Handbook of Soil Analysis

Mineralogical, Organic and Inorganic Methods

By: Marc Pansu, Jacques Gautheyrou

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Hardcover | 8 May 2006

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1016 Pages

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This new book by Marc Pansu and Jacques Gautheyrou provides a synopsis of the analytical procedures for the physicochemical analysis of soils. It is written to conform to analytical standards and quality control. It focuses on mineralogical, organic and inorganic analyses, but also describes physical methods when these are a precondition for analysis. It will help a range of different users to choose the most appropriate method for the type of material and the particular problems they have to face. The compiled work is the product of the experience gained by the authors in the laboratories of the Institute of Research for Development (IRD) in France and in tropical countries, and includes an extensive review of the literature. The reference section at the end of each chapter lists source data from pioneer studies right up to current works, such as, proposals for structural models of humic molecules, and itself represents a valuable source of information.

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You Can Find This Book In

Non-Fiction Engineering & Technology Agriculture & Farming Agricultural Science Earth Sciences, Geography, Environment, Planning Earth Sciences Geology & The Lithosphere Soil Science Science Chemistry Mineralogy & Gems Geography

Biogeography Sociology & Anthropology Anthropology

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Published: 23rd August 2016

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Mineralogical Analysis
Water Content and Loss on Ignition
Introduction	p. 3
Water Content at 105[degree]C (H[subscript 2]O[superscript -])	p. 6
Principle	p. 6
Materials	p. 6
Sample	p. 6
Procedure	p. 7
Remarks	p. 7
Loss on Ignition at 1,000[degree]C (H[subscript 2]0[superscript +])	p. 8
Introduction	p. 8
Principle	p. 11
Equipment	p. 11
Procedure	p. 11
Calculations	p. 12
Remarks	p. 12
Bibliography	p. 12
Particle Size Analysis
Introduction	p. 15
Particle Size in Soil Science	p. 15
Principle	p. 17
Law of Sedimentation	p. 18
Conditions for Application of Stokes Law	p. 24
Standard Methods	p. 26
Pretreatment of the Sample	p. 26
Particle Suspension and Dispersion	p. 31
Pipette Method after Robinson-Kohn or Andreasen	p. 35
Density Method with Variable Depth	p. 42
Density Method with Constant Depth	p. 47
Particle Size Analysis of Sands Only	p. 48
Automated Equipment	p. 50
Introduction	p. 50
Method Using Sedimentation by Simple Gravity	p. 51
Methods Using Accelerated Sedimentation	p. 53
Methods Using Laser Scattering and Diffraction	p. 54
Methods Using Optical and Electric Properties	p. 55
Methods Allowing Direct Observations of the Particles	p. 55
Methods Using Conductivity	p. 56
References	p. 56
Bibliography	p. 58
Generality	p. 58
Pre-treatment	p. 58
Pipette Method	p. 61
Hydrometer Method	p. 62
Instrumental Methods	p. 62
Fractionation of the Colloidal Systems
Introduction	p. 65
Fractionation by Continuous Centrifugation	p. 66
Principle	p. 66
Theory	p. 69
Equipment and reagents	p. 73
Procedure	p. 75
Pretreatment of the Extracted Phases	p. 79
References	p. 81
Bibliography	p. 81
Mineralogical Characterisations by X-Ray Diffractometry
Introduction	p. 83
X-Ray Diffraction and Mineralogy	p. 83
Principle	p. 86
XRD Instrumentation	p. 87
