect specifications of common wheat in pasta dried at 60°, 78°/92° C at 15% level. Pasta samples dried at 100 °C cannot be analysed by this method.

4) A further immunoassay for the determination of friabiline (specific to starch granules of soft wheat flour) will be tested in 1992 on the same pasta samples which were used in this study.

CONTRIBUTION O F THE COMMISSION


PARTICIPANTS

Institut National de la Recherche Agronomique, INRA, Montpellier, F

Nottingham Polytechnic, UK

Rhöne-Poulenc Diagnostic, Glasgow, UK. Université di Milano, I

155

PROJECT RM 340

IDENTIFICATION OF IRRADIATED FOOD

PROJECT DEFINITION

For some foodstuffs and food ingredients, irradiation enables the achievement of a greater hygienic safety and avoidance of chemical preservatives. Consumer confidence in irradiated food may be increased when there is clear evidence that the food irradiation treatment is being controlled and labelled. Because National Regulations differs, proposals for Community Legislation are under discussion. It covers only a limited number of food types. The correct application of Community Rules will require the availability of reliable methods to assess that food products are treated by irradiation and to control the trade of irradiated food in the Community. A concerted action involving some 50 laboratories of the EC and EFTA countries has been organised for a period of two years. It involves four group working on: DNA based methods, microbiological and biological methods, physical methods, chemical methods.

STATUS

The results of this concerted action is that the following methods were developed and tested: a microbiological based method for screening large quantities of samples including spices, herbs and poultry meat. The method is being tested in an intercomparison organised by MAFF and the Nordic countries. a thermoluminescence (TL) method tested in UK, Germany and in the BCR Programme was shown to reliably detect irradiation of herbs and spices. An Electron Spin Resonance (ESR) method which is applicable to meatbones, dried fruit and fish. The ESR method was validated by an extensive collaborative study and shows to be 100% reliable for meatbones and most of the dried fruits.

The work will continued to test a cheap and rapid screening method based on DNA electrophoresis. Results obtained up to 1991 are given in report EUR 13 331 (1991).



PARTICIPANTS

Bundesforschungsanstalt für Ernährung, Karlsruhe, D Center of Finland, Food Research Laboratory, Espoo, SF Department of Agriculture, Food & Agricultural Chemical Research Division, Belfast, UK -Kantonales F. Institute for Radiation Hygiene of the Federal Health Office, Neuherberg, D Irradiation Technology Branch, ENA-TIB/TIR, Roma, I Laboratoire de Chimie Analytique 2, Faculté de Pharmacie, Illkirch, F Laboratoire de Radiochimie des Constituants des Aliments, DB/SRA CEN Cadarache, Saint-Paul-lez-Durance, Laboratorium, Zurich, CH Ministry of Agriculture, Fisheries Ä Food, Torry Research Station, Aberdeen, UK

With the participation of a further 40 laboratories of the Member States.

156

PROJECT RM 341

IMPROVEMENTS IN ANALYSIS OF VITAMINS IN FOOD

PROJECT DEFINITION

Some 12 vitamins are commonly determined in foodstuffs for nutritional purposes (dietary and epidemiological surveys) and for food labelling purposes. Vitamins are included in Council Directive on Nutritional Labelling of Foodstuffs (90/496/EEC). Little is known about the reliability of such measurements and there is currently no means of ensuring traceability. The project has the general aim of method improvement and preparation of reference materials.

STATUS

The first intercomparison of chemical and microbiological methods which involved 20 specialised laboratories who determined commonly measured vitamins (retinol, B„ B2, B6, B12, C, D3, ß-carotene, α-tocopherol and niacin) in milk powder, haricot verts beans and pork muscle and a vitamin mixture has been completed. The results for retinol, α-tocopherol, C, ß-carotene & niacin agreed well for most of the materials analysed. Indicative values for these vitamins in the RMs recently certified for the major nutrients will be proposed if stability is proven (Project 239).

Methodological problems identified for folates, vitamins B„ B2 and B6 and, vitamin D are being studied in Projects 400, 401 and 402.

Reference Materials specially formulated for vitamin use have been prepared (fortified milk powder, brussels sprouts, margerine and flour) and a mixed vegetable sample (primarily for carotenoids) is under preparation. Certification measurement will begin in the second half of 1992 (see also Project 406 - Liver RMs).



PARTICIPANTS

AFRC Institute of Food Research, Norwich, UK - Biochemisches und Scheizerisches Vitamin Institut Vesal-lanum, Basel, CH - Bundesforschungansftalt für Ernährung, Stuttgart, D - Instituto del Frio CSIC, Madrid, E - Duphar B.V., Ueesp, NL - Federal Dairy Research Institute, Liebefeld-Bern, CH - Institut für Ernährungs, Giessen, D - Istituto Superiore di sanità, Roma, I - Laboratory of the Government Chemist, Teddington, UK - National Food Agency, Soborg, DK - National Food Administration, Uppsalsa, S - Produits Roche, Fontenay Sous Bois, F - Rijkskeuringsdienst van Uaren, Haastricht, NL -RijksKwaliteitsinstituut voor Land- en Tuinbouwprodukten - RIKILT, Waganingen, NL - Steins Laboratory, Holstebro, DK - Technical Research Centre of Finland, Espoo, SF - TNO Biotechnology & Chemical Institute, Zeist, NL - Unilever Research Laboratory, Colworth, UK - Université di Perugia, Perugia, I -University Col lege, Cork, IRL.

157

PROJECT RM 400

IMPROVEMENTS IN THE DETERMINATION OF FOLATES IN FOOD

PROJECT DEFINITION

The current project is undertaken as a consequence of an intercomparison made under project n° 341 which identified serious difficulties in the analysis of folate in food.

The objective is to examine through intercomparisons the performance of the different types of method with a view to identifying improved and more specific procedures for folate possibly based on HPLC or immunoassays which can offer potentially greater sensitivity. The folate content of several food RMs will be certified if it is feasible.

STATUS

The first intercomparison was completed in 1991 and showed the need to improve extraction and deconjugation procedures, calibration and identification of folate forms by HPLC and calibration in the PBA/RIA (Protein Binding Assay / Radioimmunoassay) methods. A second study will be completed in 1992.



PARTICIPANTS

AFRC Institute of Food Research, Norwich, UK Aston University, Birmingham, UK Biochemisches und Schweizerisches Vitamin Institut, Β Federal Research Center for Hutrition, Karlsruhe,D Institut für Ernährungswissenschaft, Giessen, D Instituto del Frio, CSIC, Madrid, Ε Laboratory of the Government Chemist, Teddington, UK Leatherhead Food R.A., Leatherhead, UK National Food Agency, Soborg, DK The Danish Dairy Board, Holstebro, DK TN0-CIV0, Zeist, NL Unilever Research Laboratory, Bedfordshire, UK Universität Gesamthochschule Paderborn, D University of Lund and Institute of Technology, S National Food Administration, Uppsala, S.

158

PROJECT RM 401

IMPROVEMENTS IN THE DETERMINATION OF VITAMIN B„ B, AND B4

PROJECT DEFINITION

The current project is undertaken as a consequence of an intercomparison made under project n° 341 which identified serious difficulties in the analysis of vitamins B„ B2 and B6.

The aim of this project is to improve the extraction and dephosphorylation procedures for these vitamins. The following will be investigated: choice of enzyme, pH, temperature, incubation time and samplerenzyme ratio. Further intercomparisons will involve the certification of these vitamins in reference materials prepared under project n° 341 (vitamin enriched milk powder, flour, brussels sprouts) and Project 406 (lyophilized liver).

STATUS

The first study designed to optimize the method is underway and will be completed in Spring 1992.



PARTICIPANTS

AFRC Institute of Food Research, Norwich, UK B.F.E., Stuttgart, D Bundesforschungsanstalt für Ernährung Institut für Ernährungswissenschaft Laboratory of the Government Chemist LGC, Teddington, Uli National Food Agency of Denmark, Söborg, DK RIKILT, Uageningen, NL TN0-CIV0 Institutes, Zeist, NL. Universität Giessen, 0

159

PROJECT RM 402

IMPROVEMENTS IN THE DETERMINATION OF VITAMIN D

PROJECT DEFINITION

The current project is undertaken as a consequence of an intercomparison made under project n° 341 which identified serious difficulties in the analysis of vitamin D.

The aim of the project is to improve the methods for vitamin D in food, through intercompa-risons and to certify the content of this vitamin in reference materials prepared under project n° 341 (vitamin enriched milk powder, flour, margerine) and Project 406 (lyophilized liver).

STATUS

The Erst intercomparison on the determination of vitamin D in margerine and a fortified milk powder should be completed in 1992.



PARTICIPANTS

Bundesanstalt für Hi Ichforschung, Kiel, D Bundesforschungsanstalt für Ernährung, Stuttgart, D Centro Investigación y Desarrollo la Lacteria Española, Renedo de Piélagos, E Duphar B.V., Ueesp, NL Instituto del Frió, (C.S.I.C.), Madrid, E L.H.Ε.T.I., Lisboa, Ρ Laboratory of the Government Chemist, Teddington, UK leatherhead Food RA, Leather-head, UK MAFF Food Safety Directorate, Food Science laboratory, Norwich, UK Milchwirtschaftliche Untersuchungsund Versuchsanstalt, Kempten, D National Food Agency of Denmark, Soborg, DK National Food Administration, Uppsala, S Nestec SA, Vevey, CH Produits Roche, Fontenay Sous Bois, F RIGB-Keuringsdienst van Waren, Maastricht, NL Rijkszuivelstation, Melle, Β Steins Laboratory, Holstebro, DK TNO Biotechnology & Chemical Institute, Zeist, NL Universität Basel, Basel, CH.

160

PROJECT RM 406

DEVELOPMENT OF A LIVER REFERENCE MATERIAL FOR DETERMINATION OF VITAMINS

PROJECT DEFINITION

Pig liver contains nearly all vitamins in measurable amounts which makes this matrix very suitable as a potential reference material for the whole range of water and fat soluble vitamins.

The contents of the individual vitamins in the reference material will be established progressively as the individual analytical problems are solved in the related projects (Projects 400, 401, 402).

STATUS

The conditions for processing and freeze drying of raw liver have already been established in a pilot study and a preliminary batch has been produced and checked for contents of vitamins. The preparation of the main batch of liver RM will be completed by mid. 1992.



PARTICIPANTS

Preparation of Material and Homogeneity/Stability Testing: CflNM, Geel, Β TNO Biotechnology & Chemical Institute, Zeist, NL.

Additional participants to be identified when the material has been sucessfully prepared.

161

PROJECT RM 412

DEVELOPMENT OF ADVANCED ANALYTICAL METHODS TO DETERMINE THE AUTHENTICITY OF FRUIT JUICE

PROJECT DEFINITION

The authenticity and purity of fruit juice products is extensively monitored for purposes of consumer protection, good trading practice and Community customs classification. Where they exist, the National systems of assessment for quality identity and authenticity (e.g. AFNOR, RSK, respectively in France and Germany) are generally based on previous practice of production and trade and the analytical methods are based on conventional procedures of analysis (IFU methods and recently issued CEN methods). This situation will not meet future needs because of the ingenuity of those who falsify and manipulate has become more and more sophisticated.

A number of methods used to detect the most common adulteration will be studied. They include the determination of characteristic substances:

anthocyanins and carotenoids flavonoids organic acids

and the determination of exogenous sugar by NMR, MS and detection of oligosaccharides by combined HPLC gas chromatography.

STATUS

Started in October 1991.


ECU 409 200

PARTICIPANTS

Eurofins, Nantes, F Gesellschaft für Lebensmittel forschung, Berlin, D Pernod Ricard S.A., F Rijksuniversiteit Gent, Laboratorium voor Bromatologie, Gent, Β Schutzgemeinschaft der Fruchtsaft Industrie e.V., Zorheim, D Stazione Sperimentale per l'Industria del le Conserve Alimentary, Parma, I Technische Universität München, D. Technische Universität Braunschweig, D

162

PROJECT RM 273

WATER SORPTION ISOTHERM REFERENCE MATERIAL

PROJECT DEFINITION

The Water Sorption Isotherm represents the equilibrium relationship between the water content of a food and its water activity (a,). At equilibrium, water activity is, in effect, equivalent to the relative humidity of the atmosphere surrounding the food.

Accurate definition of the water sorption isotherm is of considerable importance to processors of food and agricultural products.

Particular applications include drying of foods to ensure the required stability, mixing of foods and prediction of the sorption isotherm of the products and, packaging where the freshness of a product such as cheese depends upon the ability of the container to maintain the specified degree of humidity. The water activity subgroup of COST 90 (physical properties of foods) has developed a method for determining sorption isotherms and showed that micro crystalline cellulose (MCC) could serve as a stable and homogeneous reference material. The reference material based on MCC is designed to ensure correct application of the method.

RESULTS

The original COST 90 method has been further refined in order to improve definition of the MCC oven drying conditions. The water content of the reference material (RM 302) has been certified at 10 water activities and allows the application of the COST 90 method to be checked over the normal range of interest. The project is terminated: EUR report 12 429 (1989).


ECU 28 000

PARTICIPANTS

AFRC Institute of Food Research, Bristol, UK Bundesforschungsantalt für Ernährung, Karlsruhe, D Institut National de la Recherche Agronomique, 1NRA, Nantes, F South Bank Polytechnic, London, UK Stazione Sperimentale per l'Industria del le Conserve Alimentan', Parma, I Torry Research Station, Aberdeen, UK Universidad Politécnica ETSIA, Departamento Industrias Agricoles y Alimentaria, Valencia, E Universität München, Freising, D Universität Hohenheim, Stuttgart, D Université de Dijon, F Wageningen Agricultural University, Uageningen, NL.

163

PROJECT RM 281

REFERENCE MATERIALS FOR THE DETERMINATION OF RHEOLOGICAL PROPERTIES OF FLOURS

PROJECT DEFINITION

The minimum bread-making quality of common wheat and other basic cereals is assessed according to testing procedures given in EEC 2731/75 (as amended) regulation. The results of these quality tests rely on the accuracy of the measurement of water absorption of flour samples employing the so-called farinograph instrument following the ICC 115 standard. It should be underlined that, if samples of the same flour are evaluated with different farinographs, the results of the water absorption or the shape of the farinogram usually differ. Proper calibration and adjustment of the farinographs are required to obtain identical results. This adjustment (or calibration) must be performed with a set of reference flours of well established water absorption values. The objective of the project is to establish the feasibility of the preparation of flour reference materials as a means of calibrating the farinograph instrument. Other rheological instruments, such as alveographs and extensographs used in the Member States as complementary tests, will also be considered.

STATUS

Collaborative studies on farinograph determination carried out during 1989 with the participation of 14 European laboratories have shown that the between laboratory variation is too large. A second study on the farinograph determination has been completed and the results are being evaluated. Reference flours with certified rheological values are to be prepared in 1992.



PARTICIPANTS

Agricultural Institute, Kinsealy, IRL Agrilab, Antwerp, Β BIPEA, Paris, F Federal Research Institute of Cereal Industry, Detmold, D Flour Milling and Baking Research Association, FMBRA, Hertsfordshire, UK Grand Moulin de Pantin, ARCAM, F Institut Technique des Céréales et des Fourrages, ITCF, F Institute for Cereals, Flours and Bread TNO, Uageningen, NL Institute for Cereals, San Angelo Lodigniano, I. Jutland Technological Institute, Aarhus, DK Laboratoire ARIA, Paris, F

164

PROJECT RM 300

REFERENCE TILES FOR THE CALIBRATION O F MEASUREMENT O F COLOUR O F TOMATO PASTE AND SIMILAR PRODUCTS

PROJECT DEFINITION

The annual European production of tomato paste is valued at some 600 MECU, its principal usage being as an ingredient in food. Among several attributes, the colour of tomato paste is tightly specified by the purchasers who need to ensure that their food products have a consistent appearance. Increasingly, subjective methods for assessing colour of tomato paste by visual comparison with colour-cards are being replaced by objective methods employing colorimeters. These devices measure colour by mimicking the response of the human eye to the three primary colours, red, blue and green and allow any colour and shade to be expressed numerically in terms of "tri-stimulus" or colour values (e.g. Judd-Hunter L.a.b. values). The colour sub-group of COST 90 Bis (Physical Properties of Foods) investigated sources of disagreement in measurement of food colour. Consultation with major users of tomato paste confirmed the need for reference tiles specifically for the calibration of colorimeters used for industrial purposes.

RESULTS

A batch of 1.200 tiles having a colour very close to the target values and a narrow range of L, a and b values has been produced (26 +_ 0.5, 32.8 ±_ 0.5 and 14.4 +. 0.4 respectively). Individual colour values have been assigned to each tile by one institute using an instrument whose calibration is directly traceable to a national metrology institute. The tile was shown in a study involving 52 European Laboratories to virtually eliminate calibration errors in the measurement of tomato colour. The project is terminated: report EUR 13 392 (1991).


ECU 130 000

PARTICIPANTS

Campden Food and Drink RA, Glos, UK Ceram Research, Stoke-on-Trent, UK CS1C Inst. Agroquimica, Valencia, E Danish Research Service, Aarslev, DK Ecole Nationale Supérieure des Industries Agricoles et Alimentaires (ENSIAA), Massy, F H.J. Heinz Co Ltd, Middlesex, UK Hengstenberg GmbH, Esslingen am Neckar, D Institute of Food Research, Berks, UK Instituto del Frio, Madrid, E Londreco, Middlesex, UK Ministère des Affaires Economiques, Bruxelles, Β Ministry of Agriculture, Lykovrissi, GR Stazione Sperimentale per I'lndustria delle Conserve Alimentan, Angri, I Stazione Sperimentale Industria Conserve Alimentan', Parma, I The National Food Centre, Dublin, IRL Torry Research Station, Aberdeen, UK

52 Laboratories participated in the intercompar i son study.

165

PROJECT RM 312

DETERMINATION OF POLYPHENOUC COMPOUNDS IN AGRO-FOOD PRODUCTS

PROJECT DEFINITION

Food manufacturers need to replace colour lost during processing and to provide colour in the products which would be otherwise colourless. Community legislation only allows colours on the positive list to be added to food. Because consumers are suspicious of food additives and especially synthetic dyes, there is a trend to use natural pigments which are the same compounds as those contained in the original or similar plant material. Phenolic compounds which are present in fruit and vegetables contribute to colour and taste and are considered to be important nutritional component of the human diet. Determination of polyphenols are performed in the food industry and governmental laboratories for:

colour prediction of foodstuff when fruit concentrates are used, e.g. yoghurts, milk products, jams; detection of fruit juice adulteration; wine and spirits technologies.

The objective is to improve existing methods and to develop new methods of analysis.

STATUS

To be started in 1992.

CONTRIBUnON OF THE COMMISSION


PARTICIPANTS

AFRC Institute of Food Research, Reading, UK CERIA, Brussels, Β Departamento Tecnología de Alimentos, Universidad Politécnica, Valencia, Ε INIAER, Runa, Ρ Institut du Vin, Athens, GR Institut National de Recherches Agronomiques de Pech Rouge, Narbonne, F Institut d'Oenologie, Instituto Superior Agronomía, Lisboa, Ρ Instituto de Fermentaciones Industriales, Madrid, Ε Istituto Sperimentale per l'Enologia, Asti, 1 Leatherhead Food Research Association, Leatherhead, UK Max Von Pettenhofer Institute, Berlin, 0. RijksKwaliteitsinstituut voor Land- en Tuinbouwprodukten, Uageningen, HL Rijksuniversiteit Gent, Β TNO-CIVO, Zeist, NL Université degli studi di Perugia, Istituto per l'Industrie Agrarie, Perugia, I Universität Gesamthochschule Paderborn, D Université d'Avignon, Laboratoire des Pigments des Plantes, Institut de Chimie, Strasbourg, F Université de Bordeaux, Talence, F University of Surrey, UK

166

PROJECT RM 41β

APPLICATION AND IMPROVEMENTS OF SUPERCRITICAL FLUID EXTRACTION (SFE) TO REFERENCE MEASUREMENTS FOR FOOD AND AGRICULTURE RMs

PROJECT DEFINITION

The supercritical fluid extraction (SFE) technique offers the general advantage of selective extraction of non-volatile, non-polar up to moderately polar thermally labile compounds, compared with conventional extraction techniques. At a constant temperature, low pressures result in good extraction of non-polar compounds with low molecular weight whereas high pressures result in good extraction of moderately polar compounds with higher molecular weights thus allowing some control of extraction selectivity. Most of the major disadvantages of conventional extraction techniques are avoided if supercritical C0 2 is used as an extraction solvent. The resulting extracts are purer compared with those by conventional solvent extraction and the generation of liquid waste solvents and exposure of laboratory personnel to toxic solvents can be reduced or eliminated. The objective of the project is to improve the accuracy of the technique, to investigate its limitations in quantitative food and agricultural analysis and to explore applications for the certification of food and agricultural RMs.

STATUS

An intercomparison study on animal feed RMs naturally contaminated with aflatoxin B, at the ppb-level was used as a starting point. The study demonstrated the selective extraction of lipids using supercritical C0 2 for lipids and of aflatoxin 1^ using a mixture of supercritical COj/MeOH. The maximum recovery of aflatoxin B, in a compound feed RM was 86%. Difficulties were found to be in the diffusion of the analyte through the particles into the extraction solvent, in the solubility of the analyte in the extraction solvent, the particle size of the samples and the presence of co-extractives. Detailed studies on the applicability of SFE to current certified reference materials will be made in parallel to evaluate the limitations of the technique and its usefulness for certification measurements.

CONTRIBUnON OF THE COMMISSION


PARTICIPANTS

Carlo Erba Strumentazione SPA, Milano, I - Eindhoven University of Technology, Endhoven, NL - Faculté des Sciences Agronomiques de l'Etat, Gembloux, B - Institut des Corps Gras, Pessac, F - Instituto de Fermentación Industrial, Madrid, Ε - MAFF, Food Science Laboratory, Norwich, UK - RIKILT, Wageningen, NL - Société SEPAREX, Champígneulle, F - Universität des Saarlandes, Angewandte Physikalische Chemie, Saarbrücken, D - Université de Lyon, Lyon, F - University College of Swansea, Department of Chemistry, Swansea, UK. - University of Gent, Dept. of Organic Chemistry, Β - University of Leeds, School of

Chemistry, Leeds, UK

Agriculture

169

PROJECT RM 307

RAPESEED REFERENCE MATERIALS WITH CERTIFIED GLUCOSINOLATE AND SULPHUR CONTENTS

PROJECT DEFINITION

The presence of glucosinolates (GSL) in rapeseed cake reduces'its palatability to farm animals and is associated with interference in thyroid function and with other disorders. When the project was initiated, the Community actively encouraged the production of rapeseed varieties having low glucosinolate contents by paying a premium when the GSL content of the seed is less than 35 μπιοΐ/g. Consequently, there was a need for both rapid and official methods of analysis to ensure correct application of the Community scheme. The objective of the project was to provide rapeseeds with known glucosinolate contents as a means of verifying the various methods used both in oilseed process plant and in the official laboratories. A series of rapeseeds with certified sulphur content was required to provide a common basis for the calibration of a rapid XRF method.

RESULTS

Three rapeseed RMs were certified for their total GSL and sulphur contents. The certified contents are as follows :

RMn°

366

190

367

Total GLS contents

(μιηοΐ/g)

12.1 ± 0.8

25.5 ± 0.9

102 ± 3

Sulphur content (mg/g)

3.41 ± 0.12

4.93 ± 0.15

10.5 ± 0.4

These samples are an integral part of a proposed ISO method for XRF determination of total GSL content and the programme has supported the organisation of an ISO study. The project is terminated: report EUR 13 339 (1991).


ECU 111 000

PARTICIPANTS

Aarhus Oil, Aarhus, DK - AFRC Institute of Food Research, Norwich, UK - ATO-Agrotechnology, Uageningen, NL - BIONATPRODS Limited, Liverpool, UK - Bundesanstalt für Fettforschung, Münster, D - Centre National de ta Recherche Scientifique, Vernaïson F - Centre National de Recherche Scientifique, Vernaison, F -CETIOH, Ardon, FR Christian-Albrechts-Universität, Kiel, 0 - Danish State Seed Testing Station, Lyngby, DK - ECN Research Centre, Petten, NL - ECN, Petten NL - Faculté des Sciences Agronomiques, Gembloux, Β - Gesellschaft für Strahlenforschung, Neuherberg D. - Gesellschaft für Strahlen- und Umweltforschung GMBH, Neuherberg, D - ILLIT -Institute for Agriculture and Ecology, Kiel, D - Laboratoire U0LFF, Clichy, F - LUFA Kiel, Kiel, D - National Institute of Agricultural Botany, Cambridge, UK - N.I.A.B., Cambridge, UK - RIKILT, Uageningen, NL - RISO National Laboratory, Roskilde, DK - Royal Veterinary and Agricultural University, Frederiksberg, DK - State Laboratory Abbotstown, Dublin, IRL - Universität Kiel, Kiel, D -Universität Göttingen, Göttingen, D.

170

PROJECT RM 308

CALIBRANTS FOR GLUCOSINOLATE ANALYSIS OF RAPESEED

PROJECT DEFINITION

The proposed official method for total glucosinolate detection in rapeseed employs HPLC with UV detection to determine individual glucosinolates, these being summed to give the total content. Few of the required compounds are available for calibration purposes.

The objective of the project is to investigate the possibility of characterising the GSLs in a rapeseed extract which could then serve as a convenient chromatographic calibrant for all of the compounds of interest.

STATUS

A 36 months stability study under various conditions has been successfully completed and has demonstrated the feasibility of the project. Preparation of the final batch for certification could be started in 1992.



PARTICIPANTS

Faculté des Sciences Agronomiques, Gembloux, Β (stability studies).

Other participants to be identified for certification measurements at appropriate stage in the project.

171

PROJECT RM 310

AFLATOXIN Β, ΓΝ COMPOUND ANIMAL FEED (CRMs and Collaborative Study of Proposed Community Method)

PROJECT DEFINITION

Animal feed is subject to control in accordance with Directive 86/229/EEC which prescribes maximum levels for aflatoxin B, in finished feed of 50, 30 and 10 Mg/kg depending on the animals to be fed. The current legal method is not sufficiently sensitive to allow reliable quantitation of aflatoxin B! at 10 jig/kg and is vulnerable to interference by other feed components, notably citrus pulp and manioc. The objective of the project is: a) to provide reference materials of compound animal feed with an aflatoxin content

certified at around 10 Mg/kg, b) to organise a study of a proposed Community method for determination of the toxin

in compound feeds.

RESULTS

A preliminary intercomparison study showed that good agreement could be obtained with methods modified to eliminate interference by manioc and citrus pulp at a level of 15 μg/kg. Good results were also obtained by immuno-assay methods (test kits and immuno-affinity columns). A candidate Community method based on HPLC was successfully collaboratively tested by 25 laboratories including those officially nominated for the study by the Member States. The method will be given official Community Status in 1992. Compound feed reference materials containing aflatoxin B, at around 1 and 10 μg/kg have been prepared and shown to be homogeneous and stable. Certification measurements are completed on all materials and the materials will be issued in 1992. The project is terminated (EUR report in preparation).


ECU 42 100

PARTICIPANTS

Administration des Services Techniques de l'Agriculture, Ettelbrück, L - Central Veterinary Laboratory, Surrey, UK - CIVO/TNO, Zeist, NL - Hendrix'Voeders BV, Boxmeer, NL - Instituto Sperimentale per la Zootecnia, Roma, I - Instituto Superiore di Sanità, Roma, I - Laboratoire de Biochimie-UFAC, Vigny, F -Laboratoire Municipal de Bordeaux, Bordeaux, F - Laboratoire de la répression des fraudes. Rennes, F -Laboratorio Nacional de Engenharia e Tecnología Industrial, Lisboa, Ρ - Laboratorio de Sanidad y Producción Animal, Madrid, Ε - Laboratorio do Instituto de Qualidade Alimentan', Lisboa, Ρ -Laboratorium voor Bromatologie, Gent, Β - Laboratory of the Government Chemist (LGC), Teddington, UK -

Landwirtschaftliche Untersuchungs- und Forschunsanstalt, Kiel, D - Leatherhead Food Research Association, Surrey, UK - Ministerio de Agricultura, Madrid, Ε - Ministry of Agriculture, Athens, GR -Rijks-Kwaliteitsinstituut voor Land- en Tuinbouwprodukten (RIKILT), Uageningen, NL - Rijksinstituut

voor Volksgezondheid en Milieu Hygiene (RIVM), Bilthoven, NL - Rijksontledîngslaboratorium, Antwerpen, Β - Royal Veterinary & Agricultural University, Copenhagen, DK - State Laboratory, Dublin, IRL - Statens Foderstofkontrol, Lyngby, DK - Ufficio per la Prevenzione e La Repressione delle Frodi Agro-alimentari, Roma, I. - Universität München, Freising, D.

172

PROJECT RM 368

AFLATOXIN B, IN PEANUT MEAL (Animal Feed)

PROJECT DEFINITION

In order to keep the levels of aflatoxin M, in milk acceptably low, the levels of its precursor, anatoxin B, in cattle feed are controlled through Community legislation (DIR 74/63/EEC et seq.). Peanut meal, an important component of animal feed, is particularly vulnerable to attack by the moulds which produce aflatoxin B, and imports are consequently subject to routine monitoring both by official laboratories and the animal feed industry.

RESULTS

Two intercomparisons have been undertaken and have led to considerable improvement in between-laboratory agreement. The second study involving 18 laboratories showed, in particular, the importance of allowing for incomplete recovery. Excellent agreement was achieved with a coefficient of variation of 9% at a level of 44 ¿tg/kg. Three peanut meal reference materials have been prepared and have shown to be acceptably homogeneous. The materials are made from naturally contaminated samples and have an aflatoxin B, content of 2 ^g/kg (an effective blank), 50 and 180 ßglkg, levels corresponding to Community limits. Stability was confirmed and the certification study is completed. The materials will be issued in 1992. The project is terminated (EUR report in preparation).


ECU 70 000

PARTICIPANTS

Agricultural University, Copenhagen, DK Central Veterinary Laboratory, Surrey, UK C1V0-TN0, Zeist, NL Institut für Angewandte Botanik, Hamburg, D Instituto Superiore di Sanità, Roma, I Istituto di Scienze della Nutrizione, Piacenza, I Keuringsdienst van Waren voor het Gebied Rotterdam, Rotterdam, NL Laboratory of the Government Chemist (LGC), Middlesex, UK Laboratoire Central de la Répression des Fraudes, Massy, F Leatherhead Food Research Association, Surrey, UK MAFF, Norwich, UK Max-von-Pettenkofer-Institut, Berlin, 0 MiIchwirschaftliche Untersuchungs- und Versuchsanstalt, Kempten, D National Food Institute, Soborg, DK Netherlands Inspection Institute for Milk and Milk Products, Leusden, NL Plasmon Oíetetici Alimentan' Spa, Milano, I RHM Research Center, Bucks, UK Rijksinstituut voor Volksgezondheid en Milieu Hygiene (RIVM), Bilthoven, NL Royal Veterinary & RijksKwaliteitstinstituut voor Land- en Tuinbouwprodukten (RIKILT), Uageningen, NL Rijksuniversiteit Gent, Gent, Β State Laboratory, Dublin, IRL

The Agricultural Institute, Carlow, IRL

Tropical Development and Research Institute, London, UK

Unilever Research Laboratories, Beds, UK.

173

PROJECT RM 358

DETERMINATION OF CHLORINATED PESTICIDES IN ANIMAL FEED

PROJECT DEFINITION

The use and the production of organochlorine pesticides (OCPs) e.g. HCB, HCH, the drins, DDT etc has been banned for a long time in EC countries. However, these compounds are highly stable and therefore they are still present in the environment. As a consequence they can be detected in soils and in plants growing on land which has been treated even years ago. Finally, these pesticides bioaccumulate in the food chain. In developing countries, origin of the basic material for animal feed, chlorinated pesticides are still in use. OCPs from third world could enter the food chain through imports of raw materials. As a consequence, it is necessary to detect them in food or animal feed imported from such countries. The OCP contents in animal feed have been regulated by an EC Directive 74/63 which has been recently modified. A certified reference material is needed to improve the quality of the determination of the OCPs in feed. The candidate CRM consists in animal feed enriched with chlorinated pesticides to reach a value around the Maximum Residue Limits set in the modified EC Directive.

