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Tables of Contents for Interlaboratory Studies and Certified Reference Materials for Environmental Analysis
Chapter/Section Title
Page #
Page Count
Preface
xix
Foreword
xxi
Herbert Muntau
Abbreviations
xxv
General Introduction
The analyst and his duty
1
2
The necessity to deliver good answers
3
1
The necessity to produce reliable data
3
2
The regulatory background of quality
5
5
GLP
6
1
Certification ISO 9000
6
1
Certification ISO 14000
7
1
Accreditation ISO 25/EN 45000
8
1
International bodies for the harmonisation of standards
8
1
Conclusions
9
1
References
10
3
Quality in Chemical and Biological Analysis
Tools to achieve quality
13
5
Terms and definitions
13
1
Basic definitions
13
1
Trivial terms
14
1
Hierarchy of methods
15
1
Calibration linked classification of methods
16
1
Performance criteria of methods
17
1
Tools for QA and QC of biological and chemical measurements
18
2
First line checks
19
1
Second line checks
19
1
Third line checks
20
1
Validation of methods
20
29
Validation of instruments, computers and software
21
1
Validation of the analytical method
21
1
Full development of a method
22
1
Validating a standard procedure
22
3
Practical examples of method development and validation
25
17
Quality control of microbiological determinations
42
1
Microbiological methods
42
5
Accuracy and precision of microbiological tests
47
1
Validation of microbiological methods
48
1
Quality assurance and standardisation
48
1
Control charts
49
8
Shewart charts
50
1
Other control charts
50
1
Microbiology
51
1
High levels counts
52
4
Presence-absence reference materials
56
1
Where and when to use RMs and CRMs
57
11
Definitions by ISO
60
1
Calibration and traceability
60
2
Method validation
62
4
Statistical control
66
1
Microbiology
66
2
Conclusions
68
1
References
68
3
Use of Certified Reference Materials
General aspects
71
2
Structural role
71
1
Practical role
72
1
Types of CRMs
73
12
Calibration materials
73
1
Pure substances
73
3
Synthetic mixtures
76
1
Natural materials
77
1
When using certified calibrants
77
1
Method validation materials
78
1
Choice of the CRM
78
1
Validation of the precision of a method
79
3
Validation of the trueness of a method
82
2
Frequency of use
84
1
Validation of standardised regulatory methods
85
1
Comparison of methods and instruments
85
1
Evaluation of non-certified reference materials
86
1
CRM for microbiological methods
86
12
Types of microbiology RM
86
1
Use of BCR-CRMs in microbiology
87
1
CRMs with high levels of cfp
87
2
The number of capsules to be used
89
1
The number of replicates to be used
90
1
Practical results
91
2
Low level CRMs
93
1
Problem description
93
1
Theory of testing
94
1
The number of capsules to be used
95
1
Practical results
96
1
Frequency of use
97
1
Conclusions
97
1
References
98
17
Production of Matrix CRMs
General considerations and warnings
115
1
Preparation of the material
115
23
Choice of the material
115
1
Analytes and their concentrations
116
1
The matrix of the material
117
1
The physical status
117
1
Limits to representativeness
118
1
Artificial matrix materials
118
1
Fresh materials
118
1
Series of materials
119
1
Stabilisation of the materials
119
1
Physical and chemical effects
120
1
Microbial activity
120
2
When to stabilise the material
122
2
Limits to stabilisation
124
1
Homogenisation
124
1
Necessity for homogeneous samples
124
1
Homogenisation of fluids
125
1
Homogenisation of solids
125
3
Packaging and storage
128
1
Packaging material and vial
128
6
Temperature of storage
134
1
Safety and information
134
3
Size of batch
137
1
Transport
137
1
Study of the homogeneity
138
16
Principle
138
1
The test method
138
3
Conclusions and limits of the study
141
1
Extrapolations
142
1
Within-vial homogeneity study
142
1
Objectives and limits
142
1
Testing for the within-vial homogeneity
143
2
Between-vial homogeneity study
145
1
Principle and objective
145
1
Testing for the between-vial homogeneity
145
