电子书《Trace Quantitative Analysis by Mass Spectrometry》
Robert K. Boyd
National Research Council, Ottawa, Canada
Cecilia Basic
Basic Mass Spec., Winnipeg, Canada
Robert A. Bethem
Alta Analytical Laboratory, El Dorado Hills, CA, USA
Contents
Preface xvii
Acknowledgements xxiii
1 Measurement, Dimensions and Units 1
1.1 Introduction 1
1.2 The International System of Units (SI) 3
1.3 ‘Mass-to-Charge Ratio’ in Mass Spectrometry 6
1.4 Achievable Precision in Measurement of SI Base Quantities 9
1.5 Molecular Mass Limit for Trace Quantitation by Mass Spectrometry 11
1.6 Summary of Key Concepts 14
2 Tools of the Trade I. The Classical Tools 17
2.1 Introduction 17
2.2 Analytical and Internal Standards: Reference Materials 18
2.2.1 Analytical Standard (Reference Standard) and its Traceability 18
2.2.2 Certified (Standard) Reference Materials (CRMs) 20
2.2.3 Surrogate Internal Standard (SIS) 21
2.2.4 Volumetric Internal Standard (VIS) 25
2.3 The Analytical Balance 25
2.3.1 Balance Calibration 27
2.3.2 Sources of Uncertainty in Weighing 27
2.3.3 Weighing the Analytical Standard 31
2.4 Measurement and Dispensing of Volume 32
2.4.1 Standard Volumetric Flasks 32
2.4.2 Pipets 33
2.4.2a Classical Pipets 33
2.4.2b Micropipets 33
2.4.3 Loop Injectors for High Performance Liquid Chromatography (HPLC) 35
2.4.4 Syringes 38
2.5 Preparation of Solutions for Calibration 39
2.5.1 Matrix-Free Calibration Solutions 40
2.5.2 Matrix Matched Calibrators 40
2.5.3 Quality Control (QC) Samples 41
2.5.3a QCs in Method Development and Validation 41
2.5.3b QCs in Sample Analysis 41
2.6 Introduction to Calibration Methods for Quantitative Analysis 42
2.6.1 Calibration Using an External Standard 42
2.6.2 Calibration for the Method of Standard Additions 44
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