Part 1 - Mineralogical analysis
Chapter 1 Water Content and Loss on Ignition
1.1 Introduction ................................................ 3
1.2 Water Content at 105°С(Н2O-) ................................ 6
1.2.1 Principle ............................................. 6
1.2.2 Materials ............................................. 6
1.2.3 Sample ................................................ 6
1.2.4 Procedure ............................................. 7
1.2.5 Remarks ............................................... 7
1.3 Loss on Ignition at 1,000°C(H2O+) ........................... 8
1.3.1 Introduction .......................................... 8
1.3.2 Principle ............................................ 11
1.3.3 Equipment ............................................ 11
1.3.4 Procedure ............................................ 11
1.3.5 Calculations ......................................... 12
1.3.6 Remarks .............................................. 12
Bibliography ................................................... 12
Chapter 2 Particle Size Analysis
2.1 Introduction ............................................... 15
2.1.1 Particle Size in Soil Science ........................ 15
2.1.2 Principle ............................................ 17
2.1.3 Law of Sedimentation ................................. 18
2.1.4 Conditions for Application of Stokes Law ............. 24
2.2 Standard Methods ........................................... 26
2.2.1 Pretreatment of the Sample ........................... 26
2.2.2 Particle Suspension and Dispersion ................... 31
2.2.3 Pipette Method after Robinson-Kohn or Andreasen ...... 35
2.2.4 Density Method with Variable Depth ................... 42
2.2.5 Density Method with Constant Depth ................... 47
2.2.6 Particle Size Analysis of Sands Only ................. 48
2.3 Automated Equipment ........................................ 50
2.3.1 Introduction ......................................... 50
2.3.2 Method Using Sedimentation by Simple Gravity ......... 51
2.3.3 Methods Using Accelerated Sedimentation .............. 53
2.3.4 Methods Using Laser Scattering and Diffraction ....... 54
2.3.5 Methods Using Optical and Electric Properties ........ 55
2.3.6 Methods Allowing Direct Observations of
the Particles ........................................ 55
2.3.7 Methods Using Conductivity ........................... 56
References ..................................................... 56
Bibliography ................................................... 58
Generality ................................................. 58
Pre-treatment .............................................. 58
Pipette Method ............................................. 61
Hydrometer Method .......................................... 62
Instrumental Methods ....................................... 62
Chapter 4 Mineralogical Characterisations by X-Ray
Diffractometry
4.1 Introduction ............................................... 83
4.1.1 X-Ray Diffraction and Mineralogy ..................... 83
4.1.2 Principle ............................................ 86
4.1.3 XRD Instrumentation .................................. 87
4.2 Qualitative Diffractometry ................................. 90
4.2.1 Overview of Preparation of the Samples ............... 90
4.2.2 Preparation for Powder Diagrams ...................... 90
4.2.3 Preparation for Oriented Diagrams .................... 94
4.2.4 Pretreatment of Clays ................................ 99
4.2.5 Qualitative Diffractometry .......................... 113
4.3 Quantitative Mineralogical Analysis ....................... 118
4.3.1 Interest ............................................ 118
4.3.2 Quantitative Mineralogical Analysis by XRD .......... 118
4.3.3 Multi-Instrumental Quantitative Mineralogical
Analysis ............................................ 124
References .................................................... 126
Bibliography .................................................. 127
General ................................................... 127
Preparation of Oriented Aggregates on Porous Ceramic
Plate ............................................... 128
Saturation of Clays by Cations ............................ 129
Saturation, Solvation, Intercalation Complex,
Dissolution ......................................... 129
Preparation of Iron Oxides ................................ 130
Quantitative XRD .......................................... 130
Chapter 5 Mineralogical Analysis by Infra-Red Spectrometry
5.1 Introduction .............................................. 133
