Methodologies In Soil And Sediment Fractionation Studies -- Contents -- Chapter 1 SM&T Activities in Support of Standardisation of Operationally-defined Extraction Procedures for Soil and Sediment Analysis -- 1.1 Introduction -- 1.2 Standardisation -- 1.3 SM&T Activities for the Harmonisation of Extraction Schemes -- 1.4 The Variety of Extraction Methods and the Need for Harmonisation -- 1.5 Trends and Conclusions -- 1.6 References -- Chapter 2 Sequential Extraction Procedures for Sediment Analysis -- 2.1 Introduction -- 2.1.1 Commonly Used Sequential Extraction Procedures for Sediments -- 2.2 Preliminary Studies within BCR -- 2.3 Proposal for a Common Three-step Sequential Extraction Scheme -- 2.4 Improvement of the BCR Sequential Extraction Scheme -- 2.4.1 New Sediment Certified Reference Material for Extractable Metal Contents -- 2.4.2 Recent Applications of the Modified BCR Sequential Extraction Scheme -- 2.5 Conclusions and Further Developments -- 2.6 References -- Chapter 3 Extraction Procedures for Soil Analysis -- 3.1 Introduction -- 3.1.1 Single Extraction Procedures -- 3.1.2 Sequential Extraction Procedures -- 3.2 Preliminary Studies -- 3.2.1 Stability of Soil Extractable Contents by Single Extractants -- 3.2.2 Effect of Speed of Rotation of Mechanical Shaker -- 3.3 First Interlaboratory Studies -- 3.3.1 The Participants in the Working Group -- 3.3.2 Preparation and Characterisation of the First Test Material -- 3.3.2.1 Sample Preparation -- 3.3.2.2 Homogeneity Testing -- 3.3.2.3 Temporal Stability of Soil Extractable Contents -- 3.3.3 Extraction Procedures for the First InterlaboratoryTrials -- 3.3.4 Results of the First Interlaboratory Trial -- 3.3.5 Second Interlaboratory Trial on Calcareous Soil -- 3.3.5.1 Selection of Extractants -- 3.3.5.2 Interlaboratory Study on Calcareous Soil.

3.3.6 Conclusions of the First Interlaboratory Trials -- 3.4 Certification of Soil Reference Materials -- 3.4.1 Preparation of the Reference Materials -- 3.4.1.1 CRM 483 -- 3.4.1.2 CRM 484 -- 3.4.1.3 CRM 600 -- 3.4.1.4 BCR 700 -- 3.4.2 Homogeneity Studies -- 3.4.3 Stability Studies -- 3.4.4 Analytical Methods Used in the Certification -- 3.4.5 Technical Discussion -- 3.4.5.1 EDTA Extracts -- 3.4.5.2 Acetic Acid Extracts -- 3.4.5.3 DTPA Extracts -- 3.4.6 Certified Values -- 3.4.7 Indicative Values -- 3.5 Conclusions -- 3.6 References -- Appendix 1 Extraction Protocols -- Chapter 4 Sequential Extraction Procedures for the Characterisation of the Fractionation of Elements in Industrially-contaminated Soils -- 4.1 Introduction -- 4.2 Literature Search -- 4.2.1 Definitions and Problems -- 4.2.2 Methodologies -- 4.2.2.1 Case of Elements Giving Cationic Species -- 4.2.2.2 Case of Elements Giving Anionic Species -- 4.2.3 Conclusion -- 4.3 Experimental Study -- 4.3.1 Presentation of the Samples Studied -- 4.3.2 Application of Classical Sequential Extraction Schemes -- 4.3.2.1 Study of Elements Giving Cationic Species: Lead and Copper -- 4.3.2.2 Study of Elements Giving Anionic Species: Arsenic -- 4.3.2.3 Conclusion -- 4.3.3 Comparison of Different Reducing Agents -- 4.3.3.1 Extraction with TiCl3 -- 4.3.3.2 Extraction with Thioglycolic Acid (TGA) -- 4.3.3.3 Extraction with Ascorbic Acid (AA) -- 4.3.3.4 Conclusions -- 4.3.4 Elaboration of Simple Fraction Schemes for the Evaluation of the Risks of Pollutant Mobilisation from Industrial and Mining Site Soils -- 4.3.4.1 Simple Fractionation Scheme Specific for Elements Giving Cationic Species in IPS -- 4.3.4.2 Simple Fractionation Scheme Specific to Arsenic (Anionic Elements) -- 4.3.4.3 Application to a Certified Reference Sediment and Speciation Study -- 4.3.4.4 The Case of a Multiple Pollution -- 4.4 Conclusions.

