Quality Assurance of chemical measurements Taylor
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Table of Contents
Preface iii
CHAPTER 1. Introduction to Quality Assurance 1
CHAPTER 2. Precision, Bias, and Accuracy 7
Axioms 8
Corollaries 9
Sources of Error 9
Errors of Rounding 10
Influence of Uncertainty on Decision 10
CHAPTER 3. Statistical Control 13
CHAPTER 4. Statistical Techniques 15
Basic Requirements 15
Distributions 17
Statistics of Measurements 18
Estimation of Standard Deviation 20
Estimation of Standard Deviation from Replicate
Measurements 21
Estimation of Standard Deviation from Duplicate
Measurements 22
Estimation of Standard Deviation from the Range 23
Pooling Estimates of Standard Deviations 24
The Analysis of Variance 25
Do Two Estimates of Precision Differ? 25
What are the Confidence Limits for an Estimate of a
Standard Deviation? 26
Confidence Interval for a Mean 27
Does a Measured Value Differ from an Expected
Value? 28
Do the Means of Two Measured Values Disagree
Significantly? 29
Statistical Tolerance Intervals 31
Pooling Means to Obtain a Grand Average 32
Outliers 33
Rejection for an Assignable Cause 34
Rule of the Huge Error 34
Statistical Tests 35
Dixon Test for Outlying Observations 35
Grubbs Test for Outlying Observations 36
Youden Test for Outlying Laboratories . 37
Cochran Test for Extreme Values of Variance 38
Statistics of Control Charts 38
Control Limits 38
Central Line Considerations 38
Agreement With Established Value 38
Has the Central Line Changed? 39
Use of Random Number Tables 39
CHAPTER 5. Chemical Analysis as a System 41
Systematic Approach to Analysis 41
Effective Problem Solving 41
CHAPTER 6. The Model 45
Importance of a Model 45
Development of a Model 46
Data Quality Objectives 47
CHAPTER 7. Planning 49
General Aspects of Planning 49
Development of an Experimental Plan 51
Content of a Measurement Plan 51
CHAPTER 8. Principles of Sampling 55
Initial Considerations 55
Sampling Plan 58
Peer Review 59
Training 60
Sample Management 60
Problem of Subsampling 61
Critical Matters Related to Samples 77 61
Quality Assurance of Sampling 62
Sample Uncertainties 62
Stratification 63
Holding Time 63
Statistical Considerations in Sampling 64
Measurement Situations 64
Statistical Sampling Plan 65
Basic Assumptions 66
Guidance in Sampling 66
Cost Considerations 68
Minimum Size of Increments in a Well-Mixed
Sample 68
Size of Sample in Segregated Materials 69
Acceptance Testing 70
Matrix-Related Sampling Problems 72
Sampling Gases 73
Sampling Liquids 73
Sampling Solids 74
Sampling Multiphases 74
CHAPTER 9. Principles of Measurement 75
Terminology 75
Measurement is a Comparison Process 77
Principles of Chemical Measurement 77
Figures of Merit 78
Precision 78
Sensitivity 79
Limit of Detection and Limit of Quantitation 79
Short-term and Long-term Standard Deviation 83
Bias 83
Selectivity 84
Other Considerations 84
Importance of an SOP 85
Ruggedness Testing 85
Standardization of Methods 87
Selection of Appropriate Methodology 90
Guidelines for Selecting Instrumentation 91
Internal vs External Services 92
CHAPTER 10. Principles of Calibration 95
What Needs to be Calibrated 96
Requirements for Calibration 96
Frequency of Calibration 97
Mode of Calibration 97
Linear Relationships 98
Tests for Linearity 101
Calibration Uncertainties 103
Intercalibration 106
Additional Remarks 106
CHAPTER 11. Principles of Quality Assurance 107
CHAPTER 12. Principles of Quality Control Ill
Competence Ill
Suitable Facilities and Equipment 112
Good Laboratory and Good Measurement Practices 112
Standard Operations Procedures 113
Distinction Between GLPs, GMPs, and SOPs 114
Protocols for Specific Purposes 115
Contents of a PSP 116
Other Quality Control Techniques 118
Inspection 118
Documentation 119
Training 120
The Quality Control System 121
CHAPTER 13. Blank Correction 123
Sources of Blanks 123
Control of Blanks 123
Evaluation of Blanks 124
Statistical Treatment of the Blank 125
Significance 126
CHAPTER 14. Control Charts 129
Format 129
Control Limits 131
