Practical Inorganic Chemistry | O. J. Vorobyova, K. M. Dunaeva, E. A. Ippolitova, N. S. Tamm, V. I. Spitsyn (Ed.)

In this post we will see a book titled Practical Inorganic Chemistry by O. J. Vorobyova, K. M. Dunaeva, E. A. Ippolitova, and N. S. Tamm and was edited by V. I. Spitsyn.

Students using the
present textbook will acquaint themselves with procedures of work
in a modern laboratory. The latter include the carrying out of operations
in vacuum, synthesis in non-aqueous solvents, the conducting
of reactions in a gaseous medium (a fluidized bed, "transport" reactions)
or in liquefied gases, photolytic reduction and oxidation, and
the preparation of pure substances (sublimation, recrystallization,
extraction, chromatography, and distillation). Students will acquire
skill in handling glass and quartz ware on standard joints, cryostats,
thermostats, "dry" chambers, and simple measuring instruments.

The present book devotes a lot of space to the synthesis of the
most important inorganic compounds and the chemistry of the
elements. Since the book contains a large number of experiments and
syntheses, they cannot be performed by the students during the time
allotted for practical work, and the authors have divided the laboratory
works of each chapter into two parts. The first describes the
obligatory experiments, and the second, supplementary experiments
and syntheses.

The large number of diverse syntheses in the book enable the instructor
to vary the assignments to the students and thus expand
their chemical outlook.

The book was translated from the Russian by G. Leib and was first published by Mir in 1987.

All credits to the original uploader.

Contents:

Preface

1 Work in a Laboratory and Technique of an Experiment
1.1
1.1 Procedure of Work in a Laboratory
Laboratory Notebook (17).
Safety (18).
First Aid (18).
Laboratory Ware (19).
Heating Equipment (22).

1.2 Technique of Laboratory Work

Temperature Control (26).
Temperature Measurement and Heating Procedures (26).
Filtration (28).
Work with Laboratory Ware on Ground Joints (32).
Drying of Solids (33).
Drying of Organic Solvents (34).
Balances and Weighing (36).
Work with Glass (39).
Stoppers (40).
Producing a Vacuum (41).
Vacuum Measurement (44).
Apparatus Assembly (45).

2 Purification of Substances 47

2.1 Solids 47
Recrystallization (47).
Sublimation (48).
2.2 Purification and Distillation of Liquids
2.3 Gases
2.4 Separation and Purification of Inorganic Compounds by Ion-Exchange Chromatography
2.5 Separation and Purification of Inorganic Compounds by Extraction

3 Determination of Molecular and Atomic Masses and of Chemical 53
3.1 Molecular Masses of Gaseous Substances
3.2 Equivalents Determination of Molecular Masses of Volatile Liquids from Their Vapour Density (56)
3.3 Determination of Chemical Equivalents and Atomic Masses of Metals (58)
Determination of the Atomic Mass of Lead (60).

4 Oxygen 62

4.1 Preparation
4.2 Properties

Supplementary Experiments

Ozone (64).

5 Hydrogen 66

5.1 Preparation 66
5.2 Properties 68
5.3 Hydrogen Peroxide 69

6 Rate of Chemical Readions 70

6.1 Rate of Homogeneous Reactions 70

Effect of Reactant Concentration on Reaction Rate (70).
Effect of Catalyst on Reaction Rate (71).
Effect of Temperature on Reaction Rate (72).

6.2 Rate of Heterogeneous Reactions

Effect of the Degree of Reactant Mixing on the Reaction Rate (73).

Supplementary Experiments

1. Effect of the Surface Area on the Reaction Rate (74).
2. Effect of Light on the Decomposition of Silver Chloride (74).

7 Chemical Equilibrium 74

7.1 Effect of Reactant Concentration
7.2 Effect of Temperature

Supplementary Experiment

Reaction of Potassium Chloride with Nitric Acid (75).

8 Solutions 76

8.1 Solubility of Salts 76
8.2 Effect of Temperature on Salt Solubility 77
8.3 Preparation of Supersaturated Solutions 78
8.4 Thermal Phenomena in Dissolution of Salts 78

Supplementary Experiments 78

1. Change in Volume in Dissolution (78).
2. Determining Solubility of Air in Water (79).
3. Osmosis (80).
4. Determining the Freezing Point of Water (81).
5. Determining the Temperature of Water Crystallization from Aqueous Sugar and Sodium Chloride Solutions (82).
6. Determining the Cryohydrate Point (82).