5.1.1 Principle ........................................... 133
5.1.2 IR Instrumentation .................................. 135
5.2 IR Spectrometry in Mineralogy ............................. 138
5.2.1 Equipment and Products .............................. 138
5.2.2 Preparation of the Samples .......................... 139
5.2.3 Brief Guide to Interpretation of the Spectra ........ 146
5.2.4 Quantitative Analysis ............................... 152
5.3 Other IR Techniques ....................................... 156
5.3.1 Near-infrared Spectrometry (NIRS) ................... 156
5.3.2 Coupling Thermal Measurements and FTIR
Spectrometry of Volatile Products ................... 158
5.3.3 Infrared Microscopy ................................. 159
5.3.4 Raman Scattering Spectroscopy ....................... 159
References .................................................... 161
Chronobibliography ............................................ 162
Chapter 6 Mineralogical Separation by Selective Dissolution
6.1 Introduction .............................................. 167
6.1.1 Crystallinity of Clay Minerals ...................... 167
6.1.2 Instrumental and Chemical Methods ................... 169
6.1.3 Selective Dissolution Methods ....................... 172
6.1.4 Reagents and Synthetic Standards .................... 174
6.2 Main Selective Dissolution Methods ........................ 180
6.2.1 Acid Oxalate Method Under Darkness (AOD) ............ 180
6.2.2 Dithionite-Citrate-Bicarbonate Method (DCB) ......... 187
6.2.3 EDTA Method ......................................... 192
6.2.4 Pyrophosphate Method ................................ 196
6.2.5 Extraction in Strongly Alkaline Mediums ............. 201
6.3 Other Methods, Improvements and Choices ................... 206
6.3.1 Differential Sequential Methods ..................... 206
6.3.2 Selective Methods for Amorphous Products ............ 210
6.3.3 Brief Overview to the Use of the Differential
Methods ............................................. 214
References .................................................... 215
Chapter 7 Thermal Analysis
7.1 Introduction .............................................. 221
7.1.1 Definition .......................................... 221
7.1.2 Interest ............................................ 223
7.2 Classical Methods ......................................... 226
7.2.1 Thermogravimetric Analysis .......................... 226
7.2.2 Differential Thermal Analysis and Differential
Scanning Calorimetry ................................ 235
7.3 Multi-component Apparatuses for Thermal Analysis .......... 246
7.3.1 Concepts ............................................ 246
7.3.2 Coupling Thermal Analysis and Evolved Gas
Analysis ............................................ 247
References .................................................... 249
Chronobibliography ............................................ 250
Chapter 8 Microscopic Analysis
8.1 Introduction .............................................. 253
8.2 Preparation of the Samples ................................ 254
8.2.1 Interest ............................................ 254
8.2.2 Coating and Impregnation, Thin Sections ............. 255
8.2.3 Grids and Replicas for Transmission Electron
Microscopy .......................................... 261
8.2.4 Mounting the Samples for Scanning Electron
Microscopy .......................................... 263
8.2.5 Surface Treatment
(Shadowing, Flash-carbon, Metallization) ............ 265
8.3 Microscope Studies ........................................ 267
8.3.1 Optical Microscopy .................................. 267
8.3.2 Electron Microscopy, General Information ............ 270
8.3.3 Transmission Electron Microscopy,
Micro-diffraction ................................... 271
8.3.4 Scanning Electron Microscopy ........................ 279
8.3.5 Ultimate Micro-analysis by X-Ray Spectrometry ....... 282
References .................................................... 283
Chronobibliography ............................................ 284
Part 2 - Organic analysis
Chapter 9 Physical Fractionation of Organic Matter
9.1 Principle and Limitations ................................. 289
9.1.1 Forms of Organic Matter in Soil ..................... 289
9.1.2 Principle ........................................... 289
9.1.3 Difficulties ........................................ 291
9.2 Methods ................................................... 293
9.2.1 Classification ...................................... 293
9.2.2 Extraction of Plant Roots ........................... 293