Evaluating Control Limits 132
Control Samples 133
Frequency of Control Measurements 133
Identification of Population 136
Strategy of Use 136
Assignment of Uncertainty 138
Range Control Charts 139
Approach 139
Use of Range Control Charts 141
Subspan Range Control Charts 141
Range Performance Charts 141
Range Ratio Control Charts 77 143
Collateral Control Charts 144
Critical Collateral Measurement Control Charts 144
Recovery Control Charts 145
Other Useful Control Charts 145
Additional Remarks 145
Blinds vs Double Blinds 146
CHAPTER 15. Principles of Quality Assessment 147
Internal Techniques 147
External Techniques 149
Qualitative Identification 150
Other Techniques 150
CHAPTER 16. Evaluation Samples 153
Prime Requirements 153
Types of Evaluation Samples 153
Liquid Samples 155
Solid Samples 155
Gas Samples 155
Stability of Mixtures 156
Subsampling 156
Integrity of Evaluation Samples 157
CHAPTER 17. Reference Materials 159
Role of Reference Materials 159
Uses of Reference Materials 160
Certification of Reference Materials 163
CHAPTER 18. Traceability 165
Chemical Traceability 165
Standards Prepared by the Analyst 167
Standards Prepared by Others 167
Physical Standards 167
Reference Materials Produced by NBS 167
Reference Materials Produced by Others 168
Traceability of Analytical Results 169
Concept of the National Measurement System 169
CHAPTER 19. Quality Audits 173
Internal Audits 173
Internal Systems Audits 173
Internal Performance Audits 174
Mechanism 174
Corrective Actions 175
External Audits 175
Independent Audits 175
Forms 176
Personal Quality Assurance Profile 177
Laboratory Quality Assurance Profile 179
Quality Assurance Survey 181
Quality Assurance Practices Check List 182
Quality Assurance Training Profile 185
CHAPTER 20. Quality Circles 187
Organization 187
Objectives 187
Operation 188
Reporting 189
Agenda 191
CHAPTER 21. Validation 193
Validation of Samples 193
Validation of Methodology 193
Validation of Data 195
CHAPTER 22. Reporting Analytical Data 197
Minimum Requirements 197
Data Limitations 198
Numerical Values 199
Limits of Uncertainty for Data 199
Significant Figures 200
Guidelines for Reporting Results of Measurements 202
Guidelines for Combining Data Sets 203
Arbitrary Reporting Procedures 203
Reporting Low-Level Data 203
Report Format 205
CHAPTER 23. An Improved Approach to Performance
Testing 209
Premises 209
Advance Estimation of Precision 210
Performance Testing Plan 211
Diagnosis 211
Feedback 212
Consensus Values 213
Statistical Treatment of Data 213
CHAPTER 24. Correction of Errors and/or Improving
Accuracy 215
Identification of Problems 215
Improvement of Performance 217
Editing Data 221
CHAPTER 25. Laboratory Evaluation 225
Generic Guidelines for Evaluation 225
Accreditation 226
Self-Evaluation 228
CHAPTER 26. The Quality Assurance Program 231
Approaches to Quality Assurance 231
Quality Assurance Policy 234
Planning for Quality Assurance 234
Development of a QA Program 236
Quality Assurance Manual 238
Federally Mandated Quality Assurance Programs 239
Public Health Service 239
Food & Drug Administration 241
Environmental Protection Agency 242
Nonfederally Mandated Quality Assurance Programs 243
Quality Assurance for Measurement Programs 244
Relating Personnel to Quality Assurance 244
Appendix A. Terminology Used in Quality Assurance 245
Appendix B. Quality Assurance Program Documentation 255
B.l Example Quality Assurance Program Document 255
B.2 Outline for Use in Preparing an SOP for a
Measurement Method 262
B.3 Outline for Use in Preparing an SOP for
Calibration 263
B. 4 Outline for Use in Preparing a GLP or GMP 263
Appendix C. Statistical Tables 265
C. l Use of Range to Estimate Standard Deviation 265
C.2 Z-Factors for Two-Sided Confidence Intervals
for the Normal Distribution 266
C.3 Student t Distribution 267
C.4 Factors for Computing Two-Sided Confidence
Intervals for t, 268
C.5 Factors for Computing Two-Sided Confidence
Intervals for a Normal Distribution 269
C.6 Critical Values for the F Test 269
C.l Values for Use in the Dixon Test for Outliers 270
