Erdey / Belcher / Gordon Gravimetric Analysis

International Series of Monographs on Analytical Chemistry, Vol. 7
1. Auflage 2013
ISBN: 978-1-4832-2267-7
Verlag: Elsevier Science & Techn.
Format: PDF
Kopierschutz: 1 - PDF Watermark

E-Book, Englisch, 814 Seiten, Web PDF

Analytical Chemistry, Volume 7: Gravimetric Analysis, Part II describes the experimental procedures for the gravimetric analysis of Groups I to V cations. This book is composed of 43 chapters that also present sample preparation, separation, and precipitation protocols. The first six chapters include Group I cations, such as silver, lead, mercury, copper, bismuth, and cadmium, followed by chapters on Group II cations, including arsenic, antimony, tin, germanium, gold, platinum, selenium, and tellurium. The subsequent chapters explore the gravimetric determination of Group III cations, namely, aluminum, iron, chromium, nickel, cobalt, zinc, manganese, titanium, zirconium, hafnium, thorium, scandium, niobium and tantalum, molybdenum, tungsten, vanadium, uranium, thallium, indium, gallium, and beryllium. The remaining chapters are devoted to analysis of various forms of Groups IV and V cations. This book will prove useful to analytical and inorganic chemists, teachers, and students in the allied fields.

Autoren/Hrsg.

Erdey, László

Belcher, R.

Gordon, L.

Inhaltsverzeichnis

1;Front Cover;1
2;Gravimetric Analysis, Part II;4
3;Copyright Page;5
4;Table of Contents;6
5;Group I Cations;18
6;CHAPTER 5. SILVER – Ag – 107.870;18
6.1;5.1. Determination in the form of silver chloride, agcl;19
6.2;5.2. Determination in the form of silver bromide, AgBr;25
6.3;5.3. Determination as metallic silver after reduction with ascorbic acid;25
6.4;5.4. Determination in the form of metallic silver by electrolysis;27
6.5;5.5. Determination of silver b y fire-assay;29
6.6;5.6.-5.17. The separation of Ag;33
6.7;References;42
7;CHAPTER 6. LEAD – Pb – 207.19;43
7.1;6.1. Determination in the form of lead sulphate, PbSO4;44
7.2;6.2. Determination in the form of lead chromate, PbCrO4;50
7.3;6.3. Electrolytic deposition of lead in the form of lead dioxide, PbO2;52
7.4;6.4. Determination in the form of lead chloride, PbCl2;55
7.5;6.5. Determination in the form of lead sulphite, PbSO3;56
7.6;6.6. The separation of Pb;57
7.7;References;69
8;CHAPTER 7. MERCURY – Hg – 200.59;72
8.1;7.1. Determination in the form of mercury(II) sulphide, HgS;74
8.2;7.4. Determination in the form of mercury(I) chloride, Hg2Cl2;79
8.3;7.5. Determination in the form of metallic mercury after reduction with ascorbic acid;81
8.4;7.6. Determination in the form of metallic mercury by electrolysis;82
8.5;7.7. Determination in the form of metallic mercury by a dry method;83
8.6;7.8. Determination of mercury (I) ions in the form of mercury (I) chromate Hg2CrO4;85
8.7;7.9. Determination of mercury (I) ions in the form of mercury(I) iodate;86
8.8;7.10. The separation of Hg;87
8.9;References;89
9;CHAPTER 8. COPPER – Cu – 63.54;91
9.1;8.1. Determination in the form of metallic copper by electrolysis;92
9.2;8.2. Determination in the form of copper (I) thiocyanate, CuSCN;98
9.3;8.3. The determination of copper by precipitation in the form of its sulphide;100
