CONTENTS PART 1 - MINERALOGICAL ANALYSIS. CHAPTER 1 Water Content and Loss on Ignition. CHAPTER 2 Particle Size Analysis

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1 CONTENTS PART 1 - MINERALOGICAL ANALYSIS CHAPTER 1 Water Content and Loss on Ignition 1.1 Introduction Water Content at 105 C (H 2 O ) Principle Materials Sample Procedure Remarks Loss on Ignition at 1,000 C (H 2 O + ) Introduction Principle Equipment Procedure Calculations Remarks...12 Bibliography...12 CHAPTER 2 Particle Size Analysis 2.1 Introduction Particle Size in Soil Science Principle Law of Sedimentation Conditions for Application of Stokes Law Standard Methods Pretreatment of the Sample Particle Suspension and Dispersion Pipette Method after Robinson-Köhn or Andreasen Density Method with Variable Depth Density Method with Constant Depth Particle Size Analysis of Sands Only Automated Equipment Introduction Method Using Sedimentation by Simple Gravity Methods Using Accelerated Sedimentation Methods Using Laser Scattering and Diffraction Methods Using Optical and Electric Properties Methods Allowing Direct Observations of the Particles Methods Using Conductivity...56 References...56 Bibliography...58 Generality...58

2 VIII Contents Pre-treatment...58 Pipette Method...61 Hydrometer Method...62 Instrumental Methods...62 CHAPTER 3 Fractionation of the Colloidal Systems 3.1 Introduction Fractionation by Continuous Centrifugation Principle Theory Equipment and reagents Procedure Pretreatment of the Extracted Phases...79 References...81 Bibliography...81 CHAPTER 4 Mineralogical Characterisations by X-Ray Diffractometry 4.1 Introduction X-Ray Diffraction and Mineralogy Principle XRD Instrumentation Qualitative Diffractometry Overview of Preparation of the Samples Preparation for Powder Diagrams Preparation for Oriented Diagrams Pretreatment of Clays Qualitative Diffractometry Quantitative Mineralogical Analysis Interest Quantitative Mineralogical Analysis by XRD Multi-Instrumental Quantitative Mineralogical Analysis References Bibliography General Preparation of Oriented Aggregates on Porous Ceramic Plate Saturation of Clays by Cations Saturation, Solvation, Intercalation Complex, Dissolution Preparation of Iron Oxides Quantitative XRD CHAPTER 5 Mineralogical Analysis by Infra-Red Spectrometry 5.1 Introduction Principle IR Instrumentation IR Spectrometry in Mineralogy Equipment and Products Preparation of the Samples Brief Guide to Interpretation of the Spectra Quantitative Analysis...152

3 Contents IX 5.3 Other IR Techniques Near-infrared Spectrometry (NIRS) Coupling Thermal Measurements and FTIR Spectrometry of Volatile Products Infrared Microscopy Raman Scattering Spectroscopy References Chronobibliography CHAPTER 6 Mineralogical Separation by Selective Dissolution 6.1 Introduction Crystallinity of Clay Minerals Instrumental and Chemical Methods Selective Dissolution Methods Reagents and Synthetic Standards Main Selective Dissolution Methods Acid Oxalate Method Under Darkness (AOD) Dithionite-Citrate-Bicarbonate Method (DCB) EDTA Method Pyrophosphate Method Extraction in Strongly Alkaline Mediums Other Methods, Improvements and Choices Differential Sequential Methods Selective Methods for Amorphous Products Brief Overview to the Use of the Differential Methods References CHAPTER 7 Thermal Analysis 7.1 Introduction Definition Interest Classical Methods Thermogravimetric Analysis Differential Thermal Analysis and Differential Scanning Calorimetry Multi-component Apparatuses for Thermal Analysis Concepts Coupling Thermal Analysis and Evolved Gas Analysis References Chronobibliography CHAPTER 8 Microscopic Analysis 8.1 Introduction Preparation of the Samples Interest Coating and Impregnation, Thin Sections Grids and Replicas for Transmission Electron Microscopy Mounting the Samples for Scanning Electron Microscopy Surface Treatment (Shadowing, Flash-carbon, Metallization)

