Practical Inorganic Chemistry By Geoffrey Pass (informative)

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Geoffrey Pass
Table of Contents in Practical Inorganic Chemistry By Geoffrey Pass
Preface to the Second Edition
Preface to the First Edition
1. Typical elements
Ion size effects
The preparation of caesium dichloroiodide
Preparation: caesium dichloroiodide
The preparation of barium peroxide
Lattice energy effects
The preparation of lithium nitride
Ionization energy
The preparation of a cationic iodine compound
Preparation: dipyridineiodine(I) nitrate
Electronegativity effects
The preparation of silicon tetrachloride
Variation of bond character with oxidation state
The preparation of tin(II) chloride, and tin(IV) chloride
Preparations: tin(II) chloride
tin(IV) chloride
Charge transfer effects
The preparation of tin(IV) iodide
Preparation: tin(IV) iodide
Coordination compounds of nontransition elements
The preparation of chelate complexes of aluminium
Preparations: potassium trioxalatoaluminate
tris( acetylacetonato )aluminium
2. Oxo-acids and oxo-acid salts
Introduction
Preparations: chloric acid
iodine pentoxide
tellurium dioxide
Preparations: chromyl chloride
Bibliography
potassium monochlorochromate
sodium peroxoborate
sodium polymetaphosphate
sodium tripolyphosphate
sodium trimetaphosphate
zinc dithionite
barium dithionate
sodium thiosulphate
3. High temperature reactions
Introduction
Thermodynamic considerations
Reaction rates
Preparations: lithium nitride
barium peroxide
silicon tetrachloride
chromium metal
Bibliography
4. The elements of the first transition series
Introduction
Reactions of titanium
Reactions of vanadium
Reactions of chromium
Reactions of manganese
Reactions of iron
Reactions of cobalt
Reactions of nickel
Reactions of copper
General questions
Bibliography
S. The preparation of some manganese compounds
Introduction
Preparations: manganese(II) chloride
potassium trioxalatomanganate(III)
manganese(lII) phosphate
tris(acetylacetonato )manganese(III)
potassium manganate
potassium permanganate
6. Coordination chemistry I: typical compounds
Introduction S6
Preparations: potassium trioxalatochromate(III) S7
iron(II) oxalate S8
ferrocene 59
bis(N,N-diethyldithiocarbamato )nitrosyliron 61
Bibliography 62
7. Clathrate compounds
Introduction 63
Preparations: a sulphur dioxide-quinol clathrate compound (with detection of sulphur dioxide
by gas liquid chromatography) 64
a dicyanoamminenickel(II) clathrate compound (with separation of benzene and
p-xylene, and detection of the guest
molecule by gas liquid chromatography) 6S
Bibliography 67
8. Double salts
Introduction
Preparations: ammonium nickel(II) sulphate
ammonium copper(II) sulphate
9. The stabilization of oxidation states
Introduction 71
Insoluble compounds 72
Soluble compounds 73
Preparations: copper(I) chloride 7S
copper(I) tetraiodomercurate(II) 76
tris(thiourea)copper(I) sulphate 77
tetrapyridinesilver(II) peroxodisulphate 79
hexamminecobaIt(III) chloride 80
10. Electrochemical oxidation and reduction
Overpotential and discharge potential
Cell construction
Cell current and current density
Apparatus
Preparations: potassium peroxodisulphate
potassium chlorate
Preparations: tetrapyridinesilver(II) nitrate
titanium(III) chloride
Bibliography
11. Coordination chemistry II: stereochemistry
Introduction 91
Geometrical isomerism 91
The Trans effect 93
Preparations: cis- and trans-potassium dioxalatodiaquachromate(III) 94
tris( ethylenediamine )chromium(III)
chloride and cis-dichlorobis(ethylenediamine)chromium(III) chloride 96
tris( ethylenediamine )chromium(III) thiocyanate monohydrate and trans-dithiocyanato bis( ethylenediamine )chromi um(III)
thiocyanate 98
cis-dichlorodipyridineplatinum(II) 99
Optical isomerism 100
Resolution into optical isomers 102
Resolution: cis-dichlorobis( ethylenediamine )chromi um-(III) chloride 103
Preparation and resolution: tris(ethylenediamine)cobalt-(III) ion 104
Ionization and hydrate isomerism 105
The preparation of the hydrate isomers of chromium(III)
chloride hexahydrate 106