9.4;8.4. Determination of copper in the form of copper(I) iodide;106
9.5;8.5. Determination of copper in the form of copper(II) oxide, CuO;108
9.6;8.6. Determination of copper in the form of copper(II) quinaldinate (c10h6no2)2cu.h2o;110
9.7;8.7. Precipitation of copper(II) ions with 8-hydroxyquinoline;111
9.8;8.8. The separation of Cu;113
9.9;References;131
10;CHAPTER 9. BISMUTH – Bi – 208.98;134
10.1;9.1. Determination in the form of bismuth(III) oxide, Bi2O3;137
10.2;9.2. Precipitation in the form of basic bismuth carbonate, Bi(oH)Co3;137
10.3;9.3. Precipitation in the form of basic bismuth formate, Bio.OOCH;139
10.4;9.4. Determination in the form of bismuthyl chloride, BiOcl;141
10.5;9.5. Determination in the form of bismuthyl iodide, BiOI;142
10.6;9.6. Determination in the form of bismuth(III) phosphate, BiPo4;145
10.7;9.7. Determination in the form of bismuth(III) sulphide, Bi2S3;147
10.8;9.8. The deposition of metallic bismuth by electrolysis;149
10.9;9.9. Precipitation of bismuth in the metallic form using formaldehyde;150
10.10;9.10. The separation of Bi;151
10.11;References;158
11;CHAPTER 10. CADMIUM – Cd – 112.40;160
11.1;10.1. Determination in the form of cadmium sulphate;160
11.2;10.2. Determination in the form of cadmium sulphide, CdS;163
11.3;10.3. Determination by precipitation in the form of cadmium ammonium phosphate, CdNH4PO4.H2O;167
11.4;10.4. Deposition in the form of metallic cadmium by electrolysis;169
11.5;10.5. Determination in the form of cadmium hydrazine iodide, Cd(N2h4)2I2;172
11.6;10.6. Determination in the form of cadmium quinaldinate, Cd(C10h6N02)2;173
11.7;10.7. Precipitation of cadmium with 8-hydroxyquinoline;174
11.8;10.8. The separation of Cd;175
11.9;References;180
12;Group II Cations;182
13;CHAPTER 11. ARSENIC – As – 74.92;182
13.1;11.1. Determination of arsenic in the form of arsenic(III) sulphide, As2S3;184
13.2;11.2. Determination of arsenic in the form of arsenic(V) sulphide, As2S3;187
13.3;11.3. Determination in the form of arsenic(III) sulphide and sulphur, As2S3+2S;190
13.4;11.4. Precipitation in the form of magnesium ammonium arsenate,MgNH4aso4.6 h20;191
13.5;11.5. Determination in the form of silver arsenate, AgAsO4;197
13.6;The separation of As;199
13.7;References;214
14;CHAPTER 12. ANTIMONY – Sb – 121.75;216
14.1;12.1. Determination in the form of antimony(III) sulphide, Sb2S3;218
14.2;12.2. Determination in the form of antimony tetroxide, Sb2O4;224
14.3;12.3. The separation of Sb;226
14.4;References;228
15;CHAPTER 13. TIN – Sn – 118.69;230
15.1;13.1. Precipitation of tin in the form of stannic acid;232
15.2;13.2. Precipitation in the form of tin(IV) sulphide, SnS2;237
15.3;13.3. Determination by electrolysis from a solution containing oxalate;239
15.4;13.4. The separation of Sn;241
15.5;References;242
16;CHAPTER 14. GERMANIUM – Ge – 72.59;243
16.1;14.1. Separation of germanium from accompanying substances by distillation;246
16.2;14.2. Separation of germanium(IV) chloride, GeCl4, by extraction with carbon tetrachloride;246
16.3;14.3. Precipitation in the form of germanium(IV) sulphide, Ges2;247
16.4;14.4. Precipitation of germanium(IV) ions with tannin;249
16.5;14.5. Photometric determination of small amounts of germanium;250