9.2.3 Dispersion of the Particles ......................... 296
9.2.4 Separation by Density ............................... 309
9.2.5 Particle Size Fractionations ........................ 314
9.2.6 Precision of the Fractionation Methods .............. 320
9.3 Conclusion and Outlook .................................... 321
References .................................................... 322
Chapter 10 Organic and Total C, N (H, O, S) Analysis
10.1 Introduction ............................................. 327
10.1.1 Soil Organic Matter ............................... 327
10.1.2 Sampling, Preparation of the Samples, Analytical
Significance ...................................... 330
10.2 Wet Methods .............................................. 333
10.2.1 Total Carbon: General Information ................. 333
10.2.2 Organic Carbon by Wet Oxidation at
the Temperature of Reaction ....................... 335
10.2.3 Organic Carbon by Wet Oxidation at Controlled
Temperature ....................................... 340
10.2.4 Organic Carbon by Wet Oxidation and
Spectrocolorimetry ................................ 342
10.2.5 Total Nitrogen by Wet Method: Introduction ........ 342
10.2.6 Total Nitrogen by Kjeldahl Method and
Titrimetry ........................................ 344
10.2.7 Kjeldahl N, Titration by Spectrocolorimetry ....... 349
10.2.8 Kjeldahl N, Titration by Selective Electrode ...... 351
10.2.9 Mechanization and Automation of the Kjeldahl
Method ............................................ 353
10.2.10 Modified Procedures for NO3-, NO2- and Fixed N .... 354
10.3 Dry Methods .............................................. 355
10.3.1 Total Carbon by Simple Volatilization ............. 355
10.3.2 Simultaneous Instrumental Analysis by Dry
Combustion: CHN(OS) ............................... 356
10.3.3 CHNOS by Thermal Analysis ......................... 362
10.3.4 С and N Non-Destructive Instrumental Analysis ..... 363
10.3.5 Simultaneous Analysis of the Different С and N
Isotopes .......................................... 364
References .................................................... 365
Bibliography .................................................. 367
Chapter 11 Quantification of Humic Compounds
11.1 Humus in Soils ........................................... 371
11.1.1 Definitions ....................................... 371
11.1.2 Role in the Soil and Environment .................. 373
11.1.3 Extractions ....................................... 374
11.2 Main Techniques .......................................... 375
11.2.1 Extraction ........................................ 375
11.2.2 Quantification of the Extracts .................... 379
11.2.3 Precision and Correspondence of the Extraction
Methods ........................................... 383
11.2.4 Purification of Humic Materials ................... 389
11.3 Further Alternatives and Complements Methods ............. 392
11.3.1 Alternative Method of Extraction .................. 392
11.3.2 Fractionation of the Humin Residue ................ 392
References .................................................... 395
Humic Materials .......................................... 395
Extraction, Titration, Purification and Fractionation
of Humic Materials ................................ 396
Chapter 12 Characterization of Humic Compounds
12.1 Introduction ............................................. 399
12.1.1 Mechanisms of Formation ........................... 399
12.1.2 Molecular Structure ............................... 400
12.2 Classical Techniques ..................................... 401
12.2.1 Fractionation of Humic Compounds .................. 401
12.2.2 Titration of the Main Functional Groups ........... 408
12.2.3 UV-Visible Spectrometry ........................... 410
12.2.4 Infra-Red Spectrography ........................... 413
12.3 Complementary Techniques ................................. 415
12.3.1 Improvements in Fractionation Technologies ........ 415
12.3.2 Titration of Functional Groups .................... 418
12.3.3 Characterization by Fragmentation ................. 419
12.3.4 Nuclear Magnetic Resonance (NMR) .................. 424
12.3.5 Fluorescence Spectroscopy ......................... 433
12.3.6 Electron Spin Resonance (ESR) Spectroscopy ........ 435
12.3.7 Measurement of Molecular Weight and Molecular
Size .............................................. 437
12.3.8 Microscopic Observations .......................... 440
12.3.9 Other Techniques .................................. 441
References .................................................... 442
Molecular Models ......................................... 442
