Quality Assurance of Chemical Measurements

ISBN-13: 9780367451417 / Angielski / Miękka / 2020 / 348 str.

John K. Taylor

Opis

This definitive new book should appeal to everyone who produces, uses, or evaluates scientific data. Ensures accuracy and reliability. Dr. Taylor's book provides guidance for the development and implementation of a credible quality assurance program, plus it also provides chemists and clinical chemists, medical and chemical researchers, and all scientists and managers the ideal means to ensure accurate and reliable work. Chapters are presented in a logical progression, starting with the concept of quality assurance, principles of good measurement, principles of quality assurance, and evaluation of measurement quality. Each chapter has a degree of independence so that it may be consulted separately from the others.

Spis treści

Preface -- CHAPTER 1. Introduction to Quality Assurance -- CHAPTER 2. Precision, Bias, and Accuracy -- Axioms -- Corollaries -- Sources of Error -- Errors of Rounding -- Influence of Uncertainty on Decision -- CHAPTER 3. Statistical Control -- CHAPTER 4. Statistical Techniques -- Basic Requirements -- Distributions -- Statistics of Measurements -- Estimation of Standard Deviation -- Estimation of Standard Deviation from Replicate -- Measurements -- Estimation of Standard Deviation from Duplicate -- Measurements -- Estimation of Standard Deviation from the Range -- Pooling Estimates of Standard Deviations -- The Analysis of Variance -- Do Two Estimates of Precision Differ? -- What are the Confidence Limits for an Estimate of a -- Standard Deviation? -- Confidence Interval for a Mean -- Does a Measured Value Differ from an Expected -- Value? -- Do the Means of Two Measured Values Disagree -- Significantly? -- Statistical Tolerance Intervals -- Pooling Means to Obtain a Grand Average -- Outliers -- Rejection for an Assignable Cause -- Rule of the Huge Error -- Statistical Tests -- Dixon Test for Outlying Observations -- Grubbs Test for Outlying Observations -- Youden Test for Outlying Laboratories -- Cochran Test for Extreme Values of Variance -- Statistics of Control Charts -- Control Limits -- Central Line Considerations -- Agreement With Established Value -- Has the Central Line Changed? -- Use of Random Number Tables -- CHAPTER 5. Chemical Analysis as a System -- Systematic Approach to Analysis -- Effective Problem Solving -- CHAPTER 6. The Model -- Importance of a Model -- Development of a Model -- Data Quality Objectives -- CHAPTER 7. Planning -- General Aspects of Planning -- Development of an Experimental Plan -- Content of a Measurement Plan -- CHAPTER 8. Principles of Sampling -- Initial Considerations -- Sampling Plan -- Peer Review -- Training -- Sample Management -- Problem of Subsampling -- Critical Matters Related to Samples -- Quality Assurance of Sampling -- Sample Uncertainties -- Stratification -- Holding Time -- Statistical Considerations in Sampling -- Measurement Situations -- Statistical Sampling Plan -- Basic Assumptions -- Guidance in Sampling -- Cost Considerations -- Minimum Size of Increments in a Well-Mixed -- Sample -- Size of Sample in Segregated Materials -- Acceptance Testing -- Matrix-Related Sampling Problems -- Sampling Gases -- Sampling Liquids -- Sampling Solids -- Sampling Multiphases -- CHAPTER 9. Principles of Measurement -- Terminology -- Measurement is a Comparison Process -- Principles of Chemical Measurement -- Figures of Merit -- Precision -- Sensitivity -- Limit of Detection and Limit of Quantitation -- Short-term and Long-term Standard Deviation -- Bias -- Selectivity -- Other Considerations -- Importance of an SOP -- Ruggedness Testing -- Standardization of Methods -- Selection of Appropriate Methodology -- Guidelines for Selecting Instrumentation -- Internal vs External Services -- CHAPTER 10. Principles of Calibration -- What Needs to be Calibrated -- Requirements for Calibration -- Frequency of Calibration -- Mode of Calibration -- Linear Relationships -- Tests for Linearity -- Calibration Uncertainties -- Intercalibration -- Additional Remarks -- CHAPTER 11. Principles of Quality Assurance -- CHAPTER 12. Principles of Quality Control -- Competence -- Suitable Facilities and Equipment -- Good Laboratory and Good Measurement Practices -- Standard Operations Procedures -- Distinction Between GLPs, GMPs, and SOPs -- Protocols for Specific Purposes -- Contents of a PSP -- Other Quality Control Techniques -- Inspection -- Documentation -- Training -- The Quality