1
Practical implementation
146
5
Between-vial check through interlaboratory study
151
1
Conclusions
152
2
Study of the stability
154
10
Objectives
154
1
Multiple temperature approach
155
1
Analytical methods used for the study of stability
156
1
Isochronous studies
157
2
Extrapolations through Arrhenius law
159
2
Expiry dates
161
2
Short-term studies and conclusions
163
1
References
164
4
Procedures to Certify Reference Materials
Absolute amounts
168
13
Pure substances
168
1
Inorganic materials
168
1
Organic and organo-metallic substances
169
2
Mixtures of substances
171
1
Calibration solutions
171
1
Matrix materials
171
1
Single laboratory approach
172
1
Interlaboratory certification study
173
1
The BCR approach
173
8
Method-dependent parameters
181
2
Chemical status
182
1
Physical status
182
1
Activity-linked fractions
182
1
CRM for testing
183
1
Certification of CRM for microbiology
183
6
Types of materials
183
1
Stabilisation of microbes
184
1
Homogeneity tests
185
1
Stability tests
185
2
Certification by interlaboratory studies
187
2
Certificate and certification report
189
1
Information content
189
1
Responsibility of the producer
190
1
Producers and production systems
190
1
Producers
190
1
Production systems
191
1
Driving forces for the future
191
19
Salient features of the inquiry
198
2
Needs and recommendations
200
1
Needs for reference materials
200
5
Representativeness
205
1
Development and CRM production
206
1
Interlaboratory trials
206
1
Information/Education/Training
207
1
Networking institutes/Databases
207
1
Summary of needs
208
1
Expected trends
209
1
Conclusions
210
1
References
210
25
CRMs for Plant Analysis
Trace elements in aquatic plants
235
4
Introduction
235
1
Production of the materials
235
1
Certification
236
1
Participating laboratories
237
2
Trace elements in sea lettuce
239
4
Introduction
239
1
Production of the material
239
1
Certification
240
2
Participating laboratories
242
1
Trace elements in rye grass
243
5
Introduction
243
1
Production of the material
243
2
Certification
245
1
Participating laboratories
246
2
Trace elements in hay powder
248
3
Introduction
248
1
Production of the material
248
1
Certification
249
1
Participating laboratories
250
1
Trace elements in white clover
251
4
Introduction
251
1
Production of the material
252
1
Certification
252
1
Participating laboratories
253
2
Trace elements in beech leaves and spruce needles
255
3
Introduction
255
1
Production of the materials
255
1
Certification
256
1
Participating laboratories
257
1
Trace elements in lichen
258
6
Introduction
258
1
Interlaboratory study
259
1
Production of the material
259
1
Certification
260
2
Participating laboratories
262
2
References
264
1
CRMs for Biological Material Analysis
Trace elements in fish
265
4
Introduction
265
1
Production of the material
265
1
Certification
266
1
Participating laboratories
267
2
Methyl mercury in fish
269
4
Introduction
269
1
Production of the materials
270
1
Certification
271
1
Participating laboratories
272
1
As-species in fish
273
2
Introduction
273
1
Production of the material
273
1
Certification
274
1
Participating laboratories
275
1
CBs in fish oil
275
5
Introduction
275
1
Interlaboratory studies
276
1
Production of the materials
277
1
Certification
278
1
Participating laboratories
279
1
OCPs in cod liver oil
280
4
Introduction
280
1
Production of the material
280
2
Certification
282
1
Participating laboratories
283
1
Trace elements in mussel
284
2
Introduction
284
1
Production of the material
284
1
Certification
285
1
Participating laboratories
286
1
Organotins in mussel
286
6
Introduction
286
2
Production of the material
288
2
Certification
290
2
Participating laboratories
292
1
Trace elements in plankton
292
4
Introduction
292
1
Production of the material
292
2
Certification
294
1
Participating laboratories
295
1
Pesticides in animal fat
296
3
Introduction
296
1
Production of the material
296
1
Certification
297
1
Participating laboratories
298
1