4 X Contents 8.3 Microscope Studies Optical Microscopy Electron Microscopy, General Information Transmission Electron Microscopy, Micro-diffraction Scanning Electron Microscopy Ultimate Micro-analysis by X-Ray Spectrometry References Chronobibliography PART 2 - ORGANIC ANALYSIS CHAPTER 9 Physical Fractionation of Organic Matter 9.1 Principle and Limitations Forms of Organic Matter in Soil Principle Difficulties Methods Classification Extraction of Plant Roots Dispersion of the Particles Separation by Density Particle Size Fractionations Precision of the Fractionation Methods Conclusion and Outlook References CHAPTER 10 Organic and Total C, N (H, O, S) Analysis 10.1 Introduction Soil Organic Matter Sampling, Preparation of the Samples, Analytical Significance Wet Methods Total Carbon: General Information Organic Carbon by Wet Oxidation at the Temperature of Reaction Organic Carbon by Wet Oxidation at Controlled Temperature Organic Carbon by Wet Oxidation and Spectrocolorimetry Total Nitrogen by Wet Method: Introduction Total Nitrogen by Kjeldahl Method and Titrimetry Kjeldahl N, Titration by Spectrocolorimetry Kjeldahl N, Titration by Selective Electrode Mechanization and Automation of the Kjeldahl Method Modified Procedures for NO 3, NO 2 and Fixed N Dry Methods Total Carbon by Simple Volatilization Simultaneous Instrumental Analysis by Dry Combustion: CHN(OS) CHNOS by Thermal Analysis...362

5 Contents XI C and N Non-Destructive Instrumental Analysis Simultaneous Analysis of the Different C and N Isotopes References Bibliography CHAPTER 11 Quantification of Humic Compounds 11.1 Humus in Soils Definitions Role in the Soil and Environment Extractions Main Techniques Extraction Quantification of the Extracts Precision and Correspondence of the Extraction Methods Purification of Humic Materials Further Alternatives and Complements Methods Alternative Method of Extraction Fractionation of the Humin Residue References Humic Materials Extraction, Titration, Purification and Fractionation of Humic Materials CHAPTER 12 Characterization of Humic Compounds 12.1 Introduction Mechanisms of Formation Molecular Structure Classical Techniques Fractionation of Humic Compounds Titration of the Main Functional Groups UV Visible Spectrometry Infra-Red Spectrography Complementary Techniques Improvements in Fractionation Technologies Titration of Functional Groups Characterization by Fragmentation Nuclear Magnetic Resonance (NMR) Fluorescence Spectroscopy Electron Spin Resonance (ESR) Spectroscopy Measurement of Molecular Weight and Molecular Size Microscopic Observations Other Techniques References Molecular Models Fractionation, Determination of Molecular Weights and Molecular Sizes Functional Group of Humic Compounds Spectrometric Characterizations UV Visible, IR, Fluorescence, ESR Spectrometries Nuclear Magnetic Resonance

6 XII Contents Methods of Characterization by Fragmentation Other Methods (Microscopy, X-ray, Electrochemistry, etc.) CHAPTER 13 Measurement of Non-Humic Molecules 13.1 Introduction Non-Humic Molecules Soil Carbohydrates Soil Lipids Pesticides and Pollutants Classical Techniques Acid Hydrolysis of Polysaccharides Purification of Acid Hydrolysates Colorimetric Titration of Sugars Titration of Sugars by Gas Chromatography Quantification of Total Lipids Quantification of the Water-Soluble Organics Complementary Techniques Carbohydrates by Gas Chromatography Carbohydrates by Liquid Chromatography Fractionation and Study of the Soil Lipid Fraction Measurement of Pesticide Residues and Pollutants References Soil Carbohydrates Soil Lipids Aqueous Extract Pesticides and Pollutants CHAPTER 14 Organic Forms of Nitrogen, Mineralizable Nitrogen (and Carbon) 14.1 Introduction The Nitrogen Cycle Types of Methods Classical Methods Forms of Organic Nitrogen Released by Acid Hydrolysis Organic Forms of Nitrogen: Simplified Method Urea Titration Potentially Available Nitrogen: Biological Methods Potentially Mineralizable Nitrogen: Chemical Methods Kinetics of Mineralization Complementary Methods Alternative Procedures for Acid Hydrolysis Determination of Amino Acids Determination of Amino Sugars Proteins and Glycoproteins (glomalin) Potentially Mineralizable Nitrogen by EUF...538