16.6;14.6. Other methods for the determination of germanium;251
17;CHAPTER 15. GOLD – Au – 196.97;252
17.1;15.1. Determination in the form of metallic gold;253
17.2;15.2. The separation of Au;259
17.3;References;260
18;CHAPTER 16. PLATINUM AND THE PLATINUM METALS;262
18.1;16.1. Platinum;266
18.2;16.2. Precipitation of platinum in the form of ammonium hexachloroplatinate(IV);267
18.3;16.3. Determination of platinum by precipitation with hydrogen sulphide;269
18.4;16.4. Determination of platinum by reduction with formic acid;271
18.5;16.5. Determination by a fire-assay method;272
18.6;References;272
18.7;16.6. Ruthenium;272
18.8;16.7. Osmium;273
18.9;16.8. Palladium;273
18.10;16.9. Rhodium;274
18.11;16.10. Iridium;274
18.12;16.11. The separation of the platinum metals;277
18.13;References;277
19;CHAPTER 17. SELENIUM – Se – 78.96;278
19.1;17.1. Precipitation of selenium by reduction with hydrazine sulphate;281
19.2;17.2. Precipitat i on of selenium by reduction with sulphurous acid;282
19.3;17.3. The separation of Se;283
19.4;References;288
20;CHAPTER 18. TELLURIUM – Te – 127.60;289
20.1;18.1. Determination of tellurium by precipitation with hydrazine sulphate;291
20.2;18.2. Determination of tellurium by reduction with sulphurous acid;291
20.3;1S.3. Determination of tellurium by reduction with sodium hypophosphite;292
20.4;18.4. The separation of Te;292
20.5;References;293
21;Group III Cations;294
22;CHAPTER 19. ALUMINIUM – Al – 26.98;294
22.1;19.1. Determination in the form of aluminium oxide, Al2O3;296
22.2;19.2. Determination in the form of aluminium-8-hydroxyquinolate;313
22.3;19.3. Determination in the form of aluminium phosphate, AlPO4;316
22.4;19.4. Separation of the accompanying metallic chlorides from crystalline aluminium chloride, AlCl3.6H2O, by ether–hydrochloric acid extraction;318
22.5;19.5. The separation of Al;320
22.6;References;352
23;CHAPTER 20. IRON – Fe – 55.85;354
23.1;20.1. Precipitation in the form of iron(III) hydroxide,Fe(OH)3, and weighing as iron (III) oxide, Fe2O3;356
23.2;20.2. Precipitation of basic iron(III) salts by hydrolysis;362
23.3;20.3. Precipitation of iron(II) ions in the form of iron(II) sulphide, FeS;365
23.4;20.4. Precipitation of iron(III) ions with cupferron;366
23.5;20.5.-20.26. The separation of Fe;368
23.6;References;384
24;CHAPTER 21. CHROMIUM – Cr – 51.996;386
24.1;21.1. Determination in the form of chromium(III) oxide, Cr2O3;388
24.2;21.2. Determination of chrornate ions by precipitation in the form of mercury (I) chromate;393
24.3;21.3. Determination of chromate and dichromate ions in the form of barium chromate, BaCro4;394
24.4;21.4. Determination of chromate and dichromate ions in the form of silver chromate, AgcrO4;395
24.5;21.5. Determination of chromates in the form of lead chromate, PbCrO4;397
24.6;21.6. The separation of Cr;398
24.7;References;400
25;CHAPTER 22. NICKEL – Ni – 85.71;401
25.1;22.1. Determination in the form of the nickel dimethylglyoxime complex;403
25.2;22.2. Precipitation of nickel by electrolysis;407
25.3;22.3. The rapid determination of nickel in the form of its pyridine thiocyanate complex;408
25.4;22.4. Precipitation in the form of nickel sulphide, NiS;409
