Analytical separations and determinations: a textbook in quantitative analysis
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| Main Author: | |
|---|---|
| Format: | Book |
| Language: | English |
| Published: |
New York
Macmillan [u.a.]
1971
|
| Edition: | 1. print. |
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Physical Description: | XX, 395 S. Ill., graph. Darst. |
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| 100 | 1 | |a Kenner, Charles T. |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a Analytical separations and determinations |b a textbook in quantitative analysis |c C. T. Kenner |
| 250 | |a 1. print. | ||
| 264 | 1 | |a New York |b Macmillan [u.a.] |c 1971 | |
| 300 | |a XX, 395 S. |b Ill., graph. Darst. | ||
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| adam_text | CONTENTS
chapter 1. Introduction 1
2. The Analytical Balance 11
3. Methods of Expressing the Concentrations
of Solutions 24
4. Calculations of Gravimetric Analysis 43
5. Calculations of Titrimetric Analysis 55
6. Equilibrium 68
7. Theory of Precipitation 96
8. Gravimetry and Precipitation Titrimetry 114
9. Neutralization 126
10. Oxidation-Reduction Theory 179
11. Oxidation-Reduction Titrations 211
12. Potentiometric Measurements 225
13. Compleximetric Titrations 239
14. Colorimetric and Photometric Methods of
Analysis 249
15. Chromatography and Ion Exchange 272
ix
Contents
16. Reliability of Measurements 295
17. Laboratory Techniques 307
APPENDIXES 331
INDEX 391
DETAILED CONTENTS
chapter 1 Introduction
A. Types and Methods of Analysis 1
B. Steps in an Analysis 3
1. Obtaining the sample 3
2. Selection of the method of determination 5
3. Measurement of the sample 6
a. Selection of proper sample weight 6
b. Weighing by difference 6
c. Aliquoting procedure 7
4. Solution of the sample 8
5. Separation and measurement of the constituents being
determined 9
C. Problems 10
chapter 2 The Analytical Balance 11
A. History of Weighing 11
B. Mass and Weight 12
C. Theory of Weighing 13
D. Substitution (Single-Pan) Balance 19
xi
xii Detailed Contents
E. Balance Properties 20
F. Weighing Errors 21
G. Problems 22
chapter 3 Methods of Expressing the Concentrations
of Solutions 24
A. General 24
B. Methods of Expressing Analytical Concentrations 26
1. Weight-volume 26
2. Percentage methods 26
3. Dilution ratio 27
4. Molar and formal concentration 28
5. Normal concentration 30
6. Titer methods 31
C. Equivalent Weights 34
1. Equivalent weights for reactions in which there is no
electron transfer 34
a. Neutralization 34
b. Precipitation 35
c. General method 36
2. Equivalent weights for oxidation-reduction reactions 36
D. Conversion from One Method to Another 39
1. Weight-volume to molar or normal 39
2. Molar to normal and vice versa 40
3. Molar or normal to titer 40
4. Weight per cent to molar or normal 41
E. Problems 41
chapter 4 Calculations of Gravimetric Analysis 43
A. Gravimetric (Chemical) Factors 43
B. Calculation of Percentage by Weight 46
C. Calculation of Per Cent of Constituent for Gravimetric
Analysis 47
D. Factor Weight Samples 48
E. Quantity of Reagent Required for a Given Reaction 49
F. Indirect Analysis 50
G. Problems 53
Detailed Contents
xm
chapter 5 Calculations of Titrimetric Analysis 55
A. General 55
B. Standards 56
C. Standard Solutions 57
D. Calculation of Per Cent of Constituent from Titrimetric
Analysis 59
1. Direct titration 60
2. Indirect titration 61
E. Optimum Weight of Sample for Standardizations 62
F. Maximum Weight of Unknown Sample to Be
Weighed 64
G. Problems 66
chapter 6 Equilibrium 68
A. The Activity Concept 68
B. Equilibrium Constants 71
C. Factors Which Affect an Established Equilibrium 74
D. Applications of the Equilibrium Constant 76
1. Ionization constants 76
a. Introduction 76
b. Calculation of ionization constants from per cent of
ionization and molar concentration 77
c. Calculation of hydrogen ion concentration from
K and M 78
2. Solubility product 80
a. General 80
