Quality assurance in analytical chemistry : applications in environmental, food, and materials analysis, biotechnology, and medical engineering

著者

    • Funk, Werner
    • Dammann, Vera
    • Donnevert, Gerhild

書誌事項

Quality assurance in analytical chemistry : applications in environmental, food, and materials analysis, biotechnology, and medical engineering

Werner Funk, Vera Dammann, Gerhild Donnevert

Wiley-VCH, c2007

2nd ed

タイトル別名

Qualitätssicherung in der Analytischen Chemie

大学図書館所蔵 件 / 全2件

この図書・雑誌をさがす

注記

Includes bibliographical references (p. 209-217) and index

"Second, completely revised and enlarged edition"--Cover

内容説明・目次

内容説明

This best-selling title both in German and English is now enhanced by a new chapter on the important topical subject of measurement uncertainty, plus a CD-ROM with interactive examples in the form of Excel-spreadsheets. These allow readers to gain an even better comprehension of the statistical procedures for quality assurance while also incorporating their own data. Following an introduction, the text goes on to elucidate the 4-phase model of analytical quality assurance: establishing a new analytical process, preparative quality assurance, routine quality assurance and external analytical quality assurance. Besides updating the relevant references, the authors took great care to incorporate the latest international standards in the field.

目次

  • Preface xiii List of Symbols xvii 0 Introduction 1 0.1 General Differentiation of Analytical Processes 3 0.2 Quality of Analytical Processes and Results 4 0.3 The System of Analytical Quality Assurance 4 0.4 The Four-Phase Model of Analytical Quality Assurance 6 1 Phase I: Establishing a New Analytical Procedure 9 1.1 Introduction 9 1.1.1 Objectives of Phase I 9 1.1.2 When Are Characteristic Data Obtained? 9 1.1.3 The Progression of Phase I 10 1.1.4 Results of Phase I
  • Statistical Data 14 1.2 Calibration of the Fundamental Analytical Procedure 15 1.2.1 Establishment of an Analytical Range 16 1.2.2 Preparation of Standard Samples 16 1.2.3 Determination of the Calibration Function and Process Data 17 1.2.3.1 Process Data for the Linear Calibration Function 18 1.2.3.2 Process Data for the Second-Order Calibration Function 19 1.2.3.3 Calculating Analytical Results with the Aid of the Calibration Function 21 1.2.4 Verification of the Fundamental Calibration 23 1.2.4.1 Verification of Linearity 23 1.2.4.2 Verification of Precision 25 1.3 Analyses at Very Low Concentrations 29 1.3.1 Decision Limit 32 1.3.2 Determining the Minimum Detectable Value 34 1.3.2.1 Minimum Detectable Value, Determined Using the Distribution of Blank Values 34 1.3.2.2 Minimum Detectable Value, Obtained Using the Calibration Function 35 1.3.3 Limit of Quantification 35 1.3.4 Quick Estimation 36 1.3.5 Estimation of the Decision Limit and Limit of Quantification Using the S/N Ratio 37 1.4 Validation of Individual Process Steps and Examination of Matrix Influences 37 1.4.1 Systematic Errors 37 1.4.1.1 Constant Systematic Errors, Additive Deviations 37 1.4.1.2 Proportional Systematic Errors, Multiplicative Deviations 38 1.4.2 Establishment and Assessment of the Recovery Function 38 1.4.2.1 Prerequisites for the Interpretation of the Recovery Function 39 1.4.2.2 Testing for Systematic Errors 40 1.4.3 Application of the Recovery Function 41 1.4.3.1 Checking Individual Process Steps 41 1.4.3.2 Determination of the Recovery Function to Prove the Influence of a Matrix 45 1.5 Additional Statistical Methods 46 1.6 Use of Internal Standards 46 1.6.1 