STATUS

The material is under production, the homogeneity and stability studies started in 1991. Certification could be achieved in 1992



PARTICIPANTS

Agricultural Research Center of Finland, SF Boter- en Kaascontrolest, Leeuwarden, HL Chemisches Untersuchungsamt, Münster, D CIV0-TN0, Zeist, NL Istituto Superiore di Sanita, Roma, 1 Keuringsdienst van Waren, Utrecht, NL Laboratoire Municipal et Régional, Rouen, F L.A.R.A., Toulouse, F Milchuirtschaftliches Untersuchungs- und Versuchsanstalt, Kempten, D Ministerede l'Agriculture, Paris, F National Food Institute, Soeborg, DK Nestlé Products, La Tour de Peilx, CH RIKILT, Uageningen, NL RIVM, Bilthoven, NL Shell Research Ltd., Sittingbourne, UK Staatliche Veterinäruntersuchungsanstalt, Hannover, D Statens Livsmedelsverk, Uppsala, S The National Food Center, Dublin, IRL Universidad de Zaragosa, E

174

PROJECT RM 384

DETERMINATION OF AMINO ACIDS IN ANIMAL FEED Development of a Community Method and Reference Materials

PROJECT DEFINITION

The efficiency of animal feed, especially for intensive farming, depends heavily on the contents of several amino acids (methionine, threonine, cystine, lysine and tryptophan). These compounds are commonly added to low grade protein waste materials to produce feed with sufficient nutritive value. Community legislation (Directive 77/101/EEC and 79/373/EEC) obliges declaration of certain of these compounds in feeds for specified animals and lays down the acceptable tolerances for the accuracy of the declaration. However, several Member States have indicated that they will refuse further development of this legislation until a Community method is adopted. The objective is therefore to develop a Community method and reference feeds to assure its correct application.

STATUS

After two intercomparisons, it has been shown that there were no detectable differences in the results of 14 laboratories even though the proposed candidate method (based on ion-exchange chromatography) allowed four variations (open and closed vessel, HBr and metabisulphite oxidation). The method will be recommended as a candidate Community method. The preparation of reference materials (mixed pig feed, low fat fish meal, soya bean meal, skim milk powder and a calibration solution) has been completed and certification will be undertaken in 1992.



PARTICIPANTS

Agrilab, Antwerpen, Β - Central Laboratories Tjele, DK - CIVO-TNO Institute, Zeist, NL - Degussa AG, Hanau, D - Deutsches Institut für Lebensmitteltechnik, Quackenbruck, D - Dipartimento di Science Zootecniche dell' Universita, Firenze, I - Faculté des Sciences Agronomiques de l'Etat, Gembloux, Β -Finnish Customs Laboratory, Espoo, SF - Hewlett-Packard-GmbH, Ualdbronn, D - I.V.V.O., Lelystad, NL -Instituto Sperimentale per la Zootecnia, Roma, I - Laboratoire de la Répression des Fraudes, Rennes, F - Laboratorio Arbitral, Madrid, E - Laboratorio Nacional de Engenharia e Technologie Industrial, Lisboa, Ρ - Laboratory of the Government Chemist, Teddington, UK - LUFA, Kiel, D - National Laboratory for Agricultural Chemistry, Uppsala, S - RADAS, Oeinze, Β - Rijksontledingslaboratorium. Gentbrugge, Β - Service Technique à l'Agriculture, Ettelbrück, L - State Laboratory, Dublin, IRL - Statens Foderstofkontrol, Lyngby, DK - UK, Ministry of Agriculture, Athens, GR - Universität München, Freising, D - University Uppsala, Uppsala, S.

175

PROJECT RM 413

IMPROVEMENTS IN THE DETERMINATION OF TRYPTOPHAN IN FEED

PROJECT DEFINITION

This project is an extension of project 384 the objective of which is to develop an official Community method for amino acids in animal feed and reference samples in support of the Directives on feed labelling (77/101/EEC and 79/373/EEC). Tryptophan is destroyed during the acid hydrolysis of proteins made to liberate other amino acids and therefore must be determined by using another method with alkaline hydrolysis before ion exchange chromatography or HPLC determination.

STATUS

The first intercomparison of methods commonly used for tryptophan in 5 feed RMs has been completed and has identified a candidate official method for further evaluation. It is proposed to certify the tryptophan content in the feed samples prepared for amino acid analysis (project 384).



PARTICIPANTS

AB Analycen( Lidköping, S Bayerische Hauptversuchanstalt für Landwirtschaft, Freising, D Degussa AGf Hanau, D Faculté des Sciences Agronomiques de l'Etat, Gembloux, Β Istituto Superiore per la Zootecnia, Roma, I IWO, Lelystad, NL -Laboratoire Interrégional du DGCCRF, Rennes, F Laboratory of the Government Chemist, Middlesex, UK Landwirtschaftliche Untersuchungs- und Forschungsanstalt (LUFA), Kiel, LNETI, Lisboa, Ρ Ministerio de Agricultura, Pesca y Alimentación, Madrid, Ε Rijksontledings- laboratorium. Gentbrugge, Β State Laboratory, Dublin, IRL State Institute of Agricultural Chemistry, Vantaa, SF Statens Husdyrbrugsforsoeg, Tjele, DK TN0-CIV0 Institutes, Zeist, NL Université degli Studi di Firenze, I.

176

PROJECT RM 272

STILBENES (GROWTH HORMONES) IN FARM ANIMALS

PROJECT DEFINITION

The use of compounds having hormonal or thyreostatic action to fatten farm animals is prohibited by Community legislation (Directive 87/602/EEC et seq). However, their usage continues as is reflected by the frequency of prosecutions in several Member States. This is in spite of the extensive monitoring of farm animals (analysis of urine, bile or faeces) and of meat at import. For the stilbenes diethylstilbesterol (DES), hexoestrol (HEX), dienoestrol (DE), reliable measurements must be made at the low μg/kg level which places severe demands for sensitivity and specificity on the methods used. Official community methods are under development through the analytical sub-group of the Standing Committee on Veterinary Science (Directorate General for Agriculture, DG VI). This group has recommended the obligatory use of reference materials to confirm the correct application of the official methods and has requested that the BCR Programme should provide suitable materials to support the work of the National control laboratories.

STATUS

Lyophilised bovine urine reference materials containing (separately) DES, HEX and DE in the range 5-30 ug/1 (expressed on fresh urine) have been prepared and shown to be stable and homogeneous. Uncontaminated lyophilised urine reference materials were also prepared to test analytical sensitivity and to check immunological methods for false-positive results. Certification measurements based on GC-MS are complete and the reference materials will be issued in 1992. A batch of lyophilised bovine muscle containing DES has been shown to be stable and

homogeneous. Certification will follow in 1992.



PARTICIPANTS BCO Analytical Services BV, Breda, NL Bundesgesundheitsamt, Berlin, D Chemisches Landesuntersuchungsamt, Münster, D Inst, für Pharmakologie und Toxicologie der Universität Uürzburg, Würzburg, D Institute for Hygiene and Epidemiologie, Bruxelles, Β Laboratorium voor Bromatologie, Gent, Β Landeshauptstadt Stuttgart Chemisches Untersuchungsamt, Stuttgart, D Ministry of Agriculture, Fisheries and Food (MAFF), Surrey, UK Rijkskualiteitsinsituut voor Land- en Tuinbouwprodukten CRÍKILT), Wageningen, NL Rijksinstituut voor Volksgezondheid en Hilieu Hygiene, Bilthoven, NL RIVM, Bilthoven, NL TNO-CIVO Toxicology and Nutrition, Zeist, NL.

177

PROJECT RM 339

NOR-TESTOSTERONE ΓΝ CATTLE URINE AND MEAT RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs for support of Community Policy banning the growth promoting compounds in farm animals. Relevant Directives/regulations include : 81/602/EEC and 85/358/EEC banning the use of hormonally active compounds in farm animals, 86/469/EEC laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (sampling frequency).

Nor-testosterone, an androgenic substance with potent growth promoting ability and which does not occur naturally in farm animals, except the male horse. It is commonly found in "illegal" cocktails used for treating cattle.

The project will consist in preparing samples of muscle and of urine from cattle :

treated with nor-testosterone never treated with nor-testosterone (blank).

The reference materials are mainly intended for use by National control laboratories.

STATUS

Initial stability studies of urine RMs demonstrated instability at + 4 °C and above. A further study to investigate the use of additives to stabilize the urine RMs is underway and will be completed in 1992.



PARTICIPANTS

Bundesgesundheitsamtes, Berlin, D Central Veterinary Laboratory, Ueybridge, UK Institut d'Hygiène et d'Epidémiologie, Brussels, Β Rijks- Kwaliteitsinstituut voor Land- en Tuinbouwprodukten, Uageningen, NL Rijksinstituut voor Volksgezondheid en Milieuhygiëne, Bilthoven, NL Univ. Gent, Gent, B. Univ. Uurzburg, D Univ. Kaiserlautern, D

178

PROJECT RM 344

SULPHADIMIDINE IN PIG KIDNEY, LIVER AND MUSCLE RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals and the Directive laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (86/469/EEC).

Sulphadimidine is a member of the sulphonamide group of drugs. It is a broad spectrum antibiotic widely used in animal production either alone or in combination with other sulphonamides and antibiotics. It has a bacteriostatic action but when combined with trimethoprim, it produces a synergic effect which is both bacteriostatic and bactericidal. Its use has been widely detected in farm animals with a significant percentage of pigs having residues in excess of the tolerance of 0.1 mg/kg. It is the drug with the highest number of violations of the directive 86/469/EEC. It is routinely monitored in Member States with the National Monitoring Programs. Monitoring is primarily in meat and offal.

The objective of the project is to prepare sample of pig muscle, liver and kidney from animals: treated with sulphadimidine never treated with sulphadimidine.

Collaborative work between the major national laboratories to improve methods and results will be undertaken.

STATUS

Initial stability studies of liver RMs with additives are successfully completed and optimized lyophilization and irradiation conditions have been established. Preparation of the final batch of liver RMs is in progress. Preparation of preliminary batches of muscle and kidney RMs will be completed in 1992.



PARTICIPANTS

Preparation of materials: Veterinary Research Laboratory, Ministry of Agriculture, Food & Fisheries, Stormont, UK.

National monitoring laboratories & other specialized laboratories; to be determined.

179

PROJECT RM 346

THYROSTATICS IN CATTLE URINE AND MEAT RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals and the Directives laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (86/469/EEC).

The thyrostatics are substances with an anti-thyroid action which cause increased weight gain in cattle but without beneficial effect on edible meat (protein and fat). There are five thyrostats, tapazole and four 2-thiouracil derivatives, which could be administered in large regular doses in illegal treatment of cattle.

The objective of the project is to prepare samples of lyophilised urine and muscle of cattle: treated with thyrostatics never treated with thyrostatics.

These materials will then be used in intercomparison between the major national laboratories to improve methods and results.

STATUS

Selection of materials are completed and preliminary stability studies of urine RMs may be undertaken in 1992.



PARTICIPANTS

Preparation of materials: Rijksinstituut voor Milieu en Hygiene (RIVM), Bilthoven, NL.

National monitoring laboratories; to be identified.

180

PROJECT RM 347

TRENBOLONE IN CATTLE URINE AND MEAT RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals and the Directive laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (86/469/EEC).

Trenbolone is an exogenous androgenic substance with potent growth promoting ability. It was licensed in some Member States prior to the ban and is still licensed in some third countries including the USA It is normally administered as an implant but a solution in oil is also manufactured and may be incorporated into illegal 'cocktails'.

The project will involve the preparation of lyophilised urine and muscle from cattle: treated with trenbolone never treated with trenbolone.

The materials are mainly intended for use by the National control laboratories.

STATUS

A blank and a trenbolone containing urine RM have been prepared. Final homogeneity studies are completed and the final one year stability study is underway. Certification measurements on these materials are planned in 1992.



PARTICIPANTS

Preparation of materials: Urine: Rijksinstituut voor Milieu en Hygiene (RIVM), Bilthoven, NL.

National monitoring laboratories; to be determined.

181

PROJECT RM 362

BETA-AGONISTS IN CATTLE AND PIG TISSUES AND URINE RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals and the Directives laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (86/469/EEC) and laving down criteria for reference methods used in pursuance of the monitoring programs (87/410/EEC).

Beta-agonists are a group of pharmacologically active compounds which are well established for treatment of specific conditions such as asthma in man. They are also approved for specified veterinary treatments. A more recently discovered effect of these drugs is that they alter the growth of animals either by increasing growth rate or more importantly by repartitioning nutrients in favour of the production of more lean meat and less fat. The compounds are known to be widely used illegally in meat producing animals to yield leaner higher value meat.

They are routinely monitored in Member States with the National Monitoring programs. Monitoring may be in urine or meat. Some 12 of these compounds have been identified as having been used for illegal purposes in farm animals.

The project will consist in the preparation of a number of materials such as lyophilised urine, muscle and liver from animals:

treated with either clenbuterol or salbutamol or cimaterol (pigs only) never treated with beta-agonists.

The materials are mainly intended for use by the National control laboratories.

STATUS

Preparation of materials and initial stability studies will be completed in 1992.



PARTICIPANTS

Preparation of materials: Rijks-Kwaliteitsinstituut voor Land- en Tuinbouwprodukten (RIKILT), Wageningen, NL Rijksuniversiteit, Ghent, Β.


182

PROJECT RM 364

CHLORAMPHENICOL IN MEAT, MILK AND EGGS RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals and the Directives laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (86/469/EEC) and laying down criteria for reference methods used in pursuance of the monitoring programs (87/410/EEC).

Chloramphenicol is a broad spectrum antibiotic substance used to treat a number of bacterial infections in cattle, pigs and poultry. It is a toxic substance which can cause aplastic anaemia in humans and animals. The use of safer alternative antibiotics is strongly recommended.

The project will involve the preparation of lyophilised muscle, skimmed milk and eggs from animals:

treated with chloramphenicol never treated with chloramphenicol.

These materials will be used for collaborative exercises involving the national laboratories to improve methods and results.

STATUS

The candidate RMs have been prepared and are undergoing stability studies. Certification is expected in 1992/1993.



PARTICIPANTS

Preparation of materials: Bundesgesundheitsamt (BGA), Berlin, DE.


183

PROJECT RM 365

ZERANOL IN CATTLE URINE AND MEAT RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals. Zeranol is an exogenous oestrogenic substance with potent growth promoting ability. It was licensed in some Member States prior to the ban and is still licensed in some third countries including the USA. It is normally administered as an implant but it may be incorporated into illegal 'cocktails'. It is monitored in urine, faeces (on-site inspection), bile and in muscle. The project will involve the preparation of samples of lyophilised urine, liver and muscle from cattle:

treated with zeranol never treated with zeranol

STATUS

Preparation of materials and initial stability studies will be completed in 1992.


ECU 110 000 (estimated).

PARTICIPANTS

Preparation of materials: The National Food Center, TEAGASC, Dublin, IRL


184

PROJECT RM 366

OXYTETRACYCLINE (OTC), DIHYDROSTREPAMYCIN (DSTREP) AND AMPICILLIN IN CALF MUSCLE AND COW MILK RMs

PROJECT DEFINITION

The project is one of a series initiated at the request of the Commission's Agricultural Services (DG VI) to provide RMs in support of Community Policy banning the use of growth promoting compounds in farm animals and the Directives laying down requirements for monitoring of undesirable substances in farm animals and products in Member States (86/469/EEC) and laying down criteria for reference methods used in pursuance of the monitoring programs (87/410/EEC).

The three drugs are broad spectrum antibiotics widely used in animal production either alone or in combination with other antibiotics. A major use is for the treatment of udder infections in lactating dairy cattle. OTC is often used for pigs.

The project will involve the production of lyophilised muscle and lyophilised milk: treated with the three antibiotics never treated with the three antibiotics.

The material will be mainly used by the National control laboratories.

STATUS

Preparation of materials and initial stability studies in milk began in 1991.

CONTRTBUnON OF THE COMMISSION


PARTICIPANTS

Preparation of material: Laboratoire des Médicaments Vétérinaires, Centre National d'Etudes Vétérinaires et Alimentaires, Fougères, F.


185

PROJECT RM 381

DEVELOPMENT OF A COMMUNITY METHOD FOR THE DETERMINATION OF BETA-AGONISTS IN ANIMAL FEED

PROJECT DEFINITION

Beta-agonists are widely used in human medicine for the treatment of asthma and certain heart conditions. At higher concentrations, they also have the ability to increase the proportion of lean meat relative to fat in farm animal and to increase total weight with obvious financial benefit for the producers. Although this practice is forbidden by Community legislation (Dir EEC/86/469) there are many examples of illegal use. The compounds are added to animal feed or drinking water and recently, a major feed company was prosecuted for incorporating the compounds in their products. Claims that beta-agonists are present in animal feed have recently resulted in one Member State banning imports from another. The Community is therefore in urgent need of a method to regulate and resolve such disputes and enforce legislation. The methods need to be capable of detection of a wide range of compounds and will probably focus on immuno-affinity columns coupled to HPLC or GLC.

STATUS

The first intercomparison of methods involving 13 laboratories identified problems of extraction and clean-up. An extraction and clean-up study involving 4 laboratories was started in 1991 and should lead to a candidate "modular" Community method. The proposed method will be tested in a final intercomparison in 1992.



PARTICIPANTS

Boehringer-Ingelheim, Ingelheim, D Bundesgesundheitsamt, Berlin, D Central Veterinary Laboratory, Ueybridge, UK Centro Nacional de Alimentación, Carretera Hajadahonda, Madrid, E Chemische Untersuchungsanstalt der Stadt Stuttgart, Stuttgart, D Chemisches landesuntersuchungsamt, Münster, D Ecole Nationale Vétérinaire, Nantes, F Instituut voor Hygiene en Epidemiologie, Β I st i tuto Super ion' di Sani ta, Roma, I Isti tuto Superi ore di Sanità, Roma, I Laboratoire Interrégional du D.G.C.CR.F., Rennes, F Laboratoire Interrégional de la Répression des Fraudes, Rennes, F Ministry of Agricultural Plant, Directorate Laboratory Division, Lyngby, DK. Rijksontledingslaboratorium. Gentbrugge, Β RIKILT, Wageningen, NL RIVM, Bilthoven, NL State Laboratory, Dublin, IRL

186

PROJECT RM 309

OIL CONTENT OF RAPESEED

PROJECT DEFINITION

The price paid by seed-crushers directly depends on the oil content of rapeseed and it is therefore essential to have rapid and accurate methods that can be used ih the factory situation. Oil content is also important for reasons connected with the Common Agricultural Policy (CAP). Traditionally, oil in rapeseed has been determined by solvent extraction methods, slow and potentially hazardous procedures which are being replaced by rapid, non-destructive methods based on Nuclear Magnetic Resonance (NMR). Calibration of these methods can be conveniently made with rapeseed having an oil content determined by a solvent method. There are three similar solvent methods in use for different purposes, ISO and EEC methods and that of the trade association FOSFA. These methods differ in details which could give rise to small but significant systematic differences in the results. The object of the work is to compare the results given by the three methods and, if possible, to assign a common reference value for oil content to three rapeseed reference materials required for NMR calibration.

RESULTS

The certification of 3 rapeseed reference materials is completed. The reference materials will be available by the end 1992. The provisional certified values for the oil content (expressed on dry matter) are as follows:

CRM 446 (Low Oil Content): 42.5 ± 0.1 % CRM 447 (Medium Oil Content): 45.3 ± 0.2 % CRM 448 (High Oil Content): 49.2 ± 0.2 %

The project is terminated (EUR report in preparation).


ECU 30 000

PARTICIPANTS

Aarhus Olie, Aarhus, DK Acietes y Proteínas, Rapeloga, Portugalete, E Associazione Granaría, Milano, I Centraal Laboratorium, Brussels, Β Centre Technique Interprofessionnel des Oléagineux Métropolitains, CETIOM, Ardon, F Chemical Laboratory Dr. P. Wiertz, Hamburg, D Chemical Laboratory Dr. A, Verwey, Rotterdam, NL Danish State Seed Testing station, Lyngby, DK E.R. Bolton, London, UK Laboratoire Crépîn, Paris, F Laboratoires Wolff, Clichy, F Laboratorium Oleotest, Antwerp, Β Leatherhead Food Research Association, Surrey, UK McDonnell Co. Ltd., Drogheda, IRL Salomon & Seaber, London, UK State Laboratory, Dublin, IRL Verein Deutscher ölfabriken, Deutsche Lebensmittelwerke, Mannheim, D.

187

PROJECT RM 334

DEVELOPMENT OF A METHOD FOR THE DETERMINATION OF DRY GLUTEN IN DURUM WHEAT

PROJECT DEFINITION

The quality of durum wheat is determined by measuring its gluten and protein content Limits of these two parameters are given by the EEC Regulation on durum wheat quality (EEC 2731 modified by 2094/87).

Protein is measured by NTR or Kjeldahl methods but there is no agreed method for the gluten determination in durum wheat.

The Council asked the Commission to propose an agreed method. A procedure suggested by the Italian pasta industry will be subject of a collaborative study involving the main laboratories of the Member States working in this field.

RESULTS

An intercomparison was carried out in 1990 to study moisture, protein, wet gluten and dry gluten in durum wheat (grain and flour). The study showed that the use of different types of grinders to prepare the sample did not. affect the results as had been expected. The repeatability was 5% and the reproducibility was 20% for the dry gluten method. The project is terminated.


ECU 14 100

PARTICIPANTS

Barilla S.p.a., Parma, I BIPEA, Paris, F Bundesforschungsanstalt für Getreide- und Kartoffelverarbeitung, Institut für Müllertechnologie, Detmold, D Cereal Institute, Chemistry/Technology Department, Thessaloniki, GR Flour Milling and Baking Research Association, Chorleywood, UK Istituto Sperimentale per la Cerealicultura, Roma, I Laboratoire Central, Ministère des Affaires Economiques, Bruxelles, Β Laboratoire Institut Technique des Céréales et des Fourrages (I.T.C.F.), Paris, F Panzani, Semoulerie de Bellevue, Marseille, F Servicio Nacional de Productos Agrarios, Madrid, Ε.

188

PROJECT RM 338

NIR SPECTROMETRY FOR CEREAL AND FEED QUALITY CONTROL

PROJECT DEFINITION

Near infrared Spectrometry offers considerable potential for very fast determination of the properties of agricultural products (protein, water, fat content). However, the method requires a calibration procedure which is difficult to develop.

Intercomparisons organized by a group of laboratories under the auspices of the Commission's Agricultural Services (DG VI) for the characterization of silage gave very disappointing results.

The present project will be conducted on the determination of protein in wheats and a rather rigorous approach will be followed to calibrate the spectrometers. The objective of the project is to test methodology to establish correlation between spectrometers so that acceptable and reliable results can be obtained.

STATUS

To begin in 1992.



PARTICIPANTS

BFHBRA, Chorleywood, UK Centro Experimentale Agrario, ViUaciosa, E Danish Dairy Board, Brorup, OK Escuela Técnica Superior de Ingeniero Agrónomos y de Hontes de Cordoba, E Federal Research Center of Agriculture, Braunschweig, D Finnish Grain Board, Helsinki, SF Generalität de Catalunya, Laboratorî Agrari, Cabrila, E Institut National de la Recherche Agronomique, Nantes, F NOSCA, School of Agriculture, Aberdeen, UK Scottish Agricultural Statistics Service, SCRI, Dundee, UK Station de Haute Belgique, Lîbramont, Β Tecator, Hoganäs, SE

189

PROJECT RM 373

RENNET WHEY IN MILK POWDER

PROJECT DEFINITION

The Community pays aid of 35% to the skim milk powder used in animal feed. The addition of rennet whey powder (the dried lactose serum remaining after removal of fat and precipitation of proteins for cheese manufacture) is specifically forbidden.

Assuming an average price of 2.3 ECU/kg skim milk powder, approximately 1 χ 10' ECU of Community funds is involved. Even if only 1% of the total amount of milk powder is adulterated the loss to the Community would be around 10 million ECU.

There are at present, two HPLC methods available for the detection of rennet whey solids in skim milk and buttermilk powder but they have several disadvantages.

The objective of the project is the development of a rapid, highly specific reversed phase HPLC-method for the accurate determination of the content of rennet whey solids in milk powders which is not influenced by the ratio of the a and b variants of the glycomacropeptides in the sample.

STATUS

Work on a feasibility study for preparation of glycomacropeptides a and b in large amounts as reference materials is in hand.

A study for identification of the best extraction and clean-up method variations for determination of a and b glycomacropeptides will be finished soon.



PARTICIPANTS

Development of method:

National Institute for Dairy Research (NIZO), Ede, NL.

Evaluation of method: participants not yet identified.

190

PROJECT RM 374

IMPROVEMENTS IN INFRA-RED SPECTROSCOPIC ANALYSIS OF MILK

PROJECT DEFINITION

The fat and protein content largely determine the value of milk. These properties are determined on a daily basis in all European dairy producing countries for payment to farmers where central control laboratories are used and for quality control in industry before processing. In France, some 35 χ 10* individual samples are analyzed each year. In the UK, approximately 2 χ 10* samples are analyzed just for payments to farmers which amount to 2 χ 10' ECU per year. Infra-red spectroscopy provides a rapid and cost-effective means of determining fat, protein and lactose and is used for almost all these assays. It relies on the absorption of certain wavelengths of IR light which are characteristic of these components. In practice, minor components in milk also absorb at these wavelengths. Because of the variation in the concentration of these components with season, stage of lactation, animal species, feed, etc., it is necessary to make local calibration with samples of similar composition to those being analyzed. The objective is to study the variation in interfering components with season, geographical region and species with a view to understanding the origin of the errors in IR analysis. Chemical composition will be compared with IR spectra to identify the combination of wavelengths which yield the most specific determination of protein, fat and lactose. Success would lead to much greater efficiency and to the wider application of IR spectroscopy for milk analysis.

STATUS

A pilot study involving 11 Member State laboratories has demonstrated the feasibility of the project. The main study, involving in addition 3 EFTA countries will study geographical and seasonal influences on milk composition and IR calibration in a 12 month study involving 8 intercomparisons during 1992/1993.


ECU 175 000

PARTICIPANTS

Centro Investigación y Desarrollo La Lacteria Española, Renedo de Piélagos, E - COZ, Leusden, NL -Departamento de Tecnológica das Industrias Alimentares, Lisboa, Ρ - Ecole Supérieure d'Agriculture d'Athènes, GR - Institut National de Recherches Agronomiques UNRA/LTAN), Nantes, F - Institut National de Recherches Agronomiques (INRA), Station de Recherche en Technologie et Analyses Laitières, Poligny, F - Istituto Sperimentale Lattiero-Caserîa, Lodi (Milano), l - Laboratorio Agrario del Estado, Santander, Ε - Laboratory of Dairy Technology, Thessaloniki, GR - Milchwirtschaftliche Lehr- und

Untersuchungsanstalt, Hanover-Ahlem, D - Milk Marketing Board, Thames Ditton, UK - National Dairy

Products Research Centre, Cork, IRL - Nederlands Instituut voor Zuivelonderzoek (NIZO), Ede, NL -

Rijkszuivelstation, Melle, Β - Statens Mejeriforsog, Hillerod, DK

191

PROJECT RM 377

DETERMINATION OF AMYLOSE IN RICE

PROJECT DEFINITION

Rice is grown in ßve of the twelve Community Member States (Italy, Spain, Portugal, Greece and France) who together achieve an annual production of 1.3 million tonnes of milled rice. This figure would mean the Community is 90% self-sufficient in rice if all the crop were of the type required by the rice millers. However, short-grain varieties are produced far in excess of market requirements in the Community whereas 45% of consumption of long-grain Indica rice is imported from third country suppliers, mainly USA, Thailand and Surinam. In order to promote the selection and production in the Community of Indica rice, the Community pays a subsidy to growers which is based on morphological, chemical (amylose content) and cooking quality criteria. Decisions on whether or not EEC could give aid for each proposed variety of rice are based on minimum and maximum values for each of the criteria which are contained in the Regulation. Problems were encountered in the first year of operation of the Regulation as a result of the wide variation in test results of amylose determination obtained by Community laboratories. The determination of amylose content in rice is carried out according to ISO 6647:1987. The objective of the project is to prepare three batches of rice reference materials having amylose contents about 15 %, 20 % (critical value in the above Regulation), and 25 %.

STATUS

The 3 batches of rice reference material have been prepared. Before certification of the amylose contents is attempted, a preliminary study will be carried out during 1992 to identify any methodological problems.



PARTICIPANTS

BIPEA, Paris, F CSIC, Instituto Agroquimicà de Tecnología de los Alimentos, Valencia, E Ente Nazionale Risi, Castello d'Agogua, I FHBRA, Hertfordshire, UK Laboratoire de Technologie des Céréales, Montpellier, F TNO-IGMB, Uageningen, NL.

Additional participants to be identified.

Environment

195

PROJECT RM 238

TRACE ELEMENTS IN FISH

PROJECT DEFINITION

In addition to being an important part of the diet, fish is a product of major commercial interest in many Member States. Reliable knowledge of trace element contents is thus required for reasons of public health (toxic and nutritional elements) and to ensure that fish products satisfy national regulations e.g. the Italian legislation which specifies maximum permissible limits of 0.5 jug/kg for methyl mercury and 0.8 /ig/kg for total mercury. Reference materials (RMs) are widely required to ensure quality in trace element analyses. This RM of fish completes a series of CRMs produced to support analyses related to marine environment (e.g. mussel tissue CRM 278, sediment CRM 277 and seawater CRM 403).

RESULTS

Certification concluded (CRM 422, EUR Report in press).


ECU 72 500

PARTICIPANTS

Biologische Anstalt Helgoland, D CBMN, Β Centre National de Recherche Scientifique, CNRS, F CIVO/TNO, NL Danish Isotope Centre, DK ECN, NL Gesellschaft für Strahlen- und Umweltforschung GmbH, D IFREMER, F Institut für Spektrochemie, D IRI/TU Delft, NL Istituto Superiore di Sanita, I Labor für Spurenanalytik, D National Food Administration, Uppsala, S National Food Agency, DK PHP Sezione Chimico, Venezia, I Rijksuniversiteit Gent, Β RISK National Laboratory, DK Rijksinstituut voor Volksgezondheid en Milieu Hygiene , RIVM, NL Univ. de Oviedo, E Univ. di Pavía, I Universidad Complutense, E Universitaire Instelling Antwerpen, Β

196

PROJECT RM 249

REFERENCE MATERIALS FOR THE ANALYSIS OF PLANTS FOR ANIMAL FEED

PROJECT DEFINITION

Grass and clover for animal feed are routinely analysed to determine elements of nutritive quality (e.g. Ca, Mg, Κ, Ρ, Ν, Μη...) and of potential risk (e.g. Cd, Hg, As...). The results of determination of nutritive elements are used in the design of a well-balanced veterinary diet; the determination of the dangerous elements is necessary to avoid that the health of domestic animals is affected, which would lead to a lower production (economic loss) or even could harm man as consumer of animal products (milk, meat, etc.) Selenium is an important element for cattle; many diseases (muscle dystrophy, lack of protein production) are caused by feed with a low Se-content. Ruminants have a poor resorption of Se because their intestinal flora partly immobilises Se; hence a Se-rich diet is necessary to avoid Se-deficiency. Reference materials are helpful to avoid disputes on the quality of any of the raw materials for the preparation of animal feed. In addition, plant materials such as grasses are analysed as indicators of soil pollution with plant available element species. Hence they play an important role in environmental analysis.

RESULTS

Rye-Grass (CRM 281) was certified for: As, Cd, Cu, Hg, Mn, Pb, Se, Zn, Β, Mo, Ni, Sb (EUR Report 11839, 1988). The Hay-powder (CRM 129) was certified for: Zn, Ν, S, Ρ, Κ, Ι, Ca, Mg (EUR Report 12473, 1989).