Qualitative Diffractometry	p. 90
Overview of Preparation of the Samples	p. 90
Preparation for Powder Diagrams	p. 90
Preparation for Oriented Diagrams	p. 94
Pretreatment of Clays	p. 99
Qualitative Diffractometry	p. 113
Quantitative Mineralogical Analysis	p. 118
Interest	p. 118
Quantitative Mineralogical Analysis by XRD	p. 118
Multi-Instrumental Quantitative Mineralogical Analysis	p. 124
References	p. 126
Bibliography	p. 127
General	p. 127
Preparation of Oriented Aggregates on Porous Ceramic Plate	p. 128
Saturation of Clays by Cations	p. 129
Saturation, Solvation, Intercalation Complex, Dissolution	p. 129
Preparation of Iron Oxides	p. 130
Quantitative XRD	p. 130
Mineralogical Analysis by Infra-Red Spectrometry
Introduction	p. 133
Principle	p. 133
IR Instrumentation	p. 135
IR Spectrometry in Mineralogy	p. 138
Equipment and Products	p. 138
Preparation of the Samples	p. 139
Brief Guide to Interpretation of the Spectra	p. 146
Quantitative Analysis	p. 152
Other IR Techniques	p. 156
Near-infrared Spectrometry (NIRS)	p. 156
Coupling Thermal Measurements and FTIR Spectrometry of Volatile Products	p. 158
Infrared Microscopy	p. 159
Raman Scattering Spectroscopy	p. 159
References	p. 161
Chronobibliography	p. 162
Mineralogical Separation by Selective Dissolution
Introduction	p. 167
Crystallinity of Clay Minerals	p. 167
Instrumental and Chemical Methods	p. 169
Selective Dissolution Methods	p. 172
Reagents and Synthetic Standards	p. 174
Main Selective Dissolution Methods	p. 180
Acid Oxalate Method Under Darkness (AOD)	p. 180
Dithionite-Citrate-Bicarbonate Method (DCB)	p. 187
EDTA Method	p. 192
Pyrophosphate Method	p. 196
Extraction in Strongly Alkaline Mediums	p. 201
Other Methods, Improvements and Choices	p. 206
Differential Sequential Methods	p. 206
Selective Methods for Amorphous Products	p. 210
Brief Overview to the Use of the Differential Methods	p. 214
References	p. 215
Thermal Analysis
Introduction	p. 221
Definition	p. 221
Interest	p. 223
Classical Methods	p. 226
Thermogravimetric Analysis	p. 226
Differential Thermal Analysis and Differential Scanning Calorimetry	p. 235
Multi-component Apparatuses for Thermal Analysis	p. 246
Concepts	p. 246
Coupling Thermal Analysis and Evolved Gas Analysis	p. 247
References	p. 249
Chronobibliography	p. 250
Microscopic Analysis
Introduction	p. 253
Preparation of the Samples	p. 254
Interest	p. 254
Coating and Impregnation, Thin Sections	p. 255
Grids and Replicas for Transmission Electron Microscopy	p. 261
Mounting the Samples for Scanning Electron Microscopy	p. 263
Surface Treatment (Shadowing, Flash-carbon, Metallization)	p. 265
Microscope Studies	p. 267
Optical Microscopy	p. 267
Electron Microscopy, General Information	p. 270
Transmission Electron Microscopy, Micro-diffraction	p. 271
Scanning Electron Microscopy	p. 279
Ultimate Micro-analysis by X-Ray Spectrometry	p. 282
References	p. 283
Chronobibliography	p. 284
Organic Analysis
Physical Fractionation of Organic Matter
Principle and Limitations	p. 289
Forms of Organic Matter in Soil	p. 289
Principle	p. 289
Difficulties	p. 291
Methods	p. 293
Classification	p. 293
Extraction of Plant Roots	p. 293
Dispersion of the Particles	p. 296
Separation by Density	p. 309
Particle Size Fractionations	p. 314
Precision of the Fractionation Methods	p. 320
Conclusion and Outlook	p. 321
References	p. 322
Organic and Total C, N (H, O, S) Analysis
Introduction	p. 327
Soil Organic Matter	p. 327
Sampling, Preparation of the Samples, Analytical Significance	p. 330
Wet Methods	p. 333