Fractionation, Determination of Molecular Weights and
Molecular Sizes ................................... 443
Functional Group of Humic Compounds ...................... 445
Spectrometric Characterizations .......................... 446
UV-Visible, IR, Fluorescence, ESR Spectrometries ......... 446
Nuclear Magnetic Resonance ............................... 447
Methods of Characterization by Fragmentation ............. 449
Other Methods
(Microscopy, X-ray, Electrochemistry, etc.) ....... 451
Chapter 13 Measurement of Non-Humic Molecules
13.1 Introduction ............................................. 453
13.1.1 Non-Humic Molecules ............................... 453
13.1.2 Soil Carbohydrates ................................ 453
13.1.3 Soil Lipids ....................................... 456
13.1.4 Pesticides and Pollutants ......................... 457
13.2 Classical Techniques ..................................... 458
13.2.1 Acid Hydrolysis of Polysaccharides ................ 458
13.2.2 Purification of Acid Hydrolysates ................. 462
13.2.3 Colorimetric Titration of Sugars .................. 464
13.2.4 Titration of Sugars by Gas Chromatography ......... 467
13.2.5 Quantification of Total Lipids .................... 472
13.2.6 Quantification of the Water-Soluble Organics ...... 474
13.3 Complementary Techniques ................................. 475
13.3.1 Carbohydrates by Gas Chromatography ............... 475
13.3.2 Carbohydrates by Liquid Chromatography ............ 475
13.3.3 Fractionation and Study of the Soil Lipid
Fraction .......................................... 478
13.3.4 Measurement of Pesticide Residues and
Pollutants ........................................ 483
References .................................................... 492
Soil Carbohydrates ....................................... 492
Soil Lipids .............................................. 494
Aqueous Extract .......................................... 495
Pesticides and Pollutants ................................ 495
Chapter 14 Organic Forms of Nitrogen, Mineralizable Nitrogen
(and Carbon)
14.1 Introduction ............................................. 497
14.1.1 The Nitrogen Cycle ................................ 497
14.1.2 Types of Methods .................................. 499
14.2 Classical Methods ........................................ 500
14.2.1 Forms of Organic Nitrogen Released by Acid
Hydrolysis ........................................ 500
14.2.2 Organic Forms of Nitrogen: Simplified Method ...... 509
14.2.3 Urea Titration .................................... 511
14.2.4 Potentially Available Nitrogen:
Biological Methods ................................ 513
14.2.5 Potentially Mineralizable Nitrogen:
Chemical Methods .................................. 521
14.2.6 Kinetics of Mineralization ........................ 526
14.3 Complementary Methods .................................... 531
14.3.1 Alternative Procedures for Acid Hydrolysis ........ 531
14.3.2 Determination of Amino Acids ...................... 532
14.3.3 Determination of Amino Sugars ..................... 535
14.3.4 Proteins and Glycoproteins (glomalin) ............. 538
14.3.5 Potentially Mineralizable Nitrogen by EUF ......... 538
References .................................................... 540
Organic Nitrogen Forms: General Articles ................. 540
Nitrogen Forms by Acid Hydrolysis and Distillation ....... 541
Improvement of Acid Hydrolysis ........................... 541
Determination of Amino Acids ............................. 541
Determination of Amino Sugars ............................ 542
Glomalin ................................................. 542
Urea Titration ........................................... 543
Potentially Mineralizable Nitrogen: General Papers ....... 543
Potentially Mineralizable Nitrogen: Biological Methods ... 544
Potentially Mineralizable Nitrogen: Chemical Methods ..... 545
Potentially Mineralizable Nitrogen by EUF ................ 545
Mineralization Kinetics .................................. 546
Part 3 - Inorganic analysis - Exchangeable and Total Elements
Chapter 15 pH Measurement
15.1 Introduction ............................................. 551
15.1.1 Soil pH ........................................... 551
15.1.2 Difficulties ...................................... 553
15.1.3 Theoretical Aspects ............................... 554
15.2 Classical Measurements ................................... 556
15.2.1 Methods ........................................... 556
15.2.2 Colorimetric Method ............................... 557