b. Calculation of Ksp from solubility 81
c. Calculation of solubility from Ksp 82
d. Calculation of amount of ion or compound left
unprecipitated 83
3. Factors which affect solubility at a given
temperature 84
a. Effect of diverse ions on solubility 84
b. Effect of hydrogen ion concentrations on
solubility 84
c. Calculation of concentrations of species present at
a given hydrogen ion concentration 85
d. Effect of complex formation on solubility 88
4. Calculation of separations by fractional
precipitation 90
E. Problems 92
Detailed Contents
CHAPTER 7 Theory of Precipitation %
A. Introduction 96
B. Formation of Precipitates 98
C. Particle Size of Precipitates 98
D. Growth of an Individual Particle of a Precipitate 101
E. Impurities in or on Precipitates 103
1. Adsorption 103
2. Postprecipitation 105
3. Occlusion 106
4. Coprecipitation 106
F. Purification of Precipitates 107
G. Types of Precipitates 108
H. Rules for Precipitation 109
I. Precipitation from Homogeneous Solution 109
1. Introduction and general considerations 109
2. Types of reactions 111
a. Control of / H 111
b. Generation of other reagents 111
3. Uses of precipitation from homogeneous solution 112
a. Precipitation of hydrous oxides 112
b. Production of relatively large crystals 112
c. Study of coprecipitation 113
chapter 8 Gravimetry and Precipitation Titrimetry 114
A. Gravimetry 114
1. Determination of sulfate as barium sulfate 114
2. Determination of chloride as silver chloride 116
3. Determination of iron as ferric oxide 117
4. Precipitation of nickel dimethylglyoximate from
homogeneous solution 119
B. Precipitation Titrimetry 120
1. The Mohr method 121
2. The Fajans method (adsorption indicator
method) 122
3. The Volhard method 124
chapter 9 Neutralization 126
A. Acids and Bases 126
B. Acidity and Basicity 129
Detailed Contents xv
C. Relations AmongPcB, [H + ], PcOH, [OH~], Kw, and
pKw 130
D. Acid-Base Titrations 131
1. Conditions existing in the titrated solution at the
equivalence point 131
a. General 131
b. Concentration of salt at the equivalence
point 132
2. Solutions of salts 133
a. Hydrolysis 133
b. pcH of solutions of salts 134
(1) Salts of strong acids and strong bases 134
(2) Salts of strong bases and weak acids 134
(3) Salts of weak bases and strong acids 136
(4) Salts of weak bases and weak acids 138
(5) Amphiprotic salts 138
3. pcli of solutions of salts containing excess acid or
base 140
a. General 140
b. Solutions of a weak acid and one of its salts 140
c. Solutions of a weak base and one of its salts 142
4. Titration curves 144
a. General 144
b. Titration curve for strong acid by strong base 144
c. Titration curve for weak acid by strong base 147
d. Titration curve for weak base by strong acid 150
5. Feasibility of titrations 151
6. Titration of polyprotic acids and mixtures of
acids 152
E. Indicators 155
1. General 155
2. Explanation of indicator action 156
3. Range of indicators 157
F. Differential Titration of Alkalies 159
G. Buffers 164
1. Definitions 164
2. Types of buffers 164
3. Explanation of buffer action 164
4. Level and range of buffers 167
5. Capacity of buffers 167
6. Preparation of buffer solutions of definite pcli and
definite total molar concentration 170
H. Nonaqueous Titrations 173
I. Problems 174
xvi Detailed Contents
chapter 1O Oxidation-Reduction Theory 179
A. Balancing Oxidation-Reduction Reactions 180
B. Equivalent Weights for Oxidation-Reduction
Reactions 184
C. The Electrochemical Theory of Oxidation-Reduction 185
D. The Nernst Equation 188
E. The Effect of pcH upon the Potential of Half-Cells 191
F. The Relationship Between Standard Potentials and the
Equilibrium Constant 193
G. Typical Curve for Oxidation-Reduction Titrations 195
H. Calculation of Potentials at Various Points on the Titration
Curve 197
1. Before the equivalence point 197
2. At the equivalence point 199
3. Beyond the equivalence point 199
I. Calculation of Concentrations at Various Points on the
Titration Curve 200
1. Before the equivalence point 200