7 Contents XIII References Organic Nitrogen Forms: General Articles Nitrogen Forms by Acid Hydrolysis and Distillation Improvement of Acid Hydrolysis Determination of Amino Acids Determination of Amino Sugars Glomalin Urea Titration Potentially Mineralizable Nitrogen: General Papers Potentially Mineralizable Nitrogen: Biological Methods Potentially Mineralizable Nitrogen: Chemical Methods Potentially Mineralizable Nitrogen by EUF Mineralization Kinetics PART 3 - INORGANIC ANALYSIS Exchangeable and Total Elements CHAPTER 15 ph Measurement 15.1 Introduction Soil ph Difficulties Theoretical Aspects Classical Measurements Methods Colorimetric Method Electrometric Method Electrometric Checking and Calibration Measurement on Aqueous Soil Suspensions Determination of the ph-k and ph-ca Measurement on Saturated Pastes Measurement on the Saturation Extract Measurement of the ph-naf In Situ Measurements Equipment Installation in the Field Measurement on Soil Monoliths References Bibliography Appendix Appendix 1: Table of Electrode Potentials Appendix 2: Constants of Dissociation of Certain Equilibriums Appendix 3: Buffer Solutions Appendix 4: Coloured Indicators CHAPTER 16 Redox Potential 16.1 Definitions and Principle Equipment and Reagents Electrodes Salt Bridge for Connection System of Measurement Calibration Solutions

8 XIV Contents 16.3 Procedure Pretreatment of the Electrode Measurement on Soil Sample Measurement on Soil Monolith In Situ Measurements Measurement of Oxygen Diffusion Rate Colorimetric Test of Eh References Bibliography CHAPTER 17 Carbonates 17.1 Introduction Measurement of Total Carbonates Introduction Volumetric Measurement by Calcimetry Acidimetry Titration of Active Carbonate Principle Implementation Index of Chlorosis Potential References CHAPTER 18 Soluble Salts 18.1 Introduction Extraction Soil/solution Ratio Extraction of Saturated Paste Diluted Extracts In Situ Sampling of the Soil Water Extracts with Hot Water Measurement and Titration Electrical Conductivity of Extracts In Situ Conductivity Total Dissolved Solid Material Soluble Cations Extractable Carbonate and Bicarbonate (Alkalinity) Extractable Chloride Extractable Sulphate, Nitrate and Phosphate Extractable Boron Titration of Extractable Anions by Ionic Chromatography Expression of the Results References CHAPTER 19 Exchange Complex 19.1 Introduction Origin of Charges Ionic Exchange...630

9 Contents XV Exchange Complex Theory References Chronobibliography CHAPTER 20 Isoelectric and Zero Charge Points 20.1 Introduction Charges of Colloids Definitions Conditions for the Measurement of Charge Main Methods Measurement of ph0 (PZSE), Long Equilibrium Time Point of Zero Salt Effect (PZSE), Short Equilibrium Time References CHAPTER 21 Permanent and Variable Charges 21.1 Introduction Main Methods Measurement of Variable Charges Determination of Permanent Charges References Bibliography CHAPTER 22 Exchangeable Cations 22.1 Introduction Exchangeable Cations of Soil Extracting Reagents Equipment Ammonium Acetate Method at ph Principle Procedure Automated Continuous Extraction References Bibliography CHAPTER 23 Exchangeable Acidity 23.1 Introduction Origin of Acidity Aims of the Analysis Method Principle Reagents Procedure Other Methods References Chronobibliography

10 XVI Contents CHAPTER 24 Lime Requirement 24.1 Introduction Correction of Soil Acidity Calculation of Correction SMP Buffer Method Principle Reagents Procedure Remarks References Chronobibliography CHAPTER 25 Exchange Selectivity, Cation Exchange Isotherm 25.1 Introduction Determination of the Exchange Isotherm Principle Reagents Procedure Remarks References Chronobibliography CHAPTER 26 Cation Exchange Capacity 26.1 Introduction Theoretical Aspects Variables that Influence the Determination of CEC Determination of Effective CEC by Summation (ECEC) Principle Alternative Methods CEC Measurement at Soil ph in Not-Buffered Medium Principle Methods Using Not-Buffered Metallic Salts Procedure Using Not-Buffered Organo Metallic Cations Not-Buffered Methods Using Organic Cations CEC Measurement in Buffered Medium Buffered Methods General Information Ammonium Acetate Method at ph Buffered Methods at ph Buffered Methods at Different ph References Bibliography CEC General Theory Barium Method at soil ph Buffered Method at ph Cobaltihexamine CEC Silver-Thiourea CEC with Organic Cations (Coloured Reagents) Buffered Methods at ph Barium Chloride-Triethanolamine at ph