ECU 116 000

PARTICIPANTS

7 laboratories from 9 Member States (and the Joint Research Centre (BCMN) Geel (Β) participated in the Rye Grass certification campaign. The following laboratories participate in the certification of Hay Powder: An Foras Taluntais, UK - Aristotetian Univ. , GR - BCMN, Β - Centre de Recherche de Bordeaux, f CNR, I -CNRS, F - ECN, NL - Gesellschaft für Strahlen- und Umweltforschung, D - Inst. v. Scheikundig Onder., 0 -Ist. Sup. Sanita, I - Kernforschung, 0 - Landesanstalt für Ökologie Recklinghausen, D - NCR " Demokritos", GR - Novo Industri, DK - Plymouth Polytechnic, UK - Queen's Univ., IRL - Riso National Lab., DK - RUG, Β -TNO, NL - Univ. Cordoba, E

197

PROJECT RM 250

REFERENCE MATERIALS FOR THE ANALYSIS OF THE AQUATIC ENVIRONMENT

PROJECT DEFINITION

The analysis of water is important to detect a source of pollution, to establish its pathways for monitoring purposes. The direct analysis of water is studied in projects 264 (rain water and trace element pollutants in sea and estuarine water) and 297 (components in surface and drinking water). Direct analysis, however, presents only the actual state of water quality. Pollutant concentrations may change rapidly depending upon the nature of the source (peak effluent emissions vs. steady effluent conditions), the nature of the water (strong currents have increased pollutant levels by sediment resuspension); the ionic strength, etc. To monitor changes over a longer period of time (weeks-years) indicator organisms are frequently analysed. These organisms (e.g. plankton, aquatic plants, shellfish) are in prolonged contact with water passing their sedentary place (mussels) or with moving water (plankton). Sediments are taken when it is necessary to study long or short term history of pollution. The stratigraphie pattern of pollution in a core of a sediment represents the fluctuation of pollution in time at a certain place. Therefore, it was decided to certify the contents of trace element pollutants (As, Cd, Cu, Hg, Pb, Se, Zn) in some indicator organisms and representative types of sediment. The materials finally chosen are: sea lettuce, mussel tissue, plankton and river-, lake and estuarine sediments.

RESULTS

The sea lettuce (CRM 279) has been certified for As, Cd, Cu, Pb, Se and Zn (Report EUR 11185, 1988). Mussel tissue (CRM 278) was certified for As, Cd, Cr, Cu, Fe, Hg, Mn, Pb, Se, Zn (Report EUR 11838, 1988). Three sediment estuarine sediments (CRM 277), lake sediment (CRM 280) and river sediment (CRM 320) were certified for As, Cd, Cr, Cu, Hg, Ni, Pb, Sc, Se, Zn (Report EUR 11850, 1988).


ECU 450 000

PARTICIPANTS

Sediments: S Mussel tissue : HT

Arbeitsgr. Anal, u Umwelt, D, (S) - Aristotelian Univ., GR, (HT) - BAH, 0, (S) - Centre Recherche & Contr-Eaux, F (S) - CNRS, F (HT) - Delta Inst. Hydrobiol. Res., NL, (HT,S) - Energie Onderzoekcentr., NL, (HT) -Gesellschaft für Strahlen und Umweltf., D (MT,S) - INRA, F, (S) - Inst, für Soil Fertility, NL (S) -Isotopcentrum, OK (MT,S) - JRC, I CHT,S) - Kernforschungsanlage, D CMT,S) - Riso National - Laboratory, DK (HT,S) - RIVM, NL (MT) - RUG, INS, Β (HT,S) - SCK/CEN, Β (S) - The Agrie. Inst., IRL, (HT,S) - The Hacaulay Inst.,UK (S) - TNO, NL (HT) - Univ. di Pavia, I (HT,S) - Univ. Instellingen, Β (S) - Univ. L. Pasteur, F (HT,S) - Univ. Regensburg, D (MT,S) Uater Research Centre, UK (S)

198

PROJECT RM 264

REFERENCE MATERIALS FOR THE ANALYSIS OF SEA WATER AND ESTUARINE WATER

PROJECT DEFINITION

Marine pollution is of prime concern to the Community (e.g. 75/437/EEC, COM(80) 361, COM(76) 688, 75/438/EEC). Important indicator elements (cone, down to 0.1 Mg/kg) in monitoring sea and estuarine water pollution are: Cd, Hg, As, Pb, Se, Cu, Zn and Cr. Besides the analytical difficulties e.g. caused by the low concentrations (sea water) or the presence of colloids (estuarine water), the major difficulties in certification are caused by stability and flocculation problems of the samples. Hence feasibility studies for the preparation and the verification of the stability formed a major part of the project.

STATUS

Certification of trace elements in seawater concluded (CRM 403) (EUR report 14061, 1992). First intercomparison of trace elements in estuarine water concluded in 1991. Certification of estuarine water in progress.


ECU 140 000 (certification of CRM 403) ECU 220 000 (certification of estuarine water, estimated).

PARTICIPANTS

Sea water: SU Estuarine water: EU

Aristotelian Univ., Thessaloniki, GR (EW) - Biologische Anstalt Helgoland, D CSU, EU) - Bund, für Seeschi f f fahrt und Hydrogr., D (SU, EU) - CNRS, Service Central d'Analyse, F (SU, EU) - ECN-Research Centre, Petten, NL (SU, EU) - Estacao Agronómica Nacional, Oeiras, Ρ (EU) - Inst. Hidrográfico, Ρ (SU, EU) - Inst. für Heereskunde, Rostock, D (EU) - KEMA, Arnhem, NL (SU, EU) - Kenn'ra Denmark, DK (SU, EU) - Lab. Contox, Madrid, E (EU) - Labor für Spurenanalytik, D (SU, EU) - MAFF Fisheries Lab., UK (EU) - New Univ. Lisbon, Ρ (EU) - ΝΙ0Ζ, Texel, NL (SU, EU) Rijksuniversiteit Gent, Β (SU, EU) - Rijkswaterstaat, NL (SU, EU) - SCK Mol, Β (SU,EU) · ΤΝ0 Applied Marine Res. Lab., Den Helder, NL (SU, EU) - TNO, Delft, NL (SU, EU) - Univ. Antwerp, Β (SU, EU) - Univ. Liverpool, UK (SU, EU) - Univ. di Pisa, I (SU) - Univ. di Venezia, I (SU) -Univ. Göteborg, S (EU) - Vandkvalitetsinst. Hoersholm, DK (EU) - Uater Res. Centre, UK (SU, EU).

199

PROJECT RM 278

CHEMICAL ANALYSIS TO MONITOR DAMAGE CAUSED BY ACID DEPOSITION

PROJECT DEFINITION

The effects of acid deposition ("acid rain") are strongest on poor soils with low buffering capacity, which are traditionally in use for forestry, and on lakes. The acid increases the mobilisation of trace elements and Al, decreases the uptake of nutritive elements by the root system, and renders species such as trees, more vulnerable to attach by fungi, bacteria, etc. Besides the environmental harm the economic consequences of damaged forests (effect on prices of wood, increased risk of avalanches, decrease of touristic appeal) and dead lakes (loss of fish production, harmful effects of mobilised trace metals on potential drinking water) are considerable. In order to save forests and lakes fertilisation with dolomite can help if the acidification or the damage to trees is in a relatively early stage. Estimates of forest damage are made mainly on a visual basis, which is time consuming, requires experienced inspectors and has a poor reproducibility in time. Recently a correlation between the content of nutritive elements (Mn, N, P, K, Mg), indicator elements (e.g. Al, S, F) in tree leaves or needles, and the health of the tree has been established, which allows to use chemical methods to assess the health of forest. Reference materials consequently were requested to compare the situation of forests of different types in different countries and to allow correct assessment of trend in forest damage. Indicator elements such as Al, Cl, S (damage) and P, N, Mg, Ca, Κ and Μη (nutritive state) were certified in beech leaves and spruce needles (first year's generation) taken from moderately affected forests NNE of the Ruhr-area (D).

RESULTS

Two reference materials - beech leaves and spruce needles - (CRM 100 and 101) were certified in 1989, EUR 12680 EN.

CONTRIBUTION

ECU 250 000

PARTICIPANTS

CNRS. Vernaison, F - ECN Energiecenlrum Penen, ÑL - Greek Atomic Energy Com., Athens, GR -1NRA Scichamps, F - lnsi. ofTerrcst. Eral., UK - Landesanslalt für Ökol., D - LNETI, Ρ - Novo Industri Bagsvard, DK - Plymouth Polytechnic, UK - Queen's Univ. of Belfast, IRL - Riso Nat. Lab., Roskilde, DK RUG, Gem, Β - The Agrie. Ins!. , Cumbria, IRL - TNO, Zeist, NL - Univ. Complulense, Madrid, E -Univ. Uc Cordoba, E - Univ. de Oviedo, E - Univ. di Pavia, I - Univ. La Sapicnza Roma, I - Univ. Ulm, D

200

PROJECT RM 297

REFERENCE MATERIALS FOR THE ANALYSIS OF FRESHWATER

PROJECT DEFINITION

The quality of surface and drinking water depends amongst other parameters also on its content of major components. Many European laboratories therefore routinely monitor such components in rain, surface-, tap-, and drinking water. The need for improvement of the quality of the determinations has led the BCR to produce as a part of a larger project (i.e. project RM 250) two certified reference materials of freshwater with a low mineral content (CRM 398) and a high mineral content (CRM 399). These materials were certified for their contents of Al, Ca, Cl, Fe, Mg, Μη, Ρ, Κ, Na and S. This project is being continued by the organization of a certification campaign of nitrate in three artificial freshwaters (low, medium and high nitrate contents).

STATUS

Certification of major elements in freshwater concluded (CRM 398 and 399) (EUR Report 14062,1992). First intercomparison on nitrate in freshwater concluded in 1991. Certification to be concluded by the end of 1993 (candidate CRMs 479, 480 and 481).


ECU 73 000 (certification of CRMs 398 & 399) ECU 100 000 (certification of candidate CRMs 479, 480 & 481)

PARTICIPANTS

14 laboratories from 8 Member States participated in the fresh water certification campaign: Anglian Water

Authorities, UK - CNRS, Service Central d'Analyse, F - ECN, NL - Fondazione Clínica del Lavoro, I -Gesellschaft für Strahlen und Umweltforschung, D - Ist. Italiano di idrobiol., I - Ist. Rie. Acque, I -KIWA, NL - Minist. Affaires Economiques, Β - Porthmouth Polytechnic, UK - Risoe Nat.Laboratory, DK - RUG, Β - Universidad Complutense, Ε - Water Quality Institute, DK

22 laboratories participate in the nitrate certification:

Anglian Water Authority, UK - Aristotelian Univ., Thessaloniki, GR - Centre d'Estudis de Blanes, E CNRS,

Service Central d'Analyse, F - Compagnie Générale des Eaux, F - ECN-Research Centre, NL EPAL, Lisboa, Ρ -GSF Neuherberg, 0 - Inst. Freshwater Ecology, UK - Inst. Hidrográfico, Ρ - Kemiteknik, Aarhus, DK - KIWA, Nieuwegein, NL - Min. Affaires Econ., Brussels, Β - PMP Sezione Chimico, Venezia, I - Portsmouth

Polytechnic, UK - South West Polytechnic, UK - Swedish EPA, S - Univ. de Cordoba, Ε - Water Quality

Institute, DK

201

PROJECT RM 316

HUMAN HAIR

PROJECT DEFINITION

A number of organizations are using the analysis of .human hair to detect possible exposure of the persons to heavy elements such as mercury. Hair gives an indication of the integrated doses ingested by the person over some months and is easier to collect than blood or urine. Hair analysis has been used already in many countries for large scale monitoring of the population and for forensic purpose (e.g. As and Ti). A large campaign of that kind has been started by the Italian Government for the monitoring of people along the sea coast who might be contaminated by fish from their diet. The BCR and the JRC were requested to contribute to this work by providing reference data and reference materials for quality control. A relatively large number of local laboratories will be involved and it is indeed important that they have means of ensuring that their results are comparable and can be put together for epidemiological study. Although the reliability of the conclusions that can be drawn from the analysis of hair is disputed by some experts, the fact that organisations that had certified human hair have quickly exhausted their stocks, indicates a great interest: QC for hair analysis. The objective of the project is therefore to certify the heavy metal contents (including mercury) in a batch of human hair already existing at ISPRA.

RESULTS

Certification concluded (CRM 397) (EUR Report 13422, 1992).


ECU 71 600

PARTICIPANTS

Aristotelian Univ., GR Centre for Radiochemistry, I CNRS, Service Central d'Analyse, F Coronel Lab., NL ECU-Research Centre, NL Facultad de Ciencias Univ. Complutense Madrid, E Forschungszentrum für Umwelt und Gesundheit, D Institut für Chemie, D Institut für Spektrochemi, D Istituto Superiore di Sani ta, I

Kemiteknik-Teknologisk Institut Taastrup, DK Lab. of the Government Chemist, Teddington, UK Presidio Multizonale di Prevenzione, I Rijksuniversiteit, Β Risoe National Lab., DK

Tauw Infra Consult, NL

The Danish Isotope Centre, DK

202

PROJECT RM 326

IMPROVEMENT OF THE STATE OF THE ART IN NEUTRON ACTIVATION ANALYSIS

PROJECT DEFINITION

Neutron activation analysis (NAA) is performed in the Community in approx. 30 institutes (400-3000 analyses/year each). The sensitivity and potential accuracy of NAA make it a powerful tool in a variety of applications such as:

trace element determinations in medicine (approx. 30 % of the analyses) trace element determinations in environment, geology, archeology (approx. 20 % of the analyses).

NAA is frequently used in the certification of BCR reference materials. Whereas the availability of modern equipment should allow further improvement, difficulties were encountered for several elements including Cr, Se, V and Zn. It is therefore planned to undertake a systematic study of the various causes of error,

starting with Cr, Se and V.

STATUS

A detailed study of the causes of substantial errors in the analyses is in progress.



PARTICIPANTS Centre de Recherches de voreppe, F CNR Pavía, I Danish Isotope Centre, Copenhagen, DK ECN Petten, NL ENEA Rome, I GKSS, Geesthacht, D Hahn-Heitner Inst., Berlin, D Harwell Laboratory, Abingdon, UK Imperial College Research Centre, UK Inst. Nucleaire Wetenschappen, Gent, Β IRI Delft, NL

Kernforschungsanlage Jülich, D Laboratoire Pierre Sue, Saclay, F LNETI, Lisboa, Ρ NCR "Demokritos", Athens, GR

Risoe National Laboratory, Roskilde, DK

Technical Research Centre, Espoo, SF

Univ. Louis Pasteur, Strasbourg, F

Universität Ulm, Ulm, D

203

PROJECT RM 349

MULTI-ELEMENT CHARACTERIZATION IN CABBAGE

PROJECT DEFINITION

Multi-element plant analyses are routinely carried out in all Member States for monitoring purposes, mapping and risk assessment. It is estimated that about 60 000 laboratories were performing plant analyses in all Member States. In addition, about 1 000 plant analyses are estimated to be carried out for more than 10 elements in each laboratory. This would mean that 60 000 single element results are produced each year in Europe. For many years the multi-element reference material (kale) has been famous and after considerable success is now exhausted. Initially it was thought that only few elements or compounds were of sufficient ecotoxicological interest that they should be monitored constantly; they appeared on the so-called black and grey lists. However, with increasing understanding of environmental mechanisms, it became clear that elements not considered before (e.g. Pt-group) as being of environmental interest as well as elements which could be considered as tracers or indicators for human activities (e.g. Sc) or having synergetic or counteracting effects (e.g. Mo) should be considered as well. An example of this changing interest is given by the strong increase of the number of Pt-determinations. However, many results of this multi-element evaluation were unsatisfactory due to a lack of control of accuracy of the determinations. It has been shown that nearly 90 % of the analyses of multi-elements in the last years were wrong or insufficiently controlled. As an example, these errors were calculated to cost about 1 700 000 000 ECU in Germany each year (Chemische Rundschau, 15/89); the cost within the whole European Community was estimated to be 10 times higher. The need for reference materials characterized for as many elements as possible was therefore addressed for a quality control in such projects. It is planned to characterize the material for up to 60 elements each of them to be determined by 3 or 5 laboratories.

STATUS

In progress. The analytical work will start in 1993.



PARTICIPANTS

To be determined. Plants are being grown by Systems-Research Group, University of Osnabrück, Osnabrück, D

204

PROJECT RM 360

RENEWAL OF REFERENCE MATERIALS FOR SOILS

PROJECT DEFINITION

The sales of the existing reference materials were so fast that renewal of the stock has become necessary. The project will include again:

a light sandy soil a calcareous loam a sewage sludge material soil

STATUS

The three materials should be certified in 1992.


ECU 500 000

PARTICIPANTS

CNRS - SCA, Vernaison, F COPES, Hilano, I E.C.N., Petten, NL Ecole Européenne des Hautes Etudes, Strasbourg, F G.S.F., Neuherberg, D JRC, Ispra, I Macaulay Institute, Aberdeen, UK Ministère des Affaires Economiques, Bruxelles, Β Riso, Roskilde, DK R.U.G., Gent, Β Teagasc, Wexford CIRL)

205

PROJECT RM 369

REFERENCE MATERIAL FOR THE ANALYSIS OF WHITE CLOVER

PROJECT DEFINITION

Clover and grass for animal feed are routinely analysed to determine elements of nutritive quality (e.g. Ca, Mg, Κ, Ρ, Ν, S, Μη, Se, Mo) and of potential risks (e.g. Cd, As, Hg, Sb). The results of the determination of nutritive elements are used to improve the state of health and growth of domestic animals. Their diet must be well balanced and therefore basic feed often needs to be enriched with repect to trace and major elements. The determination of the dangerous elements is necessary to avoid health damage to the animals which would lead to a lower production (economic losses) or even could cause damage to the consumer of animal products, e.g. milk, meat, etc. Reference materials are helpful to avoid disputes on the quality of any of the raw materials for the preparation of animal feed. In addition, plant materials such as clover or grass are analysed as indicators of soil pollution with plant-available species. To control the quality of these determinations and consequently the quality of feed two CRMs have been already produced (Rye-grass, CRM 281 for the quality control of trace and toxic element analyses and Hay powder, CRM 129 for the monitoring of major elements). The certification of trace elements in clover was also found to be necessary for this purpose.

RESULTS

A white clover material was prepared and certified for its contents of As, Co, I, Mo and Se.

Certification concluded (CRM 402), EUR Report in press.


ECU 88 000

PARTICIPANTS

22 laboratories from 10 Member States (and the Joint Research Centre, BCMN, B) participate in the certification of the Hhite clover material (CRH 402)

An Foras Taluntais, IRL - Aristotelian Univ, GR - BCMN, Β - CNR, I - CNRS, F - CRF, F ECN, NL - EHICS, F - Gesellschaft für Strahlen- und Umwelt., D - INRA, F - Inst. Scheikundig Onderzoek, Β -Ist. Sup. Sanita, I - Lab. of the Government Chemist, UK - Labor für Spurenanalytik, D - Land, für Ökologie, D - Natural Env. Res. Council, UK - NRL "Oemokritos", GR - Risoe Nat. Lab., DK - RIVM, NL - Risoe Nat. Lab., DK - Univ. Complutense, E - Univ. Barcelona, E - Univ. Ulm, D

206

PROJECT RM 370

REFERENCE MATERIAL FOR THE ANALYSIS OF PLANKTON

PROJECT DEFINITION

The analyses of phyto- and zooplankton are important to investigate the transfer of toxic elements along the trophic chain and the kinetics of uptake of these elements to define the role of these organisms in the biogeochemical pathways and to compare the levels of contamination of different aquatic environments. An intercomparison on trace elements in plankton between 18 laboratories (AIOL) has revealed the presence of systematic sources of errors in the determinations. The difficulties of analysis of plankton material are not matched using other marine RMs such as sediments. Consequently, the certification of some trace elements in plankton was proposed to complete the list of CRMs already existing for marine and freswhater monitoring (see projects nr. 250 and 264).

RESULTS

A plankton material has been prepared in 1989 and certified for its contents of As, Cd, Cr, Cu, Fe, Hg, Ni, Mn, Pb, Se, V and Zn. Certification concluded (CRM 414), EUR Report in press


ECU 77 500

PARTICIPANTS

16 laboratories from 8 Member States (and the Joint Research Centre of Ispra, I) participate in the certification campaign of the plankton candidate RH 414.

Aristotelian Univ., GR

CNR 1st. Ital. Idrobiol., I Danish Isotope Centre, DK ECN, Petten, NL Gesellschaft für Strahlen- und Umwelt., 0 Ist. Sup. Sani ta, I JRC, I KFA, D Labor für Spurenanalytik, D Nat. Food Admin., S NCR "Demokritos", GR PMP Sez. Chimico, I Risoe Hat. Laboratory, DK RUG, Β Univ. Complutense, Ε

Univ. Antwerpen, Β

Univ. Pavía, I

207

PROJECT RM 372

REFERENCE MATERIALS FOR THE ANALYSIS OF RAIN WATER

PROJECT DEFINITION

Rain water is currently monitored in the Member States with regard to the acid rain problem. Important indicator components in monitoring rain water are: total acidity, NH4, NO3, K, Ca, Mg, Na, Cl and SO v Beside the analytical difficulties caused by the susceptibility to contamination with gases from the laboratory air, the major difficulties in certification are caused by stability problems of the samples. Hence a first part of the project was mainly focused on stability studies.

RESULTS

Two CRMs (low and high element contents, namely 408 & 409) were prepared and the certification campaign was carried out in 1991 (EUR-Report submitted in 1992).


ECU 80 000

PARTICIPANTS

Coordinator: KIWA, Nieuwegein, ML CNRS, Service Central d'Analyse, Vemaison, F ECN-Research Centre, Petten, NL EPAL Lab. Centrais, Lisboa, Ρ FacuLdad de Ciencias, Porto, Ρ Forschunszentrum für Umwelt und Gesundheit, Neuherberg, 0 Inst. d'Hygiène et d'Epidémiologie, Brussels, Β Inst. Terrestrial Ecology, Cumbria, UK Ist. Italiano di Idrobiologîa, Palianza, I Ist. di Ricerca sulle Acque, Brugherio, I KIUA, Nieuwegein, NL Lab. Régional d'Hydrologie, Strasbourg, F Lab. Igiene Industríale, Pavía, I Ministère des Affaires Economiques, Brussels, Β Nat. Rivers Authority, Llanelli, UK Portsmouth Polytechnic, Dept. of Analytical Chemistry, Portsmouth, UK Rijksuniversiteit Gent, I.N.U., Gent, Β RISOE Nat. Laboratory, Roskilde, DK RIVM, Bilthoven, NL Rothamsted Exp. Station, Harpenden, UK Servicio Nacional de Parques, Lisboa, Ρ Swedish EPA, Uppsala, S Univ. de Cordoba, Lab. de Química Analítica, Cordoba, Ε Univ. Complutense, Lab. de Química Analítica, Madrid, Ε Uarren Spring Lab., Stevenage, UK

208

PROJECT RM 390

RENEWAL OF REFERENCE MATERIAL FOR MELK ANALYSIS

PROJECT DEFINITION

The sales of the existing materials were so fast (particularly for the CRM 063) that the renewal of the stock has become necessary. The project deals with the production of a new batch of skim milk powder certified for its contents in major and trace elements.

STATUS

Certification to be concluded by the end of 1992 (candidate CRM 063R).


ECU 192 000

PARTiaPANTS

Coordinator: South West Polytechnic, Plymouth, UK Aristotelian University, Thessaloniki, GR BCHN, Geel, Β CNRS, Service Central d'Analyse, Vernaison, F ECN-Research Centre, Petten, NL Eidg. Forchungs. für MiIchwirtsch., Liebefeld-Bern, CH Faculdad de Farmacia, Valencia, E FORCE Institutterne, Broendby, DK Forschungszentrum für Umwelt und Gesundheit, Neuherberg, D lstituto Superiore di Sanita, Roma, I Lab. Central d'Hygiène Alimentaire, Paris, F HiIchuirtsch. Untersuch, und versuchanst., Kempten, D Milk Marketing Board, Thames Ditton, UK MT-TN0, Zeist, NL NIZO, Ede, NL Portsmouth Polytechnic, Portsmouth, UK Rijksuniversiteit Gent, INW, Gent, Β RISOE Nat. Laboratory, Roskilde, DK South West Polytechnic, Plymouth <UK) Univ. degli Studi di Pavía, Pavia, I

209

PROJECT RM 393

REFERENCE MATERIAL FOR THE DETERMINATION OF TRACE ELEMENTS IN LICHEN

PROJECT DEFINITION

Lichen is currently monitored to evaluate air pollution and to follow changes in pollution pattern. This material is found almost everywhere and accumulates trace elements from the atmosphere; it is therefore often used as a practical means for biomonitoring of pollution. The collection and analysis of lichen is much easier and cheaper than the use of air-filters; furthermore the monitoring of lichen produces data on wide geographical areas. The quality of analysis of lichen is restricted by specific matrix effects which are not matched by using other plant reference materials. Ca. 2000 papers were published in "lichenology" (involving analysis of lichen) in the last few years which revealed a high degree of variability of data. Furthermore most laboratories performing lichen analysis for governmental bodies or industries need means to implement a QC to demonstrate the accuracy of their measurements as the number of lichen analysis will probably increase in the future. A reference material will be prepared and certified for 6:10 element.

STATUS

Intercomparison to be concluded in January 1992. Certification foreseen for 1993.


ECU 150 -000 (estimated)

PARTICIPANTS

AGB, Bern, CH CIEMAT, Madrid, E DGQA, Santo André, Ρ Forsch.für Umwelt und Gesund., Neuherberg, Ist. Superiore di Sanita, Roma, I INRA, Champenoux, F Inst, für Pflanzenökologie, Giessen, 0 Kemiteknik, Taastrup, DK Lab. Government Chemist, Teddington, UK LONZA AG, Basel, CH RISOE Nat. Laboratory, Roskilde, OK Trinity College, Dublin, IRL Univ. Bradford, Bradford , UK Univ. Helsinki, Helsinki, SF Univ. de Oviedo, Oviedo, Ε Univ. Trieste, Trieste, I Zentralab. für ehem. Analysen, Jülich, D

- Aristotelian Univ., Thessaloniki, GR - DEC0NTA, Madrid, E - Fac. de Ciencias, Lisboa, Ρ - GEOCISA, Costada, Ε - Imperial College, London, UK - Inst, für Biogeographie, Saarbrücken, D - IRI/TU, Delft, NL - Kernforschungsanlage, Jülich, D - LNETI, Sacavèm, Ρ - Luton College of higher Educ, Luton, UK - Soil Survey and Land Res. Inst., Bedford, - Univ. de Barcelona, Barcelona, Ε - Univ. Bristol, Botany dept., Bristol, UK - Univ. Osnabrück, Osnabrück, D - Univ. Siena, Siena, I - Vrije Univ. Amsterdam, Amsterdam, NL

210

PROJECT RM 4 0 4

REFERENCE MATERIAL FOR THE ANALYSIS OF Hg IN SEAWATER

PROJECT DEFINITION

Important indicator elements such as Cd, Hg, As, Pb, Se, Cu, Zn and Cr are currently analysed in seawater to monitor the contamination levels. Beside the analytical difficulties e.g. caused by the low concentrations in seawater or the risks of contamination, the major difficulties in certification are caused by stability problems of the samples. Hg poses additional difficulties both in the sample preparation and the analytical step due to risks of volatilisation and is therefore being dealt separately.

STATUS

Certification to be concluded by the end of 1992 (candidate CRM 473).



PARTICIPANTS

Aristotelian Univ., Thessaloniki, GR Bund, für Seeschiffahrt und Hydrogr., Hamburg, D Chalmers Univ., Göteborg, S ECN-Research Centre, Petten, HL FORCE Inst., Brodenby, OK GKSS-Forschungszent., Geesthacht, D Gipuskoan Public Health Lab., San Sebastian, E IFREMER, Nantes, F Inst. Hidrográfico, Lisboa, Ρ Isotopcentralen, Copenhagen, DK Kernforschungsanlage, Jülich, D Labor für Spurenanalytik, Bonn, D MT-TNO, Delft, NL PMP Lab. Chimico, La Spezia, I PMP Sezione Chimico, Venezia, I Rijksuniversiteit Gent, INW, Gent, Β Rijkswaterstaat, Haren, NL Sheffield City Polytechnic, Sheffield, UK Swedish Environ. Research Inst., Göteborg, S Water Research Centre, Medmenham, UK

211

PROJECT RM 246

CHLORINATED BIPHENYLS IN SEWAGE SLUDGE

PROJECT DEFINITION

Chlorobiphenyls (cb's) are a class of 209 discrete Chemical compounds in which between one to ten chlorine atoms are attached to the biphenyl nucleus. The risk to the environment and man of the use of polychlorinated biphenyls (transformer fluids and fluids for hydraulic systems, paper and ink industry, etc.) has for long been underestimated. Large quantities of pcb-mixtures have been produced and are still in use. However, toxicological studies on individual chlorinated biphenyls (cb's) indicate that these compounds are toxic and have both carcinogenic and teratogenic properties in animals. Since a routine determination of approaching this number of components in each sample to be analysed would be prohibitive on a cost of time basis, a selection of congeners to be determined was made on the basis of their presence in industrial mixtures, occurrence in a vast number of environmental samples and toxicity of the particular congeners; these considerations have also led to legislation in some Member States. The following cb's (lUPAC-numbers) were thus chosen: 28, 52, 101, 118, 153 and 180 for certification in a sewage sludge RM. Accurate determinations are required for : checking of MAC-values (MAC = maximum allowable concentration) in raw products and food; identification of pollution sources and for the detection of time trends in environmental pollution.

RESULTS

Because of the difficulty of determining cb-congeners, the project started by a study of the various individual steps of the procedure of determination (e.g. quantification, identification, GC-separation and -injection, clean-up, concentration and extraction) used by each of the participants. In consecutive collaborative tests these procedures were studied and the sources of error were detected and consequently eliminated. Analytical feasibility studies were conducted with a variety of materials before the contents of sewage sludge was certified. The results of the certification exercise are reported in EUR 12823 EN.


ECU 150 000

PARTICIPANTS

16 laboratories from 9 Member States for the certification of cb's in sewage sludge. Pilot laboratory: Dept. Agriculture and Fisheries for Scottland, Aberdeen, UK

212

PROJECT RM 254

PURE POLYCHLORINATED DJBENZO-P-DIOXTNS RMs

PROJECT DEFINITION

Industrial and urban wastes contain organo-chlorinated by-products, the incineration of which may result in release into the atmosphere significant amounts of toxic substances such as dioxin and benzofuran derivatives. Some of these compounds such as 2, 3, 7, 8 TCDD are extremely toxic and must be readily identified and quantified in environmental samples containing hundreds of other chlorinated substances and in foodstuff, e.g. milk and cheese. There is an urgent need to develop analytical methods which not only allow identification and quantification at ppb levels, but also provide clues to the source of contamination by means of the particular pattern of isomer distribution. Such methods generally require extensive clean up to avoid interference of other chlorinated compounds. The objective of the project is to prepare reference solutions of pure dioxins congeners which could be easily handled by laboratories for calibrating their analytical methods.

RESULTS

A procedure for the gravimetric preparation of a toxic solution has been developed. Four pure PCDDs have been specially synthesized with a purity of at least 98% and used for the gravimetric preparation of nonane reference solutions are available as internal standard for trace analysis. Twelve other toxic (2, 3, 7, 8 position) TCCD (dioxins) and TCD (furans) solutions were prepared with commercially available pure substances. The purity of the compounds was weighed in two different laboratories.


ECU 350 000

PARTICIPANTS

Biochemisches Institut für Umweltcarcinogene, Ahrensburg, D Bundesanstalt für Material Forschung und Prüfung, Berlin, D Centre National de la Recherche Scientifique, CNRS, Vernaison, CNR, Istituto sull'Inquinamento Atmosférico, Roma, I Ecole Polytechnique, Palaiseau, F Institut des Radio-éléments, Fleurus, Β Joint Research Centre, Ispra, I SCK/CEN, Mol, Β TNO, Delft, NL Universität Bayreuth, D

213

PROJECT RM 274

PURE OXYGENATED-POLYCYCUC AROMATIC HYDROCARBONS

PROJECT DEFINITION

Together with the nitro PAHs, the oxygenated derivatives are considered to be amongst the major sources of potential carcinogens. More than 50 oxygenated PAHs have been detected, e.g. in the gaseous effluents from the combustion of brown coal briquettes. PAHs present in drinking water may react with ozone to form oxidized compounds if the conditions of ozonation used for the purification of water are not well controlled. The preparation of a limited number of pure oxygenated PAHs has been undertaken because such compounds are not readily available elsewhere.