9 Electrolytic Dissociation 82

9.1 Electrical Conductance of Solutions 83
9.2 Comparison of the Strength of Acids and Bases 83
9.3 Change in the Hydrogen and Hydroxyl Ion Concentration 86
9.4 Hydrolysis of Salts 87
9.5 Solubility Product 87

10 Electrochemical Properties of Solutions 88;

10.1 Electrochemical Series
10.2 Electrolysis

11 Halogens. Preparation and Properties 90·

11.1 Chlorine

Preparation Methods (90).
Preparation and Studying of Properties (91).

11.2 Bromine

Preparation (94).
Properties (94).

11.3 Iodine

Preparation (95).
Properties (96).

11.4 Fluorine

11.5 Hydrogen Compounds of the Halogens

Hydrogen Chloride (97).
Hydrogen Bromide (97).
Hydrogen Iodide (98).
Hydrogen Fluoride (98).

11.6 Oxygen Compounds of the Halogens

Chlorinated Lime (Bleaching Powder) (100).
Potassium Chlorate (100).
Iodic Acid (101).

11.7 Comparison of Oxidizing Properties of the Halogens

Supplementary Experiments and Syntheses
1. Preparation of Chlorine by Reacting Oxygen with Hydrogen Chloride (102).
2. Preparation of Purified Iodine (103).
3. Preparation of Iron(III) Chloride (104).
4. Preparation of Nickel, Cobalt, or Chromium Chloride (105).
5. Preparation of Ammonium Iodide (106).
6. Preparation of Potassium Iodide (107).
7. Preparation of Cadmium Iodide (107).
8. Preparation of Potassium Bifluoride (108).
9. Preparation of Potassium Bromate (108).
10. Preparation of Iodic Acid (109).
11. Preparation of Iodine Trichloride (109).
12. Preparation of Tetrachloroiodic Acid Tetrahydrate (110).
13. Preparation of Potassium Tetrachloroiodate Dihydrate (110).

12 Sulphur, Selenium, Tellurium

12.1 Sulphur and Its Compounds

Properties of Sulphur (111).
Hydrogen Sulphide (111).
Metal Sulphides (112).
Sulphurous Acid Anhydride (113).
Sulphuric Acid and Its Salts (114).
Sodium Thiosulphate (115).

12.2 Selenium and Tellurium
Selenium(IV) and Tellurium(IV) Oxides (116).

Supplementary Experiments and Syntheses

1. Preparation of Hydrogen Sulphide from Its Elements (117).
2. Preparation of Sodium Bisulphide (118).
3. Preparation of Sodium Sulphide (119).
4. Preparation of Sulphur Chlorides (119).
5. Preparation and Purification of Sulphur Monochloride (120).
6. Preparation of Thionyl Chloride (121).
7. Preparation of Sulphuryl Chloride (122).
8. Preparation of Sulphuric Acid by the Contact Process (123).
9. Preparation of Sulphuric ,Acid by the Chamber Process (124).
10. Preparation of Copper Sulphate Pentahydrate (Copper Vitriol) (125).
11. Preparation of Potassium Persulphate (125).
12. Preparation and Properties of Selenium(IV) Oxide (126).
13. Preparation and Properties of Tellurium(IV) Oxide (127).

13 Nitrogen 128

13.1- Preparation and Properties
13.2 Compounds

Ammonia (128).
Ammonium Salts (129).
Hydrazine and Hydroxylamine (130).
Oxygen Compounds (130).
Nitrous Acid (132).
Nitric Acid (133).

Supplementary Experiments and Syntheses
1. Liquefaction of Ammonia and Studying of Its Properties (134).
2, 3. Preparation of Magnesium Nitride by Reacting Magnesium with Nitrogen (136) and Ammonia (137).
4. Preparation of Lithium Nitride by Reacting Lithium with Nitrogen (138).
5. Preparation of Hydrazine Sulphate (139).
6. Preparation of Hydrazine Hydrate (139).
7. Preparation of Hydrazine (140).
8. Preparation of Hydroxylamine Chloride (141).
9. Preparation of Nitrogen(IV) Oxide and Nitrous Acid Anhydride (141).
10. Preparation of Nitrosyl Chloride by Reacting Nitrogen(II) Oxide with Chlorine in the Presence of an Activated Carbon Catalyst (142).
11. Preparation of Nitrosyl-Sulphuric Acid (Nitrosonium Bisulphate) (143).
12. Preparation of Nitrosyl Chloride by Reacting Nitrosyl Sulphuric Acid with Sodium Chloride (143).
13. Preparation of Nitric Acid by Oxidizing Ammonia (144).
14. Preparation of Anhydrous Nitric Acid (144).
15. Preparation of Potassium Nitrite (145).
16. Preparation of Anhydrous Copper Nitrate (146).