11 Contents XVII CHAPTER 27 Anion Exchange Capacity 27.1 Theory Measurement Principle Method Simultaneous Measurement of AEC, EC, CEC and net CEC Aim Description References CHAPTER 28 Inorganic Forms of Nitrogen 28.1 Introduction Ammonium, Nitrate and Nitrite Sampling Problems Analytical Problems Usual Methods Extraction of Exchangeable Forms Separation by Micro-Diffusion Colorimetric Titration of Ammonium Colorimetric Titration of Nitrites Colorimetric Titration of Nitrates Extracted Organic Nitrogen Other Methods Nitrate and Nitrite by Photometric UV Absorption Ammonium Titration Using a Selective Electrode Measurement of Nitrates with an Ion-Selective Electrode In situ Measurement Non-Exchangeable Ammonium References Bibliography CHAPTER 29 Phosphorus 29.1 Introduction Total Soil Phosphorus Introduction Wet Mineralization for Total Analyses Dry Mineralization Fractionation of Different Forms of Phosphorus Introduction Sequential Methods Selective Extractions Availability Indices Isotopic Dilution Methods Determination of Organic Phosphorus Retention of Phosphorus Introduction Determination of P Retention

12 XVIII Contents 29.5 Titration of P in the Extracts Introduction Titration of Ortho-phosphoric P by Spectrocolorimetry P Titration by Atomic Spectrometry Titration of Different Forms of P by 31 P NMR Separation of P Compounds by Liquid Chromatography Direct Speciation of P in situ, or on Extracted Particles References Chronobibliography CHAPTER 30 Sulphur 30.1 Introduction Sulphur Compounds Mineralogical Studies Total Sulphur and Sulphur Compounds Characteristics of Fluviomarine Soils Soil Sampling and Sample Preparation Testing for Soluble Sulphur Forms Titration of Total Sulphur Total S Solubilisation by Alkaline Oxidizing Fusion Total Solubilisation by Sodium Hypobromite in Alkaline Medium S titration with Methylen Blue Colorimetry Sulphate Titration by Colorimetry with Methyl Thymol Blue Total Sulphur by Automated Dry CHN(OS) Ultimate Analysis Titration of Total SO 2 4 -S by Ionic Chromatography Total S Titration by Plasma Emission Spectrometry Titration by X-ray Fluorescence Titration by Atomic Absorption Spectrometry Analytical Fractionation of Sulphur Compounds Titration of Organic S bound to C Titration of Organic S not bound to C Extraction and Titration of Soluble Sulphides Titration of Sulphur in Pyrites Titration of Elementary Sulphur Titration of Water Soluble Sulphates Titration of Na 3 -EDTA Extractable Sulphates Titration of Jarosite Sequential Analysis of S Forms Sulphur of Gypseous Soils Gypseous Soils Preliminary Tests Extraction and Titration from Multiple Extracts Gypsum Determination by Acetone Precipitation Sulphur and Gypsum Requirement of Soil Introduction Plant Sulphur Requirement Gypsum Requirement References Chronobibliography...890

13 Contents XIX CHAPTER 31 Analysis of Extractable and Total Elements 31.1 Elements of Soils Major Elements Trace Elements and Pollutants Biogenic and Toxic Elements Analysis of Total Elements Extractable Elements Methods using Solubilization Total Solubilization Methods Mean Reagents for Complete Dissolutions Acid Attack in Open Vessel Acid Attack in Closed Vessel Microwave Mineralization Alkaline Fusion Selective Extractions Measurement Methods Spectrocolorimetric Analysis Analysis by Flame Atomic Emission Spectrometry Analysis by Flame Atomic Absorption Spectrometry Analysis of Trace Elements by Hydride and Cold Vapour AAS Analysis of Trace Elements by Electrothermal AAS Analysis by Inductively Coupled Plasma-AES Analysis by Inductively Coupled Plasma-Mass Spectrometry Analysis on Solid Medium Method X-ray Fluorescence Analysis Neutron Activation Analysis References INDEX PERIODIC TABLE OF THE ELEMENTS...993

Marc Pansu Jacques Gautheyrou Handbook of Soil Analysis Mineralogical, Organic and Inorganic Methods

Marc Pansu Jacques Gautheyrou Handbook of Soil Analysis Mineralogical, Organic and Inorganic Methods Marc Pansu Jacques Gautheyrou Handbook of Soil Analysis Mineralogical, Organic and Inorganic Methods