4.5 References -- Appendix 2 Sequential Extraction Procedures -- Appendix 3 Single Extractions -- Appendix 4 Simplified Schemes -- Chapter 5 Sequential Extraction Procedures for Phosphorus Forms in Lake Sediment -- 5.1 Introduction -- 5.2 Selection of Sequential Extraction Procedures -- 5.3 Interlaboratory Study -- 5.3.1 Samples and Analytical Techniques Used in the Interlaboratory Study -- 5.3.2 Discussion of the Results of the First Trial -- 5.3.2.1 Williams Method -- 5.3.2.2 Golterman Method -- 5.3.2.3 Hieltjes-Lijklema Method -- 5.3.2.4 Ruttenberg Method -- 5.3.3 Reasons for Adopting the Williams Extraction Scheme -- 5.3.4 Discussion of the Results of the Second Trial -- 5.4 Certification Campaign -- 5.4.1 Preparation and Characterisation of the Reference Material -- 5.4.2 Homogeneity and Stability Studies -- 5.4.2.1 Homogeneity Study -- 5.4.2.2 Stability Study -- 5.4.3 Technical Discussion -- 5.4.3.1 General Comments -- 5.4.3.2 Results of the Trial -- 5.5 Conclusions -- 5.6 References -- Appendix 5 SMT-Protocol for Phosphorus Sequential Extraction in Fresh Water Sediments -- Chapter 6 Leaching Procedure for the Availability of Polycyclic Aromatic Hydrocarbons (PAHs) in Contaminated Soils and Waste Materials -- 6.1 Introduction -- 6.2 Materials and Methods -- 6.2.1 Materials -- 6.2.2 Extraction and Analysis of PAHs -- 6.2.2.1 Method 1: C18 Solid Phase Extraction +HPLC -- 6.2.2.2 Method 2: Liquid/Liquid Extraction with DCM + Optimised HPLC -- 6.2.3 pH-Static Leaching -- 6.2.4 Soxhlet Extraction -- 6.2.5 DOC-Flocculation -- 6.2.6 Development of the 'Availability' Leaching Test -- 6.3 Results -- 6.3.1 Total PAH Content in the Soil and Waste Materials -- 6.3.2 pH-Stat Leaching -- 6.3.4 DOC-Flocculation Experiment with OF-MSW Leachates -- 6.3.5 Relevant Properties of DOC.

6.4 Evaluation of Leaching Processes and Development of 'Availability' Leaching Test -- 6.4.1 Role of DOC in the Leaching of PAHs -- 6.4.2 Development of an 'Availability' Leaching Test -- 6.5 Conclusions -- 6.5.1 Leaching Process of PAHs -- 6.5.2 'Availability' Leaching Test -- 6.6 Acknowledgements -- 6.7 References -- Chapter 7 Harmonisation of Leaching/Extraction Procedures for Sludge, Compost, Soil and Sediment Analyses -- 7.1 Introduction -- 7.2 Scenario Approaches versus Arbitrary Approaches of Assessment -- 7.3 Total Composition versus Leaching Behaviour -- 7.4 Release Controlling Factors -- 7.5 Test Methods and Recent Developments in Standardisation -- 7.5.1 Hierarchy in Testing -- 7.5.2 Characterisation of Leaching Behaviour -- 7.5.3 Comparison of Test Methods -- 7.5.4 Quality Control System -- 7.5.5 Prediction of Release under Different Exposure Conditions -- 7.5.6 Standardisation Issues -- 7.6 Modelling of Chemical Speciation and Modelling Release -- 7.6.1 Geochemical Modelling -- 7.6.2 Modelling of Metal Organic Matter Interactions -- 7.7 Comparison of Sewage Sludge-amended Soils and Sewage Sludges -- 7.8 Judgement of Test Results and Regulatory Developments -- 7.9 Conclusions -- 7.10 References -- Laboratories Participating in the Various Reference Material Certification Studies -- Subject Index.