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Quantitative Analysis Book

Quantitative Analysis
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  • Quantitative Analysis
  • Written by author Vladimir Alexeyev
  • Published by University Press of the Pacific, April 2000
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Editorial Note9
Chapter I.Introduction
1.The Subject of Quantitative Analysis11
2.Methods of Quantitative Analysis12
3.The Analytical Balance16
4.Sensitivity, Stability, Accuracy and Precision of the Balance22
5.Rules for Handling the Analytical Balance25
6.Weighing26
7.The Damped Balance and Its Use29
8.Elimination of the Effect of Unequal Arm Length. Reduction of the Weight of an Object to Its True Value in a Vacuum33
9.Calibration of Weights35
10.General Comments on Work in a Laboratory for Quantitative Analysis37
11.Preparation of Substances for Analysis39
12.Laboratory Vessels and Their Preparation for Analysis41
13.Errors in Quantitative Analysis43
14.Treatment of Analytical Results48
15.Calculations in Quantitative Analysis53
Questions and Problems (on [sections] 1-15)56
Chapter II.Gravimetric Analysis
16.The Principle of Gravimetric Analysis59
17.Requirements for Precipitates. Choice of Precipitant60
18.Amount of Precipitant63
19.Effect of Excess Precipitant on Completeness of Precipitation66
20.The Salt Effect69
21.Effect of Temperature on Completeness of Precipitation74
22.Effect of Hydrogen Ion Concentration (pH) on Completeness of Precipitation76
23.Effect of Complex Formation on Completeness of Precipitation. Masking83
24.Amorphous and Crystalline Precipitates86
25.Conditions for Formation of Crystalline Precipitates89
26.Conditions for Formation of Amorphous Precipitates92
27.Coprecipitation94
28.Decrease of Coprecipitation103
29.Filtration105
30.Washing of Precipitates108
31.Drying and Ignition of Precipitates112
32.Calculation of Gravimetric Results116
33.Taking the Sample119
34.Dissolution. Fusion120
35.Separation of Ions in Quantitative Analysis123
Questions and Problems (on [sections] 16-35)135
Chapter III.Examples of Gravimetric Determinations
36.Determination of Water of Crystallisation in Barium Chloride140
37.Determination of Hygroscopic Water143
38.Determination of Barium in Barium Chloride144
39.Determination of Sulphur in Sulphuric Acid Solution148
40.Determination of Chlorine in Barium Chloride149
41.Determination of Iron in Ferric Chloride Solution (III)152
42.Determination of Aluminium in Alum154
43.Determination of Calcium in Calcium Carbonate156
44.Determination of Carbon Dioxide in Calcium Carbonate159
45.Determination of Magnesium in Magnesium Sulphate162
46.Determination of Phosphate in Sodium Phosphate166
47.Determination of Calcium and Magnesium When Present Together167
48.Determination of Nickel in Steel168
Questions and Problems ([sections] 36-48)171
Chapter IV.Volumetric Analysis
49.The Principle of Volumetric Analysis174
50.Requirements for Reactions Used in Volumetric Analysis175
51.Classification of Methods of Volumetric Analysis178
52.Volume Measurement179
53.Calibration of Measuring Vessels185
54.Preparation of Standard Solutions188
55.Normality of Solutions. Gram-Equivalent191
56.Calculation of the Results of Volumetric Determinations197
57.Calculations in Preparation and Dilution of Solutions202
Questions and Problems (on [sections] 49-57)206
Chapter V.The Neutralisation Method
58.The Principle of the Neutralisation Method211
59.Indicators for the Neutralisation Method215
60.Theory of Indicators217
61.Indicator Range223
62.Titration Curves. Titration of Strong Acids with Strong Alkalies (or Vice Versa)229
63.Titration of Weak Acids with Strong Alkalies (or Vice Versa)234
64.Titration of Weak Bases with Strong Acids (or Vice Versa)242
65.Titration of Weak Acids with Weak Bases (or Vice Versa)244
66.Buffer Action247
67.Indicator Error in Titration249
68.Titration of Dibasic and Polybasic Acids254
69.Titration of Salt Solutions259
70.Effects of Various Factors on Indicator Changes264
Questions and Problems (on [sections] 58-70)268
Chapter VI.Examples of Determinations by the Neutralisation Method
71.Preparation of Standard HC1 Solution271
72.Determination of Alkali in a Solution275
73.Determination of NaOH and Na[subscript 2]CO[subscript 3] in the Same Solution275
74.Determination of the Hardness of Water278
75.Preparation of Standard NaOH Solution281
76.Determinations of Acids284
77.Determination of Ammonia in Ammonium Salts284