15.2.3 Electrometric Method .............................. 560
15.2.4 Electrometric Checking and Calibration ............ 564
15.2.5 Measurement on Aqueous Soil Suspensions ........... 565
15.2.6 Determination of the pH-K and pH-Ca ............... 567
15.2.7 Measurement on Saturated Pastes ................... 567
15.2.8 Measurement on the Saturation Extract ............. 568
15.2.9 Measurement of the pH-NaF ......................... 569
15.3 In Situ Measurements ..................................... 570
15.3.1 Equipment ......................................... 570
15.3.2 Installation in the Field ......................... 570
15.3.3 Measurement on Soil Monoliths ..................... 572
References .................................................... 574
Bibliography .................................................. 575
Appendix ...................................................... 576
Appendix 1: Table of Electrode Potentials ................ 576
Appendix 2: Constants of Dissociation of Certain
Equilibriums ................................. 577
Appendix 3: Buffer Solutions ............................. 577
Appendix 4: Coloured Indicators .......................... 579
Chapter 16 Redox Potential
16.1 Definitions and Principle ................................ 581
16.2 Equipment and Reagents ................................... 583
16.2.1 Electrodes ........................................ 583
16.2.2 Salt Bridge for Connection ........................ 584
16.2.3 System of Measurement ............................. 584
16.2.4 Calibration Solutions ............................. 585
16.3 Procedure ................................................ 585
16.3.1 Pretreatment of the Electrode ..................... 585
16.3.2 Measurement on Soil Sample ........................ 586
16.3.3 Measurement on Soil Monolith ...................... 586
16.3.4 In Situ Measurements .............................. 587
16.3.5 Measurement of Oxygen Diffusion Rate .............. 588
16.3.6 Colorimetric Test of Eh ........................... 589
References .................................................... 589
Bibliography .................................................. 590
Chapter 17 Carbonates
17.1 Introduction ............................................. 593
17.2 Measurement of Total Carbonates .......................... 595
17.2.1 Introduction ...................................... 595
17.2.2 Volumetric Measurement by Calcimetry .............. 596
17.2.3 Acidimetry ........................................ 599
17.3 Titration of Active Carbonate ............................ 601
17.3.1 Principle ......................................... 601
17.3.2 Implementation .................................... 601
17.3.3 Index of Chlorosis Potential ...................... 603
References .................................................... 604
Chapter 18 Soluble Salts
18.1 Introduction ............................................. 605
18.2 Extraction ............................................... 606
18.2.1 Soil/solution Ratio ............................... 606
18.2.2 Extraction of Saturated Paste ..................... 607
18.2.3 Diluted Extracts .................................. 608
18.2.4 In Situ Sampling of the Soil Water ................ 609
18.2.5 Extracts with Hot Water ........................... 610
18.3 Measurement and Titration ................................ 610
18.3.1 Electrical Conductivity of Extracts ............... 610
18.3.2 In Situ Conductivity .............................. 613
18.3.3 Total Dissolved Solid Material .................... 614
18.3.4 Soluble Cations ................................... 615
18.3.5 Extractable Carbonate and Bicarbonate
(Alkalinity) ...................................... 616
18.3.6 Extractable Chloride .............................. 618
18.3.7 Extractable Sulphate, Nitrate and Phosphate ....... 620
18.3.8 Extractable Boron ................................. 620
18.3.9 Titration of Extractable Anions by Ionic
Chromatography .................................... 622
18.3.10 Expression of the Results ........................ 625
References .................................................... 626
Chapter 19 Exchange Complex
19.1 Introduction ............................................. 629
19.2 Origin of Charges ........................................ 630
19.2.1 Ionic Exchange .................................... 630
19.2.2 Exchange Complex .................................. 631
19.2.3 Theory ............................................ 633
References .................................................... 636
Chronobibliography ............................................ 637