Total Carbon: General Information	p. 333
Organic Carbon by Wet Oxidation at the Temperature of Reaction	p. 335
Organic Carbon by Wet Oxidation at Controlled Temperature	p. 340
Organic Carbon by Wet Oxidation and Spectrocolorimetry	p. 342
Total Nitrogen by Wet Method: Introduction	p. 342
Total Nitrogen by Kjeldahl Method and Titrimetry	p. 344
Kjeldahl N, Titration by Spectrocolorimetry	p. 349
Kjeldahl N, Titration by Selective Electrode	p. 351
Mechanization and Automation of the Kjeldahl Method	p. 353
Modified Procedures for NO[subscript 3][superscript -], NO[subscript 2][superscript -] and Fixed N	p. 354
Dry Methods	p. 355
Total Carbon by Simple Volatilization	p. 355
Simultaneous Instrumental Analysis by Dry Combustion: CHN(OS)	p. 356
CHNOS by Thermal Analysis	p. 362
C and N Non-Destructive Instrumental Analysis	p. 363
Simultaneous Analysis of the Different C and N Isotopes	p. 364
References	p. 365
Bibliography	p. 367
Quantification of Humic Compounds
Humus in Soils	p. 371
Definitions	p. 371
Role in the Soil and Environment	p. 373
Extractions	p. 374
Main Techniques	p. 375
Extraction	p. 375
Quantification of the Extracts	p. 379
Precision and Correspondence of the Extraction Methods	p. 383
Purification of Humic Materials	p. 389
Further Alternatives and Complements Methods	p. 392
Alternative Method of Extraction	p. 392
Fractionation of the Humin Residue	p. 392
References	p. 395
Humic Materials	p. 395
Extraction, Titration, Purification and Fractionation of Humic Materials	p. 396
Characterization of Humic Compounds
Introduction	p. 399
Mechanisms of Formation	p. 399
Molecular Structure	p. 400
Classical Techniques	p. 401
Fractionation of Humic Compounds	p. 401
Titration of the Main Functional Groups	p. 408
UV-Visible Spectrometry	p. 410
Infra-Red Spectrography	p. 413
Complementary Techniques	p. 415
Improvements in Fractionation Technologies	p. 415
Titration of Functional Groups	p. 418
Characterization by Fragmentation	p. 419
Nuclear Magnetic Resonance (NMR)	p. 424
Fluorescence Spectroscopy	p. 433
Electron Spin Resonance (ESR) Spectroscopy	p. 435
Measurement of Molecular Weight and Molecular Size	p. 437
Microscopic Observations	p. 440
Other Techniques	p. 441
References	p. 442
Molecular Models	p. 442
Fractionation, Determination of Molecular Weights and Molecular Sizes	p. 443
Functional Group of Humic Compounds	p. 445
Spectrometric Characterizations	p. 446
UV-Visible, IR, Fluorescence, ESR Spectrometries	p. 446
Nuclear Magnetic Resonance	p. 447
Methods of Characterization by Fragmentation	p. 449
Other Methods (Microscopy, X-ray, Electrochemistry, etc.)	p. 451
Measurement of Non-Humic Molecules
Introduction	p. 453
Non-Humic Molecules	p. 453
Soil Carbohydrates	p. 453
Soil Lipids	p. 456
Pesticides and Pollutants	p. 457
Classical Techniques	p. 458
Acid Hydrolysis of Polysaccharides	p. 458
Purification of Acid Hydrolysates	p. 462
Colorimetric Titration of Sugars	p. 464
Titration of Sugars by Gas Chromatography	p. 467
Quantification of Total Lipids	p. 472
Quantification of the Water-Soluble Organics	p. 474
Complementary Techniques	p. 475
Carbohydrates by Gas Chromatography	p. 475
Carbohydrates by Liquid Chromatography	p. 475
Fractionation and Study of the Soil Lipid Fraction	p. 478
Measurement of Pesticide Residues and Pollutants	p. 483
References	p. 492
Soil Carbohydrates	p. 492
Soil Lipids	p. 494
Aqueous Extract	p. 495
Pesticides and Pollutants	p. 495
Organic Forms of Nitrogen, Mineralizable Nitrogen (and Carbon)
Introduction	p. 497
The Nitrogen Cycle	p. 497
Types of Methods	p. 499
