Gas and liquid chromatography in analytical chemistry:
Gespeichert in:
| 1. Verfasser: | |
|---|---|
| Format: | Buch |
| Sprache: | Undetermined |
| Veröffentlicht: |
Chichester u.a.
Wiley
1988
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| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Beschreibung: | XIV, 402 S. |
| ISBN: | 0471909807 |
Internformat
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| 100 | 1 | |a Smith, Roger M. |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a Gas and liquid chromatography in analytical chemistry |
| 264 | 1 | |a Chichester u.a. |b Wiley |c 1988 | |
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| adam_text | IMAGE 1
GAS AND LIQUID
CHROMATOGRAPHY IN ANALYTICAL CHEMISTRY
ROGER M._§MITH READER IN ANALYTICAL CHEMISTRY, DEPARTMENT OF CHEMISTRY,
LOUGHBOROUGH UNIVERSITY OF TECHNOLOGY, LOUGHBOROUGH, LEICS., LEU 3TU, UK
JOHN WILEY & SONS CHICHESTER * NEW YORK * BRISBANE * TORONTO * SINGAPORE
IMAGE 2
CONTENTS
PREFACE XIII
1 INTRODUCTION 1
1.1 ANALYTICAL CHROMATOGRAPHY 1
1.2 ORIGINS OF CHROMATOGRAPHY 5
1.3 SELECTION OF A CHROMATOGRAPHIC METHOD 14
A. NATURE OF ANALYTE 15
B. MATRIX OF THE SAMPLE 16
C. REASONS FOR ANALYSIS 16
BIBLIOGRAPHY 17
REFERENCES 17
2 BASIC CONCEPTS OF CHROMATOGRAPHY 20
2.1 PRINCIPLES AND DEFINITIONS 20
A. BASIC CONCEPTS 20
B. CHROMATOGRAPHIC RETENTION 22
C. SEPARATION EFFICIENCY 27
D. RESOLUTION 30
2.2 OPTIMISATION OF SEPARATION EFFICIENCY 30
A. FACTORS AFFECTING BAND SPREADING 32
I. EDDY DIFFUSION 34
II. MOLECULAR DIFFUSION 35
III. RESISTANCE TO MASS TRANSFER 36
IV. OVERALL BAND-SPREADING EQUATION 38
V. CONCLUSIONS FROM VAN DEEMTER EQUATION 41
B. REDUCED PARAMETERS AND OTHER EQUATIONS 44
BIBLIOGRAPHY 45
REFERENCES 45
3 GAS-LIQUID CHROMATDGRAPHY: INSTRUMENTATION 47 3.1 INTRODUCTION TO
GAS-LIQUID CHROMATOGRAPHY 47
3.2 INSTRUMENTATION FOR GAS-LIQUID CHROMATOGRAPHY 48
A. THE CARRIER GAS 48
B. SAMPLE INJECTION 51
I. PACKED COLUMN INJECTION 52
IMAGE 3
VI G AS A ND L I Q U ID C H R O M A T O G R A P HY
II. OPEN-TUBULAR COLUMN INJECTION 52
III. AUTOMATIC INJECTION 57
C. COLUMN OVEN 58
BIBLIOGRAPHY 61
REFERENCES 61
4 GAS-LIQUID CHROMATOGRAPHY: COLUMNS AND STATIONARY PHASES 62
4.1 GAS CHROMATOGRAPHY COLUMNS 62
A. PACKED COLUMNS 63
I. COLUMN TUBING 63
II. SUPPORT MATERIAL 64
B. OPEN-TUBULAR COLUMNS 67
4.2 STATIONARY PHASES 71
A. NON-POLAR LIQUID PHASES 74