25.5;22.5. Precipitation of nickel with 8-hydroxyquinoline;412
25.6;22.6. The separation of Ni;413
25.7;References;420
26;CHAPTER 23. COBALT – Co – 58.93;421
26.1;23.1. Determination as metallic cobalt by electrolysis;423
26.2;23.2. Precipitation of cobalt sulphide from acetic acid medium;425
26.3;23.3. Precipitation in the form of cobalt (III) hydroxide, Co(OH)3;425
26.4;23.4. Determination in the form of tetrapyridinocobalt(II) thiocyanate;426
26.5;23.5. Determination of cobalt with á-nitroso-ß-naphtol;427
26.6;23.6. Separation of cobalt from nickel in the form of potassium cobaltinitrite, K3Co(No2)6;430
26.7;23.7. Precipitation of cobalt with 8-hydroxyquinoline;432
26.8;23.8. The separation of Co;433
26.9;References;436
27;CHAPTER 24. ZINC – Zn – 65.37;437
27.1;24.1. Precipitation of zinc ions in the form of zinc sulphide, ZnS;439
27.2;24.2. Determination by precipitation in the form of zinc ammonium phosphate, Zn(NH4)PO4;445
27.3;24.3. Determination in the form of metallic zinc by electrolysis;448
27.4;24.4. Determination in the form of zinc mercuric thiocyanate, ZnHg(SCN)4;449
27.5;24.5. Precipitation of zinc ions with 8-hydroxyquinoline;450
27.6;24.6. Determination in the form of zinc anthranilate, Zn(C7H6O2N)2;452
27.7;24.7. Precipitation of zinc in the form of zinc quinaldinate,Zn(C10H6NO2)2.H2O;454
27.8;24.8. The separation of Zn;455
27.9;References;465
28;CHAPTER 25. MANGANESE – Mn – 54.94;467
28.1;25.1. Precipitation in the form of manganese(II) sulphide, MnS;468
28.2;25.2. Precipitation in the form of manganese(II) ammonium phosphate, Mn(NH4)P04.H20;470
28.3;25.3. The separation of Mn;473
28.4;References;475
29;CHAPTER 26. TITANIUM – Ti – 47.90;476
29.1;26.1. Precipitation in the form of hydrated titanium(IV) oxide, Ti02(H20)n;478
29.2;26.2. Precipitation of titanium(IV) ions with cupferron;482
29.3;26.3. Precipitation of titanium(IV) ions with p-hydroxyphenylarsinic acid;484
29.4;26.4. The separation of Ti;485
29.5;References;489
30;CHAPTER 27. ZIRCONIUM (Zr – 9991.22) AND HAFNIUM (Hf –178.6);491
30.1;27.1. Precipitation in the form of hydrated zirconium dioxide, Zro2.NH2O;493
30.2;27.2. Determination in the form of zirconium phosphate, Zro(H2Po4)2;494
30.3;27.3. Precipitation of zirconium with mandelic acid;496
30.4;27.4. Simultaneous determination of zirconium and hafnium;498
30.5;27. The separation of Zr;499
30.6;References;503
31;CHAPTER 28. THORIUM – Th, AND THE RARE EARTHS – RE;505
31.1;28.1. Precipitation of thorium and the rare earths with ammonia;513
31.2;28.2. Precipitation of thorium and the rare earths with oxalic acid;515
31.3;28.3. The separation of thorium and the rare earths;517
32;CHAPTER 29. SCANDIUM – Sc – 44.956;524
32.1;29.1. Precipitation of scandium(III) hydroxide, Sc(OH)3, with ammonia;525
32.2;29.2. Precipitation of scandium in the form of its basic tartrate;525
32.3;29.3. Separation of scandium from other elements by ether extraction of scandium thiocyanate, Se(SCN)3;527
32.4;29.4. Photometric determination of small amounts of scandium;528
33;CHAPTER 30. NIOBIUM – Nb – 92.91 AND TANTALUM–Ta – 180.95;532
33.1;30.1. Determination in the form of tantalum(V) oxide, Ta2O5 + niobium(V) oxide, Nb2O5;536