2. At the equivalence point 201
J. Oxidation-Reduction Indicators 207
K. Problems 208
CHAPTER 11 Oxidation-Reduction Titrations 211
A. Permanganate Methods 212
1. Standardization 212
2. Determination of calcium in limestone by the oxalate-
permanganate method 212
B. Dichromate Methods 215
1. Determination of iron in an iron ore by titration
with potassium dichromate 215
C. Cerium (IV) (Ceric) Methods 217
D. Methods Involving Iodine 219
1. Indirect iodine methods involving titration with
thiosulfate 220
a. Preparation and standardization of thiosulfate
solutions 220
b. Determination of copper by the indirect iodine
method 222
Detailed Contents xvii
chapter 12 Potentiometric Measurements 225
A. Concentration Cells 226
B. Potentiometric Determination of /?H 227
1. Reference electrodes 227
2. The hydrogen electrode 229
3. Substitute hydrogen electrodes 230
a. The quinhydrone electrode 230
b. The glass electrode 231
4. Calculation of /?H 233
a. Hydrogen electrode and calomel electrode 233
b. Substitute electrodes and saturated calomel
electrode 234
C. Potentiometric Titrations 234
1. Graphical methods of selection of end point 235
D. Problems 237
chapter 13 Compleximetric Titrations 239
A. Stability and Instability Constants 240
B. Titration of Chloride with Mercuric Nitrate 241
C. Titration of Cyanide with Silver Nitrate 242
D. Titrations with Ethylenediaminetetraacetic Acid
(EDTA) 243
1. Titration methods 244
a. Direct titration 244
b. Indirect or back titration 245
c. Displacement of a metal ion 245
d. Titration of hydrogen liberated 245
e. Titration of anions 245
2. Indicators 245
3. Standardization 246
4. Determination of total hardness in water 247
5. Determination of calcium and magnesium in
limestone 247
a. Titration for sum of calcium and magnesium 248
b. Titration for calcium only 248
c. Calculations 248
xviii Detailed Contents
chapter 14 Colorimetric and Photometric Methods of
Analysis 249
A. The Nature of Radiant Energy 250
B. The Absorption Process 251
C. Nomenclature 252
D. Fundamental Laws of Absorbance 253
1. The Bougert or Lambert law 253
2. The Beer law 254
3. The combined Bougert-Beer law 255
E. Visual Colorimetric Methods 256
1. The duplication (titration) method 256
2 The dilution method 257
3. The method of balance or variable depth 257
4. The standard series method 259
F. Photometric Instruments 259
1. Light sources 260
2. The optical system 260
3. The wavelength selectors 261
a. Filters 261
b. Monochromators 262
4. Light-sensitive devices 262
a. Vacuum tube photocells (photoemissive cells) 263
b. Barrier-layer cells (photovoltaic cells) 263
c. Photomultiplier tubes 263
G. Photometric Methods 264
1. Absorption curves 264
2. Determination of concentration from absorbance 265
a. By calculation 265
b. Calibration curves 266
3. Representative procedures 267
a. Determination of manganese in cast iron or
steel 267
b. Determination of iron in limestone 268
H. Problems 269
chapter IS Chromatography and Ion Exchange 272
A. Chromatography 272
1. Column chromatography 274
a. Separation mechanism 274
b. Methods of operating chromatographic
columns 277
Detailed Contents xjx
2. Thin-layer chromatography (TLC) 280
3. Paper chromatography 281
a. General methods 282
b. Evaluation of chromatograms 282
4. Gas chromatography 284
a. Instrumentation 284
b. Evaluation 286
B. Ion Exchange 289
1. Synthetic ion-exchange materials 289
a. Structure 289
b. Mechanism of exchange 290
c. Selectivity rules 290
d. Distribution coefficients 291
2. Applications 292
a. Deionization of water 292
b. Separation of ions of opposite charge 292
c. Concentration of trace constituents 292
d. Chromatographic separations of similar
ions 293
e. Use of chelating resins 293
f. Ion-exchange membranes 293
chapter 16 Reliability of Measurements 295
A. Accuracy, Precision, and Error 295
B. Classification of Errors 296
1. Types of determinate errors 296
2. Types of indeterminate or random errors 298
C. Methods of Expressing Precision of a Set of Results 299