Classical Methods	p. 500
Forms of Organic Nitrogen Released by Acid Hydrolysis	p. 500
Organic Forms of Nitrogen: Simplified Method	p. 509
Urea Titration	p. 511
Potentially Available Nitrogen: Biological Methods	p. 513
Potentially Mineralizable Nitrogen: Chemical Methods	p. 521
Kinetics of Mineralization	p. 526
Complementary Methods	p. 531
Alternative Procedures for Acid Hydrolysis	p. 531
Determination of Amino Acids	p. 532
Determination of Amino Sugars	p. 535
Proteins and Glycoproteins (glomalin)	p. 538
Potentially Mineralizable Nitrogen by EUF	p. 538
References	p. 540
Organic Nitrogen Forms: General Articles	p. 540
Nitrogen Forms by Acid Hydrolysis and Distillation	p. 541
Improvement of Acid Hydrolysis	p. 541
Determination of Amino Acids	p. 541
Determination of Amino Sugars	p. 542
Glomalin	p. 542
Urea Titration	p. 543
Potentially Mineralizable Nitrogen: General Papers	p. 543
Potentially Mineralizable Nitrogen: Biological Methods	p. 544
Potentially Mineralizable Nitrogen: Chemical Methods	p. 545
Potentially Mineralizable Nitrogen by EUF	p. 545
Mineralization Kinetics	p. 546
Inorganic Analysis - Exchangeable and Total Elements
pH Measurement
Introduction	p. 551
Soil pH	p. 551
Difficulties	p. 553
Theoretical Aspects	p. 554
Classical Measurements	p. 556
Methods	p. 556
Colorimetric Method	p. 557
Electrometric Method	p. 560
Electrometric Checking and Calibration	p. 564
Measurement on Aqueous Soil Suspensions	p. 565
Determination of the pH-K and pH-Ca	p. 567
Measurement on Saturated Pastes	p. 567
Measurement on the Saturation Extract	p. 568
Measurement of the pH-NaF	p. 569
In Situ Measurements	p. 570
Equipment	p. 570
Installation in the Field	p. 570
Measurement on Soil Monoliths	p. 572
References	p. 574
Bibliography	p. 575
Appendix	p. 576
Table of Electrode Potentials	p. 576
Constants of Dissociation of Certain Equilibriums	p. 577
Buffer Solutions	p. 577
Coloured Indicators	p. 579
Redox Potential
Definitions and Principle	p. 581
Equipment and Reagents	p. 583
Electrodes	p. 583
Salt Bridge for Connection	p. 584
System of Measurement	p. 584
Calibration Solutions	p. 585
Procedure	p. 585
Pretreatment of the Electrode	p. 585
Measurement on Soil Sample	p. 586
Measurement on Soil Monolith	p. 586
In Situ Measurements	p. 587
Measurement of Oxygen Diffusion Rate	p. 588
Colorimetric Test of Eh	p. 589
References	p. 589
Bibliography	p. 590
Carbonates
Introduction	p. 593
Measurement of Total Carbonates	p. 595
Introduction	p. 595
Volumetric Measurement by Calcimetry	p. 596
Acidimetry	p. 599
Titration of Active Carbonate	p. 601
Principle	p. 601
Implementation	p. 601
Index of Chlorosis Potential	p. 603
References	p. 604
Soluble Salts
Introduction	p. 605
Extraction	p. 606
Soil/solution Ratio	p. 606
Extraction of Saturated Paste	p. 607
Diluted Extracts	p. 608
In Situ Sampling of the Soil Water	p. 609
Extracts with Hot Water	p. 610
Measurement and Titration	p. 610
Electrical Conductivity of Extracts	p. 610
In Situ Conductivity	p. 613
Total Dissolved Solid Material	p. 614
Soluble Cations	p. 615
Extractable Carbonate and Bicarbonate (Alkalinity)	p. 616
Extractable Chloride	p. 618
Extractable Sulphate, Nitrate and Phosphate	p. 620
Extractable Boron	p. 620
Titration of Extractable Anions by Ionic Chromatography	p. 622
Expression of the Results	p. 625
References	p. 626
Exchange Complex
Introduction	p. 629
Origin of Charges	p. 630
Ionic Exchange	p. 630
Exchange Complex	p. 631
Theory	p. 633
References	p. 636
Chronobibliography	p. 637
Isoelectric and Zero Charge Points
Introduction	p. 645