RESULTS

The purity of 7 oxygenated PAHs have been certified as follows:

CRM 337; CRM 338: CRM 339: CRM 340: CRM 341 CRM 342: CRM 347:

Dibenzo(b,d) furan 99.0 % 4H-Cyclopenta(def)phenanthrene-4-one 99,58 % 6H-Benzo(c,d)pyren-6-one 98,9 % Benzo(b)naphto(l,2-d)furan 99,7 % Benzo(b)naphto(2,l-d)furan 99,64 % Benzo(a)fluorenone 99,79 % 3-Hydroxybenzo(c)pyrene 99,4 %



PARTICIPANTS

Bundesanstalt für Hatertal Forschung und- Prüfung, Berlin, D Biochemisches Institut für Umweltcarcinogene, Ahrensburg, D Institut Curie, Paris, F Studiecentrum voor Kernenergie, Mol, Β Riso National Laboratory, DK TNO-ITC, Zeist, NL Union Technique de l'Automobile, du Motocycle et du Cycle, Montlhery, F National Physical Laboratory, Teddington, UK Microtest Research Ltd, York, UK CERCHAR, Verneuil-en-Halatte, F Istituto Superiore di Sanità, Roma, l CNR, Roma, I

214

PROJECT RM 277

DETERMINATION OF CHLORINATED DIBENZO-P-DIOXINS AND -FURANES

"DIOXINS"

PROJECT DEFINITION

The group of polychlorinated dibenzo-p-dioxins (PCDD) and corresponding furances, commonly called the "dioxins" contains some of the most toxic substances ever made by man. The group contains 210 substances of widely varying toxicity. BCR-work is concentrated on the PCDD-species with chlorine atoms in the 2,3,7,8-configuration as these are most toxic (e.g. LD50 in guinea pigs of 2,3,7,8-TCDD is: 1 Mg/g; this "dioxin" has been released mainly at the Seveso accident); 2,3,7,8-TCDD is of acute toxicity and mutagenic, teratogenic and cancerogenic effects have been described. "Dioxins" come into the environment:

a) as by-products of industrial products such as, pentachlorophenol (wood preservative), herbicides, etc. and b)through combustion processes e.g. pcb-containing, oils, waste incinerators.

As intercomparisons and disputes between industry and public authorities have shown that there is little agreement between analytical results the BCR has decided to start collaboration work, which, in view of the difficulties encountered in the analysis, is set up similarly to the work in the pcb-group (project 246) i.e. stepwise, verification of the individual steps of the anlaytical chain (quantification, identification, separation, injection, clean-up, extraction...)

STATUS

Intercomparisons to check the GC-MS procedures have been performed and various participants improved their methods consequently. The certification analyses of the dioxins in a fly ash extract have been performed in 1991; certification report submitted in 1992. An intercomparison on extraction techniques for incinerator ash will be concluded, which could lead to a certification of the TCDD with 2,3,7,8-configuration in a fly ash extract in 1992.


ECU 400 000

PARTICIPANTS

BASF, Ludwigshafen, D - Bayer AG, Leverkusen, 0 - Biocontrol, Mainz, D - 1st. Ing. Atmosf. Monterotondo,

I- CNRS, Vernaison, F Duphar BV, Weesp, NL - Ecole Polytechn., Palaiseau, F - ENEL, Pisa, I - INERIS,

Verneuil, F - 1st. Mario Negri, Milano, I - JRC, Ispra, I - Min. of Agrie. Fish & Food, Norwich, UK - MT-

TN0, Delft, NL - Schering Agrochemicals, Essex, UK - The Finnish Pulp and Paper Inst., Helsinki, S - Univ.

Amsterdam, NL - Univ. Ulm, D - VITO, Mol, Β- Uarren Spring Lab. Stevenage, UK

215

PROJECT RM 291

SHORT-TERM MUTAGENICITY TESTING

PROJECT DEFINITION

Assessment of the toxicity of new chemicals is required by the EEC Directive 79/831, 6th amendment, and includes the determination of risks which could lead to cancer or to congenital malformations caused by genetic mutation. The first level of screening consists in determining the genotoxicity of chemicals through a series of assays on micro-organisms and mammalian cells. Unfortunately, the results of these assays greatly depend upon how the methods are applied and upon the lines of bacterial strains used in performing the tests. The objectives of the project are to prepare reference materials and to certify the mutagenic activity with a well defined, optimized procedure.

STATUS

A first intercomparison on mutagenicity testing has been carried out without metabolic activation (-S9) and showed up serious difficulties in obtaining results with a good agreement. In order to prepare the 2nd intercomparison with metabolic activation (+S9) a preliminary study (with three labs) was started so as to investigate:

1) some of the most important parameters of variability of this test (-S9) like - type of solvents, agar, glucose sterilization, inducer - concentration of mutagen;

2) the appropriate S9-mix - rat strain - concentration of S9.

Part 1 of this study has been carried out Results will be available by end of May 1992. Part 2 will be terminated by end of summer 1992. The analytical protocol for the 2nd intercomparison will be adopted according to the results of the preliminary study. Two highly purified indirect mutagens (benzo(a)pyrene and 2-aminoanthracene) have been prepared as candidate reference materials. HPLC, GC-FID and GC-MS analysis indicated 99.2 % purity of benzo(a)pyrene and 99.9 % purity for 2-aminoanthracene. Homogeneity and stability studies (12 months) have been successfully completed.


ECU 120 (XX) (estimated)

PARTICIPANTS

Biochemisches Institut für Umueltcarcinogene, Ahrensburg, D - British Industrial Biological, Research Association, Carshalton, UK - Central Toxicology Laboratory, Cheschire, UK - Institut d'Hygiène et d'Epidémiologie, Bruxelles, Β - Institut Pasteur de Paris, Paris, F - Institut Pasteur de Lille, Lille, F - Inveresk Research International Ltd, Musselburgh, UK - Microtest Research Limited, Heslington, UK -National Collection of Type Cultures, London, UK - National Research Center 'Democritus', Paraskevi Attikis, GR - RCC Notox, Genetics I in Vitro Toxicology, 's-Hertogenbosch, NL - Scantox A/S, Skensveld, DK - SCK/CEN, Mol, Β - Universita di Genova, Genova, I - Universita di Pisa, Pisa, I - Universitate Autónoma de Barcelona, Bellaterra, Ε - Universitätsklinikum Essen, Essen, 0 - Université Catholique de Louvain, Bruxelles, Β

216

PROJECT RM 304

DETERMINATION OF REFERENCE SPECTRA OF POLYCYCLIC AROMATIC COMPOUNDS AND CHLORINATED AROMATIC COMPOUNDS

PROJECT DEFINITION

Identification and quantification of dangerous organic compounds in the environment, working area and consumer goods is a very difficult task because many of these compounds have isometric structures and similar chemical properties.

These compounds can be identified in complex environmental or biological matrices by their molecular spectra (UV, IR) Nuclear Magnetic Resonance Spectra or mass spectra. For instance, polycyclic aromatic compounds (PAC) detected in a complex mixture after extraction may be identified by comparing their actual fluorescence spectra with reference spectra compiled in a spectral atlas or stored in a data bank.

The objective of the project is to determine under well controlled conditions the reference spectra of organic compounds of environmental health concern such as PACs and chlorinated aromatic compounds. The measurements of UV, IR, NMR, MS spectra are to be performed by five experienced laboratories of the Member States. The compilation and edition of reference spectra and complementary data will be undertaken at the Ispra Joint Research Center.

RESULTS

A first volume of 43 PACs reference spectra was issued in 1985 as a Spectral Atlas of Polycyclic Aromatic Compounds. A second volume containing reference spectra of 45 new compounds - PAH, methylated PAH and N-heterocycles was published in 1988. The third volume of reference spectra of nitro-PAH, oxygenated PAH sulphur heterocyclics and metabolites has been published in 1991. The project is terminated.



PARTICIPANTS

Biochemisches Institut für Umweltcarcinogene, Ahrensburg, D CEA, CENG, Grenoble, F CTIS, Lyon, F Joint Research Centre, Ispra, I Laboratory of the Government Chemist, London, UK TNO-ITC, Zeist, NL Université de Bordeaux, Laboratoire de Chimie Physique, Bordeaux,

217

PROJECT RM 331

DETERMINATION OF TRACES OF PAHS IN SEWAGE SLUDGE

PROJECT DEFINITION

PAH'S generally enter the environment through combustion processes e.g. as a result of smoke production in the combustion of organic materials and in particular in Diesel engines. They may finally contaminate food, endanger many living species and eventually man through the food chain. In view of the many sources of error in the analytical procedures for a large variety of matrices from all parts of the ecosystem (e.g. sludge, water, plants, air, dusts, municipal wastes, soils, etc.) and because of the importance of measuring PAH-content for monitoring the environment (disposal of dust, ashes, waste and sewage sludge) it is necessary to support progress in the laboratories by some certified reference materials. The project will consist of: 1. Improving methodology for the determination of traces of PAH

(identification of the major causes of errors) 2. Organization of a seminar for Community laboratories to disseminate the results

of the study 3. Certification of materials of typical importance for the environment (e.g. sewage

sludge)

STATUS

The sewage sludge material will be certified in 1992.


ECU 275 000

PARTICIPANTS

Biochemisches Inst, für Umweltcarcinogene, Ahrensburg, D - Centro de Investigación y Desarrollo, Barcelona, E - CNR 1st. di Ricerche Sulla Acque, Brugherio, I - Dept. of Agriculture and Fisheries for Scotland, Aberdeen, UK - Dir. General da Qualidade do Ambiente, Lisboa, Ρ - Environmental Research Unit, Dublin, IRL -Free Univ. IVM-VU, Amsterdam, NL - Inst. Univ. de Médecine du Travail et d'Hygiène, Le Mont-sur-Lausanne,

CH - National Inst, for Occupational Health, Copenhagen, DK - Nat. per Ricerche sul Cancro, Genova, I -R.I.V.M., Bilthoven, NL - Service Nat. de la Recherche Scient., Vernaison, F - SOPRA, Milano, I - TAUW Infra Consult, Deventer, NL - Technical Research Centre of Finland, Espoo, SF - Techn. Untersuchungs- und Forschungszentrum, Essen, D - Union Techn. de l'Automobile du Motocycle et du Cycle, Monthléry, F - Univ. de Bordeaux, Talence, F - Univ. of Athens, GR - Univ. de Oviedo, E - Univ. de Cordoba, Cordoba, E Univ. Ules Baleares, Palma de Mallorca, E - VITO, Mol, Β

218

PROJECT RM 332

INDUSTRIALLY POLLUTED SOILS (COKING PLANT SOILS)

PROJECT DEFINITION

Industrial wastes are causing considerable difficulties in industrialized countries. Secret waste deposits are even of greater concern because there are many thousands of them. Reclamation of polluted areas requires considerable expenditure as well as the disposal or destruction of the wastes. In view of the problem of elimination of dangerous waste various Directives have already been adopted (e.g. 78/319/EEC, 75/442/EEC or 87/216/EEC), which deal with precautions to be taken in removal, treatment and transport of wastes. Only in NL there are more than 1600 identified sites to be treated; this is expected to be less than 10 % of all sites still uncovered. The accurate characterisation of waste has therefore considerable economic consequences. This project envisages to study the analytical problems for soils polluted by coking plants (tar, oil, PAH, phenols, cyanides) and to possibly certify reference materials.

STATUS

Two soil materials are in preparation for the certification of PAH, phenols and CN.

CONTRIBUTION OF THE COMISSION

ECU 240 000

PARTICIPANTS

VITO, Hol, Β - INERIS, Verneuil-en-Halatte, F - BRGH, Orléans, F - IRH, Nancy, F ATOCHEM, Levallois, F - Biocontrol, Mainz, D - TÜV Nordrhein-Westfalen, Essen, D - Bayer AG, Leverkusen, D - Univ. Ulm, D - Lab. of the Government Chemist, Teddington, UK - Atomic Energy Authority, Oxfordshire, UK - Inst. Hidrográfico, Lisboa, Ρ - Danish Technological Inst., Taastrup, DK - Lab. Contox, Madrid, Ε -Universidad de Santiago de Compostela, Ε - Lab. Arbit. Agroalimentarios, Madrid, Ε - Universidad de Barcelona, Ε - Inst, de Salud Carlos III, Madrid, - R.I.V.M., Bilthoven, NL - Agricultural University, Wageningen, NL - TNO-MT, Delft, NL - Free University IVM-VU, Amsterdam, NL - State Inst, of Qualtiy Control of Agricultural Products, Uageningen, NL - 1st. Sperim. per lo Studio e la Difesa del Suolo, Firenze I -FISIA, Stupinigi, I - FISIA, Orbassano, I - C.E.C, JRC, Ispra, I - 1st. suil Inquinamento Atmosférico, Monterotondo Stazione, I - E0LAS, Dublin, IRL - Agricultural Research Centre of Finland, SF - SCITEC SA, Lausanne, CH - Ecole Polytechnique Fédérale IGE, Lausanne, CH - Nat. Lab. Agriculture Chemistry, Uppsala,

219

PROJECT RM 354

PCBs IN WASTE MINERAL OIL

PROJECT DEFINITION

This project is the follow-up of project 246 in which it was foreseen to prepare a number of reference materials containing traces of PCBs and which have an importance in environment management. Waste oil with two levels of PCBs will be certified.

RESULTS

Two materials low and high level of contamination have been certified in 1992, EUR Report in press.


ECU 230 000

PARTICIPANTS

Atochem, Levai lois, CH Bureau de Recherches Géologiques et Minières, Orléans, F CSIC, Environmental Chemistry Dpt., Barcelona, E DAFS Marine Laboratory, Aberdeen, UK Oireccao General de QuaUdade do Ambiente, Lisboa, Ρ Empa, Dübendorf, CH Free University of Amsterdam, NL Inst, of Marine Research, Bergen, Ν Inst. Génie Environnement, Lausanne, CH Joint Research Centre, Ispra, I Laboratoire Cantonal, Genève, CH Laboratoire Municipal de la ville de Rouen, Rouen, F Nat. Swedish Env. Prot. Board, Solna, S Rijksinstituut voor Visserijonderzoek, Ijmuiden, NL S.G.S. Depauw & Stockoe Ecodest, Antwerpen, Β Univ. des liles Baleares, Palma de Mallorca, Ε VITO, Mol, Β

220

PROJECT RM 355

PCBs IN MILK POWDER

PROJECT DEFINITION

This project is also the follow-up of project 246.

An increasing interest is put everywhere on milk for traces of PCBs and of dioxins.

RESULTS

The material has been certified in 1992, EUR Report in press.


ECU 115 000

PARTICIPANTS Agricultural Research Center, Jokoinen, SF DAFS Marine Laboratory, Aberdeen, UK Free University of Amsterdam, NL Institut Génie Environnement, Lausanne, CH Institute of Marine Research, Bergen, Ν Instituto Químico de Sarria, Barcelona, Ε Joint Research Centre, Ispra, I

VITO, Mol, 8

Laboratoire Cantonal, Genève, CH Laboratoire Municipal de la ville de Rouen, Rouen, F Milchwirtschaftliche Untersuchungs- und Versuchsanstalt, Kempten, D National Food Agency of Denmark, Soborg, DK National Swedish Env. Proto. Board, Solna, S Rijksinstituut voor Vissen"jonderzoek, Ijmuiden, NL State Institute for Quality Control of Agricultural Products, Uageningen, NL Universität Ulm, D

221

PROJECT RM 361

DIOXINS IN FLY ASH

PROJECT DEFINITION

Following the initial work on traces of dioxins (277) it was foreseen to work on dioxins in incineratory fly ash (one of the most important dioxin pollutant) at present.

STATUS

The material has been prepared and the homogeneity and stability studies are in progress.



PARTICIPANTS

BASF, Ludwigshafen, D Bayer AG, Leverkusen, D Biocontrol Mainz, 0 CNRS-SCA, Vernaison, F Consejo Superior de Investigación Científicas, Barcelona, E Dept. of Trade and Industry, Stevenage, UK Duphar B.V., Ueesp, NL Ecole Polytechnique-DCMR, Palaiseau, F E.N.E.L., Pisa, I INERIS, Veneuîlen-Halatte, F Inst, de Salude Carlos III, Madrid, E Istituto Inquinamento Atmosférico Monterotondo Scalo, I Istituto Mario Negri, Milano, I Joint Research Centre, Ispra, I Ministry of Agriculture, Fisheries and Food, Norwich, UK MT-TNO, Delft, NL Schering Agrochemicals Ltd., Saffron Ualden, UK SCK/CEN, Mol, Β Sopra, Milano, I The Finnish Pulp and Paper Research Inst., Helsinki, SF Universiteit van Amsterdam, Amsterdam, NL Universität Ulm, 0

222

PROJECT RM 371

ORGANO-CHLORINE COMPOUNDS IN INDUSTRIAL SOILS

PROJECT DEFINITION

Polluted industrial soils are causing considerable difficulties in industrialized countries. Reclamation of polluted areas requires considerable expenditure as well as the disposal or destruction of the waste. In view of the problem of elimination of dangerous waste several Directives have already been adopted (e.g. 78/319/EEC, 75/442/EEC or 87/216/EEC) which deal with removal, treatment and transport of waste. Other Directives in this field are expected in the near future. The accurate characterization of waste has considerable economic consequences because the results of these are used to decide on the treatment to be applied for reclamation. Organo-chlorine compounds are within the most commonly encountered type of contaminants. Over the last decades large areas have been exposed, by industrial activities, to contamination by chlorobenzenes (CBs), chlorophenols (CPs), polychlorodibenzo-p-dioxins and furanes (PCDDs and PCDFs), chorinated pesticides, polychloro-biphenyls (PCBs) and the side products. This project intends to study the various analytical steps of the determination of CPs, CBs, PCDDs and PCDFs in order to highlight the sources of errors of the analytical methods. Finally two soils should be certified for CPs - CBs and dioxins when the methods applied by the participating laboratories have reached a sufficient reliability.

STATUS

A certified reference material is in preparation.



PARTICIPANTS

List not yet determined. Pilot laboratory : Biocontrol, Mainz, D

223

PROJECT RM 378

PCBs IN INDUSTRIAL SOILS

PROJECT DEFINITION

In parallel to project 371 - Organo-chlorine compounds in industrial soils - this project will investigate the determination of Polychlorobiphenyls (PCBs) in industrial soils. The certification of one soil for 12 congeners: CB 28, 52,101,105,118, 128,138,149, 153, 156, 170 and 180 is foreseen with a group of laboratories which have already worked on the certification of PCBs in sewage sludge and mineral oils.

STATUS




PARTICIPANTS

25 laboratories from 9 Member States. Pilot laboratory: IRH, Nancy, F

224

PROJECT RM 387

MODERN POLAR PESTICIDES IN WATER AND SEDIMENTS

PROJECT DEFINITION

The term "modem polar pesticides" used in this project covers a series of compounds and family of compounds:

órgano phosphorus pesticides (OPs) carbamate insecticides (CIs) triazine herbicides (THs) pyrethroid insecticides (Pis) quats

They have only in common the fact that they are polar compounds and do not belong to the group of chlorinated pesticides (OCPs) such as DDT, HCH, the Drins etc. As they chronologically appeared after the OCPs they have been grouped under the vocable "modern polar pesticides". Belonging to the second generation of (chemical) pesticides they are developed to be effective but not persistent in a natural environment. The non-chlorinated pesticides have been introduced as an ecologically preferred alternative to the organochlorine compounds. Their rapid breakdown in water and consequently their low environmental persistence were the most important arguments. A better selectivity of the target organism (animals, fungi or plants to be destroyed) was also a major progress. However the extensive use of these chemicals has resulted in a high contamination risk to various types of aquatic environment e.g. rivers, estuaries, lagoons, ground waters etc and to aquatic living organisms. During the years 1980/81 at least 640 tons of malathion, one of the most frequently applied órgano phosphorus pesticides, have been used in the EC countries. Other compounds are used in similar amounts. It appeared over the years that some of these compounds, e.g. Atrazine, have a longer half life under field conditions than expected. Therefore monitoring of the environment for such compounds has now become mandatory. The objective of the present project is to examine the possibility to stabilise some of these compounds in various matrices. After having developed stabilisation procedures for each group of pesticides, intercomparisons will be started to establish the state of the art of their determination and, where necessary, to improve the method. When the participants have improved their quality of determination, water, sediments, soils, plant materials will be certified.

STATUS

Feasibility studies concluded. First intercomparison starts in 1992.



PARTICIPANTS

25 laboratories from 11 E.C. countries + SF, CH and S. Pilot laboratories: CSIC CID, Barcelona, E

Freshwater Ecology, Dorset, UK

225

PROJECT RM 394

DIOXINS IN MILK POWDER

PROJECT DEFINITION

Recently attention has been drawn on the presence of polychloro dibenzo-p-dioxins (PCDDs) and polychlorodibenzo furanes (PCDFs) in dairy products. Trade has been hampered because of the suspected presence of higher contents of such contaminants in milk powder, cheese, etc. In some countries incineration plants have been closed because of the presence of dioxins in milk from cows grassing in the surroundings. The determination of dioxins in food products necessitates sophisticated equipment such as High Resolution Mass Spectrometry (HRMS) and High Resolution Gas Chromatography (HRGC). Sensitivities of 0.1 pg/g have to be achieved in order to accurately determine levels of 6 pg TEC/g fat in milk (TEC = toxic equivalent concentration). This latter content is the maximum tolerable limit for the milk in certain countries (e.g. NL). The extremely low levels to be determined often result in disagreement of the results of the analyses. Therefore doubt has been raised on the validity of the results of the determination of PCDDs and PCDFs and on the quality of the monitored dairy products within the E.C. The necessity has been demonstrated to set up a network of well trained laboratories involved in dioxin determinations in food and feed. This network should possibly cover all Member States. Some laboratories acting upon request of their national authorities have proposed to the Commission to start a project, within the framework of the BCR programme, on the determination of PCDDs and PCDFs in milk. This project should establish the state of the art of such determinations and should help laboratories to improve the quality of their measurements. A first intercomparison on PCDDs and PCDFs will establish the state of the art of the determination of such compounds in milk. Three batches of freeze-dried milk powder will be prepared - one natural milk powder (approx. 2 pg TEC/g fat of dioxins) - two PCDDs and PCDFs enriched samples (approx. 6 pg TEC and 20 pg TEC/g fat). According to the results of the intercomparison, additional exercises will be envisaged to increase the quality of the measurements. Possibly a milk powder, whenever necessary, will be certified for the PCDD and PCDF content.

STATUS

1st intercomparison concluded.



PARTICIPANTS

Intercompar i sons : Biocontrol Hainz, D - Chem. Landesuntersuch. Stuttgart, 0 - CNR Monterotondo Scalo, I - CNRS-SCA Vernaison, F - CSIC Barcelona, E - D.G.A. Berling, D - Ecole Polytechnic. Palaiseau, F - Free Univ. Amsterdam, NL -JRC Ispra, I - LGC Teddington, UK - HAFF, Norwich, UK - Nat. Food Admin. Uppsala, S - Nat. Food Agency Soeborg, DK - Ökometric GmbH Bayreuth, D - RIKILT Uageningen NL -RIVM Bilthoven, NL - SCK/CEN Hoi, Β - TNO Delft, NL - Univ. Ulm, D - Univ. Umea, S - Univ. Zürich, CH Pilot laboratory: RIKILT, Wageningen, NL

226

PROJECT RM 408

PAHs IN INDUSTRIAL SOIL

PROJECT DEFINITION

In parallel to projects 371 and 378 dealing with Organo-chlorine compounds in industrial soils, this project intends to investigate the determination of polycyclic aromatic hydrocarbons (PAHs) and in addition penta chlorophenol (PCP) in soil. This contamination is typical for wood (creosote treatment) preservation industry. Large areas have been polluted by the wood industry. Accurate characterization of the level of contamination is necessary before any decision on the disposal, transport or the destruction of the soils can be taken. To take such decisions results of accurate determinations of PAHs and PCP are necessary. The project will validate the methods as applied, improve them where necessary and finally certify the contents of eight PAHs (e.g. pyrene, benz(a)anthracene, benzo(a) pyrene, benzo(e) pyrene, benzo(k) fluoranthene, benzo(b) fluomathene, benzo (b) naphto (2,1-d) thiophene, indeno (1,2,3 c-d) pyrene and penta-chloro-phenol). The certification of PAHs can be done by the group already working on PAHs in sewage sludge (project 331). The certification of PCP will be done by the group working in project 371.

STATUS

The certified reference material is being prepared.



PARTICIPANTS

25 laboratories of 11 E.C. countries + SF + CH + s in each group CPAH and PCP). Pilot laboratory: IRH, Nancy, F

227

PROJECT RM 417

ORGANIC AND INORGANIC CONTAMINANTS IN HARBOUR DREDGE

PROJECT DEFINITION

Various past or recent industrial activities have caused, amongst others, that materials such as sewage sludge, harbour dredge, which in the past were used for landfill purposes or for improvement of the soil structure, have now become dangerous waste.

In view of the problem of elimination of dangerous waste several Directives have already been adopted (e.g. 78/319/EEC/, 75/442/EEC or 87/216/EEC) which deal with precautions to be taken for removal, treatment and transport of wastes.

The European Round Table held in November 1985 suggested that studies be undertaken on the impact of waste disposal and treatment facilities, and of abandoned contaminated industrial sites.

Problems related to hazardous waste are now being considered as of primary concern to DG XI.

This project will be devoted to the characterization of the risk on disposal of harbour dredge. Several inorganic (e.g. As, Pb, Hg, Cd, Cr, etc) and organic (PCBs, PAH, OCPs, dioxins, etc) toxic parameters will be certified.

STATUS:




PARTICIPANTS

List not yet determined Pilot laboratory: SGS - Depauu-Stokoe, Antuerpen, Β

228

PROJECT RM 311

THE DETERMINATION OF METHYL MERCURY SPECIES IN THE ENVIRONMENT AND IN FOOD

PROJECT DEFINITION

Mercury occurs in the environment in various forms e.g. elementary mercury (Hg"), inorganic mercury and methyl mercury (MeHg). Elementary mercury is mainly present in the air; inorganic mercury in water; and methyl mercury occurs predominantly in the contaminated food chain (e.g. shell-fish). Methyl mercury compounds are of paramount importance: their toxicity and the risk of humain exposure are high. Because of its toxicity and abundance in the food chain, the limits of exposure to MeHg are at least 5 times less than the exposure to other Hg-compounds. The objective of the project is to develop through collaborative work of a number of experienced laboratories a methodology for accurate determination of MeHg in food. It is envisaged that in a second phase reference materials will be prepared e.g. fish and shell-fish.

STATUS

Third intercomparison concluded in 1991. Certification campaign started in 1992 [mercury and methyl-mercury in tuna fish: candidate CRMs 463 (low content) and 464 (high content)].


ECU 60 000

PARTICIPANTS

Bundesanstalt für Fischerei, Hamburg, D - CNRS, Service Central d'Analyse, F - Darmarks Mi Ijoeundersogelser DHU, Soborg, DK - FORCE Institut, DK - IFREMER, Nantes, F - Kemiteknik, Taastrup, DK - Kernforschungsanlage Jülich, D - Leicester Polytechnic, UK - Max-Planck Institut, Mainz, D - Ministry of Agriculture and Fisheries, S - MRC Toxicology Unit, Carshalton, UK - National Food Agency, Soborg, DK - P.M.P. Lab. chimico. La Spezia, I - PHP Sezione Chimico, Venezia, I - Rijksuniversiteit, 1NU, Β - Rijkswaterstaat, Gravenhage, NL - RIKILT, Wageningen, NL - Sheffield City Polytechnic, UK - Swedish Environ. Research Institute, S -Swedish Nat. Food Adm., Uppsala, S - Universidad Complutense, Madrid, E - Universidad de Santiago Compostela, E - Universita di Genova, I - Univ. Umea, S - Université de Bordeaux, Talence, F - Vrije Universiteit Brussel, Β

229

PROJECT RM 313

ALKYL-TIN SPECIES IN THE MARINE ENVIRONMENT

PROJECT DEFINITION

Whereas inorganic tin species such as Sn(II) chloride, ofride or sulphate do not seem to be toxic or cancerogenic, organotin species are highly toxic. Of all organic tin species the tri-aryl compounds are most dangerous. TBT is mainly used in antifouling paints, wood preserving fungicides, desinfectants and molluscicides, whereas TBT plays a role in agriculture, (e.g. fungicides), other organotin species (e.g. dialkyl compounds) are used as stabiliser for PVC, industrial catalysts or precursors for Sn02-films or glass. The production worldwide of organotin compounds was some 35 000 tons in 1980 of which 8 000 tons were triorganotin compounds for biocidal use; 3 000 tons were produced for antifouling paints, 1 000 tons for wood preservatives, 3 000 tons for agrochemicals and 1 000 tons for desinfectants. Especially the application of TBT in antifouling paints has caused concern. Ship hulls with a TBT containing paint will not be covered under water by mussels and sea weed and therefore allow faster sailing. Also fishing nets have been treated with TBT. However, the TBT leached from the paint by water acts as a strong poison to larvae of oysters, mussels and fish. Therefore France and the UK have already legislation on the use of TBT in ship paints, Ireland announced in April 1987 that legislation on the use of organotins as antifouling agents would be banned. The objective of the project is essentially to develop, through collaborative work of expert laboratories, the methodology to obtain accurate results in the determination of the most important organic tin compounds. It is also intended to certify sediment and mussel samples.

STATUS

Second intercomparison concluded. Certification of TBT in CRM 424 (harbour sediment) to be concluded by June 1992. Certification of butyltins in coastal sediment (candidate CRM 462) to be concluded by the end of 1992. Certification of organotins in mussel (candidate CRM 477) to be concluded by the end of 1993.



PARTICIPANTS

Atochan Vlissingen, NL - BCMN - Univ. de Bordeaux, F - CSIC Barcelona, E - CIBA-GEIGY Marienberg GmbH, Bensheim, D - ENEA Roma, I - GKSS Forschungszentrum, D - Ifremer, Nantes, F - Inst, voor Visserijproducten, Ijmuiden, NL - Intern. Tin Research Inst., Uxbridge, UK - Inst, für Spektrochemie und angewandte Spektroskopie, Dortmund, D - Leicester Polytechnic, UK - MAFF Fisheries Laboratory, Burnham-on-Crouch, UK -Max-Planck Institut für Chemie, Mainz, D - Nat. Environ. Res. Inst., DK - Nat. Techn. Univ. Athens, GR -Schering, Bergkamen, 0 - Southwest Polytechnic, UK - Univ. di Genoa, I - Univ. de Sevilla, E - Univ. Instellingen Antwerpen, Β - Univ. de Pau et des Pays de l'Adour, Pau, F

230

PROJECT RM 315

SPECIATION OF TRACE METALS IN SOIL AND SEDIMENT

PROJECT DEFINITION

The bioavailability of trace metals depends on the chemical species in which they are combined. Different schemes of sequential extraction have been proposed to assess the different forms of metals (mobile/bioavailable, carbonate-bound, organic-bound, mineral...) in soil and sediments. In this project one scheme of sequential extractions has been compared by all participants with their own scheme and applied first to one polluted soil sample and one sediment. Common extraction schemes have been designed and will be used to certify sediment and soil samples.

STATUS

First intercomparison concluded. Second intercomparison on sediment in progress. Certification of extractable trace metals in two soils (sewage amended soil and terra rossa soils, candidate CRMs 483 and 484) to be concluded by the end of 1992.