14 Phosphorus 147
14.1 Allotropy
14.2 Properties
14.3 Compounds
Hydrogen Phosphide (149).
Phosphorous Anhydride and Phosphorous Acid (149).
Phosphoric Anhydride (150).
Phosphoric Acids (151).
Salts of Phosphoric Acids (153).
Phosphorus Halides (153).

Supplementary Experiments and Syntheses
1. Burning of Phosphorus under Water (155).
2. Preparation of Hydrogen Phosphide (155).
3. Preparation of Phosphonium Iodide (155).
4. Preparation of Hypophosphorous Acid (156).
5. Preparation and Separation of Phosphorus Tri- and Pentachlorides (157).
6, 7. Preparation of Phosphorus Tribromide by Reacting White Phosphorus with Bromine (159), Red Phosphorus
with Bromine (161).
8. Preparation of Phosphorus Iodide $\latex P_{2}I_{4}$ (161).
9. Preparation of Phosphorus Thiochloride (162).

15 Carbon 162

Compounds 162
Carbon(IV) Oxide (162).
Salts of Carbonic Acid (163).
Carbon(II) Oxide (163).
Carbides (165).

Supplementary Experiments and Syntheses

1. Preparation of Activated Carbon (165).
2. Comparison of Adsorptivity of Activated and Non-Activated Carbon (165).
3. Preparation of "Dry" Ice (166).
4, 5. Preparation of Calcium Carbide in an Electric Arc Furnace (166) and by Reacting Metallic Calcium with Carbon (167).
6. Preparation of Chloroform (167).

16 The Colloidal State of Substances 168

16.1 Preparation of Colloidal Solutions 170
Condensation (168).
Dispersion (169).

16.2 Properties of Colloids
Tyndall Effect (170).
Adsorption of Coloured Substances (170).
Dialysis (171).
Coagulation of an Iron(III) Hydroxide Sol (171)

17 Silicon 171

17.1 Preparation and Properties
17.2 Compounds
Silicates (172).
Silicic Acids (173).
Fluosilicic Acid (173).

Supplementary Experiments and Syntheses

1. Preparation of Crystalline Silicon (173).
2. Preparation of Silicic Acid Anhydride (174).
3. Preparation of Silicon Tetrachloride (174).
4. Preparation of Silicochloroform (175).

18 Boron 176

18.1 Preparation and Properties
18.2 Compounds

Boric Acid (177).
Boric Acid Anhydride (177).
Coloured Borax Beads (178).

Supplementary Experiments and Syntheses
1. Preparation of Boron Trichloride by Reacting Aluminium Trichloride with Boron Trifluoride (178).
2. Preparation of Boron Tribromide (179)

19 Alkali Metals 180

19.1 Properties 180
19.2 Compounds
Oxides (181).
Hydroxides (182).
Salts (182).

Supplementary Experiments and Syntheses
1. Preparation of Metallic Cesium (Rubidium) (183).
2. Preparation of Lithium Hydride (184).
3. Preparation of Lithium Peroxide (185).
4. Preparation of Sodium Peroxide (187).
5. Preparation of Lithium Iodide (187).
6. Preparation of Potassium Hydroxide by the Electrolysis of a Potassium Chloride Solution (188).
7. Preparation of Sodium Sulphate and Its Hydrates (188).
8. Determining the Transition Temperature of Sodium Sulphate Decahydrate to the Anhydrous Salt (188).
9. Preparation of Potassium Nitrate (189).

20 Beryllium, Magnesium, Calcium, Strontium, Barium

20.1 Beryllium, Magnesium, and Their Compounds
Hydroxides (190).
Carbonates (191).
Beryllium Oxyacetate (191).
Magnesium Ammonium Phosphate (192).

20.2 Calcium, Strontium, Barium

Supplementary Experiments and Syntheses
1. Preparation of Barium Peroxide (193).
2. Preparation of Calcium Hydride (193).
3. Preparation of Magnesium Chloride Hexahydrate (194).
4. Preparation of Anhydrous Magnesium Chloride (194).
5. Preparation of Anhydrous Magnesium Chloride by Reacting Hydrogen Chloride with Magnesium in Absolute Ethanol (194).
6. Preparation of Magnesium Iodide (195).
7. Preparation of Calcium Chloride Hydrate (196).
8. Processing of Barium Sulphate into Barium Chloride (197).
9. Preparation of Magnesium Perchlorate (197).
10. Preparation of Magnesia Cement (198).
11. Determining the Hardness of Water (198).
12. Solutions Used in Hardness Determination (199).