Charges of Colloids	p. 645
Definitions	p. 647
Conditions for the Measurement of Charge	p. 649
Main Methods	p. 651
Measurement of pH0 (PZSE), Long Equilibrium Time	p. 651
Point of Zero Salt Effect (PZSE), Short Equilibrium Time	p. 652
References	p. 655
Permanent and Variable Charges
Introduction	p. 657
Main Methods	p. 661
Measurement of Variable Charges	p. 661
Determination of Permanent Charges	p. 662
References	p. 664
Bibliography	p. 665
Exchangeable Cations
Introduction	p. 667
Exchangeable Cations of Soil	p. 667
Extracting Reagents	p. 668
Equipment	p. 669
Ammonium Acetate Method at pH 7	p. 671
Principle	p. 671
Procedure	p. 671
Automated Continuous Extraction	p. 674
References	p. 674
Bibliography	p. 676
Exchangeable Acidity
Introduction	p. 677
Origin of Acidity	p. 677
Aims of the Analysis	p. 678
Method	p. 680
Principle	p. 680
Reagents	p. 680
Procedure	p. 681
Other Methods	p. 683
References	p. 684
Chronobibliography	p. 685
Lime Requirement
Introduction	p. 687
Correction of Soil Acidity	p. 687
Calculation of Correction	p. 688
SMP Buffer Method	p. 690
Principle	p. 690
Reagents	p. 691
Procedure	p. 691
Remarks	p. 692
References	p. 693
Chronobibliography	p. 693
Exchange Selectivity, Cation Exchange Isotherm
Introduction	p. 697
Determination of the Exchange Isotherm	p. 702
Principle	p. 702
Reagents	p. 702
Procedure	p. 703
Remarks	p. 704
References	p. 705
Chronobibliography	p. 706
Cation Exchange Capacity
Introduction	p. 709
Theoretical Aspects	p. 709
Variables that Influence the Determination of CEC	p. 711
Determination of Effective CEC by Summation (ECEC)	p. 718
Principle	p. 718
Alternative Methods	p. 718
CEC Measurement at Soil pH in Not-Buffered Medium	p. 719
Principle	p. 719
Methods Using Not-Buffered Metallic Salts	p. 719
Procedure Using Not-Buffered Organo Metallic Cations	p. 722
Not-Buffered Methods Using Organic Cations	p. 728
CEC Measurement in Buffered Medium	p. 730
Buffered Methods - General Information	p. 730
Ammonium Acetate Method at pH 7.0	p. 732
Buffered Methods at pH 8.0-8.6	p. 738
Buffered Methods at Different pH	p. 743
References	p. 745
Bibliography	p. 750
CEC General Theory	p. 750
Barium Method at soil pH	p. 751
Buffered Method at pH 7.0	p. 751
Cobaltihexamine CEC	p. 752
Silver-Thiourea	p. 753
CEC with Organic Cations (Coloured Reagents)	p. 753
Buffered Methods at pH 8.0-8.6	p. 753
Barium Chloride-Triethanolamine at pH 8.1	p. 753
Anion Exchange Capacity
Theory	p. 755
Measurement	p. 758
Principle	p. 758
Method	p. 760
Simultaneous Measurement of AEC, EC, CEC and net CEC	p. 760
Aim	p. 760
Description	p. 761
References	p. 763
Inorganic Forms of Nitrogen
Introduction	p. 767
Ammonium, Nitrate and Nitrite	p. 767
Sampling Problems	p. 768
Analytical Problems	p. 768
Usual Methods	p. 769
Extraction of Exchangeable Forms	p. 769
Separation by Micro-Diffusion	p. 770
Colorimetric Titration of Ammonium	p. 773
Colorimetric Titration of Nitrites	p. 775
Colorimetric Titration of Nitrates	p. 778
Extracted Organic Nitrogen	p. 779
Other Methods	p. 780
Nitrate and Nitrite by Photometric UV Absorption	p. 780
Ammonium Titration Using a Selective Electrode	p. 782
Measurement of Nitrates with an Ion-Selective Electrode	p. 785
In situ Measurement	p. 788
Non-Exchangeable Ammonium	p. 790
References	p. 791
Bibliography	p. 792
Phosphorus
Introduction	p. 793
Total Soil Phosphorus	p. 794
Introduction	p. 794
Wet Mineralization for Total Analyses	p. 795
Dry Mineralization	p. 798
Fractionation of Different Forms of Phosphorus	p. 799
Introduction	p. 799
Sequential Methods	p. 800