I. HYDROCARBON PHASES 74
II. ALKYLSILICONE LIQUID PHASES 75
B. POLAR LIQUID PHASES 78
I. SUBSTITUTED SILICONE LIQUID PHASES 79
II. ESTER LIQUID PHASES 82
III. POLYETHER LIQUID PHASES 82
C. SPECIALISED LIQUID PHASES 84
I. PHASES FOR CARBOXYLIC ACIDS 85
II. PHASES FOR BASIC COMPOUNDS 85
III. HIGH-TEMPERATURE PHASES 87
D. CHIRAL PHASES 87
E. GAS-SOLID PHASES AND POLYMER PHASES 87
I. GAS-SOLID STATIONARY PHASES 87
II. POROUS POLYMER PHASES 90
4.3 COLUMN SELECTION AND THE CLASSIFICATION OF LIQUID PHASES 92
A. COLUMN SELECTION 92
B. CLASSIFICATION OF LIQUID PHASES 94
4.4 COLUMN PACKING AND TESTING 98
A. PREPARATION OF THE STATIONARY PHASE 99
B. COLUMN PACKING 99
C. COLUMN TESTING 100
BIBLIOGRAPHY 102
REFERENCES 104
5 DETECTORS FOR GAS-LIQUID CHROMATOGRAPHY 105 5.1 GENERAL CRITERIA 105
A. INTRODUCTION 0 105
B. DETECTOR PERFORMANCE 106
C. PRINCIPAL GROUPS OF DETECTORS 108
I. BULK PROPERTY DETECTORS 108
II. MASS FLOW DETECTORS 109
5.2 UNIVERSAL DETECTORS 110
A. THERMAL CONDUCTIVITY DETECTOR 110
B. FLAME IONISATION DETECTOR 112
IMAGE 4
CONTENTS VII
C. PHOTOIONISATION DETECTOR 116
5.3 SELECTIVE AND SPECIFIC DETECTORS 119
A. ELECTRON CAPTURE DETECTOR 119
B. THERMIONIC IONISATION DETECTOR 125
C. FLAME PHOTOMETRIC DETECTOR 129
D. LESS COMMONLY USED DETECTORS 131
I. ELECTROCHEMICAL METHODS 131
II. THERMAL ENERGY ANALYSER 131
III. OTHER DETECTORS 132
5.4 COUPLED DETECTORS 132
A. GC-HUMAN NOSE 133
B. GC-RADIOCHEMICAL DETECTORS 133
C. GC-ATOMIC ABSORPTION SPECTROSCOPY 133
D. GC-INFRARED SPECTROSCOPY . 133
E. GC-MASS SPECTROMETRY 135
I. INTERFACING TO THE MASS SPECTROMETER 135
II. MODES OF OPERATION 136
5.5 CRITERIA FOR THE ADOPTION OF A NEW DETECTOR 137
BIBLIOGRAPHY 140
REFERENCES 144
6 SAMPLE IDENTIFICATION AND QUANTIFICATION IN GAS-LIQUID CHROMATOGRAPHY
145
6.1 SAMPLE PREPARATION FOR GAS-LIQUID CHROMATOGRAPHY 145
6.2 SAMPLE IDENTIFICATION BY GAS-LIQUID CHROMATOGRAPHY 146
A. IDENTIFICATION BY COMPARISON WITH STANDARD COMPOUNDS 146 B.
STRUCTURE-RETENTION RELATIONSHIPS 148
C. RELATIVE RETENTION STANDARDS 150
D. RETENTION INDICES 151
6.3 SAMPLE QUANTIFICATION IN GAS-LIQUID CHROMATOGRAPHY 154
A. EXTERNAL CALIBRATION 155
B. INTERNAL CALIBRATION 156
BIBLIOGRAPHY 157
REFERENCES 158
7 GAS CHROMATOGRAPHY: SPECIAL TECHNIQUES 160 7.1 PROBLEM SAMPLES IN
GAS-LIQUID CHROMATOGRAPHY 160
7.2 DERIVATISATION REACTIONS IN GAS-LIQUID CHROMATOGRAPHY 161 A.
