1. Introduction………………….…………………………………………………..1 1.1 Historical perspective…………………………………………………………1 1.2 Overview of the handbook……………………………………………………2 1.3 Purpose and scope…………………………………………………………….2 2. Nomenclature : Terms and Parameters………………………………………..6 2.1 Introduction……………………………………………………………………6 2.2 Terms………………………………………………………………………….6 2.3 Parameters……………………………………………………………………..9 3 Samples and Sampling…………………………………………………….……15 3.1 Introduction ………………………………………………………………….15 3.2 What is a sample?……………………………………………………………15 3.3 Homogeneity and concentration ranges……………………………………...17 4. Method Selection………………………………………………………………..17 4.1 Fitness for purpose………………………………………………………..…17 4.2 Sources and strategies……………………………………………………….18 4.3 Sampling considerations…………………………………………………….19 4.4 Matrix effects………………………………………………………………..19 5 Equipment Calibration and Qualification……………...……………………...20 5.1 Qualification approaches…………………………………………………….20 5.2 A convergence of ideas………………………………………………………23 6 The mthod Development Process………………………………………………24 6.1 Mapping the analytical process and determining the key factors……………26 6.2 Simple experimental design………………………………………………….27 6.3 Multifactor experimental designs……………………………………………36 7 Method Validation………………………………………………………………37 7.1 Recommended best practice for method validation………………………….37 7.2 Describing and writing analytical methods…………………………………..39 8 Data Evaluation, Transformation and Reporting………………………….....42 8.1 Exploratory data analysis……………………………………………………43 8.2 Linear calibration models……………………………………………………48 8.3 Recording and reporting of data……………………………………………..55 9 Technology Transfer…………………………………………………………….57 9.1 Performance expectations and acceptance criteria…………………………...57 9.2 Transfer of published methods into a single laboratory………………………59 9.3 Comparison of two methods………………………………………………….60 9.4 Restricted inter-laboratory trials……………………………………………...66 9.5 Full collaborative trials……………………………………………………….69

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