Preparations: chloropentaquachromium(III) chloride 106
hexaquachromium(III) chloride 106
Linkage isomerism 107
Preparations: chloropentamminecobalt(III) chloride 107
nitro- and nitrito-pentamminecobalt (III)
chloride 108
dithiocyanato bis( triphenylarsine )palladium(II) 109
Bibliography 110
12. Homogeneous catalysis
Introduction 111
Experiment: the cobalt(II) bromide catalysed oxidation 112
ofp-xylene
A simple flow-meter construction 116
Preparations: dichlorobis(benzonitrile )palladium(II) and
di-“,-chloro-dichlorodiethylenedipalladium(II) 117
Experiment: the pentacyanocobaltate(II) ion catalysed
hydrogenation of buta-l,3-diene 118
13. Chemistry in non-aqueous solvents
Introduction
Ammonia
Experiments
Preparations: potassium tetracyanonickelate(Il)
potassium tricyanonickelate(l)
Dinitrogen tetroxide
Preparations: dinitrogen tetroxide
anhydrous copper(II) nitrate
Bibliography
14. Inorganic polymers
Introduction 133
Preparations: cyclic and linear polysiloxanes 135
diphenylsilanediol 136
The preparation and polymerization of phosphonitrilic
chloride 137
Bibliography 138
15. High vacuum techniques in chemistry
Introduction 139
Operating procedure 140
Transfer of gases to and from the system 142
Molecular weight determination 142
Spectroscopic measurements 144
Measurement of vapour pressure-temperature data 144
Experiments and
preparations: boron trifluoride with ammonia 146
nitrosonium hexachloroantimonate 148
nitrosyl chloride 148
Experiments and
preparations: nitrosyl chloride with antimony pentachloride 149
amidosulphuric acid 150
Bibliography 151
16. Inert atmosphere tecbniques
Introduction 152
Production of the inert atmosphere
Transfers to and from the glove box
The preparation of organometallic compounds
Preparations: phenyllithium
Bibliography
tetraphenyllead
triphenyllead chloride
diphenyllead dichloride
N-trimethylborazine
17. Spectroscopic tecbniques
Introduction 161
Units 162
Energy and transitions 163
Infrared spectroscopy 164
Group vibrations 165
Instrumentation 166
Sample preparation 168
Experiments 172
Electronic spectra of coordination compounds 173
The spectrochemical series 176
Instrumentation 176
Sample preparation 177
Experiments: determination of flo for the hexaquatitanium(III) ion 177
construction of part of the spectrochemical series 178
Colorimetry 179
Introduction 179
Colorimetric determination of chromium 182
Colorimetric determination of potassium permanganate 182
Experiments: rate of isomerization of trans-potassium
dioxalatodiaquachromate(I1I) to the cisisomer
Experiments: determination of the composition of complex ions in solution (Job’s method) 185
composition of the iron(III)-salicylic acid
complex 188
Bibliography 189
18. Conductance measurements
Introduction 190
Measurement of conductance 191
The cell constant 191
Preparation of the electrodes 192
The determination of the cell constant 192
Preparations and
measurements: trinitrotriamminecobalt(III) 193
the compound Co(NH3)3CI3 H2 0 193
conductivity of trinitrotriamminecobalt-
(III) and of the compound Co(NH3hCl3
H 20 194
Bibliography 194
19. Separation techniques
Introduction 195
Ion exchange 195
Experiment: Determination of the charge on the dioxalato-
diaquachromate(III) ion 197
Chromatography 198
Solid-liquid chromatography 198
Experiment: separation of hexamminecobalt(III) chloride
from chloropentamminecobalt(III) chloride
Gas chromatography
Experiments
Bibliography
20. Magnetic measurements
Introduction
The determination of magnetic susceptibilities
Calibration of the sample tube
Experiments
Preparation: chromium(II) acetate
Bibliography
21. Potentiometric titrations
Introduction
Practical considerations
Experiments: titration of phosphoric acid with base
determination of the tripolyphosphate content of sodium tripolyphosphate
Bibliography
22. Polarimetry
The nature of polarized light
Instrumentation for polarimetry
Experimental procedure
Bibliography
General bibliography
Appendix: 81 Units
Index
Atomic masses of some of the elements
Periodic table of the elements
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