PARTICIPANTS

Adas, London, UK - Agricultural Research Centre, Jokionen, S - Arbeitsbereich Umweltschutztechnik, Hamburg, D - Bedrijf slaboratorium voor Grond- en Gewasonderzoek, Oosterbeek, NL - Bundesanstalt für Materialprüfung, Berlin, D - Chalmers Univ. of technology, S - Environmental Pollution Control Lab., Thessaloniki, GR -Estacao Agronómica Nacional, Ρ - Estación Experimental del Zaidin, Granada, Ε - FCT/UNL, Honte da Capa Rica, Ρ - INRA, Arras, F - I.N.R.A., Bordeaux, F - Inst, de Géologie du Bassin d'Aquitaine, Talence, F -Institute for Soil Fertility, Haren, NL - Institute of Plant Nutrition and Soil Science, Braunschweig, D -Instituto de Chimica Agraria, Bari, I - 1st. Chimico del Terreno, I - Joint Research Centre, I -Kemitechnik, Taastrup, DK - Laboratoire Central des Ponts et Chaussées, Bougenais, F - Lab. de Chimie Analytique, Paris, F - Laboratorium und Umweltschutz, Nordenham, D -Laboratory of the Government Chemist, Teddington, UK - Landbouw Universiteit Wagem'ngen, NL - Queen Mary College, London, UK - Rothamsted Experimental Station, Herts, UK - State University of Gent, Β - Station Fed. de Rech, en Chimie Agricole, CH - The Agricultural Institute Centre, Wexford, IRL - The Macaulay Institute for Soil Research, Aberdeen, UK - Univ. de Barcelona, Ε - Univ. de Cordoba, Ε - Universita di Genova, Genova, I - Vrije Universiteit Brussel, Β - Water Research Centre, Hedmenham, UK

231

PROJECT RM 336

SPECIATION OF ARSENIC

PROJECT DEFINITION

Arsenic is an element of which the various forms (species) have a widely differing toxicity. Inorganic As (III) is highly toxic, e.g. amounts 0.15-0.3 g are acutely lethal to humans whereas As (V) is less toxic and organic arsenic compounds such as arsenobetaine and choline have no effect on the human body. Therefore it is of paramount importance to determine the form and binding in which the arsenic is present ("speciation") before concluding on the hazard of disposal or of removing an arsenic-contaminated food from the market. As203 is used as herbicide, pesticide, fungicide and desinfecting agent in sheep growing; Na-arsenite is still in use to desinfect soils. ASjOs is used in the cotton industry and to protect wood. In view of the different toxicological behaviour of various As containing compounds and their different toxicity it is necessary to determine the speciation rather than the total contents. This holds especially for fish intended for human consumption; high contents of As are tolerable if all arsenic is in the form of arsenobetaine. The fate of arsenic-containing herbicides and pesticides in the environment and the conversion of these compounds is of particular interest to the herbicide-industry but requires the development of suitable speciation methodology. The programme will include the methodologies for the determination of: As(V) and As(III); mono and dimethylarsenic acids and salts; arsenocholine and arsenobetaine Then the study will continue with the extraction from real samples (mussel tissue, fish, soil, sediments). It is intended to certify up to 4 materials.

STATUS

Four intercomparisons on solutions of As compounds have been conducted.


ECU 375 000

PARTICIPANTS

C.M.R.S., Vernaison, F Ecole Européenne des Hautes Etudes, Strasbourg, F IFREHER, Nantes, F Inst. Pasteur de Lille, F 1st. Sup. di Sani ta, I Ministry of the Environment, Soburg, DK National Techn. Univ. Athens, GR Rijksuaterstaat. Haren, NL School of Analytical Sciences, Dublin, IRL School of Chemistry, Leicester, UK Sheffield City Polytechnic, UK The State Lab., Dublin, IRL Univ. de Barcelona, E Univ. of Southampton, UK

232

PROJECT RM 345

IMPROVEMENT OF THE DETERMINATION OF CR IN ENVIRONMENTAL MATRICES

PROJECT DEFINITION

The toxicity of Cr has led to the implementation of Directives which set maximum values for this element in different matrices (potable and effluent water, sewage sludge, compost, soils for agriculture). In view of the increasing concern about the role of Cr, the BCR programme intended in various cases to certify the total Cr-content (e.g. in soils, sludges, plants and coal). However, in most cases the results could not be accepted because the spread was too large or a methodological bias could not be excluded. Owing to the poor performance encountered, a programme has started which aim was to (i) identify CRMs for which an additional certification of Cr would be useful, (ii) verify the homogeneity of the materials selected, (iii) develop a method of good reliability (IDMS) to be able to remove methodological bias amongst methods where detected and (iv) optimise the AAS measurements for Cr determination (ETAAS and FAAS).

STATUS

Selection of CRMs, development of IDMS and AAS optimisation to be concluded by the end of 1992. Additional certification in various CRMs may follow.



PARTICIPANTS

For the preliminary study: ECN-Research Centre, Petten (NL) - Univ. de Barcelona (E) For future work: participants to be determined

233

PROJECT RM 34β

SPECIATION OF LEAD

PROJECT DEFINITION

Lead has various chemical forms (species) displaying a wide range of toxical impact to biota and humans. Ethyllead compounds are highly toxic, e.g. 80 μg/g (as Pb) of tetraethyllead (TEL) and 20 iig/g (as Pb) of triethyllead (TriEL) are acutely lethal to rats. Similar observations were made with trimethyllead (TML) species (lethal concentration of 36 Mg/g as Pb). The lethal dose for human is presently not known but was estimated at 0.25 g of TEL and more than 1 g of TML. The toxicity of inorganic lead for humans is 10-time less than tetra-alkyllead compounds. The toxicity of organolead species as well as their environmental distribution are not well known because of the lack of adequate analytical methodology. The need for reliable techniques is widely recognized. The project will start with a stability study of methyl- and trimethyllead compounds. Subsequently an intercomparison will be organized to improve methods of determination. Finally the intention is to certify some of the major lead compound in road dust and in artifical rainwater.

STATUS

First intercomparison in progress.



PARTICIPANTS

CNR, Pisa, I CNRS, Service Central d'Analyse, F GKSS Forschungszentrum, o Kemiteknik, Taastrup, OK Leicester Polytechnic, UK Nat. Inst. Occupational Health, Umea, S Philipps-Univ., Harburg, D Rijkswaterstaat, Haren, NL South West Polytechnic, UK The Assoc. Octel Company, UK Univ. Antwerp, Β Univ. Zaragoza, Ε Univ. Umea, S

234

PROJECT RM 351

IMPROVEMENT OF THE DETERMINATION OF ALUMINIUM AND AL-SPECIES

PROJECT DEFINITION

Aluminium is an ubiquitous element of which the various forms (e.g. complexed forms of Al) have a widely differing toxicity to biota and humans. The evaluation of this toxicity with regards to Al-species and total Al is often hampered by the lack of available analytical methodology. Aluminium is toxic to plants and accumulates especially in roots. The toxicity may be caused by interferences in cell multiplication in the root, binding of phosphorus, decrease in enzymatic activities, changes in the cell walls and interferences in resorption and transport of Ca, Mg, Ρ, Κ and even water. Al which is accessible to aquatic biota (e.g. fish) is known to be highly toxic to them. Aluminium is toxic to humans. Patients submitted to dialysis are the most exposed to Al contamination (dementia, anemia). Al is also suspected to be linked with Alzheimer's disease (senile dementia). The project will start with a feasibility study consisting of the study of the stability of a number of complexed forms of Al in aqueous solutions. Following this, intercomparisons will be organized for the determination of Al-species in solutions. At the end of the project it is hoped to study the speciation of Aluminium in soil.

STATUS

Feasibility study to be concluded by the end of 1992.



PARTICIPANTS

For the initial study :

Southwest Polytechnic, UK Univ. Cordoba, Ε Univ. Oviedo, Ε

The other participants to be determined.

235

PROJECT RM 385

IMPROVEMENT OF THE DETERMINATION OF SELENIUM SPECIES IN ENVIRONMENTAL MATRICES

PROJECT DEFINITION

Selenium is an essential element; e.g. deficiency in Se can produce ischaemia, heart disease, liver damage and Se is supposed to play a role in DNA-repair thus reducing the risk of cancer, but higher amounts of Se may be dangerous. The various forms of Se have a widely differing toxicity e.g. the toxicity of Se(VI) is 100-1000 times higher than that of Se(IV). In aqueous solution, Se may be present as Se(IV), Se(VI), methylated Se-species and other forms of organic Se such as Se-cysteine and Se-methionine. In view of the different toxicological behaviour of various Se containing compounds and their different toxicity it is necessary to determine the speciation rather than the total contents to judge the environmental danger caused by Se. The difficulty of the determination of Se species with various techniques highlights the need to perform speciation studies to improve analytical methodology. In a first stage, the project is focused on the methodologies for the determination of Se(IV) and Se(VI) in water. Then the study will continue with the improvement of methods for the determination of organic Se-species in water and possibly in fish.

STATUS

Feasibility study for Se(IV) and Se(VI) to be concluded by the end of 1992. First intercomparison planned in 1993.



PARTiqPANTS

Preliminary study: Univ. Complutense, Madrid, E LNETI, Sacavèm, Ρ

Other participants: to be determined later.

236

PROJECT RM 405

IMPROVEMENT OF THE DETERMINATION OF CHROMRJM SPECIES IN ENVIRONMENTAL MATRICES

PROJECT DEFINITION

Chromium is an element of which the various forms Cr(III) and Cr(VI) have a widely differing toxicity. Generally speaking, the toxicity of Cr(VI) is 100-1000 times higher than that of Cr(III). On the other hand Cr is an essential nutritional element at lower levels (e.g. glucose tolerance factor in diabetes). The project consists in first studying the stability of Cr(III) and Cr(VI) in solutions. Following this, collaborative work will be organised to improve methods of determination. If this is successful the project should proceed with the certification of Cr(III) and Cr(VI) in water in a first stage. Other studies are carried out for the improvement of determination of Cr(VT) in dust (filters loaded with Cr(VI)-containing dust) which could also lead to certification. This project will possibly be followed by the certification of Cr (VI) in soils.

STATUS

Stability studies of Cr(III) and Cr(VI) in water concluded in 1991. First intercomparison to be concluded by the end of 1992. Feasibility study on Cr(VI) on filter in progress.



PARTICIPANTS

Preliminary studies: Rijksuniversiteit Gent, INU, Β

Bund, für Seeschiffahrt und Hydrogr., Hamburg, D CIBA-GEIGY, Basel, CH Ecole Nat. de Chimie, Strasbourg, F Health and Safety Executive, London, UK Inst. Occupational Health, Birmingham, UK Inst. Occupational Health, Helsinki, SF

Lab. Government Chemist, Teddington, UK Min. Emploi et du Travail, Brussels, Β NCR Demokritos, Agia Paraskevi, GR

Perkin-Elmer, Überlingen, D Severn-Trent Lab., Coventry, UK S0PRA, Milano, I SPECTRO, Kleve, D Thomson Lab., Milton Keynes, UK Univ. of Dublin, IRL Vandkvalitetsinst., Hoersholm, DK Zentralinst, für Arbeitsmedizin, Hamburg, D

- ΒΙΑ, Skt Augustin, D - Chalmers Univ. of Technology, Göteborg, S - CNRS, Serv. Cent. d'Analyse, Vernaison, F - Fond. Clínica del Lavoro, Pavía, I

- Inst, für Gefahrstoff-Forsch., Bochum, - Inst, for Occupât. Health, Copenhagen, - Inst. Nac. de Seguridad e Higiena enl el Trabajo, Barcelona, E - Lab. National d'Essai, Paris, F - Nat.Inst. Occupational Health, Oslo, Ν - Oceanography Laboratory, Liverpool, UK

- Philipps-Univ., Marburg, D

- Sheffield City Polytechnic, Sheffield,

- South West Polytechnic, Plymouth, UK

- State Laboratory, Dublin, IRL

- Univ. Cordoba,Faculdad de Ci eneas,Cordoba, Ε

- Univ. Regensburg, Regensburg, D

- VITO, Mol, Β

D

DK

UK

237

PROJECT RM 286

REFERENCE MATERIALS FOR MICROBIOLOGICAL TESTING OF WATER

PROJECT DEFINITION

Various sorts of water (e.g. bathing water, tap water) are frequently monitored for their microbiological quality. False analytical results may have economic and public health consequences such as: unnecessary delay in taking repaired drinking water system back into use, unnecessary corrective actions after tests with false positive results, unnecessary condemnation of water sources for e.g. food industry, unnecessary constraints on the trade of mineral water or shellfish, unnecessary condemnation of bathing beaches, illness caused by undetected microbes in polluted water, etc. Intercomparisons have indicated that 5-15 % of all results are incorrect. Stability is the main difficulty in developing microbiological RM's. There is evidence that good stability can be achieved by isolating microbes in milk in gelatine capsules.

STATUS

Five intercomparisons have been conducted to study the stability of the materials during transport, reconstitution of lethally stressed micro flora and the various official tests for total coli and thermo tolerant coliforms. E. coli, E. Faecum and E. cloacae have been studied. The certification of E. faecum is foreseen for 1992.


ECU 330 000

PARTICIPANTS

45 laboratories from 11 Member States + S and CH Pilot Laboratory: Or A Havelaar, Bilthoven, NL

238

PROJECT RM 389

SEAWATER MICROBIOLOGY

PROJECT DEFINITION

The Council of the European Communities has adopted a Directive (Council Directive 76/260/EEC) for the harmonization of the legislations of the Member States in this field. The fundamental objectives of this Directive are:

to protect the environment and the public health by reducing the pollution of bathing waters and to prevent further degradation; to inform the public on the quality of bathing waters e.g. "operation blue flag".

Large discrepancies due to a lack of harmonization of methods and a lack of expertise of the laboratories induce several difficulties:

production of unreliable results and impossibility to harmonise the situation as requested by the Directive; general doubt expressed by the responsible officials when contamination is detected; damage to the credit given to sanitary control of bathing waters and which consequently does not stimulate national and local authorities to improve the situation;

and finally, it ruins any effort to inform the public and sheds doubt with the general public on the quality of all bathing waters.

It is not possible to circulate seawater samples with a guarantee of sufficient stability to the different laboratories within the EC. Therefore, it is necessary to bring all participating laboratories in an intercomparison on the determination of faecal microorganisms to the same place in order to provide them with adequate samples.

The host laboratory has the task to provide all participants with the necessary hardware so that they can apply their own method of determination in the same conditions as at home.

7 intercomparisons for a step by step approach are foreseen.

STATUS

Feasibility studies finished (2 intercomparisons: 1 with 5 labs; 1 with 34 labs)



PARTICIPANTS

34 official laboratories from 11 E.G. countries + SF Pilot laboratory; Institut Pasteur, Lille, F

239

PROJECT RM 235

S0 2 IN AIR

PROJECT DEFINITION

Community Directive 80/779/EEC specifies maximum, permissible levels of sulphur dioxide in the ambient air. Intercomparisons organized by DG XI in support of the implementation of this Directive have shown differences in excess of 10 % between central laboratories and in excess of 30 % between network monitors. The aim of the project was to improve the analytical technique and agreement between results.

STATUS

In the first intercomparison the values obtained ranged from 78 to 94 nmol/mol. In the final stage the sampling procedure had been improved (dead volume miriimised, length of sampling line rninimised, sufficient equilibration time). AU laboratories agreed to within a range of 4 nmol/mol.


ECU 84 000

PARTICIPANTS

L'Air Liquide Belge, Schelle, Β Boe Special Gases, London, Uk Bundesgesundheitsamt, Institut für Wasser-, Boden- und Lufthygiene, Berlin, D Joint Research Centre, Ispra, I Laboratoire National d'Essais, Paris, F Messer-Griesheim, Duisburg, D Risoe National Laboratory, Roskilde, DK SIAD, Bergamo, 1 Umweltbundesamt, Offenbach am Main, D Van Swinden Laboratorium, Delft, NL

240

PROJECT RM 265 (a)

AROMATIC HYDROCARBONS IN TENAX

PROJECT DEFINITION

Occupational exposure of industry workers to potentially harmful vapours may be highly variable from one worker to another. Therefore periodic monitoring of the exposure of each individual worker is legally required. Community legislation is being developed; a draft CEN standard requires an overall accuracy of 30 %; as the sampling is expected to be the larger source of error, analyses should be accurate to within appr. 10 %. Intercomparisons with leading laboratories from government and from chemical industry have shown much larger errors.

Therefore several projects were started to improve the accuracy of workplace air monitoring. The intention was to cover a limited number (e.g. 10) of classes of compounds, which were measured in a wide range of industries and which covered the various types of technical difficulties encountered. Aromatic hydrocarbons were selected for the first project in this series, as they are universally used as solvents (toluene, xylene,...) or present in gasoline and exhaust gases (benzene). "Personal monitoring" of exposure to aromatic hydrocarbons is usually performed by trapping vapours on a sorbing agent, from wich they are desorbed either by heat (a) or by solvent extraction (b) for the final gas chromatographic determination.

RESULTS

Three successive intercomparisons were organised, each followed by a meeting where the measurement methods were discussed. The main sources of error were:

evaporation of liquids during the preparation of the standard solutions use of uncalibrated equipment (e.g. syringes) not readily detected instrument malperformances (leaks in the thermal desorber, malfunctioning analytical balance; unoptimised flame ionisation detector).

A reference material was certified consisting of Tenax tubes with: (1.053 +/- 0.014) Mg benzene; (1.124 +/- 0.015) μ.% toluene and (1.043 +/- 0.015) μg m-xylene. Certification report : EUR 12308, 1990.


ECU 316 000

PARTICIPANTS

ΑΚΖ0 Research Labs, Arnhem, NL - BP Research Centre, Sunbury-on-Thames, UK - Directoraat - Generaal van de Arbeid, Voorburg, NL - Dow Chemical (Nederland), Terneuzen, NL - E0LAS, Dublin, IRL - The State Laboratory, Dublin, IRL - HSE-0MHL, London, UK - ICI Chemicals & Polymers, Runcorn, UK - Koninklijke Shell Laboratoria, Amsterdam, NL - Lab. of the Government Chemist, Teddington, UK - National Inst, of Occupational Health, Hellerup, DK - Rhône-Poulenc Industrialisation, Décines-Charpieu, F - TN0-MT, Delft, NL -Univ. Urbion (1st. Scienze Chimiche), I

241

PROJECT RM 265 (b)

AROMATIC HYDROCARBONS IN CHARCOAL

PROJECT DEFINITION

This project, which is similar to project RM 265 (a)„ aims at the certification of a reference material for use in solvent desorprion procedures.

STATUS

In progress.


ECU 230 000

PARTICIPANTS

AKZO Research Labs., Arnhem, HL

Bayer, Leverkusen, D

ΒΙΑ, Skt. Augustin, D

Bundesanstalt für Arbeitsschutz, Dortmund, D CTT-Servicos Saude Occupacional, Ρ Directoraat-Generaal v.d. Arbeid, Voorburg, NL

Drägerwerk, Lübeck, D EOLAS, Dublin, I Fondazione Clínica del Lavoro, I

Fraunhofer-Inst. Umweltchemie Ökotoxikologie, Schmallenberg, D HSE-OMHL, London, UK INRS, Vandoeuvre, F INSKT, Baracaldo, E INSHT-Centro Nacionaal de Condiciones de Trabajo, Barcelona, E INSHT - Hygiene Industrial, El Palmar, E Inst, für Arbeits- und Sozialmedizin, Erlangen, D Inst, de Médecine et Hygiène du Travail, Lausanne, CH Institut Wasster-, Boden- und Lufthygiene, Berlin, D Jysk Teknologisk/Kemitechnik, Aarhus, DK K.U. Leuven, Lab. Arbeidshygiëne en -toxicologie, Leuven, Β Lab. Toxicologie Industrielle, Bruxelles, Β

LIS Nordrheinwestfalen, Essen, D

Miljoe-Kemi, Galten, OK

Ministry of Labour, Athens, GR

Nat. Inst. Occupational Health, Copenhagen, DK

Niedersächsisches LIS, Hannover, D SCK-Leefmilieu, Mol, Β Shell UK, Occupational Hygiene Unit, Chester, UK

TI-Environmental Technology, Taastrup, DK

Univ. Gesamthochschule Paderborn, D

Univ. Urbino (1st. Scienze Chimiche), I

242

PROJECT RM 329

CHLORINATED HYDROCARBONS

PROJECT DEFINITION

This project is similar to project 265. Chlorinated hydrocarbons are widely used as solvents; intercomparisons have shown considerable errors in leading laboratories. Unexpected problems are encountered in calibration. Therefore a sequence of intercomparisons and technical discussions was undertaken, and the certification of one reference material is planned. Compounds of interest: dichloromethane; 1,1,1-trichloroethane; trichloroethene; tetrachloroethylene.

STATUS

In progress.


a) Thermal desorption : ECU 310 000 (estimated) b) Solvent desorption : ECU 230 000 (estimated)

PARTICIPANTS

(a) Thermal desorption:

AKZ0 Research, Arnhem, NL BP Research, Sunbury-on-Thames, UK Carlo Erba, Ródano, I DANI, Monza, I Directoraat-Generaal van de Arbeid, Voorburg, NL EOLAS, Dublin, IRL HSE-OMHL, London, UK ICI, Runcorn, UK JRC, Ispra, I

Laboratoires Wolff, Clichy - F LIS Nordrhein-Westfalen, Essen, D National Inst. Occupational Health, Copenhagen, DK Perkin-Elmer, Beaconsfield, UK Rhône Poulence, Décines-Charpieu, F The State Laboratory, Dublin, IRL TN0-HT, Delft, NL Univ. Urbino, Urbino, I VTT, Espoo, SF

b) Solvent desorption:

Expected to be largely the same as in project 265 (b)

243

PROJECT RM 335

WORKPLACE AIR SAMPLING

PROJECT DEFINITION

Most techniques used for the monitoring of the exposure of individual workers to harmful vapours consist of a sampling step (trapping of the vapours on a sorbing agent or with a reagent) and an analysis step (desorption and determination of the trapped compounds). Whereas the larger errors are expected in the sampling step, reference materials are helpful only in the analysis step. The purpose of this project is to offer a means of quality control for the sampling step also. The work consists of intercomparisons in which a uniform test atmosphere is generated in a purpose-built system, where all participants can sample at the same time in the same polluted air, each with their own devices and procedures. It is expected that this will lead to the identification of sources of error. This work will at the same time offer the possibility to validate the various types of samplers (this is especially necessary for the "passive" samplers where vapours are collected by diffusion without measuring a volume of air) and to check the performance of "direct reading" devices (e.g. length-of-stain tubes).

STATUS

Two intercomparisons were organised so far, the analytes being aromatic hydrocarbons and chlorinated hydrocarbons.


ECU 130 000

PARTICIPANTS

Arbejdsnriljoeinstituttet, Koebenhaven, DK - BASF AG, Ludwigshafen, D - ΒΙΑ, Skt. Augustin, D -BP International, Guilford, UK - B.P. Research Centre, Middlesex, UK - Bundesanstalt für Arbeitsschutz, Dortmund, D - Dept. de Ingeniena Química, Hurcia, E - Drägerwerk, Lübeck, D - EOLAS, Dublin, IRL -ICI Chemicals & Polymers, Runcorn, UK - ICI Dept. of Research & Tech., Runcorn, UK - Health and Safety Executive, London, UK - IKP, Stuttgart, D - INCOHINSA, Madrid, ES - INERIS, Verneuil-en-Halatte, F - INSHT, Baracaldo, ES - Inst. Arbeits- und Sozialmedizin, Erlangen, D - Instituto Nacional de Seguridad e Hygiene en el Trabajo, Barcelona, ES - KYAE, Athens, GR - Laboratorio di Igiene Industríale, Pavía, I - LIS, Essen, D - Miljoe Kemí, Galten, DK - Min. de l'Emploi et du Travail, Bruxelles, Β - Niedersächsisches Landesamt, Hannover, D - Rhône Poulenc Industrialisation, Décines-Charpíeu, F -Severn-Trent Laboratories, Finham Coventry, UK - State Laboratory, Dublin, IRL - TNO Afd. Binnenmilieu, Delft, NL - TÜV, Hamburg, D -Tyotervejslaitos, Helsinki, SF - Universita degli studi di Urbino, Urbino, I - VITO-LMB, Mol, Β - Warren Spring Laboratory, Stevenage, UK -

244

PROJECT RM 388

IMPROVEMENT OF THE DETERMINATION OF FLUORIDE AND CHLORIDE IN COAL AND FLY ASH

PROJECT DEFINITION

Coal and fly ash are currently analysed to assess air and ground water pollution, to evaluate mass balance in coal production and as indirect control of emission (based on the differences in concentrations found in coal and fly ash respectively). Some areas suffer from a severe pollution by emission of fluoride into the atmosphere and its subsequent transport into the ground water. In the past materials such as incineration ash were used as fillers for concrete and road constructions. Nowadays the quantity produced is such that deposition is necessary which in turn becomes a problem because of the possible toxicity. Chloride is responsible for burner corrosion and has to be determined to assess this risk. In some cases raw materials may be rejected if the chloride and fluoride contents are too high which is a source of economic concern. The control of the quality of measurements is therefore of paramount importance which underlines the need for RMs certified for their contents in CI and F.

STATUS

A series of intercomparisons has demonstrated that the certification of F and CI in coal and fly ash was feasible. The certification will be concluded by the end of 1992 (fly ash and coal, candidate CRMs 038 and 460).


ECU 80 000

PARTICIPANTS

Coordinator: NV KEMA, Arnhem, NL Bund, für Materialforschung und Prüfung, Berlin, D CNRS, Service Central d'Analyse, vernaison, F ECN-Research Centre, Petten, NL ELSAM, Aabenraa, DK Ente Nazionale per l'Energía Elettrica, Pisa, ! Gordinne & Cie, Rozenburg, NL INERIS, verneuil en Halatte, F Inst, de Carboquimica, Zaragoza, E Laborelec, Linkebeek, Β Ministère des Affaires Economiques, Brussels, Β Rheinisch-Westfälischer TÜV, Essen, 0 Rijksuniversiteit Gent, INW, Gent, Β Ruhrkohle AG, Essen, 0 South West Polytechnic, Plymouth, UK Stazione Sperimentale per i Combustibili, San Donato, I Technical Res. Centre (VTT), Espoo, SF Universidad de Oviedo, Oept. de Qiumica Analítica, Oviedo, Ε

245

PROJECT RM 396

IMPROVEMENT OF THE DETERMINATION OF FLUORIDE AND CHLORIDE IN CLAY

PROJECT DEFINITION

The clay materials used in the brick industries are currently monitored to avoid air and ground water pollution. Some areas suffer from a severe pollution by emission of fluoride into the atmosphere and its subsequent transport into the ground water as clay may contain 200 to 1200 Mg/g of F. As an example, the brick and ceramic industry is responsible for 50 % of the total F emission in The Netherlands. The emissions are calculated from the difference in the F content of clay and the final product Cbrick). Chloride is responsible for corrosion and has to be determined to assess this risk. Problems have been observed during baking of clay. In some cases, raw materials are rejected if the CI and F contents are too high which cause an economic concern. As a consequence, many European countries have implemented legislations for the maximum authorised values in gaseous emission of F and CI from brick industries, which strongly stresses the need for the control of the quality of measurements and therefore for the production of reference materials.

STATUS

Certification to be concluded by the end of 1992 (candidate CRM 461).


ECU 53 000

PARTICIPANTS

Coordinator: NV KEMA, Arnhem, NL Bund, für Materialforschung und Prüfung, Berlin, D CNRS, Service Central d'Analyse, Vernaison, F ECN-Research Centre, Petten, NL ELSAM, Aabenraa, DK Gordinne & Cíe, Rozenburg, NL INERIS, Verneuïl en Halatte, f lnst. de Carboquimica, Zaragoza, E Ente Nazionale per l'Energia Elettrica, Pisa, I Min. des Affaires Econ., Brussels, Β Rijksuniversiteit Gent, INU, Gent, Β Rheinisch-Westfälischer TÜV, Essen, 0 Ruhrkohle AG, Essen, D South West Polytechnic, Plymouth, UK Stazione Soerimentale per i Combustibili, San Donato, l Techn. Centrum voor de Keramische Industrie, De steeg, NL Technical Res. Centre (VTT), Espoo, SF Universidad de Oviedo, Dept. de Qiumica Analítica, Oviedo, E

246

PROJECT RM 397

ALDEHYDES IN WORKPLACE AIR

PROJECT DEFINITION

The common methods for the personal monitoring of the exposure of workers to aldehydes in workplace air uses sampling through solids or liquids where the aldehydes are chemically converted to less reactive compounds which are then determined in the laboratory. The most widely used reagent is 2,4-dinitrophenylhydrazine (DNPH) which reacts with aldehydes to form hydrazones which are then determined by HPLC. It is difficult for laboratories to check if they meet the planned CEN requirement of 30 % overall accuracy; no quality assurance schemes or reference materials exist.

Intercomparisons will therefore be organised in which solutions of hydrazones, and impregnated filters containing the reaction products of formaldehyde, will be distributed. Reference materials will be certified (simulated sampling solutions, simulated sampling filters for formaldehyde, and pure substances). A type of diffusive samplers, which is already validated for formaldehyde, will be validated for other aldehydes as well. The analytes studied will be: formaldehyde, acetaldehyde, acrolein and glutaraldehyde (and acetone which is a common interfèrent).

STATUS

Feasibility study (preparation of pure and homogeneous batches; study of stability upon long term storage) in progress.



PARTICIPANTS (provisional list)

Arbetsmiljoeinstitutet, Umea, S - BASF, Ludwigshafen, D - BP Research Centre, Sunbury-on-Thames, UK - CEC Joint Research Centre, lspra, I - Dansk Teknol.Inst., DK - Directoraat-Generaal van de Arbeid, Den Haag, NL - EOLAS, Dublin, IRL - Fondazione Clínica del Lavoro, Pavia, I - HSE-OMHL, London, UK - INERIS, Verneuil-en-Halatte, F - INRS, Vandoeuvre, F - INSHT, Barcelona, ES - INSHT, Madrid, ES - Inst. Arbeits- und Sozialmedizin, Erlangen, D - Inst. Milieuwetenschappen TNO, Delft, NL - Inst. Nac. de Saude Dr Ricardo Jorge, Porto, Ρ - Inst. Univ. de Medicine et d'Hygiène du Travail, Lausanne, CH - Kemiteknik, Aarhus, DK -Miljoe-Kemi, Galten, DK - Min. Emploi et Travail, Brussels, Β - Nottingham Polytechnic, UK - Tampere Regional Inst. Occup. Health, Tampere, SF - Thomson - Laboratories, Milton Keynes, UK - Turku Regional Inst, of Occupational Health, Turku, SF - VIT0-LMB, Mol, Β - Uarren Spring Laboratory, Stevenage, UK

247

PROJECT RM 398

ISOCYANATES IN WORKPLACE AIR

PROJECT DEFINITION

The common methods for the personal monitoring of the exposure of workers to isocyanates in workplace air uses sampling through solids or liquids containing a reagent such as l-(2-methoxyphenyl)-piperazine (2-MP) which reacts with the isocyanates to form stable compounds which are then determined by HPLC. It is difficult for laboratories to check if they meet the planned CEN requirement of 30 % overall accuracy; no sufficiently validated methods or reference materials exist.

Intercomparisons will therefore be organised in which simulated evaporation residues of 2-MP sampling solutions will be distributed. Reference materials will be certified (simulated evaporation residues of sampling solutions, and pure substances). The analytes of interest will be: 2,4- and 2,6-toluene diisocyanate (TDI), 4,4'-diphenyl-methane diisocyanate (MDI) and hexamethylene diisocyanate (HDI).

STATUS

Feasibility study (preparation of pure and homogeneous batches; study of stability upon long term storage) in progress.



