Spectrochemical Trace Analysis FOR Metals and Metalloids: Wilson & Wilson's Comprehensive Analytical Chemistry

Wilson & Wilson's
COMPREHENSIVE ANALYTICAL CHEMISTRY
VOLUME XXX
SPECTROCHEMICAL TRACE ANALYSIS

FOR
METALS AND METALLOIDS
by
R. LOBINSKI and Z. MARCZENKO
1996
ELSEVIER
AMSTERDAM - LAUSANNE - OXFORD - NEW YORK - SHANNON - TOKYO
Contents
Editor's Preface
Authors' Preface
List of Abbreviations
xxi
xxiii
xxvii
Part I. General
Chapter 1. Sampling
References
3
4
Chapter 2. Decomposition Idissolution techniques

2.1. Acid attack
2.1.1. Acids
2.1.2. Dissolution techniques
2.2. Fusion
2.2.1. Alkaline fusion
2.2.2. Acidic fusion
2.2.3. Reductive fusion (fire assay)
2.3. Decomposition in gas streams
2.3.1. Oxidation (dry ashing)
2.3.2. Decomposition with halogens
References
5
5
5
8
10
10
11
11
13
13
14
14
Chapter 3. Separation and preconcentration

3.1. Solvent extraction
3.1.1. Extractants and extraction solvents
3.1.2. Separation oftraces
3.1.3. Separation ofthe matrix
3.1.4. Practical aspects
3.2. Precipitation and coprecipitation
3.2.1. Coprecipitation oftraces
3.2.2. Precipitation of macrocomponents
3.3. Volatilization
3.3.1. Volatilization of trace elements
17
18
18
20
22
22
24
24
26
27
27
ix
3.3.2. Volatilization of macrocomponents

3.4. Sorption
3.4.1. Sorption via physical interactions
3.4.2. Simple ion-exchange
3.4.3. Chelating sorbents
3.4.4. Practical aspects
3.5. Chromatographie techniques
3.5.1. Gas chromatography
3.5.2. Liquid chromatography
3.5.3. Supercritical fluid chromatography
3.6. Electrochemical methods
References
Chapter 4. Spectrometric determination techniques
4.1. Basic coneepts
4.2. Sample and sample introduetion
4.2.1. Gaseous samples
4.2.2. Liquids and Solutions
4.2.3. Slurries
4.2.4. Solid samples
4.3. Spectrophotometry
4.3.1. Sample and colour Systems
4.3.2. Instrumentation
4.3.3. Measurement and calibration
4.3.4. Analytical characteristics
4.4. Atomic absorption spectrometry (AAS)
4.4.1. General
4.4.2. Flame AAS
4.4.3. Graphite furnace AAS
4.4.4. Quartz furnace AAS
4.5. Atomic emission spectrometry
4.5.1. Sample and sample introduetion
4.5.2. Flame AES
4.5.3. Inductively coupled plasma AES
4.5.4. Other atomic emission techniques
4.6. Fluorescence spectrometry
4.6.1. Molecular fluorescence spectrometry (spectrofluorimetry)
4.6.2. Atomic fluorescence spectrometry (AFS)
4.6.3. X-ray fluorescence spectrometry (XRF)
4.7. Activation spectrometry
4.7.1. Irradiation and measurement
4.7.2. Analytical characteristics
4.8. Mass spectrometry
4.8.1. Inductively coupled plasma mass spectrometry
4.8.2. Other MS techniques
References
x
29
30
30
31
32
33
33
34
35
38
38
39
45
45
47
47
48
50
51
53
53
54
55
56
57
57
59
62
66
66
67
67
68
73
73
74
75
77
82
82
83
85
85
91
Chapter 5. Quantification techniques

5.1. Calibration graph
5.2. The method of Standard additions
5.3. Internal standardization
5.4. Isotope dilution analysis
References
105
105
105
106
107
108
Chapter 6. Speciation analysis

6.1. Instrumental approaches
6.1.1. Gas chromatography-atomic absorption spectrometry . .
6.1.2. Gas chromatography-atomic emission spectrometry . . .
6.1.3. Gas chromatography-mass spectrometry
6.1.4. Liquid chromatography-mass spectrometry
6.1.5. Supercritical fluid chromatography-mass spectrometry .
6.2. Sample preparation for speciation analysis
References
109
110
110
111
111
112
112
113
114
Chapter 7. Flow-injection analysis

7.1. General purpose FI manifold
7.2. Liquid-liquid extraction
7.3. Liquid-gas extraction
7.4. Sorption
7.5. Precipitation
7.6. Microwave digestion
7.7. Speciation analysis
7.8. Calibration
References
115
115
117
117
118
119
119
120
121
121
Chapter 8. Quality assurance in trace analysis

8.1. Standard Solutions
8.1.1. Aqueous Standards
8.1.2. Non-aqueous Standards
8.2. Contamination
8.3. Losses
8.4. Accuracy verification
References
123
123
123
124
124
126
127
128
PART II. Multielement Trace Analysis of Real Samples