Selective Extractions - Availability Indices	p. 804
Isotopic Dilution Methods	p. 813
Determination of Organic Phosphorus	p. 814
Retention of Phosphorus	p. 818
Introduction	p. 818
Determination of P Retention	p. 819
Titration of P in the Extracts	p. 821
Introduction	p. 821
Titration of Ortho-phosphoric P by Spectrocolorimetry	p. 823
P Titration by Atomic Spectrometry	p. 828
Titration of Different Forms of P by [superscript 31]P NMR	p. 828
Separation of P Compounds by Liquid Chromatography	p. 829
Direct Speciation of P in situ, or on Extracted Particles	p. 830
References	p. 830
Chronobibliography	p. 833
Sulphur
Introduction	p. 835
Sulphur Compounds	p. 835
Mineralogical Studies	p. 838
Total Sulphur and Sulphur Compounds	p. 839
Characteristics of Fluviomarine Soils	p. 839
Soil Sampling and Sample Preparation	p. 840
Testing for Soluble Sulphur Forms	p. 841
Titration of Total Sulphur	p. 842
Total S Solubilisation by Alkaline Oxidizing Fusion	p. 843
Total Solubilisation by Sodium Hypobromite in Alkaline Medium	p. 844
S titration with Methylen Blue Colorimetry	p. 845
Sulphate Titration by Colorimetry with Methyl Thymol Blue	p. 850
Total Sulphur by Automated Dry CHN(OS) Ultimate Analysis	p. 853
Titration of Total S0[subscript 4][superscript 2-]-S by Ionic Chromatography	p. 855
Total S Titration by Plasma Emission Spectrometry	p. 857
Titration by X-ray Fluorescence	p. 857
Titration by Atomic Absorption Spectrometry	p. 857
Analytical Fractionation of Sulphur Compounds	p. 858
Titration of Organic S bound to C	p. 859
Titration of Organic S not bound to C	p. 861
Extraction and Titration of Soluble Sulphides	p. 863
Titration of Sulphur in Pyrites	p. 865
Titration of Elementary Sulphur	p. 867
Titration of Water Soluble Sulphates	p. 869
Titration of Na[subscript 3]-EDTA Extractable Sulphates	p. 871
Titration of Jarosite	p. 873
Sequential Analysis of S Forms	p. 876
Sulphur of Gypseous Soils	p. 878
Gypseous Soils	p. 878
Preliminary Tests	p. 879
Extraction and Titration from Multiple Extracts	p. 881
Gypsum Determination by Acetone Precipitation	p. 882
Sulphur and Gypsum Requirement of Soil	p. 883
Introduction	p. 883
Plant Sulphur Requirement	p. 884
Gypsum Requirement	p. 886
References	p. 888
Chronobibliography	p. 890
Analysis of Extractable and Total Elements
Elements of Soils	p. 895
Major Elements	p. 895
Trace Elements and Pollutants	p. 897
Biogenic and Toxic Elements	p. 899
Analysis of Total Elements	p. 900
Extractable Elements	p. 901
Methods using Solubilization	p. 901
Total Solubilization Methods	p. 901
Mean Reagents for Complete Dissolutions	p. 903
Acid Attack in Open Vessel	p. 906
Acid Attack in Closed Vessel	p. 911
Microwave Mineralization	p. 913
Alkaline Fusion	p. 915
Selective Extractions	p. 920
Measurement Methods	p. 925
Spectrocolorimetric Analysis	p. 927
Analysis by Flame Atomic Emission Spectrometry	p. 931
Analysis by Flame Atomic Absorption Spectrometry	p. 932
Analysis of Trace Elements by Hydride and Cold Vapour AAS	p. 937
Analysis of Trace Elements by Electrothermal AAS	p. 940
Analysis by Inductively Coupled Plasma-AES	p. 941
Analysis by Inductively Coupled Plasma-Mass Spectrometry	p. 946
Analysis on Solid Medium	p. 952
Method	p. 952
X-ray Fluorescence Analysis	p. 954
Neutron Activation Analysis	p. 962
References	p. 969
Index	p. 975
Periodic table of the elements	p. 993
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Handbook of Soil Analysis

Mineralogical, Organic and Inorganic Methods

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