Questions and Problems (on [sections] 71-77)287
Chapter VII.Oxidation-Reduction Methods (Oxidimetry)
78.Oxidation Potentials and Reaction Direction290
79.Influence of Concentrations and the Reaction of the Medium295
80.Equilibrium Constants of Oxidation-Reduction Reactions300
81.Oxidation-Reduction Titration Curves303
82.Indicators Used in Oxidation-Reduction Methods308
83.Rate of Oxidation-Reduction Reactions312
84.Side Reactions in Oxidation-Reduction Titrations316
Questions and Problems (on [sections] 78-84)319
Permanganate Titrations
85.General Principles of the Method321
86.Preparation and Storage of Standard KMnO[subscript 4] Solution322
87.Standardisation of KMnO[subscript 4] Solution323
88.Determination of Ferrous Iron, Hydrogen Peroxide and Nitrites325
89.Determination of Iron in Ferric Chloride Solution327
90.Determination of Chromium in Potassium Dichromate Solution330
91.Determination of Calcium in Calcium Carbonate332
92.Determination of Manganese in Steel (or Cast Iron)334
Dichromate Titrations
93.General Principles of the Method337
94.Determination of Iron in an Ore339
Iodometry
95.General Principles of the Method341
96.Preparation of Standard Solutions346
97.Standardisation of Na[subscript 2]S[subscript 2]O[subscript 3] Solution349
98.Determination of Active Chlorine in Bleaching Powder352
99.Determination of Copper in Copper Sulphate353
100.Determination of Arsenic in Sodium Arsenite Solution354
101.Determination of Sodium Sulphite356
Bromatometry
102.General Principles of the Method357
103.Determination of Antimony in Tartar Emetic358
104.Determination of Magnesium in a Solution of Mg Salt359
Questions and Problems (on [sections] 85-104)362
Chapter VIII.Methods of Precipitation and Complex Formation
105.General Principles366
106.Titration Curves in the Precipitation Method367
107.Methods of Determining the Equivalence Point371
108.Adsorption Effects in Titration. Adsorption Indicators375
109.Standardisation of Silver Nitrate Solution by the Mohr Method379
110.Standardisation of Ammonium Thiocyanate Solution381
111.Thiocyanate Determination of Halides382
112.Determination of Halides by Titration with Silver Nitrate in Presence of Adsorption Indicators383
113.Mercurometric Determination of Chlorides384
114.Mercurimetric Determination of Chlorides386
115.Determination of Zinc by Precipitation with Potassium Ferrocyanide387
116.Complexometric Determination of the Total Hardness of Water389
Questions and Problems (on [sections] 105-116)392
Chapter IX.Colorimetry
117.The Principle of the Method394
118.Laws of the Absorption of Light by Solutions398
119.Conditions for Applicability of the Lambert-Beer Law. Influence of the Medium pH401
120.Influence of Extraneous Ions on the Colour of Solutions403
121.Methods of Colour Comparison406
122.Colorimeters411
123.Photocolorimetry413
124.Determination of Copper in Copper Sulphate Solution416
125.Determination of Titanium in Titanium Sulphate Solution417
126.Determination of Iron in a Solution of an Iron Salt418
127.Determination of Hydrogen Ion Concentration (pH)423
Questions and Problems (on [sections] 117-127)429
Chapter X.Electrochemical Methods of Analysis
128.General Principles of Electrogravimetric Analysis431
129.Chemical Processes During Electrolysis432
130.The Laws of Electrolysis434
131.Decomposition Voltage436
132.Electrolytic Separation of Metals441
133.Effect of Solution pH443
134.Significance of Current Density in Electrolysis. Accelerated Electrolysis445
135.Determination of Copper in Copper Sulphate Solution448
136.Separation and Determination of Copper and Nickel in Solution452
137.Separation of Ions at a Mercury Cathode. Determination of Titanium in Steel454
138.Internal Electrolysis456
139.The Principle of the Polarographic Method of Analysis459
Questions and Problems (on [sections] 128-139)463
Appendices
I.Atomic Weights466
II.Dissociation Constants and Strength Exponents (pK) of Some Weak Electrolytes468
III.Solubilities and Solubility Products of Some Sparingly Soluble Electrolytes at Room Temperature470
IV.Instability Constants of Certain Complexes472
V.Specific Gravities of Solutions of Strong Acids, Alkalies and Ammonia at 15[degree]C473
VI.Standard Oxidation Potentials474
VII.Buffer Mixtures for pH Determination476
VIII.Values of t[subscript alpha] for Different Values of Confidence ([alpha]) and Different Numbers of Determinations (n)477
IX.Logarithms478
X.Antilogarithms481
Index484


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