HYDROXYL GROUPS 161
I. ALKYLATION TO FORM ETHERS 162
II. ACYLATION 162
III. SILYLATION * 162
B. CARBOHYDRATES 164
C. CARBOXYLIC ACIDS 165
I. DIAZOMETHANE 165
II. ACID-CATALYSED ESTERIFICATION 167
III. ON-COLUMN ESTERIFICATION REACTIONS 167
IV. DERIVATISATION FOR THERMIONIC DETECTION 167
IMAGE 5
VIII GAS AND LIQUID CHROMATOGRAPHY
D. AMINES 168
I. ACYLATION 168
II. ARYLATION 168
III. SILYLATION 169
E. AMINO ACIDS 169
F. OTHER FUNCTIONAL GROUPS * 169
G. CHIRAL SEPARATIONS 170
H. ABSTRACTION TECHNIQUES 170
7.3 SAMPLE PYROLYSIS 171
7.4 MATRIX PROBLEMS 173
A. HEADSPACE ANALYSIS 173
B. TRAPPING OF VOLATILE SAMPLES 174
7.5 COLUMN SWITCHING - 175
BIBLIOGRAPHY 177
REFERENCES 178
8 LIQUID CHROMATOGRAPHY 179
8.1 LIQUID CHROMATOGRAPHIC METHODS 179
A. NORMAL-PHASE CHROMATOGRAPHY 182
B. REVERSED-PHASE CHROMATOGRAPHY 182
8.2 RELATED SEPARATION TECHNIQUES 184
A. ION-EXCHANGE CHROMATOGRAPHY 184
B. SIZE EXCLUSION CHROMATOGRAPHY 186
8.3 PREPARATIVE SEPARATIONS 188
8.4 SELECTION OF AN ANALYTICAL METHOD - 189
BIBLIOGRAPHY 190
REFERENCES 191
9 THIN-LAYER CHROMATOGRAPHY 192
9.1 SEPARATIONS ON THIN-LAYER CHROMATOGRAPHY 192
A. ADSORPTION-PHASE TLC 195
B. REVERSED-PHASE TLC 196
C. HIGH-PERFORMANCE TLC 196
D. MOBILE PHASES 197
9.2 ANALYTE DETECTION 198
A. DIRECT EXAMINATION 198
B. GENERAL DETECTION REAGENTS 198
C. SELECTIVE DETECTION REAGENTS 200
D. INSTRUMENTAL DETECTION 201
9.3 SAMPLES AND APPLICATIONS 202
A. QUALITATIVE ANALYSIS AND IDENTIFICATION 203
B. QUANTIFICATION 206
9.4 NEW IDEAS AND TECHNIQUES 206
BIBLIOGRAPHY 207
REFERENCES 208
10 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 209 I 10.1 MODES OF OPERATION
OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 209 10.2 INSTRUMENTATION FOR
LIQUID CHROMATOGRAPHY 211
IMAGE 6
CONTENTS - IX
A. ELUENT 212
I. ELUENT PURITY 212
II. ELUENT DEGASSING 215
B. PUMPS 218
I. RECIPROCATING PUMPS 218
II. DIAPHRAGM PUMPS 219
III. SYRINGE PUMPS 220
IV. PRESSURE AMPLIFICATION PUMPS * 221
V. PROGRAMMED ELUTION . 221
C. SAMPLE INJECTION SYSTEMS 222
D. CONNECTING TUBING 224
E. COLUMNS 225
I. ANALYTICAL COLUMNS 225
II. MICROBORE COLUMNS 225
III. CAPILLARY COLUMNS 227
IV. PRE- AND GUARD COLUMNS 227
V. COLUMN OVENS 228
VI. PACKING COLUMNS 229
BIBLIOGRAPHY 230
REFERENCE 231
11 DETECTION IN HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 232
11.1 GENERAL CRITERIA 232