Chapter 20 Isoelectric and Zero Charge Points
20.1 Introduction ............................................. 645
20.1.1 Charges of Colloids ............................... 645
20.1.2 Definitions ....................................... 647
20.1.3 Conditions for the Measurement of Charge .......... 649
20.2 Main Methods ............................................. 651
20.2.1 Measurement of pHO (PZSE), Long Equilibrium
Time .............................................. 651
20.2.2 Point of Zero Salt Effect (PZSE), Short
Equilibrium Time .................................. 652
References .................................................... 655
Chapter 21 Permanent and Variable Charges
21.1 Introduction ............................................. 657
21.2 Main Methods ............................................. 661
21.2.1 Measurement of Variable Charges ................... 661
21.2.2 Determination of Permanent Charges ................ 662
References .................................................... 664
Bibliography .................................................. 665
Chapter 22 Exchangeable Cations
22.1 Introduction ............................................. 667
22.1.1 Exchangeable Cations of Soil ...................... 667
22.1.2 Extracting Reagents ............................... 668
22.1.3 Equipment ......................................... 669
22.2 Ammonium Acetate Method at pH 7 .......................... 671
22.2.1 Principle ......................................... 671
22.2.2 Procedure ......................................... 671
22.3 Automated Continuous Extraction .......................... 674
References .................................................... 674
Bibliography .................................................. 676
Chapter 23 Exchangeable Acidity
23.1 Introduction ............................................. 677
23.1.1 Origin of Acidity ................................. 677
23.1.2 Aims of the Analysis .............................. 678
23.2 Method ................................................... 680
23.2.1 Principle ......................................... 680
23.2.2 Reagents .......................................... 680
23.2.3 Procedure ......................................... 681
23.3 Other Methods ............................................ 683
References .................................................... 684
Chronobibliography ............................................ 685
Chapter 24 Requirement
24.1 Introduction ............................................. 687
24.1.1 Correction of Soil Acidity ........................ 687
24.1.2 Calculation of Correction ......................... 688
24.2 SMP Buffer Method ........................................ 690
24.2.1 Principle ......................................... 690
24.2.2 Reagents .......................................... 691
24.2.3 Procedure ......................................... 691
24.2.4 Remarks ........................................... 692
References .................................................... 693
Chronobibliography ............................................ 693
Chapter 25 Exchange Selectivity, Cation Exchange Isotherm
25.1 Introduction ............................................. 697
25.2 Determination of the Exchange Isotherm ................... 702
25.2.1 Principle ......................................... 702
25.2.2 Reagents .......................................... 702
25.2.3 Procedure ......................................... 703
25.2.4 Remarks ........................................... 704
References .................................................... 705
Chronobibliography ............................................ 706
Chapter 26 Cation Exchange Capacity
26.1 Introduction ............................................. 709
26.1.1 Theoretical Aspects ............................... 709
26.1.2 Variables that Influence the Determination of
CEC ............................................... 711
26.2 Determination of Effective CEC by Summation (ECEC) ....... 718
26.2.1 Principle ......................................... 718
26.2.2 Alternative Methods ............................... 718
26.3 CEC Measurement at Soil pH in Not-Buffered Medium ........ 719
26.3.1 Principle ......................................... 719
26.3.2 Methods Using Not-Buffered Metallic Salts ......... 719
26.3.3 Procedure Using Not-Buffered Organo Metallic
Cations ........................................... 722
26.3.4 Not-Buffered Methods Using Organic Cations ........ 728
26.4 CEC Measurement in Buffered Medium ....................... 730