Trace elements in milk
299
4
Introduction
299
1
Production of the material
299
1
Certification
300
2
Participating laboratories
302
1
CBs in milk
303
4
Introduction
303
1
Production of the material
304
1
Certification
304
2
Participating laboratories
306
1
Dioxins in milk
307
3
Introduction
307
1
Production of the material
307
1
Certification
308
2
Participating laboratories
310
1
Microbiological parameters in milk
310
6
Introduction
310
1
Production of the materials
310
1
Milk containing Salmonella
310
1
Milk containing Enterococcus
311
2
Certification
313
1
Milk containing Salmonella
313
1
Milk containing Enterococcus
314
1
Participating laboratories
315
1
Trace elements in human hair
316
3
Introduction
316
1
Production of the material
317
1
Certification
317
2
Participating laboratories
319
1
References
319
2
CRMs for Water Analysis
Major elements in freshwater
321
3
Introduction
321
1
Production of the materials
321
1
Certification
322
1
Participating laboratories
323
1
Nitrate in freshwater
324
5
Introduction
324
1
Feasibility study
324
3
Production of the materials
327
1
Certification
328
1
Participating laboratories
329
1
Major elements in rainwater
329
4
Introduction
329
1
Production of the materials
329
2
Certification
331
1
Participating laboratories
332
1
Trimethyllead in rainwater
333
7
Introduction
333
1
Feasibility study
334
1
Interlaboratory studies
335
1
Production of the materials
336
2
Certification
338
2
Participating laboratories
340
1
Major elements in groundwater
340
4
Introduction
340
1
Feasibility study
340
1
Production of the materials
341
1
Certification
342
1
Participating laboratories
343
1
Trace elements in groundwater
344
7
Introduction
344
1
Interlaboratory study
345
1
Production of the materials
346
1
CRMs for trace elements
346
2
CRMs for bromide
348
1
Certification
348
2
Participating laboratories
350
1
Trace elements in estuarine water
351
9
Introduction
351
1
Feasibility study
352
1
Interlaboratory studies
352
4
Production of the material
356
1
Certification
357
2
Participating laboratories
359
1
Trace elements in seawater
360
5
Introduction
360
1
Interlaboratory studies
360
1
Production of the material
361
2
Certification
363
1
Some remarks on the analysis of the material
363
1
Participating laboratories
364
1
Mercury in seawater
365
6
Introduction
365
1
Feasibility study
365
1
Interlaboratory studies
366
1
Preliminary work
366
1
Production of the material
367
2
Certification
369
1
Participating laboratories
370
1
Cr-species in lyophilised water
371
4
Introduction
371
1
Preliminary investigations
371
1
Interlaboratory study
372
1
Production of the material
373
1
Certification
374
1
Participating laboratories
375
1
Se-species in solution
375
7
Introduction
375
1
Preliminary investigations
376
2
Interlaboratory study
378
1
Production of the materials
378
2
Certification
380
1
Participating laboratories
381
1
Unstable pesticides in lyophilised water
382
3
Introduction
382
1
Production of the material
383
1
Certification
384
1
Participating laboratories
385
1
References
385
4
CRMs for Sediment Analysis
Trace elements in river and lake sediment
389
4
Introduction
389
1
Production of the materials
389
1
Certification
390
3
Participating laboratories
393
1
Fluoride in clay
393
3
Introduction
393
2
Production of the material
395
1
Certification
395
1
Participating laboratories
396
1
Organotins in estuarine sediment
396
6
Introduction
396
1
Preliminary investigations
396
1
Production of the material
397
2
Certification
399
3
Further developments
402
1
Participating laboratories
402
1
Methyl mercury in estuarine sediment
402
6
Introduction
402
1
Interlaboratory study
403
1
Production of the material
403
1
Certification
404
3
Participating laboratories
407
1
Extractable trace elements in river sediment
408
4
Introduction
408
1
Interlaboratory study
408
2
Production of the material
410
1
Certification
410
1
Participating laboratories
411
1
PCBs in sediment
412
4
Introduction
412
1