11.2 SPECTROPHOTOMETRIC DETECTORS 235
A. ULTRAVIOLET-VISIBLE SPECTROPHOTOMETRIC DETECTORS 235
I. FIXED-WAVELENGTH DETECTORS 237
II. VARIABLE-WAVELENGTH DETECTORS 238
III. DIODE ARRAY SPECTROPHOTOMETRIC DETECTORS 239
IV. ELUENT RESTRICTIONS WITH ULTRAVIOLET DETECTION 242
B. FLUORESCENCE DETECTORS 244
11.3 ELECTROANALYTICAL DETECTORS 247
A. CONDUCTOMETRIC DETECTORS 247
B. AMPEROMETRIC AND COULOMETRIC DETECTORS 248
11.4 REFRACTIVE INDEX DETECTORS 251
11.5 OTHER LIQUID CHROMATOGRAPHY DETECTORS 257
11.6 COUPLED LIQUID CHROMATOGRAPHY DETECTORS 258
A. LC-INFRARED SPECTROSCOPIC DETECTION 258
B. LC-MASS SPECTROMETRIC DETECTION 258
BIBLIOGRAPHY 260
12 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY SEPARATION METHODS; COLUMNS
AND MOBILE PHASES. 263 12.1 SELECTION OF A SEPARATION METHOD 263
12.2 NORMAL-PHASE SEPARATION METHODS 266
A. STATIONARY PHASE MATERIALS 267
B. MOBILE PHASES FOR NORMAL-PHASE SEPARATIONS 270
12.3 REVERSED-PHASE SEPARATION METHODS 273
A. HYDROCARBONACEOUS BONDED-PHASE MATERIALS 273
IMAGE 7
GAS AND LIQUID CHROMATOGRAPHY
B. OTHER BONDED-PHASE MATERIALS 277
C. POLYMER STATIONARY PHASES 281
D. DYNAMICALLY COATED COLUMNS 282
E. SOLVENT SELECTION FOR REVERSED-PHASE CHROMATOGRAPHY 284 12.4
SEPARATION OF IONISABLE COMPOUNDS 287
A. ION SUPPRESSION 287
B. MASKING AGENTS 289
C. ION-PAIR CHROMATOGRAPHY 290
I. MECHANISM OF ION-PAIR SEPARATIONS 291
II. TYPICAL SEPARATION SYSTEMS 293
12.5 ION CHROMATOGRAPHY AND ION-EXCHANGE CHROMATOGRAPHY 295 A.
SEPARATION OF CATIONS AND ANIONS 295
I. WEAK ION-EXCHANGE COLUMNS 296
II. ION CHROMATOGRAPHY WITH SUPPRESSED DETECTION 296 III. INDIRECT
PHOTOMETRIC DETECTION 299
B. SILICA AS AN ION-EXCHANGE MEDIUM 300
12.6 SEPARATION OF MACROMOLECULES AND BIOPOLYMERS 300
12.7 OPTIMISATION TECHNIQUES 302
A. MAPPING OPTIMISATION METHODS 306
B. ITERATIVE OPTIMISATION METHODS 307
C. SIMPLEX OPTIMISATION METHODS 307
BIBLIOGRAPHY 308
REFERENCES 310
13 QUANTITATIVE AND QUALITATIVE APPLICATIONS OF HIGH-PERFORMANCE LIQUID
CHROMATOGRAPHY 311 13.1 APPLICATIONS OF HIGH-PERFORMANCE LIQUID
CHROMATOGRAPHY 311 13.2 SAMPLE PREPARATION 312
13.3 SAMPLE IDENTIFICATION 314
A. RELATIVE RETENTION FACTORS 317
B. RETENTION INDICES IN HPLC 318
13.4 QUANTITATIVE ANALYSIS BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 319
13.5 MEASUREMENT OF PHYSICAL PARAMETERS 321
BIBLIOGRAPHY 321
REFERENCES 322