PARTICIPANTS (provisional list)

AKZO Corporate Res., Arnhem, NL - ArbetsmiIjoeinstitutet, Umea, S - BASF, Ludwigshafen, D - Bayer, Leverkusen, D - ΒΙΑ, Skt-Augustin, D - BP Research Centre, Sunbury-on-Thames, UK - Dansk Teknologisk Inst.-Kemiteknik, Aarhus, DK - Directoraat-Generaal van de Arbeid, Den Haag, NL - EOLAS, Dublin, IRL - Fondazione Clínica del Lavoro, Pavia, I - HSE-OMHL, London, UK - ICI Specialties, Manchester, UK - INERIS, Verneuil-en-Halatte, F - INRS, Vandoeuvre, F - INSHT, Barcelona, E - INSHT, Madrid, E - Inst. Arbeits- und Sozialmedizin, Erlangen, D - Inst. Gefahrstoffforschung der Bergbau-Berufsgenossenschaft, Bochum, D - Inst. Milieuwetenschappen TNO, Delft, NL - Inst. Nac. de Saude Dr Ricardo Jorge, Porto, Inst. Occup. Medicine, Edinburgh, UK - Inst. Univ. de Medicine et d'Hygiene du Travail, Lausanne, CH - Miljoe-Kemi, Galten, DK Min. Emploi et Travail, Brussels, Β - Rhône-Poulenc Industrialisation, Décines-Charpieu, F - Tampere Regional Inst, of Occup. Health, Tampere, SF - Thomson Laboratories, Milton Keynes, UK - Turku Regional Inst, of Occupational Health, Turku, SF - Warren Spring Laboratory, Stevenage, UK

248

PROJECT RM 411

NO, FROM BOILERS

PROJECT DEFINITION

A European standard method is being developed for measuring the NO, emission from domestic boilers. The standard would in principle require that the ambient temperature and humidity (possibly even pressure) are fixed. As this is in practice not feasible (for economic reasons), a model will be included to convert the NO, emission measured at given ambient conditions to the standard conditions by calculation. This model requires a data base of measurements on the same boilers under different ambient conditions. As the available empirical data were far insufficient, a systematic study was undertaken in two laboratories where the temperature and humidity can be varied in a fairly wide range.

STATUS

In progress.


ECU 87 000

PARTiaPANTS

CETIAT, Villeurbanne, F VEG Gasinstituut, Apeldoorn, NL

Biomedical Analysis

251

PROJECT RM 303

MAGNESIUM AND LITHRIM IN HUMAN SERUM

PROJECT DEFINITION

Magnesium deficiency is a clinically serious condition which leads to a variety of muscular and neurological disorders. It may result e.g. from insufficient magnesium intake, from impaired absorption or from prolonged diuretic treatment. More and more use is made of determinations of serum magnesium in clinical practice. Lithium salts are used as drugs to treat recurrent depressive conditions. The range of therapeutic blood concentrations is narrow and an accurate monitoring of the dosage given to the patient is necessary. The project first consists of intercomparisons to assess the methods used to determine Mg & Li in serum. The project should be concluded by a certification campaign on two lyophilized serum reference materials. The CRMs 303 & 304 previously certified for their total calcium concentration should be used for this purpose.

RESULTS

The project was completed in 1991. Twelve European laboratories contributed to the establishment of the certified concentration values in each of the two serum reference materials:

CRM 303 : Mg(II) (1.131 ± 0.022) mmol/1 Li(I) (0.523 ± 0.024) mmol/1

CRM 304 : Mg(II) (1.85 ± 0.03) mmol/1

Li(I) (0.985 ± 0.029) mmol/1

Details on the certification exercise are published in the report EUR 14 186 (1992).



PARTICIPANTS Coordinator : Rijksuniversiteit Gent, Laboratoria v. Medische Biochemie / Klinische Analyse, Gent, Β Centre National de la Recherche Scientifique, Service central d'Analyse, Vernaison, F Energieonderzoek Centrum Nederland, Petten, NL Frederiksberg Hospital, Clinical Chemistry Department, Copenhagen, DK Gartnavel General Hospital, Biochemistry Department, Glasgow, UK Hospital de la Santa Creu i San Pau, Barcelona, E Institute für Wasser-, Boden- und Lufthygiene, Bundesgesundheitsamt, Berlin, D Istituto Superiore di Sanità, Laboratorio de Tossicologia Applicata, Roma, I Istituto Superiore di Sanità, Laboratorio di Biochimica Clínica, Roma, I Joint Research Centre Geel CBNM, CEC, GEEL, Β Royal Victoria Hospital, Endocrine Laboratory, Belfast, UK St. Radboud Ziekenhuis, Internal Medicine, Clinical Chemistry Lab., Nijmegen, NL

252

PROJECT RM 380

IONISED CALCIUM IN HUMAN BLOOD, SERUM AND PLASMA

PROJECT DEFINITION

Measurements of plasma concentrations of potassium, sodium, calcium and chloride ions are amongst the most common requests made to routine clinical biochemistry laboratories. There is a growing need to monitor these parameters in patients severely ill and during and following major surgery. Since 1982 calcium can be measured directly for whole blood, serum and plasma by electrochemical Potentiometrie analysers based on ion-selective electrodes (ISEs) rather than by flame photometry of diluted plasma samples. Results, however, depend on the analyser used. The International Federation of Clinical Chemistry (IFCC) has addressed that problem and is currently developing a reference method for the determination of blood ionised calcium. The project aims at working out, through collaborative studies, the details and specifications of the IFCC measurement procedure. A reference cell will be circulated together with recommendations for its use. It might be concluded by the certification of reference samples to help implement the IFCC recommendations.

STATUS

The project has started in 1990. It is expected to be completed in 1993. A first interlaboratory study was concluded. It revealed discrepancies between results obtained using the reference cells as well as between results yielded by commercial ISE instruments. An additional intercomparison is due to start in 1992, implementing the conclusions of the first study (modifications on reference cell, protocol, etc.).



PARTICIPANTS

Coordinators : Technical University of Eindhoven, NL and University of Newcastle, UK

"Eginitio" University Hospital, Athens, GR Allgemeines Krankenhaus, Hamburg, D AVL Biomedical Instruments, Schauffhausen, CH Centre Hospitaller de Meaux, F Centre Hospitaller Universitaire Necker-Enfants Halades, Paris, F Children Hospital "Aglaia Kiriakou", Athens, GR Ciba-Diagnostics Ltd., Suffolk, UK Faculdad de Ciencias, Valladolid, E Faculdade de Ciencias, Lisboa, Ρ Herlev Hospital, DK Institut de Pharmacie, Université Libre de Bruxelles, Β Instrumental Analysis, Eindhoven, NL Instrumentation Laboratory SpA, Milano, I Kone Corporation, Espoo, SF Medizinische Hochschule Hannover, D Ospedale Niguarda Ca

1 Granda, Milano, I

Radiometer A/S, Copenhagen, DK St. James University Hospital, Leeds, UK St. Vincent Hospital, Dublin, IRL Swiss Federal Institute of Technology, Zurich, CH University of Linkoping, S

253

PROJECT RM 174

PROGESTERONE IN HUMAN SERUM

PROJECT DEFINITION

Progesterone is a steroid hormone derived from cholesterol. In adult women, it is produced in the ovaries. An important reason for determining progesterone in serum is the assessment of female infertility. The project includes the development of an isotope dilution - mass spectrometry (ID-MS) method for the determination of progesterone in human serum. Two serum pools will be prepared from blood collected from selected populations of donors. Each batch is to contain only endogenous progesterone.

RESULTS

The project has been completed in 1989. Six laboratories contributed to the establishment of the certified value for the progesterone concentration in each of the two serum pools. Four intercomparison exercises were necessary to set up an ID-MS procedure in each participating laboratory. The between-laboratory CV was initially of about 6 %. The certified concentrations of progesterone in the serum reference materials are : CRM 347 (10.13 ± 0.21) nmol/1 CRM 348 (40.3 ± 1.0) nmol/1 Details on the certification exercise are published in report EUR 12282 (1989).


ECU 144 000

PARTICIPANTS

Academisch Ziekenhuis, Groningen, NL Centro di Spettrometrîa di Massa, Firenze, I Fondation de Recherche en Hormonologie, Fresnes, F Institut für Klinische Biochemie, Bonn, D National Institute for Biological Standards and Control, Potters Bar, UK Rijksuniversiteit Gent, Β Tenovus Institute for Cancer Research, Cardiff, UK

254

PROJECT RM 353

17 /9-OESTRADIOL IN HUMAN SERUM

PROJECT DEFINITION

Oestradiol is a C18-steroid and is found in both females and males. In females, throughout puberty, it stimulates growth of the sex organs and development of secondary sexual characteristics, while in adult females its main biological action is on the functioning of the reproductive tract. In the male the role of oestradiol is thought to be involved with testosterone in the regulation of gonadotrophin secretion. Oestradiol assay is the most widely used test for the assessment of oestrogen status in infants and adults. Oestradiol analysis is also essential for monitoring ovulation inducing therapies and hormone replacement after castration or in the post-menopausal period of life. The project aims at the certification of 17/3-oestradiol concentrations in human serum materials, by method procedures using isotope dilution - mass spectrometry (ID-MS).

STATUS

The feasibility of preparation and conservation of human serum based samples was sucessfully demonstrated. The method development achieved allows to envisage a certification exercise in 1992. The project is actually at the stage of collecting the required human sera. Certification is expected in 1993 - 1994.



PARTICIPANTS

Centro di Spettrometria di Massa, Fierenze, I Fondation de Recherche en Hormonologie, Fresnes, F Instand, Düsseldorf, D Institut für Klinische Biochemie, Bonn, D National Institute for Biological Standards and Control, Potters Bar, UK Rijksuniversiteit Gent, Β Tenovus Institut for Cancer Research, Cardiff, UK

255

PROJECT RM 217

THYROXINE IN HUMAN SERUM

PROJECT DEFINITION

Thyroxine is a hormone secreted by the thyroid gland. It controls a great many metabolic processes in the body. In the newborn, it has been shown to play a key role for the growth and development of the brain. In the field of hormonology, the determination of serum thyroxine is amongst the most frequent tests. The project comprises the set-up of an isotope dilution - mass spectrometry method (ID-MS), including the preparation of labelled thyroxine. Three batches of human serum, each of them corresponding to a particular thyroxine level will be certified. Thyroxine levels selected are those found in hypothyroid subjects, normal individuals and hyperthyroid patients respectively.

STATUS

Methodological developments are completed. Three laboratories are using ID-MS for the determination of serum thyroxine. Two intercomparison exercises have been carried out. Certification is expected in 1992.


ECU 150 000

PARTICIPANTS

Institut für Klinische Biochemie, Bonn, D National Institute for Biological Standards and Control, Potters Bar, UX Rijksuniversiteit Gent, Β University of Birmingham, UK

256

PROJECT RM 320

HUMAN LUTEINIZING HORMONE

PROJECT DEFINITION

Luteinizing hormone (LH) is a glycoprotein secreted by the anterior portion of the pituitary gland. In the male, LH controls testosterone secretion. In the female, at about the midpoint of the cycle, as a result of the action of LH, an ovum is released and progesterone secretion begins. Measurement of serum LH has proved useful in a variety of conditions including hypogonadism, ovulation and infertility studies. Serum assay of glycoproteic hormones is complicated by the fact that these molecules are circulating under different forms that vary according to the physiological and pathological status of the patients. The project is intended to improve the comparability of the assays of LH in serum. The means to achieve this objective involve the epitope mapping of several preparations of LH using monoclonal antibodies (mAbs). This should permit to identify mAbs reacting with epitopes constantly present on the surface of all LHs or conversely with epitopes expressed by LH in specific situations. The bioactivity and structure of LH isoforms will probably be assessed.

STATUS

In 1988 an interlaboratory study was launched, between 23 laboratories, to determine LH in different serum samples. The results showed a wide scatter between methods. Work for epitope mapping has been completed. A set of sera corresponding to different physio-pathological situations has been collected and assayed by a series of kits, making use of monoclonal antibodies. The results are presented in a report which is being prepared. In parallel a study has started (in 1992), on the determination of LH epitopes involved in its biological activity. The results should be available by the end of 1992.



PARTICIPANTS

For the epitode mapping: Coordinator: Université de Marseille, F

Academisch Ziekenhuis, Vrije Universiteit, Brussel, Β AKZO, Organon Teknika N.V., Turnhout, Β

Amerlite Diagnostics Ltd,

Buckinghamshire, UK

Amersham Int.pic, Cardiff, UK

Β i omér i eux, Charbonni ères-1es-Ba i ns, F Boehringer Mannheim GmbH, Penzberg, D CIS-ΒΙΟ International, Gif sur Yvette, F

Dakopatts A/S, Glostrup, DK

Eurogentec, Liège, Β Fondation de Recherche en Hormonologie,

Fresnes, F

Hoechst AG, Frankfurt, D

Hospital de la Santa Creu i San Pau,

Barcelona, Ε

Hybritech Europe, Liège, Β Immunotech, Marseille, F

Institut de Médecine de la Reproduction, Marseille, F IRE-Medgénix, Fleurus, Β Ludwig-Maximilians Universität München, D

Novo, Biolabs, Cambridge, UK ORIS-Industrie Bagnols sur Cèze, F Pharmacia-Uallac ΟΥ, Turku, SF Policlinico Padre Sacco, Milano, I

Rijksinstituut voor Volksgezondheit

& Milieuhygiene, Bilthoven, NL

Serono Diagnostics Ltd, Woking, UK

Sorin Biomedica SpA, Saluggia, I

St. Thomas Hospital, London, UK

Universidade de Coimbra, Ρ

For interlaboratory trials :

see project ne 321 for FSH.

257

PROJECT RM 321

HUMAN FOLLICLE STIMULATING HORMONE

PROJECT DEFINITION

Follicle stimulating hormone (FSH) is also a pituitary glycoproteic hormone. It acts synergetically with LH to control gonadal functions. High concentrations of FSH in plasma would suggest gonadal failure in both males and females. FSH and LH are structurally very close. The aim of this project is identical to that on LH and it should proceed along the same lines.

STATUS

In 1988 an interlaboratory trial was organised involving 22 laboratories, to determine FSH in different serum samples. The results showed a marked difference in means between the all radioimmunoassay (RIA) and the all immunometric assay (IMA) groups. This suggests that the all laboratory trimmed mean (ALTM) is unlikely to provide a suitable target value, at least for high concentration of FSH. Work may continue with epitope mapping studies such as those carried out for LH when the studies on the latter are completed.



PARTICIPANTS

Akademisch Ziekenhuis, Brussel, Β

Amersham International pic, Cardiff, UK

BioMérieux, Charbonières-les-Bains, F Bleuland Ziekenhuis, Gouda, NL Boehringer Mannheim GmbH, Penzberg, D Charing Cross Hospital, London, UK Cliniques Universitaires St Luc, Bruxelles, Β Copenhagen County Hospital, Glostrup, DK

Dakopatts, Glostrup, DK

Edinburgh Royal Infirmary, UK

Eurogentec S.A., Liège, Β Hospital de La Santa Creu i San Pau, Barcelona, Ε

Hybritech Europe, Liège, Β Hoechst AG, Frankfurt, D

Immunotech, Marseille, F

Institut Gustave Roussy, Villejuif, F

Institut des Radïoéléments-Medgenix, Fleurus, Β Klinikum Grosshadern, München, D Laboratoires d'Analyses Biologiques Spécialisées, Nice, F Medizinische Hochschule Hannover, D Medizinische Universität Lübeck, D National Athletic Research Centre, Athens, GR National Institute for Biological Standards and Control, Potters Bar, UK Novo Biolabs Ltd., Cambridge, UK Nuclear Research Centre Demokritos, Athens, GR ORIS-Industrie, Bagnols-sur-Ceze, F Queen Elizabeth Hospital, Birmingham, UK Seratec GmbH, Göttingen, D

Serono Diagnostics Ltd., Woking, UK Soriη Biomedica SpA, Salluggia, I

Statens Seruminstitut, Copenhagen, DK

St. Radboud Ziekenhuis Nijmegen, NL

St. Thomas Hospital, London, UK

Universidade de Coimbra, Ρ

Université Aïx-Marseille 2, F

258

PROJECT RM 322

HUMAN PROLACTIN

PROJECT DEFINITION

Human prolactin (PRL) is a polypeptide hormone also secreted by the pituitary. Its role is mainly related to the control of lactation and gonadal function. Serum prolactin has been found elevated in some women with breast cancer. High concentrations of serum prolactin are a clear indication of a pituitary tumour. The objective of the project is to help harmonize results of assays of prolactin in serum. The project will involve intercomparison studies in the first instance to assess currently used assay methods. It should later evolve in the same direction as project n° 320 on LH.

STATUS

In 1988 an interlaboratory study was launched between 21 laboratories to determine PRL in different serum samples. The results showed that the mean values for the various method groups are in satisfactory agreement with the all laboratory consensus mean. Work may start in a similar way to the one for LH and FSH when the studies on LH are completed.



PARTICIPANTS

See project n° 321 for FSH.

259

PROJECT RM 323

α-FOETOPROTEIN

PROJECT DEFINITION

α-Foetoprotein (a-FP) is a fetal globulin synthetized by the embryonic liver. In human beings the transition form a-FP to albumin as the dominant serum protein begins normally at the thirteenth week of gestation. Elevated serum levels of a-FP in adults have been found in patients with primary liver cancer, gonadal tumours and carcinomas of other tissues. The project will include the assessment of the suitability of a-FP purified from a hepatoma cell culture for calibration of serum a-FP assays. The project could lead to the preparation and certification of serum reference samples.

STATUS

A purified a-FP preparation form hepatoma cell line has been produced at the Sclavo Institute (Siena, I). The material as stated by the manufacturer, is > 99 % pure. It is foreseen to use it as calibrator for the determination of the mass concentration of a-FP in serum reference materials. Further assessment of the identity and purity of the a-FP has been carried out while comparison of methods for measuring serum a-FP proceeds. Some 20 laboratories were involved in interlaboratory studies. A lot of 2500 ampoules of lyophilized purified a-FP is prepared. 9 laboratories will be involved in the value assignment campaign and certification is expected in 1993.



PARTICIPANTS

Amersham International pic, Cardiff, UK

BioMérieux, Charbonnières-les-Bains, F Bleuland Ziekenhuis, Gouda, NL Boehringer Mannheim GmbH, Penzberg, D Centre du Médicament, Nancy, F Charing Cross Hospital, London, UK Cliniques Universitaires St. Luc, Bruxelles, Β Copenhagen County Hospital, Glostrup, DK


Diagnostics Pasteur-Kallestad,

Marnes La Coquette, F

Edinburgh Royal Infirmary, UK

Eurogentec, S.A. Liège, Β Herlev Hospital, DK

Hospital de la Santé Creu i San Pau, Barcelona, Ε Hoechst AG, Frankfurt, D

Immunotech, Marseille, F

Institut Gustave Roussy, Villejuif, F

Institut des Radioéléments-Medgenix, Fleurus, Β Klinikum Grosshadern, München, D

Laboratoire d'Analyses Biologiques Spécialisées, Nice, F Max Planck Institut für Biophysikalische Chemie, Göttingen, D Medizinische Hochschule Hannover, D Medizinische Universität Lübeck, D National Athletic Research Centre, Athens, GR National Institute for Biological Standards and Control, Potters Bar, UK Novo Biolabs Ltd., Cambridge, UK Oris-Industrie, Gif sur Yvette, F Sclavo S.A., Siena, I Seratec GmbH, Göttingen, D Serono Diagnostics Ltd., Woking, UK Sorjn Biomedica, S.A. Salluggia, I

Statens Serumsinstitut Copenhagen, DK St. Radboud Ziekenhuis, Nijmegen, NL Universidade de Coimbra, Ρ Universität Freiburg, D Universität Hamburg, D Vrije Universiteit Amsterdam, NL

260

PROJECT RM 324

CARCINOEMBRYONIC ANTIGEN

PROJECT DEFINITION

Carcinoembiyonic antigen (CEA) is a glycoprotein found in the fetal gastrointestinal tract during the first six months of gestation. In the normal adult small amounts of CEA are present in serum. Serum levels increase in case of malignant tumours associated with various cancers e.g. of the colon, rectum, stomach, pancreas, ovaries. The CEA test is particularly useful to monitor the response to therapy in patients with diagnosed malignancies. CEA is the most widely used among the tumour marker tests. The aim of the project is to investigate means to improve the reliability of assays of serum CEA. The project will comprise studies to produce a purified, well characterised CEA material, while examining and improving the specificity of monoclonal antibodies (mAbs) used for the immunological assay of CEA in serum. Techniques of cell culture and genetic engineering will be employed for these purposes. The next step might include the certification of serum reference samples.

STATUS

The work to purify CEA from the human colon adenocarcinoma cell line LS 174 Τ is completed. The purification scheme first included the treatment of the cell line by a phosphatidylinositol phospholipase-C to release CEA from the cell membrane. Further steps comprised anion exchange, irnmunoaffinity and gel filtration chromatographies. The purified material is currently examined for its immunological properties. In parallel, work was undertaken to prepare a synthetic peptide (77 aminoacid residues long) as an immunogenic material. The peptide was selected as representing the portion of the CEA molecule that is the most characteristic of it, i.e. presenting the least homology with other CEA-like proteins. The preparation was to be made by genetic engineering and was successful. The procedure is at present optimized to increase the production yield. The project should be completed in 1994.



PARTICIPANTS

For the purification work: Immunotech S.A., Marseille, F Seratec and Max-Planck Institut, Göttingen, D

For interlaboratory studies: See project n" 323 for a-FP.

261

PROJECT RM 325

HUMAN CHORIONIC GONADOTROPIN

PROJECT DEFINITION

Human chorionic gonadotropin (hCG) is a glycoprotein normally produced by the placenta. The physiological effects induced by hCG are similar to those produced by luteinizing hormone (LH), including induction of ovulation. Indirect measurement of the rapidly rising hCG concentration early in pregnancy forms the basis of most "pregnancy tests" employed today. In men or in non-pregnant women increased levels of serum hCG indicate the presence of a tumour (for example, a choriocarcinoma of the uterus). The determination of serum hCG is of particular value in monitoring the response of the tumour to chemotherapy. The aim is similar to that of projects n° 320 and 321. The approach will be the same as described for project n° 320.

STATUS

In 1988 an interlaboratory study was set up with 19 laboratories, to determine hCG in different serum samples. The results showed that the mean values for the major method groups are in good agreement with the all laboratory consensus means, at least in relation to lower concentrations. Future work including epitope mapping studies may start after the completion of studies on LH.



PARTICIPANTS

See project n" 321 for FSH.

262

PROJECT RM 403

EPIDERMAL GROWTH FACTORS AND GROWTH FACTOR RECEPTORS

PROJECT DEFINITION

The presence of steroid hormone receptors correlates with various biological characteristics in breast and endometrium cancer. Certain tumours produce growth factors, which cause growth stimulation in an autocrine way. It is generally acknowledged that the receptor status of a tumour has prognostic significance and is used in the decision whether endocrine treatment will be given. The project will focus on the standardization of the measurement of epidermal growth factors (EGF) and growth factor receptors (EGFR) in malignant breast cancer tumours. This consists of three Phases: Phase I: The preparation of the iodinated radio active ligand, the preparation of the lyophilized reference membrane sample and research for a reference parameter for expressing assay results. Phase II: Validation and design of the assay in such a way that it may be even implemented by not highly specialized laboratories. Phase HI: Organization of the relative Quality control (QC) programme involving a large number of laboratories from the Members States. In addition, the statistical evaluation of the data provided by the aforementioned laboratories is foreseen.

STATUS

Six iodination methods have been evaluated and three of them resulted in 125I-mEGF molecules showing identical binding behaviour to the EGFR when compared to native EGF. Also no or negligible amounts of oxidized EGF moieties were demonstrated by HPLC. Tracers prepared by any of these methods are equally suitable to measure EGFR in human tissue membrane preparations. In addition the hydroxilapatite (HAP) method, for separating bound and free ligand in the assay of EGFR, was evaluated and assessed to be satisfactory. With respect to the software to calculate receptor binding data obtained with HAP-assay, consensus was reached by the participants to try to use the same one in every laboratory. Completion of this phase of the project is expected in mid 1992. Subsequently the design of a complete assay for the EGFR may be envisaged with a large number of participants involved.



PARTICIPANTS

Phase I Coordinator: - University of Nijmegen, Nijmegen, NL - Dokter Daniël den Hoed Kliniek, Rotterdam, NL - University of Glasgow, Glasgou, UK Phase 11 As above and : - Centre Oscar Lambret, Lille, F - Hospital Universitario San Carlos, Madrid, E - University of Crete, Crete, GR Phase 111 As above (Phases I and II), and a large number of laboratories from EC.

263

PROJECT RM 260

CREATINE KINASE

PROJECT DEFINITION

Creatine kinase (CK) is an enzyme which is present in the cells of most organs. The determination of creatine kinase, and particularly of the three isoenzymes from brain (CK-BB), skeletal muscle (CK-MM) and heart muscle (CK-MB) respectively, is currently performed in clinical chemistry laboratories. The brain isoenzyme (CK-BB) is found elevated in serum of patients with certain neurological diseases. The project consists of the purification of creatine kinase isoenzyme CK-BB from human placenta. The aim is to certify the catalytic activity concentration of creatine kinase in this well characterized purified enzyme preparation. The method used for the assay is that recommended by the International Federation of Clinical Chemistry (IFCC).

RESULTS

The feasibility study could establish that a stable purified enzyme preparation could be produced in lyophilized form. An interlaboratory study was carried out on that preparation with a view to assigning a value to the CK catalytic activity concentration of the reconstituted material. Nine laboratories participated. The agreement between laboratories was judged satisfactory, permitting to propose the preparation for certification with the following value and uncertainty : CRM 299 (325 ± 10) U/l. The report describing the preparation and the certification exercise has been published as report EUR 13886 (1992).


ECU 30 000

PARTICIPANTS

Coordinator: Hospices Civils de Lyon, F Boehringer Mannheim GmbH, Penzberg, 0 Centre Hospitalier Universitaire Vaudois, Lausanne, CH Centre du Médicament, Nancy, F Medizinische Hochschule Lübeck, D Metaxas Memorial Cancer Hospital, Piraeus, GR National Institute for Biological Standards and Control, Potters Bar, UK Odense University Hospital, DK St Radboud Ziekenhuis, Nijmegen, NL Universidad Autónoma de Barcelona, E

264

PROJECT RM 282

ALRAUNE PHOSPHATASE

PROJECT DEFINITION

Alkaline phosphatase (AP) is an enzyme found in particular in the cells which are responsible for the bone formation (osteoblasts). This enzyme is involved in the process of calcification of the bone. The catalytic activity of the enzyme is measured in serum primarily for the diagnosis of bone disease. It is an adjunct for the detection of bone cancer. The project involves the purification of alkaline phosphatase extracted from porcine kidney, its stabilization in an albumin matrix and the production of a batch of samples for certification. The catalytic activity concentration of AP in the partly purified preparation will be certified according to the method of the International Federation of Clinical Chemistry (IFCC).

RESULTS

The project was completed in 1988. A stable preparation of partly purified alkaline phosphatase was produced. The material is in lyophilized form. A strict procedure for reconstitution of the lyophilized enzyme preparation was specified to avoid time -and temperature -dependent increase of activity of the reconstituted AP preparation. The catalytic concentration activity of the reconstituted material was measured by 14 laboratories according to the IFCC method. The certified value and uncertainty were established as : CRM 371 (254 ± 6) U/l. Details on the preparation of the partly purified enzyme and on the results of the certification campaign are presented in the report EUR 11774 (1988).


ECU 75 000

PARTICIPANTS

Boehringer Mannheim GmbH, Penzberg, 0 Centre du Médicament, Nancy, F Fondaζi one Centro San Romanello, Milano, I

Hospices Civils de Lyon, F

Medizinische Hochschule Hannover, D

Medizinische Hochschule Lübeck, D Metaxas Memorial Cancer Hospital, Piraeus, GR National Institute for Biological Standards and Control, Potters Bar, UK Odense University Hospital, DK Royal Free Hospital, London, UK Royal Postgraduate Medical School, London, UK St Radboud Ziekenhuis, Nijmegen, NL Universidad Autónoma de Barcelona, E Université de Liège, Β

265

PROJECT RM 293

LACTATE DEHYDROGENASE

PROJECT DEFINITION

Lactate dehydrogenase (LD) activity determinations in serum are being used, since years, for diagnosing many diseases involving heart, erythrocytes, liver and for detecting tumours. The serum contains in variable proportions five LD isoenzymes, formed from monomelic polypeptides Β and A. The B4 isoenzyme - LD1 - is more abundant in the cells of heart muscle, kidney, brain and in erythrocytes. The LD1 determination in serum is particularly useful in the biochemical diagnosis of myocardial infarction. The objective of the project is to work both on a reliable method for the determination of the catalytic concentration of LD and on a reference enzyme preparation enabling the transfer of that method. The LD1 isoenzyme will be purified from human erythrocytes.

STATUS

A preliminary study has shown that a stable LD1 could be prepared. A batch of about 1500 samples is available for certification. A first intercomparison with 11 laboratories has been performed in 1989 with the following results : between :laboratory CV = 13.9 % and within-laboratory CV = 4.2 % on average. The followed method was that recommended by the French Society for Clinical Biology (SFBC). After several points of the methodology have been assessed (e.g. linearity of the reaction and purity of the reagents), much improvement was recorded. 8 participants will be involved in the value assignment campaign (due in 1992) with the SFBC method. Certification is expected in 1993.



PARTICIPANTS

Coordinator: Hospices Civils de Lyon, F Boehrînger Hanheim GmbH, Penzberg, 0 Centre Hospitalier Universitaire Vaudoïs, Lausanne, CH Centre du Médicament, Nancy, F Fondazione Centro San Romanello del Honte Tabor, Milano, I Hôpital Necker-Enfants Malades, Paris, F National Institute for Biological Standards and Control, Potters Bar, UK Universidad Autónoma de Barcelona, Barcelona, Ε Université Louis Pasteur, Strasbourg, F

266

PROJECT RM 294

ALANINE AMINOTRANSFERASE

PROJECT DEFINITION

Alanine aminotransferase (ALT) is mainly located in the liver cells. This enzyme is normally present in serum but its concentration increases in cases of hepatic injuries. In acute hepatitis, ALT is the first enzyme with increased activity in serum. ALT can also be a useful indicator of the effect of drugs on the liver. With that of aspartate aminotransferase, ALT determination is the most frequent of the enzymatic tests performed in clinical chemistry laboratories. The project consists in preparing a partially purified ALT from pork heart. Stability of the isolated enzyme will be assessed before the certification of the catalytic concentration of ALT can start. The method used for the ALT measurement is the IFCC recommended method.

RESULTS

Following a preliminary study that showed that a stable ALT could be prepared, the certification campaign was completed in 1991, on a new batch of 2 000 samples. 13 laboratories participated and the following value and its uncertainty are proposed for certification: CRM 426 (129 ± 4) U/l. The report describing the preparation and the certification exercise is being finalized for publication.


ECU 120 000

PARTICIPANTS

Coordinator : Centre du Médicament, Nancy, F Boehringer Mannheim GmbH, Penzberg, D Centre Hospitalier Universitaire Vaudois, Lausanne, CH Fondazione Centro San Romanello, Milano, I Hôpital Necker-Enfants Malades, Paris, F Hôpital de la Chaux-de-Fonds, CH Medizinische Hochschule Hannover, D Metaxas Memorial Cancer Hospital, Piraeus, GR National Institute for Biological Standards and Control, Potters Bar, UK Odense University Hospital, DK Sint Radboud Ziekenhuis, Nijmegen, NL Universidad Autónoma de Barcelona, E Université Louis Pasteur, Strasbourg, F University of Thessaloniki, GR

267

PROJECT RM 295

PROSTATIC ACID PHOSPHATASE

PROJECT DEFINITION

Measurement of the enzyme prostatic acid phosphatase (PAP) in serum is an established procedure in monitoring metastatic carcinoma of the prostate and is also useful in confirming suspected early stage disease. The project aims at preparing purified acid phosphatase form human prostate. The project also includes the investigation and subsequent development of an assay method of sufficient reliability and robustness for assigning a value to the PAP concentration in the enzyme material.

RESULTS

The purification of acid phosphatase from human prostatic tissue has been successful. A batch of 3000 samples in lyophilised form was prepared for certification. The method used was the one with 4-nitrophenyl phosphate as substrate and measurements were carried out at 37° C. 9 laboratories were involved and the following value and its uncertainty were proposed for certification: CRM 410 (28.0 ± 0.7) U/l. The report describing the preparation and the certification exercise is being finalized for publication.