21 Aluminium 201

21.1 Properties 201
21.2 Compounds 201
Aluminium Hydroxide (201).
Potassium Aluminium Alum (201).
Other Compounds (201).

Supplementary Experiments and Syntheses
1. Preparation of Iron by Aluminothermic Process (202).
2. Preparation of Aluminium Hydroxide (202).
3. Preparation of Sodium Aluminate (203).
4. Preparation of Aluminium Sulphate from Kaolin (203).
5. Preparation of Aluminium Chloride in a Fluidized Bed (203).
6. Preparation of Aluminium Bromide (204).

22 The Rare-Earth Elements 205

22.1 Cerium(III) Compounds 205.
Hydroxide (205).
Salts (205).

22.2 Cerium(IV) Compounds
Hydroxide (206).
Salts (206).

Supplementary Experiment
Preparation of Cerium(III) Sulphate by the Photochemical Reduction of Cerium(IV) Compounds with Ethanol (206).

23 Titanium, Zirconium, Hafnium 206

23.1 Titanium(IV) Compounds 207
23.2 Titanium(IIl) Compounds 207

Supplementary Experiments and Syntheses 208
1. Preparation of Titanium Tetrachloride and Studying of Its Properties (208).
2. Preparation of Zirconium (Hafnium) Bromide (Iodide) (209).
3. Preparation of Ammonium Heptafluozirconate(IV) (210).

24 Vanadium, Niobium, Tantalum 210

24.1 Vanadium Compounds 211

Supplementary Experiments and Syntheses 212
1. Preparation of Vanadium by the Aluminothermic Process (212).
2. Preparation of Vanadium(V) Oxide (212).
3. Preparation of Sodium Vanadate (212).
4. Preparation of Vanadium Oxychloride and Studying of Its Properties (212).
5. Preparation of Ammonium Fluovanadate(III) (213).
6. Preparation of Anhydrous Dioxovanadium Nitrate (V0 2NO a) (214).
7. Preparation of Niobium (Tantalum) Chloride and Purification from Iron Impurities (214).

25 Chromium, Molybdenum, Tungsten, Uranium 215

25.1 Chromium
Chromium(II) Compounds (215).
Chromium(III) Compounds (216).
Chromium(VI) Compounds (218).

25.2 Molybdenum and Tungsten Compounds

25.3 Uranium Compounds

Supplementary Experiments and Syntheses

1. Preparation of Chromium (221).
2. Properties of Chromium (222).
3. Preparation of Chromium(II) Acetate (222).
4. Preparation of Chromium(III) Chloride Hydrate (223).
5. Preparation of Anhydrous Chromium(III) Chloride (224).
6. Preparation of Chromium (III) Nitride (224).
7. Preparation of Chromium (III) Sulphide (224).
8. Preparation of Potassium Trioxalatochromate(III) (225).
9. Preparation and Properties of Chromyl Chloride (225).
10. Preparation of Potassium Chlorochromate (225).
11. Preparation of Chromium(VI) Oxysulphate (225).
12. Preparation and Properties of Molybdenum (Tungsten) (227).
13. Preparation of Molybdenum(VI) Oxide (227).
14. Preparation of Sodium Paramolybdate (229).
15. Preparation of Normal Ammonium Tungstate (229).
16. Preparation of Sodium Paratungstate (229).
17. Preparation of Sodium Metatungstate (229).
18. Preparation of Tungsten Bronzes (230).
19. Preparation of Potassium Hexachloromolybdate(III) (231).
20. Preparation of Molybdenum Pentachloride and Tungsten Hexachloride (232).
21. Preparation of Molybdenum(III) Bromide (233).
22. Preparation of Uranium(IV) Fluoride (233).
23. Preparation of Uranium(IV) Chloride (234).

26 Manganese 235

26.1 Manganese(II) and Manganese(IV) Compounds
26.2 Manganese(VI) and Manganese(VII) Compounds

Supplementary Experiments and Syntheses
1. Preparation of Manganese by the Aluminothermic Process (237).
2. Preparation of Manganese Chloride in an Ethanol Solution (238).
3. Preparation of Manganese Oxalate (238).
4. Preparation of Manganese(II) Oxide (238).
5. Preparation of Sodium Manganate(V) (239).
6. Preparation of Sodium Manganate(VI) by the Solid-Phase Reaction of Manganese Dioxide with Sodium Peroxide (239).
7. Preparation of Potassium Permanganate by the Hydrolysis of Potassium Manganate (240).
8. Preparation of Potassium Permanganate by the Anodic Oxidation of Manganese (240).

