Trace Analysis -- Contents -- Chapter 1 Achieving Valid Trace Analysis -- 1.1 Introduction -- 1.1.1 What is Trace Analysis? -- 1.1.2 The Importance of Trace Analysis in Today's World -- 1.1.3 Difficulty of Achieving Reliable Trace Analysis -- 1.1.4 How Can the Reliability of Trace Analysis be Improved? -- 1.1.5 The Purpose and Structure of This Book -- 1.1.6 References -- 1.2 The Approach to Quality -- 1.2.1 Overview -- 1.2.2 Fitness for Purpose -- 1.2.3 The Resources for Trace Analysis -- 1.2.4 Laboratory Operations -- 1.2.5 Quality Control, Monitoring, and Auditing -- 1.2.6 References -- 1.3 The Approach to Trace Analysis -- 1.3.1 The Special Needs of Trace Analysis -- 1.3.2 The Structure of Trace Analysis Methods -- 1.3.3 Classification by Analyte and Matrix -- 1.3.4 Reference -- 1.4 Analytical Methodology -- 1.4.1 Terminology -- 1.4.2 Method Selection and Development -- 1.4.3 Method Validation -- 1.4.4 References -- Chapter 2 Sample Handling -- 2.1 Sample Storage and Stability -- 2.1.1 Introduction and Overview -- 2.1.2 Storage Conditions -- 2.1.3 Storage Containers -- 2.1.4 References -- 2.2 Sample Pre-treatment, Homogenisation, Sub-sampling, and Potential Sources of Contaminants -- 2.2.1 Introduction and Overview -- 2.2.2 Sample Pretreatment -- 2.2.3 Ensuring Homogeneity of the Bulk Material and Taking a Sub-sample -- 2.2.4 Sample Particle Size Reduction -- 2.2.5 Sample Reduction (Division) and Particle Size Separation (Sieving) -- 2.2.6 Sources of Contamination and Uncertainty -- 2.2.7 References -- Chapter 3 Inorganic Analytes: Sample Preparation -- 3.1 Introduction -- 3.1.1 Overview -- 3.1.2 Where Errors Occur -- 3.1.3 Precautions Against Errors -- 3.1.4 Choice of Acids -- 3.1.5 Handling Acids Safely -- 3.1.6 Reference -- 3.2 The Destruction of Organic Matrices -- 3.2.1 Overview -- 3.2.2 Comparison of Techniques.

3.2.3 General Precautions -- 3.2.4 Practical Advice -- 3.2.5 References -- 3.3 Decomposition and Dissolution of Inorganic Matrices and Residual Inorganic Material from Organic Matrices -- 3.3.1 Overview -- 3.3.2 Comparison of Techniques: Acid Decomposition -- 3.3.3 General Precautions -- 3.3.4 Critical Aspects -- 3.3.5 Uncertainty -- 3.3.6 References -- 3.4 Separation and Preconcentration in Inorganic Analysis -- 3.4.1 Overview -- 3.4.2 Comparison of Techniques -- 3.4.3 References -- Chapter 4 Inorganic Analytes: Determination -- 4.1 Introduction -- 4.1.1 Overview -- 4.1.2 Sample Presentation: the Form of the Matrix -- 4.1.3 The Analyte -- 4.1.4 Summary -- 4.2 Atomic Spectroscopy -- 4.2.1 Overview -- 4.2.2 Comparison of Techniques for Different Sample Types -- 4.2.3 Comparison of Techniques -- 4.2.4 Interferences and How to Deal with Them -- 4.2.5 Hints and Tips -- 4.2.6 Factors Affecting Quality -- 4.2.7 Safety Features -- 4.2.8 Applications -- 4.2.9 References -- 4.3 Elemental Mass Spectrometry -- 4.3.1 Overview -- 4.3.2 Comparison of Techniques -- 4.3.3 Physical and Spectral Interferences in ICP-MS -- 4.3.4 Modes of Sample Introduction -- 4.3.5 Modes of Data Acquisition in ICP-MS -- 4.3.6 Isotope Ratio and Isotope Dilution Analysis -- 4.3.7 Calculation of Elemental Concentration from Isotope Dilution Measurements -- 4.3.8 Analysis of Organic Samples by ICP-MS -- 4.3.9 Uncertainty (Errors) -- 4.3.10 Applications -- 4.3.11 References -- 4.4 The Chromatography of Ions -- 4.4.1 Introduction and Overview -- 4.4.2 Ion Separation Mechanisms -- 4.4.3 Methods of Detection -- 4.4.4 Critical Aspects -- 4.4.5 Practical Advice -- 4.4.6 References -- Chapter 5 Organic Analytes: Sample Preparation -- 5.1 Introduction to Planning and Preparation for Organic Analyses -- 5.1.1 Overview -- 5.1.2 Potential Difficulties with Organic Analyses.