Chapter 9. Environmental and geological materials
9.1. Air
9.1.1. Sampling and sample handling
9.1.2. Determination techniques
9.2. Water
9.2.1. Sampling and storage
9.2.2. Preconcentration
133
133
134
135
136
138
140
143
xi
9.3.
Rocks, soils and Sediments

9.3.1. Sampling and physical sample preparation
9.3.2. Sample decomposition
9.4. Ashes, slags and solid wastes
9.5. Speciation
9.5.1. Water
9.5.2. Sediments and soils
9.6. Quality control and assurance
9.6.1. Contamination
9.6.2. Losses
9.6.3. Reference materials
References
151
152
152
156
165
166
166
169
171
171
172
172
174
Chapter 10. Biological and clinical materials

10.1. General considerations
10.1.1. Sampling and storage
10.1.2. Direct analysis
10.1.3. Digestion
10.1.4. Separation and/or preconcentration
10.1.5. Determination
10.1.6. Microanalysis
10.2. Biomedical materials
10.2.1. Body fluids
10.2.2. Tissues
10.3. Ecological materials
10.3.1. Plant materials
10.3.2. Animal tissues
10.4. Foodstuffs
10.5. Speciation
10.6. Quality assurance
References
187
187
187
188
188
188
188
189
189
190
194
196
196
200
204
207
208
212
Chapter 11. Inorganic industrial materials

11.1. Metals and alloys
11.1.1. Ferrous metals and alloys
11.1.2. Non-ferrous metals and alloys
11.1.3. Refractory metals and alloys
11.1.4. Precious metals
11.2. Semiconducting materials and related products
11.2.1. Semiconducting materials
11.2.2. Electronic grade gases and chemicals
11.3. Analysis of ceramics and their basic products
11.3.1. General analytical approaches
11.3.2. Industrial ceramics
11.3.3. Catalysts
223
223
224
227
232
235
237
237
242
242
242
246
248
XU
11.4. Nuclear materials

11.5. Quality control and assurance
References
Chapter 12. Organic industrial materials
12.1. Petroleum and petroleum products
12.1.1. Sample handling prior to measurement
12.2. Energy-related solid materials
12.2.1. Sample handling prior to measurement
12.3. Polymers
12.4. Speciation analysisof fossil fuels
12.5. Quality assurance
References
243
252
253
261
261
261
263
266
266
267
268
269
269
272
Part III. D e t e r m i n a t i o n of Individual E l e m e n t s

Chapter
13.1.
13.2.
13.3.
13. Aluminium
277
Separation and preconcentration
277
Determination techniques
278
Analysis of real samples
279
13.3.1. General considerations
281
13.3.2. Water, dialysis fluids and pharmaceutical samples . . . 281
13.3.3. Biological samples
283
13.4. Speciation
285
References
288
Chapter 14. Antimony

14.1. Separation and preconcentration
14.2. Determination techniques
14.3. Analysis of real samples
References
293
293
295
297
299
Chapter
15.1.
15.2.
15.3.
303
303
306
308
308
309
315
315
321
Chapter 16. Barium

16.1. Analytical techniques
329
329
15. Arsenic
Separation and Preconcentration
Determination techniques
Analysis of real samples
15.3.1. Environmental and geological materials
15.3.2. Biological samples
15.3.3. Industrial materials
15.4. Speciation
References
xiii

References
331
332
Chapterl7. Beryllium
References
333
333
335
337
Chapter 18. Bismuth

References
339
339
340
341
342
Chapter 19. Boron . . . . ;

References
347
348
349
352
357
Chapter 20. Cadmium

20.4. Speciation
References
361
361
362
363
374
374
Chapter 21. Caesium

References
377
377
378
379
380
Chapter 22. Calcium and magnesium

22.1. Determination
References
383
383
385
Chapter 23. Chromium

23.3. Speciation
23.4. Analysis of real samples . . .
References
387
387
389
391
393
398
Chapter 24. Cobalt

405
405
xiv

References
406
408
411
Chapter 25. Copper

25.4 Speciation
References
413
413
414
416
419
422
Chapter 26. Gallium

References
427
427
429
430
Chapter 27. Germanium

References
433
433
434
436
436
Chapter 28. Gold

28.3.1. Geological materials
28.3.2. Other materials
28.3.3. Accuracy considerations
References
439
440
441
443
443
447
450
451
Chapter 29. Hafnium

29.1. Determination
References
455
455
457
Chapter 30. Indium

References
459
459
460
461
461
Chapter 31. Iridium

References
465
465
466
467
470
xv
Chapter 32. Iron

32:2. Analysis of real samples
32.3. Speciation
References
473
473
476
476
476
Chapter 33. Lead

33.3.2. Biological materials
33.4. Speciation oforganolead Compounds
33.4.1. Instrumental approaches
33.4.2. Analysis of real samples
References
481
481
483
485
485
487
488
489
489
490
493
Chapter 34. Lithium