Production of the material
413
1
Certification
414
1
Participating laboratories
415
1
PAHs in sediment
416
3
Introduction
416
1
Production of the material
416
1
Certification
417
1
Participating laboratories
418
1
References
419
2
CRMs for Soil and Sludge Analysis
Introduction
421
1
Trace elements in soils
421
6
Introduction
421
1
Production of the material
422
3
Certification
425
1
Participating laboratories
426
1
Extractable trace elements in sewage sludge amended soils
427
7
Introduction
427
2
Production of the material
429
2
Certification
431
1
Participating laboratories
432
2
CBs in sewage sludge
434
4
Introduction
434
1
Production of the materials
435
1
Certification
436
1
Participating laboratories
437
1
PAHs in sewage sludge
438
4
Introduction
438
1
Production of the materials
439
1
Certification
440
1
Participating laboratories
441
1
References
442
3
Other Types of CRMs
Coal materials
445
11
Introduction
445
1
Trace elements in coal
445
1
Production of the materials
445
1
Certification
446
1
Participating laboratories
446
2
Minor and major elements in three coals
448
1
Introduction
448
1
Production of the reference materials
448
1
Certification
449
1
Participating laboratories
450
1
Sulphur in six coals
451
1
Introduction
451
1
Production of the reference material
452
1
Certification
452
2
Participating laboratories
454
1
Fluorine in coal
454
1
Introduction
454
1
Production of the reference material
454
1
Certification
455
1
Participating laboratories
455
1
Ash materials
456
10
Introduction
456
1
Trace elements, fluorine and chlorine in ash
456
1
Introduction
457
1
Production of the reference material
457
1
Certification
458
3
Participating laboratories
461
1
Dioxins in fly ash extract
462
1
Introduction
462
1
Preparation of the reference material
462
2
Certification
464
1
Participating laboratories
465
1
Dust materials
466
8
Trimethyllead in urban dust
466
1
Introduction
466
1
Feasibility study
466
1
Interlaboratory study
467
1
Production of the material
467
2
Certification
469
1
Participating laboratories
470
1
Cr(VI) in welding dust
470
1
Introduction
470
1
Preliminary investigations
471
1
Production of the material
472
1
Certification
473
1
Participating laboratories
473
1
PCBs in mineral oil
474
4
Introduction
474
1
Production of the materials
475
1
Certification
476
1
Participating laboratories
477
1
References
478
3
Interlaboratory Studies
Introduction
481
1
Definitions
481
1
General principles
481
9
Participants
482
1
Organiser
482
1
Objective of the study
482
1
Choice and preparation of the test materials
483
1
Selection of the test material
483
1
Representativeness
483
1
Preparation
484
1
Assigned values
484
2
Analytical protocol
486
1
Collection and evaluation of data
486
1
Collection of results
486
1
Technical evaluation
487
1
Statistical evaluation
488
1
Conclusions and actions
488
2
Method performance studies
490
8
Definition
490
1
Fields of application
490
1
Method and protocol
491
1
Participants
491
1
Materials
491
1
Reporting and exploitation of the data
492
1
Examples of method performance study
492
1
Extraction tests for soil and sediment analysis
492
6
Evaluation of methods of microbiological parameters
498
1
Laboratory performance studies
498
9
Definition
498
1
Field of application
499
1
Objective and organisation
499
1
Evaluation of performance
500
1
Relation to accreditation
501
2
Example of laboratory performance study: Proficiency testing scheme for marine monitoring
503
1
Introduction
503
1
Framework
504
1
Test materials
505
1
Performance evaluation
505
1
Developments
506
1
Conclusion
507
1
Material certification studies
507
1
Improvement schemes
508
8
Aims and principles
508
1
Organisation
508
1
General principles
509
1
Example of improvement scheme: Methyl mercury in environmental matrices
510
1
Aim of the project
510
1
The interlaboratory programme
510
5
Example of improvement scheme: Seawater microbiology
515
1
Conclusions
516
1
References
516
21
Index
537
14
Laboratory Index
551