14 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY: SPECIAL TECHNIQUES 323
14.1 DERIVATISATION REACTIONS FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY
323
A. REACTIONS TO O ENHANCE ULTRAVIOLET DETECTION 326
I. PRE-COLUMN REACTIONS 327
II. POST-COLUMN REACTIONS 328
B. REACTIONS TO ENHANCE FLUORESCENCE DETECTION 329
I. PRE-COLUMN REACTIONS 329
II. POST-COLUMN REACTIONS 331
, C. REACTIONS TO ENHANCE ELECTROCHEMICAL DETECTION 331
D. REACTIONS TO ENHANCE SEPARATION 332
IMAGE 8
CONTENTS XI
14.2 SEPARATION OF CHIRAL COMPOUNDS 332
A. DERIVATISATION FOR CHIRAL SEPARATIONS 333
B. CHIRAL STATIONARY PHASES 333
14.3 COLUMN SWITCHING AND SAMPLE TRAPPING 337
A. COLUMN TRAPPING 337
B. COLUMN SWITCHING, HEART-CUT AND BACK-FLUSHING METHODS 338
BIBLIOGRAPHY 339
15 DATA HANDLING AND AUTOMATION IN CHROMATOGRAPHY 341
15.1 COMPUTERS IN CHROMATOGRAPHY 341
15.2 INTEGRATION AND DATA HANDLING 341
A. PEAK DETECTION 342
B. INTEGRATOR PARAMETERS 350
15.3 DATA ANALYSIS 351
15.4 AUTOMATIC CONTROL AND INJECTION METHODS 352
15.5 NEW APPLICATIONS OF COMPUTERS IN THE CHROMATOGRAPHY LABORATORY 352
A. DATA BANKS 353
B. EXPERT SYSTEMS 353
C. ROBOTICS AND SAMPLE PREPARATION 355
BIBLIOGRAPHY 355
16 FUTURE DEVELOPMENTS IN CHROMATOGRAPHY 357 16.1 ADVANCES IN EXISTING
CHROMATOGRAPHIC METHODS 357
A. GAS-LIQUID CHROMATOGRAPHY 357
B. HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 358
C. THIN-LAYER CHROMATOGRAPHY 360
16.2 NEW SEPARATION METHODS 360
A. SUPERCRITICAL FLUID CHROMATOGRAPHY 360
B. FIELD FLOW FRACTIONATION 364
C. AFFINITY CHROMATOGRAPHY 365
BIBLIOGRAPHY 365
APPENDIX 1 SOURCES OF CHROMATOGRAPHIC METHODS 368 AL.L LITERATURE OF
CHROMATOGRAPHY 368
A. PRIMARY LITERATURE 369
B. REVIEW JOURNALS IN CHROMATOGRAPHY 370
C. BOOKS ON CHROMATOGRAPHY 371
A1.2 GENERAL BOOKS ON CHROMATOGRAPHY APPLICATIONS 371
A. GENERAL APPLICATIONS 371
B. PHARMACEUTICAL, CLINICAL AND BIOMEDICAL APPLICATIONS 371 C. FOOD,
AGRICULTURAL AJID ENVIRONMENTAL APPLICATIONS 372
D. MISCELLANEOUS APPLICATIONS 372
AL.3 APPLICATIONS OF GAS-LIQUID CHROMATOGRAPHY 373
A. GENERAL APPLICATIONS 373
B. PHARMACEUTICAL, CLINICAL AND BIOMEDICA) APPLICATIONS 373 C. FOOD,
AGRICULTURAL AND ENVIRONMENTAL APPLICATIONS 373
D. MISCELLANEOUS APPLICATIONS 374
IMAGE 9
XII GAS AND LIQUID CHROMATOGRAPHY
AL .4 APPLICATIONS OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 374 A.