Control System -- CHAPTER 13. Blank Correction -- Sources of Blanks -- Control of Blanks -- Evaluation of Blanks -- Statistical Treatment of the Blank -- Significance -- CHAPTER 14. Control Charts -- Format -- Control Limits -- Evaluating Control Limits -- Control Samples -- Frequency of Control Measurements -- Identification of Population -- Strategy of Use -- Assignment of Uncertainty -- Range Control Charts -- Approach -- Use of Range Control Charts -- Sub span Range Control Charts -- Range Performance Charts -- Range Ratio Control Charts -- Collateral Control Charts -- Critical Collateral Measurement Control Charts -- Recovery Control Charts -- Other Useful Control Charts -- Additional Remarks -- Blinds vs Double Blinds -- CHAPTER 15. Principles of Quality Assessment -- Internal Techniques -- External Techniques -- Qualitative Identification -- Other Techniques -- CHAPTER 16. Evaluation Samples -- Prime Requirements -- Types of Evaluation Samples -- Liquid Samples -- Solid Samples -- Gas Samples -- Stability of Mixtures -- Subsampling -- Integrity of Evaluation Samples -- CHAPTER 17. Reference Materials -- Role of Reference Materials -- Uses of Reference Materials -- Certification of Reference Materials -- CHAPTER 18. Traceability -- Chemical Traceability -- Standards Prepared by the Analyst -- Standards Prepared by Others -- Physical Standards -- Reference Materials Produced by NBS -- Reference Materials Produced by Others -- Traceability of Analytical Results -- Concept of the National Measurement System -- CHAPTER 19. Quality Audits -- Internal Audits -- Internal Systems Audits -- Internal Performance Audits -- Mechanism -- Corrective Actions -- External Audits -- Independent Audits -- Forms -- Personal Quality Assurance Profile -- Laboratory Quality Assurance Profile -- Quality Assurance Survey -- Quality Assurance Practices Check List -- Quality Assurance Training Profile -- CHAPTER 20. Quality Circles -- Organization -- Objectives -- Operation -- Reporting -- Agenda -- CHAPTER 21. Validation -- Validation of Samples -- Validation of Methodology -- Validation of Data -- CHAPTER 22. Reporting Analytical Data -- Minimum Requirements -- Data Limitations -- Numerical Values -- Limits of Uncertainty for Data -- Significant Figures -- Guidelines for Reporting Results of Measurements -- Guidelines for Combining Data Sets -- Arbitrary Reporting Procedures -- Reporting Low-Level Data -- Report Format -- CHAPTER 23. An Improved Approach to Performance -- Testing -- Premises -- Advance Estimation of Precision -- Performance Testing Plan -- Diagnosis -- Feedback -- Consensus Values -- Statistical Treatment of Data -- CHAPTER 24. Correction of Errors and/or Improving -- Accuracy -- Identification of Problems -- Improvement of Performance -- Editing Data -- CHAPTER 25. Laboratory Evaluation -- Generic Guidelines for Evaluation -- Accreditation -- Self-Evaluation -- CHAPTER 26. The Quality Assurance Program -- Approaches to Quality Assurance -- Quality Assurance Policy -- Planning for Quality Assurance -- Development of a QA Program -- Quality Assurance Manual -- Federally Mandated Quality Assurance Programs -- Public Health Service -- Food & Drug Administration -- Environmental Protection Agency – Non federally Mandated Quality Assurance Programs -- Quality Assurance for Measurement Programs -- Relating Personnel to Quality Assurance -- Appendix A. Terminology Used in Quality Assurance -- Appendix B. Quality Assurance Program Documentation -- B. l Example Quality Assurance Program Document -- B.2 Outline for Use in Preparing an SOP for a -- Measurement Method -- B.3 Outline for Use in Preparing an SOP for -- Calibration -- B.4 Outline for Use in Preparing a GLP or GMP -- Appendix C. Statistical Tables -- C.l Use of Range to Estimate Standard Deviation -- C.2 Z-Factors for Two-Sided Confidence Intervals -- for the Normal Distribution -- C.3 Student t Distribution -- C.4 Factors for Computing Two-Sided Confidence -- Intervals for E. -- C.5 Factors for Computing Two-Sided Confidence -- Intervals for a Normal Distribution -- C.6 Critical Values for the F Test -- C. 7 Values for Use in the Dixon Test for Outliers -- C.8 Values for Use in the Grubbs Test for Outliers -- C.9 Values for Use in the Youden Test for Outliers -- C.10 Values for Use in the Cochran Test for Extreme -- Variance -- C.11 Short Table of Random Numbers -- Appendix D. Study Aids -- D. l Seventy-Five Terms Commonly Used in -- Discussing Quality Assurance -- D.2 Seventy-Five Top

O autorze

Taylor, John K.