33.2;30.2. The separation of Ta and Nb;538
33.3;References;541
34;CHAPTER 31. MOLYBDENUM – Mo – 95.94;543
34.1;31.1. Precipitation in the form of molybdenum(VI) sulphide, MoS3;545
34.2;31.2. Determination in the form of lead molybdate, PbMoO4;549
34.3;31.3. Determination in the form of silver molybdate, Ag2moO4;551
34.4;31.4. Determination in the form of molybdenum oxinate, MoO2(C9H6On)2;552
34.5;31.5. The separation of Mo;554
34.6;References;558
35;CHAPTER 32. TUNGSTEN – W – 183.85;559
35.1;32.1. Precipitation in the form of tungstic acid H2WO4.H2O;561
35.2;32.2. Precipitation in the form of mercury(I) tungstate, Hg2Wo4;564
35.3;32.3. Precipitation in the form of benzidine tungstate;565
35.4;32.4. Determination in the form of tungsten oxinate, Wo2(C9H6ON)2;567
35.5;32.5 The separation of W;567
35.6;References;572
36;CHAPTER 33. VANADIUM – V – 50.94;573
36.1;33.1. Precipitation in the form of mercury(I) vanadate, Hg2(Vo3)2;576
36.2;33.2. Determination in the form of silver vanadate, Ag3vo4;578
36.3;33.3. Precipitation in the form of vanadium cupferronate;579
36.4;33.4. The separation of V;581
36.5;References;583
37;CHAPTER 34. UBANIUM – U – 238.03;584
37.1;34.1. U(VI) – Separation of uranium from Cu, Bi, Pb, As, Sb and other cations of groups I and I I;586
37.2;34.2. U(VI) – Separation of uranium from iron(III) and the cations whose carbonates are insoluble in water;586
37.3;34.3. U(VI) Separation of uranium by ether extraction;586
37.4;34.4. Separation of uranium with cupferron;588
37.5;34.5. Determination of uranium by precipitation in the form of ammonium diuranate, (NH4)2U7O7;588
37.6;34.6. Precipitation in the form of uranium(IV) cupferrate, U(C6H502N2)4. Analysis of pitch blende;590
37.7;34.7. Determination in the form of uranyl oxinate, U02(C9H6NO)2C9H7NO;592
37.8;34.8. Other separations of U;595
37.9;References;596
38;CHAPTER 35. THALLIUM – TI – 204.39;597
38.1;35.1. Determination in the form of thallium(I) chromate, TI2Cr04;600
38.2;35.2. Determination in the form of thallium(I) iodide, TlI;601
38.3;35.3. Determination in the form of thallium(III) oxide, T!203;603
38.4;35.4. The separation of Tl;604
38.5;References;607
39;CHAPTER 36. INDIUM – IN –114.82;609
39.1;36.1. Precipitation in the form of indium(III) hydroxide, In(OH)3;612
39.2;36.2. Determination in the form of indium(IH) sulphide, In2S3;613
39.3;36.3. Determination in the form of indium(III) oxinate, In(CgH6ON)3;615
39.4;36.4. Separation of indium from the accompanying ions by extraction;616
39.5;36.5. Determination of indium by polarography;617
39.6;References;617
40;CHAPTER 37. GALLIUM – GA – 69.72;619
40.1;37.1. Precipitation of gallium(III) hydroxide with ammonia and by other hydrolysis methods;622
40.2;37.2. Precipitation with cupferron;625
40.3;37.3. Determination of gallium by precipitation with 8 -hydroxyquinoline ;626
40.4;37.4. Determination of gallium with 5-7-dibromo- 8-hydroxyquinoline;627
40.5;37.5. Precipitation of gallium in the form of its camphoric acid salt;627
40.6;37.6. Separation of gallium from other ions by ether extraction;628
40.7;37.7. Other Separation of gallium Ga–Fe(Al) ;629
40.8;References;630
41;CHAPTER 38. BERYLLIUM – Be – 9.012;631