ECU 110 000

PARTICIPANTS

Coordinator : Royal Postgraduate Medical School, London, UK Boehringer Mannheim GmbH, Penzberg, D Centre Hospitaller Universitaire Vaudois, Lausanne, CH Fondazione Centro San Romanello, Milano, I Kopital Mecker-Enfants Malades, Pan's, F Metaxas Memorial Cancer Hospital, Piraeus, GR National Institute for Biological Standards and Control, Potters Bar, UK Odense University Hospital, DK Universidad Autónoma de Barcelona, E University of Thessaloniki, GR

268

PROJECT RM 296

ASPARTATE AMINOTRANSFERASE

PROJECT DEFINITION

Aspartate amino transferase (AST) is another enzyme widely used in clinics to assess the severity of liver disorders and myocardial infarction. It is used to detect relapsing hepatic cirrhosis. To produce a candidate reference material for this enzyme the experimental approach will be through genetic engineering and molecular biology techniques. Previous knowledge of the molecular structure and activity of gamma-glutamyltransferase would be a template for the preparation of AST. Subsequent steps will follow the same pattern as for the other enzyme preparations.

STATUS

The first step, the feasibility study on gamma-glutamyltransferase (GGT) used as a model, was completed in 1989. The expression of GGT cDNA in E. Coli and yeast appeared to be possible. Cell culture using the HepG2 hepatoma cell line was successful and could yield a GGT material whose kinetic and immunological properties were shown to be close to those of human serum GGT. The results are presented in report EUR 12842 (1990). The application to AST should follow after completion of the project n° 294 on ALT.



PARTICIPANTS

For the purification work : Centre du Médicament, Nancy, F

269

PROJECT RM 318

PANCREATIC α-AMYLASE

PROJECT DEFINITION

In most European countries, the amylase test is the main enzymatic test in the diagnosis of pancreatic disease. Furthermore, it has been reported that elevated α-amylase in serum also occurs in mumps, renal disease and abdominal disorders such as cholecystitis. Usually total serum amylase activity is measured without discriminating the organ sources. Recently the use of inhibitors or monoclonal antibodies has enabled the pancreatic amylase to be specifically measured, enhancing the diagnostic value of the test. Measurement of amylase in serum is carried out in a majority of the European clinical chemistry laboratories (about 75 % ) . The project aims at producing a preparation of purified α-amylase from human pancreatic tissue. The project will also include the study of assay methods to select that which should be used for assigning the value to the concentration of amylase in the enzyme material.

STATUS

Purified α-amylase was obtained from human pancreas. Two pilot batches (one liquid and one lyophilized) were prepared for an interlaboratory exercise -which gave good agreement- and a stability study, showing that the material is adequately stable. Results of this feasibility study have been published as report EUR 13629 (1991). A final lot is currently being lyophilized and certification is expected in 1992-1993.



PARTICIPANTS

Coordinator : Universidad Autónoma de Barcelona, E

Association Pharmaceutique Belge, Bruxelles, Β Boehrînger Mannheim GmbH, Penzber, D Centre du Médicament, Nancy, F Hôpital de la Chaux-de-Fonds, La Chaux-de-Fonds, CH Hôpital Νecker Enfants-Malades, Paris, F Hospices Civils de Lyon, Lyon, F

Medizinische Universität zu Lübeck, Lübeck, D Metaxas Memorial Cancer Hospital, Piraeus, GR National Institute for Biological Standards and Control, Potters Bar, UK Ospedale San Raffaele, Milano, I Regional Hospital, Corck, IRL Royal Postgraduate Medical School, London, UK Université Louis Pasteur, Strasbourg, F

270

PROJECT RM 319

PANCREATIC UPASE

PROJECT DEFINITION

Lipase determination is at least as useful as amylase ,in the diagnosis of pancreatic disease. Methodology for lipase assay is however currently less developed. Serum lipase is less widely implemented. About 25 % of the European clinical chemistry laboratories perform this analysis probably because of methodological difficulties. The project aims at preparing purified lipase by two routes : a conventional purification procedure from pancreatic juice and employing the techniques of cell and molecular biology. Methodological investigations will also be conducted for assigning a value to the lipase concentration in the enzyme material.

STATUS

Purification work is in progress. By the conventional purification procedure of pancreatic juice, a purified lipase could be obtained. The enzyme appears to be more than 95 % pure and its catalytic activity seems stabilized. In parallel, assay conditions for pancreatic Upase are being established using a continuous pH-stat technique. Work is also in progress using genetic engineering. The human lipase cDNA has been cloned in an eukaryotic expression vector. This recombinant vector was used to transform V79 and CHO cells. Future efforts will focus on the characterization of these cell lines in terms of lipase production. Completion of the project is expected in 1993.



PARTICIPANTS

For the purification work : Centre du Médicament, Nancy, F Université Louis Pasteur, Strasbourg, F University of Thessaloniki,"Aretaieon" University Hospital, Athens, GR

For the certification : as in project n" 318 for α-amylase.

271

PROJECT RM 375

MONOSPECIFIC ANTIBODIES TO HUMAN CREATINE KINASE Β

PROJECT DEFINITION

In clinical medicine, the distribution of creatine kinase (CK) -MB, -MM or -BB isoenzyme activity in the circulation is used as an important and reliable parameter in the diagnosis of (acute) myocardial and brain infarction, acute or chronic inflammatory and non-inflammatory myopathies, brain and/or muscle traumas and, more recently, presence of lung, brain or prostate tumours. Since no uniform method is being applied for the discrimination between CK isoforms and the determination of their respective concentration the techniques of genetic engineering will be used to first produce biochemically pure CK-B. This material will then serve to prepare highly specific immunoprecipitating and immunoinhibiting monoclonal antibodies against CK-B. Thereafter it is planned to use these materials to set up an immunoenzymatic assay.

STATUS

The project has started in 1990 and is expected to be completed within 1992. The progress so far attained concerns: 1) the establishment of a procedure for routine production of 0-galactosidase CK-B fusion protein as CK-B antigenic material in E.Coli host bacteria; 2) the development of two alternative routes for the purification of this antigenic fusion protein, namely via HPLC (yielding protein with CK-B enzymatic activity) or via preparative SDS-acrylamide electrophoresis (yielding SDS-inactivated material). The next steps will determine the procedure for upscaling the production and will evaluate the antigenic potential of the produced material. In parallel, a synthetic antigenic material was produced by conjugation of synthetic CK-B peptide to a Bovine Serum Albumin carrier molecule. This conjugate will be used in immunization experiments to produce highly specific antibodies to CK-B.



PARTICIPANTS

For the purification work : Sint Radboud Ziekenhuis, Nijmegen, NL

272

PROJECT RM 262

GLYCATED HAEMOGLOBINS

PROJECT DEFINITION

In patients who suffer from diabetes, important indicators of the overload of sugar are the fractions of haemoglobin called "glycated haemoglobins". The glycation process may affect other proteins than haemoglobin. The determination of glycated haemoglobins is therefore relevant also to prevent the long-term complications associated with diabetes by helping to control the overall carbohydrate metabolism of the patients. The project comprises a methodological assessment aiming at the selection of techniques capable to provide reliable and reproducible results for the determination of glycated haemoglobin fractions. The project should be concluded by the preparation of a reference material.

RESULTS

Six interlaboratory trials have been carried out to improve the consistency of the results obtained by affinity chromatography and by high performance liquid chromatography (HPLC). A reference preparation has been produced from a blood haemolysate. A value was attributed to the preparation using a HPLC procedure. A fully detailed report is due within 1992.


ECU 30 000

PARTICIPANTS

Bio-Rad Labs. GmbH, München, D Centre Hospitalier Universitaire Cochin, Paris, F Centre de Transfusion Sanguine, Nancy, F Diabetes Forschungsinstitut, Düsseldorf, D Hôpital Universitaire Erasme, Bruxelles, Β Hvidore Hospital, Klampenborg, DK

Medizinische Klinik der Technischen Universität München, D Novo Biolabs Ltd., Cambridge, UK Queen's Medical Centre, Nottingham, UK Royal Sussex County Hospital, Brighton, UK Universita di Milano, I University of Surrey, Guildford, UK

Ziekenhuis de Ueezenlanden, Zwolle, NL

273

PROJECT RM 292

APOLIPOPROTEINS

PROJECT DEFINITION

Cardiovascular diseases still represent the major cause of death and invalidity in our Western society. Clinical and epidemiological studies have established that the prevalence and incidence of these diseases are associated with serum lipoprotein concentrations. In the last years there has been a growing interest for the protein moiety of the lipoproteins called the "apolipoproteins", the determination of which offers a more discriminative diagnosis for coronary heart disease. The aim of the project is to assist in the standardization of apolipoprotein (Apo) assays. The project includes the preparation of purified Apo AI, Apo All and possibly Apo Β to be used as calibrators for the determination of these Apo's in serum. The next step will concern methodological development and might result in the certification of serum reference materials.

RESULTS

The purification of Apo AI and Apo All is completed. The stability of the lyophilized preparations appears to be satisfactory. The certification analysis is performed by aminoacid analysis to assign a mass concentration to each of the purified Apo's. The Apo materials have been certified with the following mass concentrations :

for Apo AI CRM 393 (1.06 ± 0.05) g/1 for Apo All CRM 394 (0.321 ± 0.019) g/1.

The results are presented in EUR report 13393 (1991).


ECU 230 000

PARTiaPANTS

Coordinator : University of Glasgow, UK Algemeen Ziekenhuis Sint Jan, Brugge, Β Behringwerke AG, Marburg, 0 Boehringer Mannheim GmbH, Penzberg, D Diagnostics Pasteur-Kallestad, Steenvoorde, F Institut Pasteur, Lille, F Universita di Milano, I University of Lund, Department of Clinical Chemistry, S

274

PROJECT RM 298

SECOND REFERENCE RABBIT THROMBOPLASTIN

PROJECT DEFINITION

The thromboplastin is a lipoprotein, used in the assay known as the prothrombin time test to induce the formation of the clot in a blood plasma specimen. The test is performed to monitor patients receiving oral anticoagulant therapy. To prevent thrombosis while avoiding bleeding, appropriate dosage of anticoagulant must be ensured. The project aims at renewing the stock of reference rabbit thromboplastin now exhausted, by producing and certifying a new preparation in essentially the same manner as that used for CRM 149.

RESULTS

The project was successfully completed in 1988. A new lot of 10 000 ampoules containing lyophilized thromboplastin from rabbit brain was produced. The stability and homogeneity of the batch were demonstrated. Eleven laboratories took part in the certification exercise whereby the new rabbit thromboplastin was correlated to the International Reference Preparation for thromboplastin (IRP 67/40). The certified parameters establishing the relationship between CRM 149R and IRP 67/40 are: slope : 1.343 ± 0.035 intercept : - 0.382 ± 0.042. Details of the campaign are presented in the report EUR 11686 (1988).


ECU 35 500

PARTICIPANTS

Academisch Ziekenhuis Leiden, NL Centralsygehuset i Esbj'erg, DK Centre Hospitaller Universitaire de Paris, F Hippocration Hospital, Athens, GR Hospital de la Santa Creu i Sant Pau, Barcelona, E Instituto Nacional de Saude, Lisboa, Ρ Katholieke Universiteit Leuven, Β Klinikum der Albert-Ludwigs-Universität, Freiburg, D Ospedale Regionale di Parma, I Thame Thrombosis and Haemostasis Research Foundation, UK Uithington Hospital, Manchester, UK

275

PROJECT RM 306

THYROGLOBULIN

PROJECT DEFINITION

Thyroglobulin is a protein of the thyroid gland which plays the major role in the synthesis of the thyroid hormones. The determination of serum thyroglobulin (Tg) is particularly important in the follow-up of patients who suffered from thyroid cancer. After successful therapy, the monitoring of serum Tg is carried out to assess recurrent episodes of the cancer. Elevated serum Tg levels may be an indication of metastases. Such an information gives an opportunity to treat the disease at an early stage. The project aims at providing clinical chemists with a means of assessing (calibrating) their assay of serum thyroglobulin. The project starts with the preparation of a purified Tg extracted from human thyroid glands. Next steps might include the certification of serum reference materials.

STATUS

Following two pilot studies that concluded to the feasibility of preparing purified and stable thyroglobulin in a reproducible way, a final lot of purified Tg has been produced. The work to certify its mass concentration has started and it should be completed by the end of 1992.



PARTICIPANTS

Coordinator: Frederiksberg Hospital, Copenhagen, DK Academisch Hedisch Centrum, Amsterdam, NL Cattedra di Chimica Fisiológica, Catanzaro, I Centre Hospitalier Régional, Marseille, F Facultad Autónoma de Medicina, Madrid, E Faculté de Medicine Grange Blanche, Lyon, F Henning Berlin GmbH, Berlin, D Hôpital St. Pierre, Bruxelles, Β Institut Gustave Roussy, Villejuif, F Instituto Portugués de Oncología, Lisboa, Ρ Universitäts Poliklinik, Heidelberg, D Université Libre de Bruxelles, Β Université Catholique de Louvain, Unité Hormones et Métabolisme; Bruxelles, Β University of Birmingham, UK University of Athens, GR University of Pisa, Livorno, I

276

PROJECT RM 350

REFERENCE MATERIAL FOR 14 HUMAN PLASMA PROTEINS

PROJECT DEFINITION

There are over fifty proteins in blood circulation which have either a protective function or a metabolic role. The latter includes transport of hormones and nutrients. The protective proteins help the organism to respond to inflammation or trauma and assist in the defense against infection. Quality Assessment surveys in Western Europe countries during the last five years have indicated considerable variation in analyte values between commercial calibrants for plasma proteins, in particular for immunoglobulins (10 - 20% CV between laboratory). Consequently a proposal was put forward to the Commission to prepare a serum material to be used by manufacturers to validate their kits or assay systems for measurements of 14 plasma proteins. Certification will involve calibration against the existing WHO International Reference Preparation for plasma proteins and against pure proteins where available.

STATUS

The collection of serum is completed. An interlaboraty study for assessment of the assay methods was successfully performed as well as a value assignment campaign. The certification programme and the relative report should be completed in 1992.



PARTICIPANTS

Coordinators Hospices Civils de Lyon, F

The University of Leeds, UK

Abbott Diagnostic Products GmbH,

Uiesbaden-Delkenheim, D

Academisch Ziekenhuis der Vrije Universiteit,

Amsterdam, NL

Behringwerke AG, Marburg, D

Boehringer Mannheim GmbH, Penzberg, D

Centre Hospitalier de Luxembourg, L

Cliniques Universitaires St. Luc,Bruxelles, Β


Danderyds Hospital, Danderyd, S

Diabetes Forschungsinstitut, Düsseldorf, D Diagnostics Pasteur-Kallestad, Marnes la Coquette, F Faculdade de Medicina de Coimbra, Ρ General Hospital of Athens, GR

Hoffmann-La Roche & Co, Ltd., Basle, CH

Hôpital Lariboisière, Pan's, F

Hospital de la Santa Cruz y San Pablo, Barcelona, Ε Institut für Klinische Chemie und Haematologie, St. Gallen, CH Klinikum der Philipps-Universität, Marburg, D

Krankenhaus Nordwest, Frankfurt, D Odense University Hospital, DK Ospedale Ν i guarda Ca' Granda. Milano, Ospedale de Stradella, I

Our Lady's Hospital, Crumlin, Dublin,

Royal Hallamshire Hospital, Sheffield,

St. Antonius Hospital, Nieuwegein, NL

Sundby Hospital, Copenhagen, DK

Universiteit Ziekenhuis Antwerpen, Β

University of Birmingham, UK

University Hospital, Lund, S

1RL

UK

277

PROJECT RM 379

FEASIBILITY STUDY OF A PREPARATION OF PURIFIED HUMAN OSTEOCALCIN BY GENETIC ENGINEERING

PROJECT DEFINITION

Osteocalcin (bone-gla protein, BGP), a non-collagenous protein from bone matrix, was suggested to be a reliable non-invasive marker for prevention and diagnosis in many bone diseases such as osteoporosis. Indeed, osteoporosis is one of the most common metabolic bone diseases resulting in bone loss responsible for vertebral or femoral fractures in post-menopausal women or in women and men over 70 years. For example, in France, about 30.000 hip fractures per year were reported in osteoporotic people and about 1.000.000 women were carriers of vertebral crushes. In Sweden, the Netherlands and Great Britain, similar incidences were described. The aim of the project is to employ the techniques of genetic engineering and cell biology to produce purified human osteocalcin. The cDNA coding for osteocalcin will be cloned and appropriate vectors will be tried to express the cDNA in eukaryotic cells. Additionally, the possibility of obtaining osteocalcin route from osteoblast cultures will be investigated.

STATUS

The project has started in 1990. Using polymerase chain reaction and specific oligonucleotides as primers, amplification of the human BGP gene sequences was successfully achieved. The human BGP gene was then cloned in the pBR 322 plasmid and ligated to an eukaryotic expression vector. Gene transfer experiments are in progress. At the completion of the project, a limited amount of purified material should be available for further studies.



PARTiaPANTS

For the purification work : Centre du Medicament, Nancy, F Stabiligen S.A., Nancy, F

278

PROJECT RM 376

CREATININE IN HUMAN SERUM

PROJECT DEFINITION

Creatinine is a conversion product of creatine. Between 1 and 2 % of muscle creatine is converted to creatinine daily. Creatinine is thus related to creatine content of body or muscle mass. Free creatinine appearing in the blood is not reutilized but ultimately excreted into urine. Characteristic for this excretion process is its remarkably constant rate. There exist however clinicopathological situations in which creatininuria is increased, e.g. renal failure, hyperthyroidism and severe muscular disease. In relation to the renal excretion process, serum creatinine is an excellent screening test for adequate renal function. The project will start by intercomparisons between laboratories selected by organizers of External Quality Assessment Schemes (EQAS). Next step should involve methodological developments at both routine and reference levels. The preparation of serum reference materials is envisaged.

STATUS

Laboratories (see below) nominated by national/regional European EQAS organizers so far participated in two intercomparisons. Results showed a considerable scatter between methods. The observed highest and lowest values relative to isotope dilution -mass spectrometry (ID-MS) target values (+28 %; -16 % respectively) questioned if such a routine analytical performance was acceptable as a basis for clinical decision. In order to improve the analytical state of the art values obtained by "reference" methodologies are needed. Refinement of ID-MS and HPLC measurement procedures was considered to be useful. 11 laboratories are now involved in collaborative studies with such methods. The progress achieved is promising and a certification campaign of serum reference materials is foreseen for 1993.



PARTICIPANTS

"Aretaieon" University Hospital, Athens, GR "Evangel ismos" Hospital, Athens, GR Addenbrookes Hospital, Cambridge, UK Clínica San Camilo, Madrid, E East Birmingham Hospital, UK Faculteit Farmaceutische Wetenschappen, Gent, Β Hôpital Herriot, Lyon, F Hôpital Necker-Enfants Malades, Paris, F Hospital Comarcal de Bidasoa, Guipúzcoa, Ε Hospital General Vail d'Hebron, Barcelona, Ε

Hospital de Santa Maria, Lisboa, Ρ

Hospital de Terrassa, Barcelona, Ε

Insitut für Klinische Biochemie, Bonn, 0 Instand, Düsseldorf, D Instituto Nacional de Saude, Lisboa, Ρ

Istituto Scientifico San Raffaele, Milano, I

Laboratoire National de la Santé, Luxembourg, L Laboratorium voor Medische Biochemie, Wilrijk, Β Medizinisch-Chemisches Laboratorium, Zürich, CH Medizinische Hochschule Hannover, D Meilakti Hospital, Helsinki, SF Ospedale Niguarda Ca' Granda, Milano, I Our Lady's Hospital for Sick Children, Dublin, IRL Rigshospitalet Copenhagen, DK Sint Radboud Ziekenhuis, Nijmegen, NL St. James Hospital, Dublin, IRL University Hospital, Uppsala, S

279

PROJECT RM 386

6 p-HYDROXYCORTISOL IN HUMAN URINE

PROJECT DEFINITION

Some drugs, administered to humans, have the capacity to induce the production of enzymes in much larger amounts than normally. The enzyme induction capacity is determined in pharmacological studies since it can represent either a benefit or a potential danger for the tested drug. In humans, induction processes can be explored using different exogenous or endogenous substances. These last compounds such as plasma gamma glutamyltransferase, urinary glucaric acid or urinary 6 ß-hydroxycortisol are particularly interesting. 6 /S-hydroxycortisol is a polar, unconjugated metabolite of Cortisol which is dependent on the cytochrome P-450IILA3 activity. Its urinary excretion is considered as a good test to evaluate inductive effects of drugs in humans and has been demonstrated to be clearly increased in subjects treated by inducers such as phénobarbital or rifampicin. The project consists of an interlaboratory study of urinary 6 /3-hydroxycortisol determination, using an immunoenzymatic technique (ELISA) more rapid and more sensitive than other existing methods. High performance liquid chromatography (HPLC) will be used as a "reference method". It is probable that a reference material adapted to the immunoenzymatic method will be considered in the future.

STATUS

The project started in July 1990. The results of a first intercomparison of measurements of urinary 6 /3-hydroxycortisol yielded a satisfactory analytical variation (4-12% day to day coefficient of variation) for ELISA method. However significant differences were observed between the results obtained by ELISA and HPLC respectively. Additional work for method comparison was recommended.



PARTICIPANTS

Coordinator : Centre du Médicament, Nancy, F "De Wever" Hospital, Heerlen, NL Biochemistry Department, Trinity College, Dublin, IRL Centre Hospitalier Universitaire Jean Minjoz, Besançon, F Centre Hospitalier Universitaire Necker, Paris, F Clinical Chemistry and Hematology, Kantonsspital, St.Gallen, CH Department of Biochemistry, University of Birmingham, Birmingham, UK Department of Pharmacology, Copenhagen, DK Department of Biochemistry, Faculty of Medical Sciences, Lisbonne, Ρ Department of Pharmacology, Facultad de Medicina, Badajoz, Ε Facultad de Medicina, Departamento de Bioquímica, Sevilla, Ε Hoechst A.G., Allgemeine Pharma Forschung, Frankfurt, D Laboratoire d'Analyses Médicales, Luxembourg, L Laboratoire de Chimie Médicale, Institut de Pathologie, Liège, Β Laboratorio di Biochimica clínica, Ospedale Niguarda ca'Granda, Milano, l

280

PROJECT RM 391

CHOLESTEROL IN HUMAN SERUM

PROJECT DEFINITION

Cholesterol is an important component of cellular membraneous structures. Its sterol nucleus is the precursor of steroid hormones and the bile acid(s). Only about 1/4 of the total cholesterol body burden is due to alimentation, the larger quantity - the so-called endogenous cholesterol - is synthetised by the organism. Approximately 70 % of the plasma cholesterol is in the form of cholesterol esters. Under pathological situations lipid deposits (atheromatous plaques) appear in large arteries. This leads to degeneration, progressive sclerosis and the formation of calcified plaques. The arteries become extremely hard (arteriosclerosis) and they are easily ruptured. The atheromatous plaques provocating obstacles to the blood flow initiate thrombus or embolus formation. Almost half of human beings die of the consequences of arteriosclerosis. Therefore cholesterol became one of the most frequently analyzed plasma parameters. The project will start by intercomparisons between laboratories (see below) nominated by national/regional European organizers of External Quality Assessment Schemes (EQAS). Next step should focus on methodological improvement at both routine and reference levels. The project could lead to the preparation of certified serum reference materials.

STATUS

The intercomparison exercise particular feature of which was the circulation of both fresh and lyophilized serum samples is completed. Differences amounting to 22% have been observed between results provided by "routine" methods.lt was also noted that even non-routine methods (e.g. ID-MS and HPLC) gave some discrepant results which was taken as an incentive to undertake methodological improvement. Additional intercomparison exercises are now in progress.



PARTICIPANTS

Amtssygehuset, Koge, DK

C.A.P. Dr. Robert, Badalona, E Holbaek Hospital, DK Hôpital du Bocace, Dijon, F Hôpital de la Croix-Rousse, Lyon, F Hospital Consorcio de Terrasa, Barcelona, E Instand, Düsseldorf, D Institut für Klinische Chemie und Haematologie, St. Gallen, CH Institut für Klinische Biochemie, Bonn, Instituto Nacional de Saude, Lisboa, Ρ Istituto di Farmacología, Milano, I Lab. ν. Hedische Biochemie en Radiofarmacie, Wilrijk, Β

Laboratoire d'Analyses Médicales, Luxembourg, L Laboratorio de Química Clínica, Hospital de Santa Cruz, Carnaxide, Ρ

Laboratorio de Análisis Clínicos S.L., Tarragona, Ε Labquality, Helsinki, SF

Ospedale di Rho, Milano, I

Queen Elizabeth Hospital, Birmingham, UK

Regional Hospital, Cork, IRL

Regional Hospital Lund, S

Rijksuniversiteit Gent, Β

Royal Infirmary, Glasgow, UK

Spedali Civil i di Brescia, I

St. Radboudziekenhuis, Nijmegen, NL

St. Mary's Hospital, London, UK

Trinity College, Dublin 2, IRL

Universidad de Barcelona, Dept. Bioquímica, Barcelona, E University Hospital Dijkzicht, Rotterdam, NL

281

PROJECT RM 314

COLLABORATIVE STUDY ON HEPATITIS Β VACCINES

PROJECT DEFINITION

Hepatitis Β vaccines prepared by purification of 22 run Hepatitis Β surface antigen (HB,Ag) particles from the plasma of chronically infected individuals or by recombinant DNA (rDNA) technology are in use throughout Europe. A collaborative study was undertaken primarily as a support to DG III in relation to their work for the harmonization of procedures for testing new vaccines produced by rDNA technology. It was not intended to develop the study into a project. The aim was to examine the suitability of a plasma derived Hepatitis Β vaccine as immunogenicity reference for material derived by rDNA methods in yeast and mammalian cells.

RESULTS

Seven European laboratories participated in the collaborative study which was terminated in 1989. The vaccines examined were the WHO International Reference Reagent (IRR) with plasma derived HB/ig, two vaccines containing HBAg produced by rDNA in yeast and a vaccine with HB̂ Ag prepared in mammalian cells. The potencies of the tested vaccines were to be reported relative to the IRR. Estimates of potency by the 7 participating laboratories varied by a factor of 10 generally. The variation in the dilution of vaccine required to induce antibodies in 50% of test animals varied by a factor of 25 between the laboratories. The IRR was deemed suitable as immunogenicity reference for all tested. HB,Ag vaccines. The results are presented in report EUR 12857 (1990).


ECU 1 100

PARTICIPANTS

Coordinator : National Institute for Biological Standards and Control, Potters Bar, UK

Instituto de Salud Carlos III, Madrid, Ε Instituut voor Hygiene & Epidemiologie, Brussel, Β Istituto Superiore di Sanità, Roma, I Laboratoire National de la Santé, Paris, F Paul Ehrlich Institut, Frankfurt, D Rijksinstituut voor Volksgezondheid t, Milieuhygiene, Bilthoven, NL

282

PROJECT RM 352

ANTINEUTROPHIL CYTOPLASMIC ANTIBODIES (ANCA)

PROJECT DEFINITION

In the case of autoimmune diseases the organism raises antibodies against its own cells. In 1985 it was reported that anti-Neutrophil Cytoplasmic Antibodies (ANCA) -directed against components of the cytoplasm of the neutrophils- were present in the serum of patients with Wegener's granulomatosis (inflammatory vascular disease of the upper airways and lungs, also affecting the kidneys). ANCA are now commonly measured to diagnose this disease. The project consists of a collaborative study with the aim of developing a set of assays for the detection of ANCA. The methods will be assessed in order to determine their ability to detect and quantify ANCA in a spectrum of diseases that are characterised by the inflammatory state of the blood vessels, the kidneys or the joints. This will be achieved through an interlaboratory trial to test the selected assays (in a large number of laboratories) on an elevated number of patient sera.

STATUS

The project has started in 1990 and is expected to be completed before the end of 1994. Currently performed assays were compared on a limited number of patient serum samples. At present the selection of a set of solid phase assays is performed in parallel with the characterization of the antigens.



PARTICIPANTS

Coordinator : Academisch Ziekenhuis, Leiden, NL Academisch Ziekenhuis Groningen, Groningen, NL Gentofte Hospital, Hellerup, 0K Hôpital Necker, Paris, F Hospital Clinic i Provincial, Barcelona, E National Bacteriological Laboratory, Stockholm, S Rheumaklinik Bad Bramstedt, D Royal Postgraduate Medical School, London, UK San Carlo Borromeo General Hospital, Milano, I Statens Seruminstitut, OK University of Ioannina Medical School, loannina, GR University Hospital, Heidelberg, D University of Cambridge, UK Utech & Lüdeman GbR, Raisdorf, D Vrije Universiteit Brussel, Brussel, Β

283

PROJECT RM 416

BLOOD GROUPING REAGENTS

PROJECT DEFINITION

The safety of blood transfusion in the European Community relies in part on the quality of the reagents used for ABO and Rh(D) typing and compatibility testing. Mistyping of donors or patients caused by defective substandard reagents can lead to clinically significant transfusion reactions, and in some cases, fatality. There are no European reference materials available for the control of the quality of the reagents in use. The aim of this project is to prepare, with the collaboration of representatives from blood transfusion laboratories and reagent manufacturers operating within Europe, anti-A, anti-B and anti-D certified reference materials. The certification will be conducted according to agreed specifications and will include the evaluation, validation and stability study of the proposed materials. Similar work may then be envisaged for three additional standards (anti-IgG, papain and control weak anti-D and red cell panels for anti-D evaluation).

STATUS

Candidate pilot freeze-dried materials for anti-Α, anti-B and anti-D are being tested and compared to existing FDA and WHO standards by the participants. The results are expected to be reported by mid 1992. Certification to be completed in 1993.



PARTICIPANTS

Coordinator: International Blood Group Reference laboratory, Bristol, UK

Aalborg Sygehus, Aalborg, DK Baxter/Dade, Düdingen, CH Biotest Diagnostics, Dreieich, D Blood Transfusion Service Board, Dublin, IRL Central Laboratory of the Netherlands, Amsterdam, NL Croix Rouge de Belgique, Liège, Β Diagnostics Transfusion, Les Ulis, F East Anglia Blood Transfusion Centre, Cambridge, UK Finnish Red Cross Blood Transfusion, Helsinki, SF Greek National Blood Transfusion Centre, Athens, CR Institut Cátala de la Salut, Barcelona, Ε Institut für Transfusionmedizin, Aachen, D Institut National de Transfusion Sanguine, Paris, F Instituto National de Sangue, Porto, Ρ National Institute for Biological Standards and Control, Potters Bar, UK Organon Teknica, Turnhout, Β Ortho Diagnostic Systems, Antwerp, Β Primo Centro Transfusioni, Milano, I Red Cross Blood Transfusion Service, L Scottish National Blood Transfusion Service, Edinburgh, UK University Hospital Blood Bank, Lund, S Zentral laboratorium Blutspendedienst, Bern, CH

Metals and Industrial Products

287

PROJECT RM 189

OXYGEN IN SEMICONDUCTOR SILICON

PROJECT DEFINITION

The oxygen content of silicon is an important parameter for the manufacturing of integrated circuits and other electronic devices. The measurements are based on infrared absorption spectrometry. Results of infrared absorption measurement often differ by several percent between different laboratories. Industry has therefore requested the BCR programme to produce silicon reference materials (zero specimens needed in the measurements as well as samples to check infrared spectrometers).