References
501
501
502
504
505
Chapter 35. Manganese

References
509
509
510
511
514
Chapter 36. Mercury

36.1.1. Volatilization
36.1.2. Other methods
36.3. Analysis of real samples for total mercury content
36.3.1. Environmental and geological materials . . :
36.4. Speciation
36.4.1. Analytical techniques
36.4.2. Speciation analysis of real samples
References
517
517
518
519
519
522
522
525
526
529
529
535
536
Chapter 37. Molybdenum

543
543
xvi

References
544
547
551
Chapter 38. Nickel

References
555
555
556
558
563
Chapter 39. Niobium

References
567
567
568
569
569
Chapter 40. Osmium

40.1. Separation
References
571
571
572
573
576
Chapter 41. Palladium

References
579
579
580
581
586
Chapter 42. Platinum

References
589
589
590
592
598
Chapter 43. Rare earth elements

References
601
602
604
611
617
Chapter 44. Rhenium

References
623
623
625
627
Chapter 45. Rhodium

References
629
629
630
631
633
xvii
Chapter 46. Rubidium

References
635
635
637
637
Chapter 47. Ruthenium

References
639
639
640
642
643
Chapter 48. Scandium

References
645
645
646
648
646
Chapter 49. Selenium

49.3.3. Industrial samples
49.4. Speciation
References
649
649
651
653
654
654
661
661
663
Chapter 50. Silicon

References
671
671
673
674
Chapter 51. Silver

References
677
677
678
679
685
Chapter 52. Sodium and potassium

References
687
687
688
689
Chapter 53. Strontium.

691
691
692
xviii

References
693
693
Chapter 54. Tantalum

54.2. Determination
References
695
695
696
698
Chapter 55. Technetium

References
699
699
700
701
704
Chapter 56. Tellurium

References
707
707
708
709
711
Chapter 57. Thallium

References
713
713
714
716
718
Chapter 58. Thorium

References
721
721
722
724
727
Chapter 59. Tin

59.4. Speciation
59.4.1. Sample preparation
59.4.2. Instrumental techniques
59.4.3. Speciation analysis of real samples
References
729
729
730
732
736
736
737
738
742
Chapter 60. Titanium

References
747
747
748
749
xix
Chapter 61. Transuranium elements

61.3. Analysis of environmental samples
References
751
751
752
753
757
Chapter 62. Tungsten

References
761
761
763
763
Chapter 63. Uranium

References
765
765
766
768
773
Chapter 64. Vanadium

References
777
777
778
780
784
Chapter 65. Zinc

References
787
787
789
791
Chapter 66. Zirconium

References
797
797
798
799
799
Index
803
xx

Spectrochemical Trace Analysis FOR Metals and Metalloids: Wilson & Wilson's Comprehensive Analytical Chemistry

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Spectrochemical Trace Analysis FOR Metals and Metalloids: Wilson & Wilson's Comprehensive Analytical Chemistry

Uploaded by

Copyright:

Available Formats

Wilson & Wilson's

COMPREHENSIVE ANALYTICAL CHEMISTRY

SPECTROCHEMICAL TRACE ANALYSIS

Chapter 2. Decomposition Idissolution techniques

Chapter 3. Separation and preconcentration

3.3.2. Volatilization of macrocomponents

Chapter 5. Quantification techniques

Chapter 6. Speciation analysis

Chapter 7. Flow-injection analysis

Chapter 8. Quality assurance in trace analysis

PART II. Multielement Trace Analysis of Real Samples

Rocks, soils and Sediments

Chapter 10. Biological and clinical materials

Chapter 11. Inorganic industrial materials

11.4. Nuclear materials

Part III. D e t e r m i n a t i o n of Individual E l e m e n t s

Chapter 14. Antimony

Chapter 16. Barium

16.2. Analysis of real samples

Chapter 18. Bismuth

Chapter 19. Boron . . . . ;

Chapter 20. Cadmium

Chapter 21. Caesium

Chapter 22. Calcium and magnesium

Chapter 23. Chromium

Chapter 24. Cobalt

24.2. Determination techniques

Chapter 25. Copper

Chapter 26. Gallium

Chapter 27. Germanium

Chapter 28. Gold

Chapter 29. Hafnium

Chapter 30. Indium

Chapter 31. Iridium

Chapter 32. Iron

Chapter 33. Lead

Chapter 34. Lithium

Chapter 35. Manganese

Chapter 36. Mercury

Chapter 37. Molybdenum

37.2. Determination techniques

Chapter 38. Nickel

Chapter 39. Niobium

Chapter 40. Osmium

Chapter 41. Palladium

Chapter 42. Platinum

Chapter 43. Rare earth elements

Chapter 44. Rhenium

Chapter 45. Rhodium

Chapter 46. Rubidium

Chapter 47. Ruthenium

Chapter 48. Scandium

Chapter 49. Selenium

Chapter 50. Silicon

Chapter 51. Silver

Chapter 52. Sodium and potassium

Chapter 53. Strontium.

53.3. Analysis of real samples

Chapter 54. Tantalum

Chapter 55. Technetium

Chapter 56. Tellurium

Chapter 57. Thallium

Chapter 58. Thorium