Definition, Purpose 46 1.6.2 Conditions and Limitations of the Use of Internal Standards 47 1.6.3 Procedure 47 1.7 Preparing for Routine Analysis 49 1.7.1 Examination of the Time Dependency of Measured Values 49 1.7.1.1 Comparison of the "Within Batch" Standard Deviation (sw) with the "Between Batches" Standard Deviation (sb) 49 1.7.1.2 Determining the Need for Daily Adjustment of Analytical Equipment 51 1.7.1.3 The Trend Test 51 1.8 Summary of the Results of Phase I (Process Development): Documentation 54 2 Phase II: An Analytical Process Becomes Routine
  • Preparative Quality Assurance 57 2.1 Introduction 57 2.1.1 Objectives of Phase II 57 2.1.2 Execution of Phase II 57 2.1.3 Progression of Phase II 57 2.1.4 Results of Phase II 58 2.2 Selection of the Analytical Procedure 59 2.2.1 Specificity of the Procedure 60 2.2.2 Selectivity of the Analytical Procedure 60 2.2.3 Working Range 60 2.2.4 Calibration Function, Sensitivity, and Precision of the Procedure 60 2.2.5 Minimum Detectable Value and Limit of Quantification 61 2.2.6 Risk of Systematic Error 61 2.2.7 Effort, Costs 61 2.3 The "Training" Phase of the Process 62 2.4 Establishment of Quality Objectives to be Adhered to in Routine Usage 64 2.4.1 External Quality Requirements 65 2.4.2 Internal Quality Requirements 66 2.5 Control Samples for Internal Quality Assurance 66 2.5.1 Requirements of Control Samples 66 2.5.2 Types of Control Samples 67 2.5.2.1 Standard Solutions 67 2.5.2.2 Blank Samples 67 2.5.2.3 Natural Samples 67 2.5.2.4 Spiked Natural Samples 68 2.5.2.5 Synthetic Samples 68 2.5.2.6 Certified Reference Materials (CRMs) 68 2.5.3 Requirements for Producers of Control Materials 69 2.5.4 Applicability of Control Sample Types 69 2.6 The Control Chart System 70 2.6.1 Introduction: History of the Control Chart 70 2.6.2 Principle of a Control Chart 72 2.6.3 Average Run Length (ARL) and Evaluation of Control Charts 73 2.6.4 Derivation of the Average Run Length (ARL) 74 2.6.4.1 Examples of Theoretical Calculations 75 2.6.4.2 Analytical Example 76 2.6.5 Concept for the Preparation of Routine Quality Control 78 2.6.6 Evaluation of the Preliminary Period 80 2.6.6.1 Variance Analysis 80 2.6.6.2 Adherence to Required Quality Objectives 80 2.6.7 Types of Control Charts and Their Applications 80 2.6.7.1 Shewhart Charts 81 2.6.7.2 R-Chart (Range Control Chart) 89 2.6.7.3 Difference Chart 96 2.6.7.4 Standard Deviation Chart (s-Chart) 98 2.6.7.5 Target Value Charts 99 2.6.7.6 Cusum Chart 100 2.6.8 Summary of the Characterization of Control Charts 112 3 Phase III: Routine Quality Assurance 115 3.1 Introduction 115 3.1.1 Setting the Objectives of Phase III 115 3.1.2 Execution of Phase III 115 3.1.3 Progression of Phase III 115 3.2 Fundamental Measures of Internal Quality Assurance 118 3.2.1 The Laboratory and Laboratory Management 118 3.2.2 Personnel 119 3.2.3 Outfitting and Equipment 119 3.2.3.1 Performance Monitoring, Calibration and Adjustment of Measuring Equipment 119 3.2.3.2 Maintenance of Equipment 120 3.2.4 Materials 121 3.2.4.1 Certifying Sample Quality 121 3.2.4.2 Analysis-Related Materials 121 3.2.4.3 Control Samples for Routine Quality Control 122 3.2.5 Instituted Analytical Processes 122 3.2.6 Testing the Equivalency of Analytical Results 122 3.2.6.1 Testing the Equivalency for a Single Matrix 123 3.2.6.2 Testing the Equivalency in Different Matrices 126 3.2.7 Uncertainty of Measurements 130 3.2.7.1 New Terms According to the EURACHEM Guide 131 3.2.7.2 Overview of Common Procedures for the Determination of Measurement Uncertainty 133 3.2.7.3 