27 Iron, Cobalt, Nickel 241

27.1 Properties
27.2 Compounds
Preparation and Properties of Hydroxides (241).
Salts (242).
27.3 Complex Compounds
Compounds with Complex Cations (244).
Compounds with Complex Anions (245).

Supplementary Experiments and Syntheses
1. Preparation of Reduced Iron (Cobalt, Nickel) (245).
2. Preparation of Pyrophoric Iron (246).
3. Preparation of Iron(II) Oxide (246).
4. Preparation of Macrocrystalline Iron(III) Oxide (246).
5. Preparation of Nickel(III) Oxide (247).
6. Preparation and Properties of Sodium Ferrite (247).
7. Preparation of Anhydrous Cobalt (Nickel) Chloride in an Ethanol Solution (247).
8. Preparation of Anhydrous Iron(III) Chloride in a Fluidized Bed (247).
9. Preparation of Potassium Trioxalatoferrate(III) (247).
10. Preparation of Tetraamminecarbonatocobalt(III) Nitrate (248).
11. Preparation of Ammonium Hexafluocobaltate(II) (248).
12.Preparation of Hexaaminenickel(II) Chloride (248).
13. Preparation of Nickel Carbonyl (249).

28 Copper, Silver, Gold 250
28.1 Copper 250
Copper(I) Compounds (251). Copper(II) Compounds (252)

28.2 Silver 253
Properties (254).
Compounds (254).
Silver Plating (255)

28.3 Gold 255
Properties (255).
Compounds (256).

Supplementary Experiments and Syntheses 256
1. Preparation of Copper(II) Fluoride (256).
2. Preparation of Copper(II) Nitride (256).
3. Preparation of Copper(II) Bromide (257).
4. Preparation of Copper(II) Acetylide (257).
5. Preparation of Silver from Silver Chloride (257).

29 Zinc, Cadmium, Mercury 258

29.1 Zinc and Cadmium Compounds 258

29.2 Mercury Compounds (259)

Supplementary Experiments and Syntheses 260
1. Preparation of Zinc Amalgam (260).
2. Preparation of a Low Melting Alloy (260).
3. Preparation of Zinc Chloride (260).
4. Preparation of Zinc Oxychloride (261).
5. Preparation of Zinc Choride Crystallohydrate (261).
6. Use of Zinc Chloride in Soldering (262).
7. Preparation of Zinc Iodide in Absolute Ether (262).
8. Preparation of Zinc Oxyacetate (262).
9. Preparation of Crystalline Cadmium Sulphide (263).
10. Preparation of Autocomplex Cadmium Iodide (263).
11. Preparation of Cadmium Pigments (263).
12. Purification of Mercury by Filtration (264).
13. Chemical Purification of Mercury (264).
14. Preparation of Mercury (I) Nitrate (264).
15. Preparation of Mercury (II) Nitrate (264).
16. Preparation of Mercury(II) Iodide (264).

30 Tin, Lead 265
30.1 Tin 265-
30.2 Lead 266-
Oxides and Hydroxides (266).
Salts and Their Properties (267).

Supplementary Experiments and Syntheses 267
1. Preparation of Tin by Reduction with Charcoal (267).
2. Preparation and Properties of Tin (II) Oxide (267). 3,
4. Preparation of $latex \alpha$ and $latex \beta$ Stannic Acid (268).
5. Preparation of Tin(II) Chloride (268).
6. Preparation of Tin (IV) Chloride (268).
7. Preparation of Chlorostannic Acid (268).
8. Preparation of Ammonium Chlorostannate (269).
9. Soldering (269).
10. Preparation of Lead (270).
11. Properties of Lead (270).
12. Preparation of Lead(II) Oxide (Yellow and Red Modifications) (270).
13. Preparation of Lead(II) Acetate (Lead Sugar) (271).
14. Preparation and Properties of Lead(lV) Oxide (271).
15. Preparation and Properties of Red Lead Oxide (Minium) (271).
16. Preparation of Ammonium Hexachloroplumbate (272).
17. Preparation of Lead Tetrachloride (272).
18. Preparation of Lead Tetraacetate (272).

31 Arsenic, Antimony, Bismuth 273
31.1 Arsenic 273
31.2 Antimony 275
31.3 Bismuth 276
Supplementary Experiments and Syntheses 276
1. Preparation of Antimony (276).
2. Preparation of Antimony(V) Oxide (277).
3. Preparation of Antimony(III) Iodide (277).
4. Preparation of Bismuth and Studying of Its Properties (277).

Appendix 1. Selected Tables 278

Appendix 2. CCourse Projects in Inorganic Chemistry 303,

Literatur