G. Svehla-Vogel's Qualitative Inorganic Analysis-Prentice Hall (1996), chem

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Vogel's
Qualitative Inorganic Analysis
Seventh Edition
Revised
by
G. Svehla
PhD, DSC, FRSC
formerly Professor ofAnalytical Chemistry.
University Col/ege. Cork
199712 4692
543.062 VOG
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Addison Wesley Longman Ltd
Edinburgh Gate, Harlow
Essex CM20 21E, England
and Associated Companies throughout the world
©
Longman Group Limited 1979, 1987, 1996
All rights reserved; no part of this publication may be reproduced, stored in a retrieval system, or
transmitted in any form or by any means, electronic, mechanical, photocopying, recording,
or otherwise without either the prior written permission of the Publishers or a licence permitting
restricted copying in the United Kingdom issued by the Copyright Licensing Agency Ltd.,
90 Tottenham Court Road, London WI P 9HE.
Trademarks
Throughout this book trademarked names are used. Rather than put a trademark symbol in
every occurrence of a trademarked name, we state that we are using the names only in editorial
fashion and to the benefit of the trademark owner with no intention of infringement of the
trademark.
First published under the title
A Text-book of Qualitative Chemical Analysis 1937
Second edition 1941
Reissue with Appendix 1943
Third edition under the title
A Text-book of Qualitative Chemical Analysis including Semimicro
Qualitative Analysis 1945
Fourth edition under the title
A Text-book of Macro and Semimicro Qualitative Inorganic
Analysis 1954
Fifth edition 1979
Sixth edition under the title
Vogel's Qualitative Inorganic Analysis 1987
Seventh edition 1996
Reprinted 1997
British Library Cataloguing in Publication Data
A catalogue entry for this title is available from the British Library.
ISBN 0-582-21866-7
Library of Congress Cataloging-in-Publication Data
A catalog entry for this title is available from the Library of Congress.
Set by 22 in 10/12pt Times
Produced by Longman Singapore Publishers (Pte) Ltd.
Printed in Singapore
Contents
Preface to seventh edition
ix
From preface to the first edition
x
From preface to the fifth edition
x
From preface to the sixth edition
xi
Chapter 1 Introduction
1
Chapter 2 Experimental techniques
3
2.1 Introduction
3
2.2 Dry tests
4
2.3 Wet reactions; macro apparatus and analytical operations on a
15
macro scale
2.4 Semimicro apparatus and semimicro analytical operations
23
2.5 Micro apparatus and microanalytical operations
39
2.6 Spot test analysis
45
2.7 Detection of metals by flame atomic spectrometric methods
54
Chapter 3 Reactions of the cations
59
3.1 Classification of cations (metal ions) in analytical groups
59
3.2 Notes on the study of the reactions of ions
60
3.3 First group of cations: lead(II), mercury(IL and silver(l)
61
3.4 Lead, Pb
(A,: 207.19)
62
3.5 Mercury, Hg
(A,:
200.59) - mercury(l)
67
3.6 Silver, Ag
(A,:
107.868)
71
3.7 Second group of cations: mercury(IIL lead(IIL bismuth(lliL
76
copper(II), cadmium(IIL arsenic(III) and (VL antimony(III)
and (VL and tin(II) and (IV)
3.8 Mercury, Hg
(A,:
200.59) - mercury(II)
77
3.9 Bismuth, Bi
(A,: 208.98)
79
3.10 Copper, Cu
(A,: 63.55)
83
3.11 Cadmium, Cd
(A,: 112.40)
88
3.12 Arsenic, As
(A,:
74.92) - arsenic(III)
91
3.13 Arsenic, As
(A,:
74.92) - arsenic(V)
93
3.14 Special tests for small amounts of arsenic