Indication of Measurement Uncertainty in Test Reports 142 3.2.7.4 Interpretation of Measurement Uncertainty in the Context of Limit Value Monitoring 143 3.2.7.5 Summary 144 3.2.8 Reporting Analytical Results 145 3.3 Routine Quality Control 145 3.3.1 Trueness Control 146 3.3.1.1 General 146 3.3.1.2 Blank Value Monitoring 146 3.3.1.3 _x-Chart 148 3.3.1.4 Recovery Rate Control Chart 148 3.3.2 Precision Control 148 3.3.2.1 General 148 3.3.2.2 Precision Control Using an R-Chart 149 3.3.2.3 Securing Precision Using a Standard Deviation Control Chart 149 3.3.3 Revision of Quality Control Charts 150 3.3.4 Quality Assurance in the Case of Time-Consuming or Infrequent Analyses 150 3.4 Special Quality Problems in Routine Analysis 151 3.4.1 Matrix Effects 151 3.5 Corrective Measures 154 3.5.1 Sources of Error in Analytical Laboratories 154 3.5.2 Systematic Troubleshooting 155 3.5.2.1 Analytical Errors That Can Be Detected Using Statistical Quality Control Methods 161 3.5.2.2 Plausibility Checks 162 3.6 Documentation and Archiving 166 4 Phase IV: External Analytical Quality Assurance 169 4.1 Introduction 169 4.2 Audits 169 4.3 Interlaboratory (or Round Robin) Tests 170 4.3.1 Interlaboratory Tests for Process Standardization 171 4.3.2 Interlaboratory Tests as Proof of Laboratory Performance 171 4.3.3 Other Interlaboratory Tests 172 4.3.4 Planning and Execution of Interlaboratory (or Round Robin) Tests 173 4.3.4.1 Quality Management System of the Provider of an Interlaboratory Test 173 4.3.4.2 Planning the Interlaboratory Test 174 4.3.4.3 Interlaboratory Test Samples 175 4.3.5 Procedures for the Execution and Evaluation of Interlaboratory Tests 176 4.3.5.1 Interlaboratory Test Programs According to ISO 5725-2 177 4.3.5.2 The Youden Method of Interlaboratory Tests 179 4.3.5.3 Interlaboratory Tests According to ISO Guide 43 188 4.4 Effects of Internal Quality Assurance on the Results of Interlaboratory Tests 191 4.5 Conclusion 194 5 Definitions 195 5.1 Quality and Quality Management 195 5.2 Analytical Terms 197 5.3 Analytical Results 201 5.4 Deviation, Uncertainty 202 5.5 Materials, Samples 205 5.6 Statistical Tests 206 6 References Appendix 1 A1 Sample Calculations 219 A1.1 Fundamental Calibration 219 A1.2 Linearity Tests 221 A1.2.1 Visual Linearity Test 221 A1.2.2 Second-Order Calibration Function 222 A1.2.3 Linearity Test: Goodness-of-Fit Test 224 A1.2.4 Variance Homogeneity Test 226 A1.2.5 Outlier Tests for Linear Calibration 228 A1.2.6 Securing the Lower Range Limit 230 A1.2.7 Decision Limit, Minimum Detectable Value, and Limit of Quantification 231 A1.2.8 Recovery Function 236 A1.2.9 Testing Analytical Results for Temporal Stability 239 A1.2.10 Trend Test 242 A1.2.11 Practice Phase: Checking the Analysis Quality Achieved Based on the Process Standard Deviation 243 A1.3 Phases II and III: Control Charts 244 A1.3.1 Blank Value Control Chart 245 A1.3.2 x-Chart for Standard Solutions 246 A1.3.3 Recovery Rate (RR) Control Chart 247 A1.3.4 Verifying Precision by Means of R-Charts and s-Charts 249 A1.3.5 Testing for Series-Internal Drift 251 A1.3.6 RR-Control Chart by Addition of a Standard 253 A1.3.7 Cusum Chart 254 A1.3.8 Equivalency 258 A1.3.9 Standard Addition 261 Appendix 2 A2 Statistical Tables 263 A2.1 t-Table 263 A2.2 F-Table (95%) 264 A2.2 F-Table (99%) 265 A2.3 Grubbs Table 267 A2.4 2-Table 268 Appendix 3 A3 Contents of the CD 269 A3.1 Checklists 269 A3.2 Instructions for Using the Calculation Examples 269 A3.3 Statistical Table Values 270 Subject Index 271

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