5.1.3 Planning a Trace Organic Analysis -- 5.2 Methods of Extraction of Organic Analytes from Solid Samples -- 5.2.1 Overview -- 5.2.2 Choice of Extraction Technique -- 5.2.3 Choice of Solvent -- 5.2.4 Hints and Tips -- 5.2.5 Uncertainty Associated with Extraction -- 5.2.6 References -- 5.3 Methods of Extraction of Organic Analytes from Liquid Samples and Clean-up of Liquid Extracts -- 5.3.1 Overview -- 5.3.2 Comparison of Techniques -- 5.3.3 Critical Aspects and General Precautions -- 5.3.4 Hints and Tim -- 5.3.5 Associated Uncertainty -- 5.3.6 References -- 5.4 Concentration of Organic Extracts -- 5.4.1 Overview -- 5.4.2 Comparison of Techniques -- 5.4.3 Critical Aspects and General Precautions -- 5.4.4 Associated Uncertainty -- 5.4.5 References -- Chapter 6 Organic Analytes: Determination -- 6.1 Introduction to The Determination of Organic Analytes -- 6.1.1 Overview -- 6.1.2 Choice of Technique -- 6.2 Gas Chromatography -- 6.2.1 Overview -- 6.2.2 Comparison of Techniques -- 6.2.3 Gas Chromatographic Injection -- 6.2.4 Columns and Stationary Phases -- 6.2.5 Gas Chromatographic Detectors -- 6.2.6 Associated Uncertainty -- 6.2.7 References -- 6.3 High Performance Liquid Chromatography -- 6.3.1 Overview -- 6.3.2 Comparison of Techniques -- 6.3.3 Solvents and Mobile Phases -- 6.3.4 Practical Advice -- 6.3.5 Hints and Tips -- 6.3.6 Associated Uncertainty -- 6.3.7 References -- 6.4 Thin Layer Chromatography -- 6.4. I Overview -- 6.4.2 Comparison of Techniques, General Precautions, and Critical Aspects -- 6.4.3 References -- 6.5 Organic Mass Spectrometry -- 6.5.1 Overview -- 6.5.2 Comparison of Mass Spectrometers -- 6.5.3 Methods of Introducing the Sample into the Mass Spectrometer -- 6.5.4 Ionisation Techniques -- 6.5.5 Scanning Modes -- 6.5.6 Tandem Techniques -- 6.5.7 General Precautions -- 6.5.8 Critical Aspects -- 6.5.9 Hints and Tips.

6.5.10 Uncertainty in Identification -- 6.5.11 Uncertainty in Quantitation -- 6.5.12 Applications -- 6.5.13 References -- 6.6 Isotope Dilution Mass Spectrometry (IDMS) -- 6.6.1 Overview -- 6.6.2 Comparison of Techniques -- 6.6.3 General Precautions -- 6.6.4 Critical Factors -- 6.6.5 Hints and Tips -- 6.6.6 Uncertainty -- 6.6.7 Applications -- 6.6.8 References -- Chapter 7 The Analysis of Speciated Elements -- 7.1 Introduction -- 7.2 Extraction of the Analyte and Preparation of a Test Solution -- 7.3 Comparison of Determination Techniques -- 7.3.1 Separation Methods -- 7.3.2 Methods of Detection -- 7.4 Critical Factors when using Coupled Techniques -- 7.4.1 Length of Transfer Lines when Coupling to LC Systems -- 7.4.2 Use of the Correct Nebuliser -- 7.4.3 The Spray Chamber -- 7.4.4 Coupling Lines for GC -- 7.4.5 Mass Spectrometer Cones and Lens Stacks -- 7.4.6 The Use of Organic Solvents -- 7.5 General Precautions and Tips -- 7.6 References -- Chapter 8 Techniques Suitable for Both Inorganic and Organic Analytes -- 8.1 Absorption and Emission of Ultraviolet and Visible Radiation -- 8.1.1 Overview -- 8.1.2 Scope of UV/Visible Absorption Spectrophotometry -- 8.1.3 Quantitative Applications of UV/Visible Spectrophotometry -- 8.1.4 Photoluminescence and Chemiluminescence -- 8.1.5 UV/Visible Absorption Spectrophotometry in Practice -- 8.1.6 Colorimetric Procedures -- 8.1.7 Photoluminescence and Chemiluminescence Analyses -- 8.1.8 Checking and Maintaining Instrument Performance -- 8.1.9 References -- 8.2 Electrochemical Techniques -- 8.2.1 Overview -- 8.2.2 Potentiometric Methods -- 8.2.3 Potentiometric Techniques: Hints and Tips -- 8.2.4 Voltammetric Methods -- 8.2.5 Stripping Voltammetry -- 8.2.6 Pulsed Voltammetry -- 8.2.7 Voltammetry: Hints and Tips -- 8.2.8 Bioelectroanalysis -- 8.2.9 References -- 8.3 Bioanalytical Techniques -- 8.3.1 Overview.

8.3.2 Enzyme/Subtrate Reactions -- 8.3.3 Immunoassays -- 8.3.4 DNA Analysis -- 8.3.5 References -- Chapter 9 From Signal Processing to Reporting -- 9.1 Signal Processing -- 9.1.1 Overview -- 9.1.2 Good Automated Laboratory Practice (GALP) -- 9.1.3 Signal Integrity -- 9.1.4 Spectroscopic Signals -- 9.1.5 Chromatographic Signals -- 9.1.6 References -- 9.2 Data Handling -- 9.2.1 Overview -- 9.2.2 Statistical Methods -- 9.2.3 Measurement Uncertainty -- 9.2.4 Sources of Uncertainty -- 9.2.5 References -- 9.3 Reporting of Results -- 9.3.1 Overview -- 9.3.2 Customer Requirements -- 9.3.3 References -- Appendix 1: Some Frequently Used Acronyms and Technical Abbreviations -- Appendix 2: Some Sources of Reference Materials -- Subject Index.