95
3.15
Antimony, Sb
(Ar:
121.75) -
antimony(llI)
99
3.16
Antimony, Sb
(Ar:
121.75) -
antimony(V)
102
3.17
Special tests for small amounts of antimony
104
3.18
Tin, Sn
(Ar:
118.69) -
tin (II)
104
3.19
Tin, Sn
(Ar:
118.69) -
tin(IV)
107
3.20
Third group of cations: iron(ll) and (III). aluminium(III),
108
chromium(lll) and (VI), nickel(ll). cobalt(ll). manganese(lI)
and (VII). and zinc(lI)
3.21
Iron, Fe
(Ar:
55.85) -
iron(ll)
109
3.22
Iron, Fe
(Ar:
55.85) -
iron(lll)
113
3.23
Aluminium, AI
(Ar: 26.98)
118
3.24
Chromium, Cr
(Ar:
51.996) -
chromium(lIl)
122
3.25
Oxoanions of Group III metals: chromate and permanganate
127
3.26
Cobalt, Co
(Ar: 58.93)
127
3.27
Nickel, Ni
(Ar:
58.71)
131
3.28
Manganese, Mn
(Ar:
54.938) -
manganese(lI)
135
3.29
Zinc; Zn
(Ar: 63.38)
139
3.30
Fourth group of cations: barium(ll). strontium(II), and calcium(lI)
143
3.31
Barium, Ba
(Ar: 137.34)
144
3.32
Strontium, Sr
(Ar: 87.62)
147
3.33
Calcium, Ca
(Ar: 40.08)
149
3.34
Fifth group of cations: magnesium(II), sodium(I), potassium(I),
152
and ammonium(l)
3.35
Magnesium, Mg
(Ar: 24.305)
152
3.36
Potassium, K
(Ar: 39.098)
156
3.37
Sodium, Na
(Ar: 22.99)
159
3.38
Ammonium, NHt
(M
r
: 18.038)
160
Chapter
4
Reactions of the anions
163
4.1
Scheme of classification
163
4.2
Carbonates,
CO~-
164
4.3
Hydrogen carbonates, HC03'
166
4.4
Sulphites,
SO~-
168
4.5
Thiosulphates, S20~-
171
4.6
Sulphides, S2-
174
4.7
Nitrites, N02'
176
4.8
Cyanides, CN-
179
4.9
Cyanates, OCN-
181
4.10
Thiocyanates, SCN-
182
4.11
Hexacyanoferrate(ll) ions, [Fe(CNl6l4-
185
4.12
Hexacyanoferrate(lll) ions, [Fe(CN)6l
3
-
187
4.13
Hypochlorites, OCI-
188
4.14
Chlorides, CI-
190
4.15
Bromides, Br-
192
4.16
Iodides, 1-
195
4.17
Fluorides, F-
198
4.19
Chlorates, CI0
3
199
202
4.20
Bromates, Br03
204
4.21
Iodates, 10
3
206
4.22
Perchlorates, CI0
4
207
4.23
Borates,
BO~-, B40~-,
B02'
208
4.24
Sulphates, SO~-
211
4.25
Peroxodisulphates,
S20~-
214
4.26
Silicates,
SiO~-
215
4.27
Hexafluorosilicates (silicofluorides), [SiF
6
1
2
-
217
4.28
Orthophosphates,
PO~-
218
4.29
Pyrophosphates,
P20~-,
and metaphosphates, P0
3
221
4.30
Phosphites, H PO~-
221
4.31
Hypophosphites, H
2
P02'
223
4.32
Arsenites, AsO~-, and arsenates, AsO~-
224
4.33
Chromates, CrO~-, and dichromates, Cr20~-
224
4.34
Permanganates, Mn04
228
4.35
Acetates, CH
3
COO-
229
4.36
Formates, HCOO-
232
4.37
Oxalates, (COO)~-
234
4.38
Tartrates,
C4H40~-
236
4.39
Citrates, C6H50~-
239
4.40
Salicylates, C
6
H
4
(OH)COO- or C
7
H
5
Oi
240
4.41
Benzoates, C
6
H
5
COO- or C
7
H
5
02'
242
4.42
Succinates, C
4
H4
O~-
243
4.43
Hydrogen peroxide, H
2
0
2
(the per hydroxyl ion, OOH-)
244
4.44
Dithionites,
S20~-
247
Chapter
5
Selected tests and separations
249
5.1
Introd uction
249
5.2
Preliminary tests on liquid samples (samples in solution)
249
5.3
Preliminary tests on non-metallic solid samples
250
5.4
Preliminary tests on metal samples
252
5.5
Dissolution of the sample
253
5.6
Examination of the insoluble residue
254
5.7
Testing for a single cation in solution
256
5.8
Separation and identification of cations in mixtures
258
5.9
Special tests for mixtures of anions
265
Chapter
6
Reactions of some less common ions
274
6.1
Introduction
274
6.2
Thallium, TI
(Ar:
204.34) -
thallium(l)
274
6.3
Thallium, TI
(Ar:
204.34) -
thallium(III)
276
6.4
Tungsten, W
(Ar:
183.85) -
tungstate
276
4.18
Nitrates, N0
3
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