26.4.1 Buffered Methods - General Information ............ 730
26.4.2 Ammonium Acetate Method at pH 7.0 ................. 732
26.4.3 Buffered Methods at pH 8.0-8.6 .................... 738
26.4.4 Buffered Methods at Different pH .................. 743
References .................................................... 745
Bibliography .................................................. 750
CEC General Theory ....................................... 750
Barium Method at soil pH ................................. 751
Buffered Method at pH 7.0 ................................ 751
Cobaltihexamine CEC ...................................... 752
Silver-Thiourea .......................................... 753
CEC with Organic Cations (Coloured Reagents) ............. 753
Buffered Methods at pH 8.0-8.6 ........................... 753
Barium Chloride-Triethanolamine at pH 8.1 ................ 753
Chapter 27 Anion Exchange Capacity
27.1 Theory ................................................... 755
27.2 Measurement .............................................. 758
27.2.1 Principle ......................................... 758
27.2.2 Method ............................................ 760
27.3 Simultaneous Measurement of AEC, EC, CEC and net CEC ..... 760
27.3.1 Aim ............................................... 760
27.3.2 Description ....................................... 761
References .................................................... 763
Chapter 28 Inorganic Forms of Nitrogen
28.1 Introduction ............................................. 767
28.1.1 Ammonium, Nitrate and Nitrite ..................... 767
28.1.3 Sampling Problems ................................. 768
28.1.4 Analytical Problems ............................... 768
28.2 Usual Methods ............................................ 769
28.2.1 Extraction of Exchangeable Forms .................. 769
28.2.2 Separation by Micro-Diffusion ..................... 770
28.2.3 Colorimetric Titration of Ammonium ................ 773
28.2.4 Colorimetric Titration of Nitrites ................ 775
28.2.5 Colorimetric Titration of Nitrates ................ 778
28.2.6 Extracted Organic Nitrogen ........................ 779
28.3 Other Methods ............................................ 780
28.3.1 Nitrate and Nitrite by Photometric UV
Absorption ........................................ 780
28.3.2 Ammonium Titration Using a Selective Electrode .... 782
28.3.3 Measurement of Nitrates with an Ion-Selective
Electrode ......................................... 785
28.3.4 In situ Measurement ............................... 788
28.3.5 Non-Exchangeable Ammonium ......................... 790
References .................................................... 791
Bibliography .................................................. 792
Chapter 29 Phosphorus
29.1 Introduction ............................................. 793
29.2 Total Soil Phosphorus .................................... 794
29.2.1 Introduction ...................................... 794
29.2.2 Wet Mineralization for Total Analyses ............. 795
29.2.3 Dry Mineralization ................................ 798
29.3 Fractionation of Different Forms of Phosphorus ........... 799
29.3.1 Introduction ...................................... 799
29.3.2 Sequential Methods ................................ 800
29.3.3 Selective Extractions - Availability Indices ...... 804
29.3.4 Isotopic Dilution Methods ......................... 813
29.3.5 Determination of Organic Phosphorus ............... 814
29.4 Retention of Phosphorus .................................. 818
29.4.1 Introduction ...................................... 818
29.4.2 Determination of P Retention ...................... 819
29.5 Titration of P in the Extracts ........................... 821
29.5.1 Introduction ...................................... 821
29.5.2 Titration of Ortho-phosphoric P by
Spectrocolorimetry ................................ 823
29.5.3 P Titration by Atomic Spectrometry ................ 828
29.5.4 Titration of Different Forms of P by 31P NMR ...... 828
29.5.5 Separation of P Compounds by Liquid
Chromatography .................................... 829
29.6 Direct Speciation of P in situ, or on Extracted
Particles ................................................ 830
References .................................................... 830
Chronobibliography ............................................ 833
Chapter 30 Sulphur
30.1 Introduction ............................................. 835
30.1.1 Sulphur Compounds ................................. 835
30.1.2 Mineralogical Studies ............................. 838