RESULTS

Intercomparisons have been organized to improve the measurements of the actual oxygen content and of the infrared absorption. Two reference materials have been certified. CRM 368: silicon with very low 0 content, to be used as "zero"

specimens: 69 + / - 19 ng/g Certification report: EUR 12927 (1990)

CRM 369: silicon with 0 contents in the range of industrial interest, for testing the accuracy (photometry + software) or the IR Instruments: absorption coefficients in the range 2.2 - 3.8 cm' oxygen contents in the range 8 - 1 3 ¿¿g/g Certification report : EUR 12928 (1991)


ECU 240 000

PARTICIPANTS

Atomic Energy Research Establishment, Harwell, UK Bundesanstalt für Materialforschung und -prüfung, Berlin, D Centre d'Etudes et de Recherches par Irradiation, Orléans, F Dynamit Nobel Silicon, Novara, l Ecole Normale Supérieure, Paris, F Instituut voor Nucleaire Wetenschappen (RUG), Gent, Β Interdisciplinary Research Centre Semiconductor Materials, London, UK J.J. Thomson Physical Laboratory, Reading, UK Joint Research Centre, Central Bureau for Nuclear Measurements, Geel, Β J.U. Goethe Universität, Institut für Kernphysik, Frankfurt, 0 Laboratorium voor Kristallografie en Studie van de Vaste Stof (RUG), Gent, Β Max-Planck-Institut für MetalIforscnung, Dortmund, D Philips Components, Southampton, UK Royal Signals and Radar Establishment, Great Malvern, UK Siemens AG, München, D Telefunken Electronic, Heilbronn, D Wacker-Chemitronic, Burghausen, D

288

PROJECT RM 210

IMPURITIES IN COPPER

PROJECT DEFINITION

The purity of electrolytically refined copper (e.g. for use in electric cables) must comply with internationally agreed norms which require the determination of 19 elements: Ag, As, Bi, Cd, Co, Cr, Fe, Mn, Ni, O, Ρ, Pb, S, Sb, Se, Si, Sn, Te and Zn. Most of these are routinely determined by optical emission spectrometry, but the results of various laboratories do not always agree well. Considering the economic importance, industry has requested the BCR to certify reference materials.

RESULTS

Two reference materials have been certified for 15 elements: CRM 074: electrolytically refined copper CRM 075: copper with added impurities (levels close to specified maxima) A separate reference material (CRM 017) was certified for S and Ρ (10 resp. 7 mg/kg). Certification reports: EUR 12318 (1989) (CRM 017)

EUR 14055 (1992) (CRMs 074 and 075)


ECU 121 000

PARTICIPANTS

BICC Environmental Services, Prescot, UK

Bundesanstalt für Materialforschung und -prüfung, Berlin, D Central Bureau for Nuclear Measurements, Geel, Β Centre d'Etudes Nucléaires, Fontenay-aux-Roses, F Energieonderzoekcentrum Nederland, Petten, NL GSF Forschungszentrum für Umwelt und Gesundheit, Neuherberg, D Hüttenwerke Kayser, Lünen, D IMI Refiners, Walsall, UK Instituut voor Nucleaire Wetenschappen (RUG), Β Isotopcentralen, Copenhagen, DK

Kernforschungsanlage Jülich, D Prof. Kraft, Kronberg, D Hax-Planck-Institut für HetalIforschung, Dortmund, D Metallurgie Hoboken-Overpelt, Hoboken, Β Metallurgie Hoboken-Overpelt, Ölen, Β Norddeutsche Affinerie, Hamburg, D

Philips Natuurkundig Laboratorium, Eindhoven, NL

Risoe National Laboratory, Roskilde, OK

Universität Regensburg, D VG Elemental, Winsford, UK

289

PROJECT RM 221

ANALYSIS OF COAL

PROJECT ΡΕΠΝΓΠΟΝ

The upsurge of interest in trace elements in coal has accompanied the increase of use of coal over the last 10-15 years. Trace elements should be taken into account during coal mining, preparation, storage and in application (coking, power production or liquefaction). For example, the quality of steel produced with cokes could be impaired by too high contents of As and P. The current concern on environmental consequences of the usage of coal has increased the need for information on the fate of trace elements especially during combustion in power plants. Elements of mainly environmental interest (fly ash, ashes, slag,...) are As, Cd, Cr, Pb, Hg, Ni, Se. Coal combustion yields gaseous components (e.g. S02, NO„ HCl, HF...) which, upon emission, undergo chemical reactions to finally form acid deposition. The elements S, N, CI are also important from the point of view of corrosion of e.g. furnaces, boilers. Aspects like calorific value and the contents of carbon and hydrogen are frequently determined because they are of prime importance to the user as energy carriers; therefore these values dictate the price of coal in a positive manner. The contents of ash, sulphur, etc. have a negative effect on the market price of coal. The project involves certification of important parameters in coals. The coals chosen are typical for the main sectors of usage of coal: coking for e.g. the steel industry, combustion in the power industry and liquefaction.

RESULTS

The contents of C, H, N, CI, As, Cd, Mn, Hg, Pb, Se, V and Zn have been certified in three coals: Gas Coal (CRM 180), Coking Coal (CRM 181) and Steam Coal (CRM 182) as well as their ash content and their gross calorific value. The certification of the sulphur contents of six coals, together providing a range of appr. 0.3 to 5 % by mass, was terminated in 1990 (EUR 12646 EN, 1990).


ECU 375 000

PARTICIPANTS

In the certification exercises concluded in 1987, 30 laboratories from 8 Member States participated. Participants in the certification of sulphur:

British Coal, London, UK - British Gas, London, UK - Centre d'Etudes & Recherche Charb., Verneuil, F - CISE SPA, Segrate, I - ENA, Madrid, E - Energiecentrum, Petten, NL - Ente Hai. En. Elet., Pisa, -- Hoogovens Groep Β.V., Ijmuiden, NI - URS, Dublin, IRL - KEMA, Arnhem, NL · Min. Affaires économiques, Brussels, Β -Ruhrkohle AG, Essen, D - TNO Maatschappij, Zeist, NL

290

PROJECT RM 231

LOW OXYGEN IN COPPER

PROJECT DEFINITION

The determination of the low levels of oxygen in OFMC Copper poses particular problems for industry. In 1978, the BCR has certified a reference material (CRM 054) with approx. 1 μ{*^ oxygen in copper. This material has become exhausted in 1986 which shows that this CRM still responds to a need of industry. The BCR has therefore undertaken the certification of a replacement material.

RESULTS

The certification of the replacement material (CRM 054R) was certified as (0.47 +/-0.04) Mg/g. Certification report : EUR 12240 (1989)


ECU 14 000

PARTICIPANTS

Bundesanstalt für Materialforschung und -prüfung, Berlin, D Central Bureau for Nuclear Measurements, Geel, Β Centre d'Etudes et de Recherches par Irradiation, Orléans, F Instituut voor Nucleaire Wetenschappen (RUG), Gent, Β J.W. Goethe Universität, Institut für Kernphysik, Frankfurt, D Kabel- und Metallwerke Gutehoffnungshüte, Osnabrück, D Max-Planck-Institut, Dortmund, D

291

PROJECT RM 232

IMPURITIES IN ZINC AND ZINC ALLOYS

PROJECT DEFINITION

The composition of zinc and its alloys is routinely determined by optical emission spectrometry. All types of emission spectrometer require series of calibrants covering a range of concentrations. The European zinc industry has used standards supplied by a French organisation for several decades. When these standards became exhausted, the BCR has accepted to produce and certify new series of reference materials for unalloyed zinc and for the zinc alloys ZnAl4 and ZnAl4 Cul.

RESULTS

17 reference materials in the form of disks have been certified:

7 grades of unalloyed zinc (CRM 321 to 327; varying impurity levels) 5 grades of ZnAl4 (CRM 351 to 355; varying impurity levels) 6 grades of ZnAWCul (CRM 356 to 361; varying impurity levels) Certified elements: Al, Cd, Cu, Fe, In, Mg (alloys only), Ni (alloys only),

Pb, Sn and Tl. Certification reports: EUR 12817 (1990) (unalloyed zinc) and EUR 12818

(1990) (zinc alloys)


ECU 470 000

PARTICIPANTS

BudeIco, Budel-Dorplein, NL Bundesanstalt für Materialforschung und -prüfung, Berlin, D Energieonderzoek Centrum Nederland, Petten, NL Ever Ready Ltd, Stanley, UK Fonderie de Voreppe (Péchiney), Foreppe, F Joint Research Centre, Central Bureau for Nuclear Measurements, Geel, Β Prof. Kraft, Kronberg, D

Laboratoire National d'Essais, Paris, F

Metaleurop, Noyelles-Godault, F

Metateurop Weser Blei, Nordenham, 0

Metaleurop Harz-Metall, Goslar, D

Philips, Eindhoven, NL

Ruhr-Zink, Datteln, D

Vieilie Montagne, Balen, Β

VieiΙ le Montagne, Overpelt, Β

Vieille Montagne France, Auby-lez-Douai, F

292

PROJECT RM 234

GROSS CALORIFIC VALUE OF NATURAL GAS

PROJECT DEFINITION

Large quantities of natural gas are imported by and traded between the Member States of the Community. The price of the natural gas is related to the energy content. The discrepancies between laboratories can be as large as +/- 0.5 %. Real disputes are not frequent because the contracts specify how differences between their measurements will be handled, but the sum dealt with in such settlements is estimated at several 107 ECU per year, hence the need for improving the accuracy of the measurements. An intercomparison was held to assess if improvement of the measurements could be achieved.

RESULTS

The GCV (Gross Calorific Value) of 2 batches of natural gas was determined by 14 European laboratories using two methods:

direct calorimetry; determination of the gas composition by chromatography and calculation of the GCV.

For calorimetry the spread of results was within + / - 0.15 % (coefficient of variation). The laboratories using the most accurate methodologies agreed within + / - 0.09 %. For gas chromatography, the spread of results Was + / - 0.15 %, for the most accurate results + / - 0.03 %.The difference between the mean results of calorimetry and the mean value derived from gas chromatography was 0.01 - 0.02 %. Final report in print.


ECU 10 000

PARTICIPANTS

British Gas, London, UK Bundesanstalt für Materialforschung und -prüfung, Berlin, D Dantest, Koebenhavn, DK Distrigas, Brussels, Β ENAGAS, Zaragoza, Ε

Gas and Oil Measuring Branch, Dept. of Energy, Uigston, UK

Gaz de France - CERSTA, La Plaine St-Denis, F

Irish Gas Board, Cork, IRL

Nederlandse Gasunie, Groningen, NL

Physikalisch-Technische Bundesanstalt, Braunschweig, D

Ruhrgas AG, Essen, D

SNAH, San Donato, Milano, I

Thyssengas GmbH, Duisburg, 0

VEG Gasinstituut, Apeldoorn, NL

293

PROJECT RM 261

TITANIUM AND TITANIUM ALLOYS

PROJECT DEFINITION

Titanium and its alloys (mainly TÍA16V4) are increasingly used in, respectively, chemical industry and aerospace applications. The industrial analytical laboratories often use techniques like emission spectrometry (for unalloyed Ti) or X-ray fluorescence (for alloys). These techniques require standards, but the preparation of homogeneous standards is difficult. The BCR has therefore undertaken the production of reference materials (in the form of disks) through powder metallurgy.

RESULTS

Two reference materials have been certified: CRM 89: Ti alloy with 6% Al and 4% V CRM 90: unalloyed Ti with 300-750 mg/kg of AI, Co, Cr, Cu, Fe, Mn, Mo, Nb, Ni, Si, Sn, V, W and Zr and approx. 10 mg/kg Β. Certification report: EUR 14056 (1992).

PARTICIPANTS

Aciéries d'Imphy, Imphy, F Aérospatiale, Suresnes, F Bundesanstalt für Materialforschung und -prüfung, Berlin, 0

Central Bureau for Nuclear Measurements (CEC Joint Research Centre), Geel, Β Compagnie européenne du Zirconium CEZUS, Usine de Venthon, Albertville, F Etablissement Technique Central de l'Armement, Centre de Recherches et d'Etudes d'Arcueil, Arcueil,F GSF, Forschungszentrum für Umwelt und Gesundheit, Neuherberg, D Instituut voor Nucleaire Wetenschappen (RUG), Gent, Β Krupp Industrietechnik, Sparte Systemtechnik, Essen, D

Laboratoire National d'Essais, Paris, F

Mannesmann Forschungsinstitut, Duisburg, D

Metallwerk Plansee GmbH, Reutte/Tirol, A

Risoe National Laboratory, Roskilde, DK

Wehrwissenschaftliches Institut für Materialuntersuchungen, Erding, D

294

PROJECT RM 327

COAL BOTTOM ASH

PROJECT DEFINITION

One of the major characteristics determining the quality of coal is the composition of the ash which remains in the furnace after the combustion ("bottom ash"). The contents of the major elements must be known to allow the proper setting of the combustion process parameters. The contents of trace elements such as As, Pb and Zn must be known to evaluate the environmental risks associated with the disposal of the ash (e.g. contamination of surface or ground water). At the request of industry, the Commission has undertaken the certification of a coal bottom ash reference material for Al, As, Ca, Fe, Κ, Mg, Na, Ρ, Pb, S, Si, Ti an Zn.

STATUS

In progress


ECU 118 000

PARTICIPANTS

British Coal Corp., Burton-on-Trent, UK

CERCHAR, Verneuil-en-Halatte, F

C.N.R.S., Vernaison, F

Donato Mi láñese, I E.C.N., Petten, NL Empr. Nac. de Electricidad, Madrid, E Endstaedvaerket ELSAM, Vodskov, DK Eniricerche, San Ente Naz. per l'Energia Elettr., Pisa, I E.S.B. Powerstation, Clare, E Ets. Gordinne S Cie, Rozenburg, NL EOLAS, Glasnevin, E Hoogovens Umuiden, NL I.R.S.I.D., Maizières-les-Metz, F 1st. de Carboquimica, Zaragoza, E Laborelec, Linkebeek, Β Ministère des Affaires économiques, Bruxelles, Β N.V. KEMA SBA, Arnhem, NL

Rijksuniversiteit Gent, Β

Ruhrkole, Herne, D

Stazione Milanese per I Conbust., San Donato Milanese, I

Stichting Steenkolbank, Eygelshoven, NL

295

PROJECT RM 337

ALKALI LEACHING FROM PHARMACEUTICAL GLASS CONTAINERS

PROJECT DEFINITION

Glass containers for injectable solutions must comply with specifications of the European Pharmacopoeia (also ISO 4802) which limit the release of alkaline constituents into pure water when applying a specific test. The test method consists of:

applying a specified temperature cycle to containers, partially filled with pure water (in equilibrium with the atmosphere), in an autoclave subsequent determination of total alkalinity (titration) of the water or of specified elements (Na and possibly others).

The test method imposed by the European Pharmacopoeia is not ideal. The test is very sensitive to minor differences in the temperature cycle applied. It appears in fact that most cases of observed high leaching are caused by measurement errors and not by poor quality of the glass. Potential sources of error have been identified and largely eliminated in preliminary intercomparisons. A reference material will be certified to enable laboratories to check if the method is applied correctly.

STATUS

In progress


125 000 ECU (estimated)

PARTICIPANTS

Institut National du Verre, Charleroi, Β Upjohn, Puurs, Β BSN Entoilage, Givon, F Bünder Glas, Bünde, D Forschungsgemeinschaft für technisches Glas, Wertheim, D Glaskontor, Hüllheim, D Schott Glaswerke, Mainz, D Schott Ruhrglas, Mitterteich, 0 Kimble Italiana, Pisa, 1 Stazione Sperimentale del Vetro, Venezia, I Vetreria Parmense Bormioli Rocco, Parma, I Glasforskningsinstitutet, Växjö, S British Glass, Sheffield, UK

296

PROJECT RM 363

DEVELOPMENT OF NEAR INFRARED METHODOLOGY FOR THE DETERMINATION OF THE COMPOSITION OF FIBRE BLENDS

PROJECT DEFINITION

The current analytical methods of PES/cotton and wool/acrylic blends, described in the ISO standard 1833 and the directive 71/307/CEE are based on the selective chemical degradation of one of the components, after which the residue is weighed and the blend ratio evaluated from the loss of mass. If performed properly, the technique can be accurate ( ± 1 % ) . In many cases, products (such as fats, waxes, etc) are added to the blend for fabrication purposes and make the détermination more difficult. By comparison NIRA, in which the material absorption pattern is measured as a function of wavelength in the 1400 to 2400 nm range, offers a method with many advantages. The project will consist in analysing samples from different origins and from different production stages. They will be tested by NIR and by the classical method. The NIR will be evaluated from these results.

RESULTS

The study has revealed that NIRA can be applied as a fast (within one minute) and moderately accurate (SEP = ± 1.5%) analysis method for the determination of binary fibre blends. The technique is especially useful in applications where a high number of analyses needs to be performed such as in production control and first screening analysis of trade samples. However, the study also indicates that the accuracy of the technique and the coefficients used in the equations need to be controlled regularly by the use of reference samples or by performing chemical analysis.


ECU 42 800

PARTICIPANTS

Centexbel, Β

297

PROJECT RM 415

REPLACEMENT OF COKE CRMs

PROJECT DEFINITION

The BCR reference materials CRM 001-004, metallurgical cokes (certified for ash content, gross calorific value (GCV), and contents of several elements) are nearly exhausted, which indicates that they continue to respond to a need of industry. Therefore 4 new materials will be prepared and certified, covering the following ranges: 5 to 8 % ash content; 0.5 to 1 % sulphur content; 0.2 to 0.8 % hydrogen content. The certified parameters will include ash content, GCV, and the contents of carbon, hydrogen and sulphur.

STATUS

Preparation and homogeneity/stability testing in progress.



PARTICIPANTS

Preparation: British Coal Research Establishment, Chetltenham, UK. Certification: approx. 10 laboratories from various Member states (to be identified in 1992).

Surface Analysis

301

PROJECT RM 193

ENERGY AND INTENSITY CALIBRATIONS FOR XPS AND AES

PROJECT DEFINITION

The aims of the projects were to provide traceable energy and intensity scales for X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES).

RESULTS

i) Energy scales For both XPS and AES energy scales traceable to the UK national voltage standard have been realised by the accurate measurement of the positions of strong characteristic peaks of gold, silver and copper. When applied via intercomparison, the XPS scale demonstrated that on commercial machines the principle sources of errors were in the setting of the zero and the establishment of scaling factors. The corresponding scale for AES reduced the scatter seen in an ASTM intercomparison by more than a factor of 5 for all instruments surveyed and a factor of 17 for high resolution instruments.

ii) Energy-intensity response functions The response function of an electron spectrometer to a given flux of electrons depends upon their energy and the details of the spectrometers construction. To enable individual XPS spectrometer's relative energy-intensity response functions to be determined a well defined procedure again based on the characteristic peaks of Au, Ag and Cu was derived. Using this procedure it was demonstrated in an intercomparison that results from different instruments could, for the first time, be compared to within one standard deviation of 4%. For the AES case a fully instrumented electron spectrometer capable of determining absolute spectral intensities was developed. The intensity scale derived with this instrument enabled 38 laboratories using a wide range of equipments to reproduce quantitative analyses for Au, Ag and Cu to within 3% over the energy range 10 to 2500 ev and 2% over the range 100 to 1000 ev when using the direct mode. However when working in the differential mode the agreement degraded to worse than 10% (see Project 287).


ECU 186 000

PARTICIPANTS

Wore than 40 laboratories in the Member States plus an equal number in Japan, USA and Canada via the VAHAS initiative with coordination by NPL.

302

PROJECT RM 287

AUGER ELECTRON SPECTROSCOPY INTENSITY CALIBRANT

PROJECT DEFINITION

The AES work undertaken in Project 193 allows analysts working in the direct mode to agree on absolute peak intensities to within ± 3%. However, for the differential mode this agreement degrades to worse than ± 10 % even when operating under reference conditions. Since many instruments are only capable of working in the differential mode, it is necessary to improve the traceability of the intensity scale in this mode and to establish procedures which relate the scale established under reference conditions to those under other operating conditions. This the project is attempting to do via the production of a reference material which will allow traceability to an absolute AES intensity scale which is comprised of peaks throughout the spectrum which correspond to known intensities irrespective of the operating conditions.

RESULTS

The development of a fully instrumented electron spectrometer to measure absolute spectral intensities for AES and XPS significantly changed the approach taken in this project. Instead of considering the relative energy-intensity response functions of the spectrometer under different operating conditions it was possible to consider the problem in terms of absolute intensities.

The reference material consists of a copper substrate containing a gold insert. Using this material 5 laboratories demonstrated with a range of cylindrical mirror analyzers and concentric hemispherical spectrometers that it is possible to produce absolute peak intensity calibrations in the AES differential mode to within +. 4.4 % . This should be compared to the 10 % achieved earlier for relative intensity calibrations and should facilitate accurate comparisons between data from different instruments.



PARTICIPANTS

National Physical laboratory, UK (Coordinator) University of Kaiserslaten, D University of Nodena, I University of Loughborough, UK BNR Ltd, UK

303

PROJECT RM 288

THE ANALYSIS OF MONOLAYER SEGREGANTS IN STEELS

PROJECT DEFINITION

The presence of impurities at grain boundaries in steels can cause intergranular brittle failure in stress corrosion, impact and creep situations. Identification and quantification of these segregants is often carried out using Auger electron spectroscopy. However, the lack of reproducibility of AES instruments in the quantitative mode frequently makes it difficult to relate measurements in different laboratories. A reference material with known and reproducible segregants for the major impurities encountered in practice (P, Sn, Sb and S) has therefore been produced.

RESULTS

Difficulties in the fabrication of the low alloy steel restricted the segregant elements to Ρ and Sn. When heat treated at 200 °C for 2 hours, water quenched and further heat treated for 48 hours at 580 °C a reproducible segregation of the impurity elements was achieved. The samples were then broken under high vacuum and analyzed using AES.

After calibration of the spectrometer energy and intensity scales using the procedures developed under project RM 193, the laboratories participating in the intercomparison agreed to within +. 15 % on concentrations of the segregated Ρ and Sn equivalent to approximately 30 % of a monolayer. This represents an improvement of over an order of magnitude.

The calibration of the material is based upon the intercomparison and literature values for the Auger electron yields. Absolute certification of the material is therefore not possible but it is made available to AES users for the validation of their instrumental factors and procedures.


ECU 50 000

PARTICIPANTS

National Physical Laboratory, UK (Coordinator) Max PLanck Institute, Dusseldorf, 0 University of Bristol, UK Berkeley Nuclear laboratories, UK AEA Technology, Harwell, UK British Steel, UK

304

PROJECT RM 290

SILICON DIOXIDE REFERENCE MATERIAL FOR XPS

PROJECT DEFINITION

Project 193 was concerned with the development for XPS of a traceable energy scale and a procedure for the determination of spectrometer energy-intensity response functions relative to that of a spectrometer of a specific design. Having achieved these it is now possible to compare results from different instruments provided that they are operated under standard conditions. To enable true quantification to be achieved and for comparison of results made under practical operating condition, it is necessary to produce a small number of reference materials which will provide peaks of known intensity throughout the spectrum. This may be achieved by utilizing the well-defined stoichiometry of fuzed quartz and the ability to graft onto the surface exact monolayers of stable organic compounds containing fluorine. By employing both planar and granular materials the effects of surface roughness also become quantifiable.

RESULTS

Fuzed quartz either in its as cleaned state or with a hydrolysed surface was shown to not to be sufficiently stable for use as a surface analysis reference material without the need for ion etch cleaning. Similarly when surface layers of either alkylsilanes, perfluorinated silanes or chlorosilanes were grafted onto Si02 layers their stability in the atmosphere or under X-ray irradiation was not high enough to enable them to be used as reference materials for either XPS or SIMS. By contrast when the polymers were grafted onto a chromium surface they were found to be much more stable.


ECU 61 200

PARTICIPANTS

Inst, de Physique Nucléaire de Lyon, F

305

PROJECT RM 299

THE EFFECTS OF CRYSTALUNITY ON THE QUANTIFICATION OF AUGER ELECTRON SPECTROSCOPY

PROJECT DEFINITION

Quantification of AES may be impaired by 3 effects of specimen crystallinity which result in peak intensities varying by a factor of 2 or more when exarnining single crystals, fracture surfaces or polycrystalline materials of grain size larger than the beam diameter. The first of these effects is anisotropy of Auger electron emission and the second and third the diffraction and channelling of the incident and emergent beam, respectively. The aim of the project was to isolate and examine these effects separately for a wide range of materials in order to determine their underlying mechanisms and relative contributions to peak intensity attenuation. With this knowledge procedures were developed to minimize the effects of crystallinity when performing quantitative AES as well as looking to see how the effects could be used to characterize materials.

RESULTS

The project demonstrated that the effects responsible for the crystalline contrast are too complex to be incorporated into generally applicable correction procedures being dependent both the specimen and the type of spectrometer used. Thus Auger electron diffraction is nearly always negligible in a cylindrical mirror analyzer but may be of comparable magnitude to channelling in concentric hemispherical analyzer. As a result the existence of crystallographic effects must be recognised in individual cases and strategies evolved to account for them. This is particularly true when, as in the measurement of the stoichiometry of a crystalline substrate, the relative intensities of all Auger peaks will be affected by diffraction. In some limited cases amorphization of the sample by ion bombardment was shown to be effective in removing the effects of crystallinity but care has to be taken to avoid preferential sputtering which itself may be orientation dependent. On the other hand, by using low beam energies and normalizing the signals from surface layers (e.g. segregant layers) to the N(E) background at a high energy, reliable surface coverage data can be obtained. In order to understand the interaction of the various effects of crystallinity theoretical calculations were also undertaken. These confirmed the complex nature of the effects but gave insight into how they could both be controlled and used to characterize materials.


ECU 255 000

PARTICIPANTS

CEA, F Thomson CSF, F Univ of Lyon, F Kax Planck Düsseldorf, D UKAEA Harwell, UK

306

PROJECT RM 305

INTERCOMPARISON OF SURFACE ANALYSIS MEASUREMENTS OF OXIDE FILMS OF ALUMINIUM

PROJECT DEFINITION

This project continues the theme of Project 193 by determining the reproducibility of the determination of thin oxide film thickness using AES and XPS whilst at the same time improving quantification procedures and determining important reference data for the oxide system studied.

RESULTS

Samples of 230 run thick A l ^ on Al were produced and characterized using nuclear reaction analysis. XPS was then used to determine Al and O peak positions, intensities, chemical shifts and the oxide thickness using the spectrometer energy calibration determined in project 193. In addition the layer was sputter depth profiled using AES and the BCR 260 Ta205 oxide thickness reference material.

The very consistent results gave the following:

the binding energies of the metallic states Al 2p and Al 4f7/2 are 73.0 ± 0.1 eV and 118.0 ± 0.2 eV; the chemical shifts of Al3+ in the oxide layer are 2.8 ± 0.1 eV and 2.5 ± 0 . 1 eV; using the oxide thickness obtained with nuclear reaction analysis and the ratios of the oxide thickness to electron attenuation length from XPS, the attenuation lengths for ALA, are (Al2p)MiI0l = 17.7°A and ( A L J ^ = 20.5°A; the ratios of the photoelectron yields of oxygen to aluminium are YCO^/YCAl^ = 6.1 ± 0.7 and Y(0J /Y(AU = 5.0 ± 0.7; the LMM and KLL AES energies of Al in A1203 53.5 ± 2.8 eV and 1389.5 ± 3.5 eV, the corresponding values for Al metal being 66.4 ± 2.8 eV and 1394.4 ± 4.0 eV; the relative etching rate between A1203 and Ta205 is 0.69 ± 0 . 1 7


ECU 22 977

PARTICIPANTS

Univ. Pierre S Marie Curie, F IRSID, F Univ. Delft, NL Hax PLanck Inst. Düsseldorf, D Max Planck Inst. Stuttgart, D CEGB, UK Alean, UK Univ. Surrey, UK Chalmers Univ., S VAU AG, D Ecole Polyytechnique Fédérale, CH

307

PROJECT RM 317

ESTABLISHMENT OF A PRACTICAL BACKGROUND SUBSTRACTION ALGORITHM FOR XPS AND AES

PROJECT DEFINITION

The quantification of surface analytical AES and XPS was the subject of several earlier projects. As such, they are effective if the peak height is not influenced by the matrix. When interference is present, one needs improved methods for substracting the background from the actual spectra. Improved methods are now available in the form of practical algorithms. The aim of the proposed project is to test the application of these algorithms, initially with pure metals and then with increasingly complex materials, both homogeneous and non-homogeneous. At each stage, the application of the new methods will be revised in the light of the results. The work will be initially carried out by XPS. It will be extended to AES in a later phase.

STATUS

An intercomparison on the use of the new background subtraction algorithms in comparison to existing ones is being carried out for data produced on a wide range of makes and models of XPS instruments.


ECU 161 000

PARTICIPANTS

Fysik Institut, Odense Univ., DK (pi Lot laboratory) + 20 Laboratories in aLl Member States

308

PROJECT RM 343

SECOND XPS INTENSITY INTERCOMPARISON

PROJECT DEFINITION

Project 193 established for the first time traceable energy and intensity scales for two of the three surface analytical techniques primarily used in industry, namely X-ray photoelectron spectroscopy (XPS) and Auger Electron Spectroscopy CAES). The results of this work have been accepted as a significant step forward in the quantification of these techniques. More recently, as a direct result of the methodology adopted for the AES energy/intensity project, NPL has been able to establish an AES/XPS instrument which is fully characterised and can provide absolute spectra. Using these, it will be possible via an intercomparison to establish for the first time absolute energy/intensity transmission functions for different spectrometers as distinct to the relative ones. Having done so, the way will be open to proceed towards improved quantification by, in addition, making use of background substruction (project 317). Absolute spectra will be obtained under strictly controlled conditions for the materials used in the XPS and AES intercomparisons (Ag, Au and Cu). An intercomparison will then be held in which participants with different designs of instrument will determine the same spectra for a wide range of operating conditions. The results will be analysed to determine if it is possible to produce master calibrations for each spectrometer type or if, at the 3% accuracy level, individual calibrations are required.

STATUS

In progress.



PARTICIPANTS

National Physical Laboratory, UK + 25 laboratories from Community Member States

309

PROJECT MR 359

REFERENCE SPECTRA FOR AUGER ELECTRON SPECTROSCOPY

PROJECT DEFINITION

BCR's contribution to surface analysis has been consistently aimed at the quantification of 3 techniques, namely AES, XPS and SIMS, which are the most widely used in industry. To date work has been undertaken to develop traceable calibrations for the energy and intensity scales of AES and XPS and to examine the effects of artifacts such as those produced by crystallinity. In addition, work is in progress to develop appropriate background substraction routines to enable the true quantification of analyses. As part of the work on AES, a reference instrument will full traceability to national voltage and other standards has been established at the National Physical Laboratory. The existence of this instrument allows the deconvolution of the instrumental factors from an AES spectrum so that the measured peak heights are no longer dependent upon the energy at which they are determined and thus the energy-intensity response function of the detecting spectrometer. The heights of peaks within the spectra obtained in this way therefore represent the actual relative sensitivities for the different Auger transitions. With this knowledge one should be able to obtain the same elemental analysis whether one uses the high or low energy peaks in the analysis for a given element in a sample. Moreover, using the procedures which were derived in earlier projects to establish energy/intensity response functions relative to the reference instrument, reference spectra related to this instrument can be transferred to any other machine. The present project is therefore to produce reference AES spectra for all the vacuum stable, non radioactive elements of the periodic table.

STATUS

In progress.



PARTICIPANTS

National Physical Laboratory, UK CNRS, F

European Communities - Commission

EUR 14800 - The BCR programme on applied metrology and chemical analysis

Projects and results 1988-92

Luxembourg: Office for Official Publications of the European Communities

1992 - xvi + 312 pp. - 15.0 χ 21.0 cm

BCR information series

ISBN 92-826-4968-7

Price (excluding VAT) in Luxembourg: ECU 28.50

This book summarizes the results of research projects which were carried out under the European Community BCR programme between 1988 and 1992. It covers 145 projects related to chemical analyses, mainly concerned with environment, food, agriculture and medical care, 106 projects related to metrology, and 20 projects related to testing of various industrial products.

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This book summarizes the results of research projects

which were carried out under the European Community's

BCR programme between 1988 and 1992. It covers 145

projects related to chemical analyses, mainly concerned

with environment, food, agriculture and medical care,

106 projects related to metrology, and 20 projects related

to testing of various industrial products.

The purpose of all these projects was to improve existing

methods of measurement and testing to improve the way

in which they are implemented, or to develop new

methods when the economic need to do so was

established. A number of projects have led to the

development of certified reference materials which can

be used by laboratories to verify if their own results are

correct. Finally, projects in the field of metrology have

improved the harmonization of the calibrations provided

by official laboratories to industry throughout the

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