GENERAL APPLICATIONS 374
B. PHARMACEUTICAL, CLINICAL AND BIOMEDICAL APPLICATIONS 374 C. FOOD,
AGRICULTURAL AND ENVIRONMENTAL APPLICATIONS 375
D. APPLICATIONS TO THE SEPARATION OF POLYMERS 375
A1.5 APPLICATIONS OF THIN-LAYER CHROMATOGRAPHY 376
APPENDIX 2 PRACTICAL PROBLEMS IN CHROMATOGRAPHY 377 A2.1 PROBLEMS IN
CHROMATOGRAPHY 377
A. PROBLEM PREVENTION 378
B. PROBLEM RECOGNITION 378
C. PROBLEM LOCATION AND RECTIFICATION 378
I. SAMPLE PREPARATION 379
II. INJECTION TECHNIQUE 379
A2.2 EQUIPMENT PROBLEMS IN GAS-LIQUID CHROMATOGRAPHY 381
A. CARRIER GAS 381
B. COLUMN OVEN 382
C. COLUMNS 382
D. DETECTORS 383
A2.3 EQUIPMENT PROBLEMS IN HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY 385
A. PUMPS AND FLOW PROBLEMS 385
B. SAMPLES AND SOLVENT 386
C. INJECTOR VALVE 387
D. COLUMN AND ELUENT 387
A2.4 RECORDS AND DATA INTERPRETATION 390
A2.5 OPERATOR PROBLEMS 390
BIBLIOGRAPHY 391
APPENDIX 3 TERMS AND DEFINITIONS 393
SUBJECT INDEX 395
|
| any_adam_object | 1 |
| author | Smith, Roger M. |
| author_facet | Smith, Roger M. |
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| author_sort | Smith, Roger M. |
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| building | Verbundindex |
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| discipline | Chemie / Pharmazie Chemie |
| format | Book |
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| id | DE-604.BV001287268 |
| illustrated | Not Illustrated |
| indexdate | 2024-08-01T16:23:48Z |
| institution | BVB |
| isbn | 0471909807 |
| language | Undetermined |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-000776231 |
| oclc_num | 246944602 |
| open_access_boolean | |
| owner | DE-12 DE-384 DE-355 DE-BY-UBR DE-862 DE-BY-FWS DE-83 DE-11 |
| owner_facet | DE-12 DE-384 DE-355 DE-BY-UBR DE-862 DE-BY-FWS DE-83 DE-11 |
| physical | XIV, 402 S. |
| publishDate | 1988 |
| publishDateSearch | 1988 |
| publishDateSort | 1988 |
| publisher | Wiley |
| record_format | marc |
| spellingShingle | Smith, Roger M. Gas and liquid chromatography in analytical chemistry Analytische Chemie (DE-588)4129906-1 gnd Gaschromatographie (DE-588)4019330-5 gnd Flüssigkeitschromatographie (DE-588)4017622-8 gnd |
| subject_GND | (DE-588)4129906-1 (DE-588)4019330-5 (DE-588)4017622-8 |
| title | Gas and liquid chromatography in analytical chemistry |
| title_auth | Gas and liquid chromatography in analytical chemistry |
| title_exact_search | Gas and liquid chromatography in analytical chemistry |
| title_full | Gas and liquid chromatography in analytical chemistry |
| title_fullStr | Gas and liquid chromatography in analytical chemistry |
| title_full_unstemmed | Gas and liquid chromatography in analytical chemistry |
| title_short | Gas and liquid chromatography in analytical chemistry |
| title_sort | gas and liquid chromatography in analytical chemistry |
| topic | Analytische Chemie (DE-588)4129906-1 gnd Gaschromatographie (DE-588)4019330-5 gnd Flüssigkeitschromatographie (DE-588)4017622-8 gnd |
| topic_facet | Analytische Chemie Gaschromatographie Flüssigkeitschromatographie |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=000776231&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT smithrogerm gasandliquidchromatographyinanalyticalchemistry |
Inhaltsverzeichnis
Schweinfurt Magazin
| Signatur: |
2801 1991:2679 |
|---|---|
| Exemplar 1 | ausleihbar Verfügbar Bestellen |