1. Average deviation and relative average deviation 299
2. Methods of calculating standard deviations 300
a. Sum of squares method 300
b. Deviations from average method 301
c. From the range 301
D. Confidence Limits 302
1. Method using student s / value 303
2. Method using range and tw 303
E. Method for Discarding Deviant Results in Sets of 10 or
Less 303
F. Rules for Significant Figures 304
G. Problems 305
XX
Detailed Contents
CHAPTER 17 Laboratory Techniques 307
A. General 307
B. Transfer of Liquids from Beakers 308
C. Filtration 309
1. Gravity filtration 309
2. Suction filtration 309
D. Washing 312
E. Preparation of Gooch Crucibles 314
1. General 314
2. Preliminary steps 314
3. Preparation of asbestos mat in crucible 315
F. Ignition of Precipitates 315
G. Drying and the Use of Desiccators 318
H. Evaporation and Digestion 320
I. Use of the Volumetric Apparatus 321
1. General 321
2. Burettes 321
3. Pipettes 325
4. Volumetric flasks 327
APPENDIXES 331
1. The Equal-Arm Balance 331
2. Inorganic Nomenclature 341
3. General Solubility Rules 344
4. Densities of Some Common Materials 345
5. Literature of Analytical Chemistry 346
6. Table of Solubility Products 350
7. Table of lonization Constants of Weak Acids
and Bases 353
8. Table of Stability Constants of Complexes 356
9. Table of Standard Potentials 359
10. Use of Logarithms 362
11. Table of Five-Place Logarithms 371
INDEX 391
|
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| id | DE-604.BV000935591 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T15:21:30Z |
| institution | BVB |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-000572597 |
| oclc_num | 16198950 |
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| owner_facet | DE-19 DE-BY-UBM DE-355 DE-BY-UBR DE-188 |
| physical | XX, 395 S. Ill., graph. Darst. |
| publishDate | 1971 |
| publishDateSearch | 1971 |
| publishDateSort | 1971 |
| publisher | Macmillan [u.a.] |
| record_format | marc |
| spelling | Kenner, Charles T. Verfasser aut Analytical separations and determinations a textbook in quantitative analysis C. T. Kenner 1. print. New York Macmillan [u.a.] 1971 XX, 395 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Chemistry, Analytic Quantitative Chemie (DE-588)4009816-3 gnd rswk-swf Quantitative Analyse (DE-588)4125311-5 gnd rswk-swf Quantitative Analyse (DE-588)4125311-5 s Chemie (DE-588)4009816-3 s DE-604 HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=000572597&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Kenner, Charles T. Analytical separations and determinations a textbook in quantitative analysis Chemistry, Analytic Quantitative Chemie (DE-588)4009816-3 gnd Quantitative Analyse (DE-588)4125311-5 gnd |
| subject_GND | (DE-588)4009816-3 (DE-588)4125311-5 |
| title | Analytical separations and determinations a textbook in quantitative analysis |
| title_auth | Analytical separations and determinations a textbook in quantitative analysis |
| title_exact_search | Analytical separations and determinations a textbook in quantitative analysis |
| title_full | Analytical separations and determinations a textbook in quantitative analysis C. T. Kenner |
| title_fullStr | Analytical separations and determinations a textbook in quantitative analysis C. T. Kenner |
| title_full_unstemmed | Analytical separations and determinations a textbook in quantitative analysis C. T. Kenner |
| title_short | Analytical separations and determinations |
| title_sort | analytical separations and determinations a textbook in quantitative analysis |
| title_sub | a textbook in quantitative analysis |
| topic | Chemistry, Analytic Quantitative Chemie (DE-588)4009816-3 gnd Quantitative Analyse (DE-588)4125311-5 gnd |
| topic_facet | Chemistry, Analytic Quantitative Chemie Quantitative Analyse |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=000572597&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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