41.1;38.1. Precipitation of beryllium in the form of beryllium hydroxide, Be(OH)2;633
41.2;38.2. Determination of beryllium in the form of beryllium pyrophosphate, Be2P207;638
41.3;38.3. The separation of Be;640
41.4;References;641
42;Group IV Cations;642
43;CHAPTER 39. CALCIUM – Ca – 40-08;642
43.1;39.1. Precipitation in the form of calcium oxalate, CaC204 · H20;645
43.2;39.2. Precipitation in the form of calcium molybdate, CaMo04;655
43.3;39.3. The separation of Ca;656
43.4;References;671
44;CHAPTER 40. STRONTIUM;673
44.1;40.1. Determination in the form of strontium oxalate, SrC204-H20;674
44.2;40.2. Determination in the form of strontium sulphate, SrS04;676
44.3;40.3. Determination in the form of strontium carbonate, SrC03;678
44.4;40.4. The separation of Sr;679
44.5;References;683
45;CHAPTER 41. BARIUM – Ba – 134-34;684
45.1;41.1. Determination in the form of barium sulphate, BaS04;685
45.2;41.2. Determination in the form of barium chromate, BaCr04;696
45.3;41.3. The separation of Ba;698
45.4;References;704
46;Group Y Cations;705
47;CHAPTER 42. MAGNBSIUM – Mg – 24-31;705
47.1;42.1. Precipitation in the form of crystalline magnesium ammonium phosphate, MgNH4P04· 6H20;706
47.2;42.2. Precipitation in the form of magnesium oxinate, Mg(C9HeON)2-4 H20;712
47.3;42.3. The separation of Mg;716
47.4;References;724
48;CHAPTER 43. SODIUM – Na – 22.99;725
48.1;43.1. Determination in the form of sodium chloride, NaCl;727
48.2;43.2. Determination in the form of sodium sulphate, Na2S04;728
48.3;43.3. Determination in the form of sodium zinc uranyl acetate, NaZn(U02)3.(C2H302)9.6-5 B2O;730
48.4;43.4. Determination in the form of sodium magnesium uranyl acetate, NaMg(U02)3(c2H302)9-6.5 H20;733
48.5;References;735
49;CHAPTER 44. POTASSIUM – K – 39.10;736
49.1;44.1. Determination in the form of potassium chloride, KCl;738
49.2;44.2. Determination in the form of potassium sulphate, K2S04;739
49.3;44.3. Determination in the form of potassium hexachloroplatinate( IV), K2PtCl6;740
49.4;44.4. Determination in the form of potassium perchlorate, KClo4;744
49.5;44.5. Determination in the form of potassium tetraphenylborate, K[B(C6H5)4];747
49.6;References;751
50;CHAPTER 45. LITHIUM – LI – 6.94;753
50.1;45.1. Determination in the form of lithium chloride, LiCl;754
50.2;45.2. Determination in the form of lithium sulphate, li2so4;755
50.3;References;755
51;CHAPTER 46. AMMONIUM ION – NH+4 – 18.039;756
51.1;References;757
52;CHAPTER 47. METHODS OF SEPARATION OF THE CATIONS OF THE ALKALI METAL GROUP;758
52.1;47.1. Na, K – Separation of sodium and potassium from cations of the groups I–IV and magnesium;758
52.2;47.2. Separation of sodium from potassium and simultaneous determination;763
52.3;47.3. Separation of lithium from Na, K, (Rb, Cs) by extraction;769
52.4;47.4. Separation and determination of lithium and sodium by indirect analysis;773
52.5;47.5. Separation and determination of lithium and potassium by indirect analysis;774
52.6;47.6. Separation of Na, K, Li, from SOI", PO|~;774
52.7;47.7. Separation of Na, K, Li from complex cyanides;775
52.8;47.8. Separation of Na, K, Li from other ions;775
52.9;47.9. Separation of NHJ from other ions;776
53;Author Index;778
54;Subject Index;790
55;Other Titles in the Series;814