Valid

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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 andSampling…………………………………………………….……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 Matrixeffects………………………………………………………………..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 experimentaldesigns……………………………………………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 ofdata……………………………………………..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

Appendix:Statistical Tables…………………………………………………..76 10. Selected Publications of AMC………………………………………………..78 References………………………………………………………………………….79 Subject Index……………………………………………………………………….83

Valid Analytical Methods and Procedures

1 Introduction
1.1 Historical perspective
The development of standard methods of analysis has been a prime objective of the Analytical Division of the Royal Society of Chemistryand its precursors, the Society of Public Analysts and the Society for Analytical Chemistry, since the earliest of days and the results of this work have been recorded in the pages of The Analyst since its inception in 1876. An ‘Analytical Investigation Scheme’ was proposed by A. Chaston Chapman in 1902. This later evolved into the Standing Committee on Uniformity of Analytical Methods and wascharged with developing standard chemicals and securing comparative analyses of these standard materials. In 1935, the Committee was renamed the Analytical Methods Committee (AMC) but the main analytical work was carried out by sub-committees composed of analysts with specialised knowledge of the particular application area. The earliest topics selected for study were milk products, essential oils,soap and the determination of metals in food colourants. Later applications included the determination of fluorine, crude fibre, total solids in tomato products, trade effluents and trace elements, and vitamins in animal feeding stuffs. These later topics led to the publication of standard methods in a separate booklet. All standard and recommended methods were collated and published in a volumeentitled Bibliography o Standard, Tentative and Recommended or f Recognised Methods o Analysis in 1951. This bibliography was expanded to f include full details of the method under the title Oficial, Standardised and Recommended Methods o Analysis in 1976 with a second edition in 1983 and a f third edition in 1994. The work of the AMC has continued largely unchanged over the years with new...
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