30.2 Total Sulphur and Sulphur Compounds ...................... 839
30.2.1 Characteristics of Fluviomarine Soils ............. 839
30.2.2 Soil Sampling and Sample Preparation .............. 840
30.2.3 Testing for Soluble Sulphur Forms ................. 841
30.2.4 Titration of Total Sulphur ........................ 842
30.2.5 Total S Solubilisation by Alkaline Oxidizing
Fusion ............................................ 843
30.2.6 Total Solubilisation by Sodium Hypobromite in
Alkaline Medium ................................... 844
30.2.7 S titration with Methylen Blue Colorimetry ........ 845
30.2.8 Sulphate Titration by Colorimetry with Methyl
Thymol Blue ....................................... 850
30.2.9 Total Sulphur by Automated Dry CHN(OS) Ultimate
Analysis .......................................... 853
30.2.10 Titration of Total SO42--S by Ionic
Chromatography ................................... 855
30.2.11 Total S Titration by Plasma Emission
Spectrometry ..................................... 857
30.2.12 Titration by X-ray Fluorescence .................. 857
30.2.13 Titration by Atomic Absorption Spectrometry ...... 857
30.2.14 Analytical Fractionation of Sulphur Compounds .... 858
30.2.15 Titration of Organic S bound to С ................ 859
30.2.16 Titration of Organic S not bound to С ............ 861
30.2.17 Extraction and Titration of Soluble Sulphides .... 863
30.2.18 Titration of Sulphur in Pyrites .................. 865
30.2.19 Titration of Elementary Sulphur .................. 867
30.2.20 Titration of Water Soluble Sulphates ............. 869
30.2.21 Titration of Na3-EDTA Extractable Sulphates ...... 871
30.2.22 Titration of Jarosite ............................ 873
30.2.23 Sequential Analysis of S Forms ................... 876
30.3 Sulphur of Gypseous Soils ................................ 878
30.3.1 Gypseous Soils .................................... 878
30.3.2 Preliminary Tests ................................. 879
30.3.3 Extraction and Titration from Multiple Extracts ... 881
30.3.4 Gypsum Determination by Acetone Precipitation ..... 882
30.4 Sulphur and Gypsum Requirement of Soil ................... 883
30.4.1 Introduction ...................................... 883
30.4.2 Plant Sulphur Requirement ......................... 884
30.4.3 Gypsum Requirement ................................ 886
References .................................................... 888
Chronobibliography ............................................ 890
Chapter 31 Analysis of Extractable and Total Elements
31.1 Elements of Soils ........................................ 895
31.1.1 Major Elements .................................... 895
31.1.2 Trace Elements and Pollutants ..................... 897
31.1.3 Biogenic and Toxic Elements ....................... 899
31.1.4 Analysis of Total Elements ........................ 900
31.1.5 Extractable Elements .............................. 901
31.2 Methods using Solubilization ............................. 901
31.2.1 Total Solubilization Methods ...................... 901
31.2.2 Mean Reagents for Complete Dissolutions ........... 903
31.2.3 Acid Attack in Open Vessel ........................ 906
31.2.4 Acid Attack in Closed Vessel ...................... 911
31.2.5 Microwave Mineralization .......................... 913
31.2.6 Alkaline Fusion ................................... 915
31.2.7 Selective Extractions ............................. 920
31.2.8 Measurement Methods ............................... 925
31.2.9 Spectrocolorimetric Analysis ...................... 927
31.2.10 Analysis by Flame Atomic Emission Spectrometry ... 931
31.2.11 Analysis by Flame Atomic Absorption
Spectrometry ..................................... 932
31.2.12 Analysis of Trace Elements by Hydride and Cold
Vapour AAS ....................................... 937
31.2.13 Analysis of Trace Elements by Electrothermal
AAS .............................................. 940
31.2.14 Analysis by Inductively Coupled Plasma-AES ....... 941
31.2.15 Analysis by Inductively Coupled Plasma-Mass
Spectrometry ..................................... 946
31.3 Analysis on Solid Medium ................................. 952
31.3.1 Method ............................................ 952
31.3.2 X-ray Fluorescence Analysis ....................... 954
31.3.3 Neutron Activation Analysis ....................... 962
References .................................................... 969
Index ......................................................... 975
Periodic table of the elements ................................ 993
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