Analysis with supercritical fluids: extraction and chromatography
Gespeichert in:
| Weitere Verfasser: | |
|---|---|
| Format: | Buch |
| Sprache: | English |
| Veröffentlicht: |
Berlin ; Heidelberg ; New York ; London ; Paris ; Tokyo ; Hong Kong ; Barcelona ; Budapest
Springer
1992
|
| Schriftenreihe: | Springer laboratory
|
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Beschreibung: | XIV, 213 S. Ill. |
| ISBN: | 3540554203 0387554203 |
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| 245 | 1 | 0 | |a Analysis with supercritical fluids |b extraction and chromatography |c Bernd Wenclawiak (ed.) |
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CONTENTS
1 SFC AND SFE: AN INTRODUCTION FOR NOVICES
BERND WENCLAWIAK 1
2 PHYSICO-CHEMICAL PRINCIPLES
OF SUPERCRITICAL FLUID SEPARATION PROCESSES
GERHARD M
.
SCHNEIDER 9
2.1 INTRODUCTION 9
2.2 PHYSICO-CHEMICAL PROPERTIES
OF PURE SUPERCRITICAL SOLVENTS 10
2.2.1 THERMODYNAMIC PROPERTIES 10
2.2.2 DIELECTRIC PROPERTIES 10
2.2.3 TRANSPORT PROPERTIES 12
2.3 PHASE EQUILIBRIA OF FLUID MIXTURES 13
2.3.1 PHASE-THEORETICAL ASPECTS 13
2.3.2 CLASSIFICATION OF BINARY CRITICAL PHASE BEHAVIOR
BY "FAMILIES" 14
2.3.3 TERNARY SYSTEMS 16
2.3.4 QUATERNARY SYSTEMS 19
2.3.5 SOLUBILITY OF SOLIDS IN SUPERCRITICAL SOLVENTS 21
2.3.6 ISOTHERMAL PRESSURE (CONCENTRATION)
PHASE DIAGRAMS 21
2.3.7 CALCULATION AND CORRELATION
OF FLUID PHASE EQUILIBRIA 24
2.4 PHYSICO-CHEMICAL APPLICATIONS OF SFC 26
2.4.1 CAPACITY RATIOS 26
2.4.2 DIFFUSION COEFFICIENTS 28
REFERENCES 30
3 BASIC PRINCIPLES OF ANALYTICAL SUPERCRITICAL FLUID
EXTRACTION
JERRY
W.
KING
AND
JOHN
E.
FRANCE
32
3.1 THE DEVELOPMENT OF ANALYTICAL SFE 32
3.1.1 SAMPLE PREPARATION IN ANALYTICAL CHEMISTRY 32
3.1.2 UTILIZATION OF SUPERCRITICAL FLUIDS
IN ANALYTICAL-SCALE EXTRACTIONS 33
3.1.3 FEATURES OF ANALYTICAL SFE 33
HTTP://D-NB.INFO/920748325
VIII CONTENTS
3.2 FLUID PROPERTIES IN SFE 34
3.2.1 SELECTION OF THE SUPERCRITICAL FLUID 34
3.2.2 UNIQUE PROPERTIES OF SUPERCRITICAL FLUID
CARBON DIOXIDE 36
3.2.3 THE USE OF COSOLVENTS IN SFE 37
3.3 OPTIMIZING EXPERIMENTAL CONDITIONS
FOR ANALYTICAL SFE 39
3.3.1 OBJECTIVES OF THE EXTRACTION 39
3.3.2 CRITICAL PARAMETERS PERTINENT TO SFE 41
3.3.3 A THEORETICAL APPROACH FOR OPTIMIZING SFE 42
3.4 THE RELEVANCE OF SFC-DERIVED DATA
TO ANALYTICAL SFE 43
3.4.1 RELEVANT MEASUREMENTS BY SFC 44
3.4.2 IMPLICATIONS FOR SFE 45
3.5 THE PRACTICE OF ANALYTICAL SFE 46
3.5.1 EQUIPMENT REQUIREMENTS 46
3.5.2 EXPERIMENTAL CONSIDERATIONS IN ANALYTICAL SFE . 49
3.6 SAMPLE MATRIX EFFECTS IN SFE 51
3.6.1 PHYSICAL MATRIX EFFECTS 52
3.6.2 CHEMICAL CHANGES IN THE SAMPLE MATRIX 52
3.6.3 IMPACT OF MATRIX ON EXTRACTION KINETICS 53
3.7 PROBLEMS AND FUTURE RESEARCH NEEDS
IN ANALYTICAL SFE 55
REFERENCES 57
4 COUPLED SUPERCRITICAL FLUID EXTRACTION-CAPILLARY
GAS CHROMATOGRAPHY (SFE-GC)
STEVEN B. HAWTHORNE 6
1
4.1 INTRODUCTION 61
4.2 PERFORMING SFE-GC 61
4.2.1 INSTRUMENTATION AND METHODS 61
4.2.2 FLUIDS AND EXTRACTION CONDITIONS
USED FOR SFE-GC 64
4.3 ABILITIES AND LIMITATIONS OF SPLIT AND ON-COLUMH
SFE-GC 65
4.3.1 CHROMATOGRAPHIE PEAK SHAPES OBTAINED
USING SFE-GC 65
4.3.2 QUANTITATION USING SFE-GC 67
4.3.3 SPEED OF SFE-GC ANALYSES 67
4.3.4 SENSITIVITY AND SAMPLE SIZES 68
4.3.5 SAMPLE TYPES AND MATRIX CONSIDERATIONS 70
4.4 SUMMARY 72
REFERENCES 72
CONTENTS IX
5 GRADIENTS IN SFC
ERNST KLESPER
AND
FRANZ
P.
SCHMITZ
74
5.1 OVERVIEW 74
5.2 TEMPERATURE GRADIENTS 79
5.3 PRESSURE GRADIENTS 81
5.4 DENSITY GRADIENTS 87
5.5 VELOCITY GRADIENTS 94
5.6 REFERENCES 97
6 INJECTION TECHNIQUES IN SFC
TYGE GREIBROKK 100
6.1 INTRODUCTION 100
6.2 THE PHYSICAL STATE OF THE SAMPLE 100
6.3 INTRODUCTION OF SUPERCRITICAL FLUID EXTRACTS 100
6.4 INTRODUCING A SOLUTION 101
6.5 PEAK FOCUSING 102
6.6 DIRECT INJECTION 103
6.7 OPEN SPLIT (DYNAMIC SPLIT) INJECTION 103
6.8 TIMED SPLIT INJECTION 105
6.9 SOLVENT EFFECTS ON PEAK SHAPE 106
6.10 SOLVENT VENTING WITH A PRECOLUMN 107
6.11 SOLVENT BACKFLUSH 109
6.12 SOLVENT VENTING WITH GAS PURGING 111
6.13 SAMPLE LOSSES IN THE INJECTOR 114
REFERENCES 115
7 STATIONARY PHASES FOR PACKED COLUMN
SUPERCRITICAL FLUID CHROMATOGRAPHY
COLIN F. POOLE, JOHN W. OUDSEMA,
THOMAS
A.
DEAN,
AND
SALWA
K.
POOLE
116
7.1 INTRODUCTION 116
7.2 PHYSICAL PROPERTIES OF COLUMN PACKINGS 116
7.3 INFLUENCE OF SUBSTRATE MORPHOLOGY ON THE
PROPERTIES OF CHEMICALLY BONDED PHASES IN SFC . 121
7.4 INFLUENCE OF SURFACE HETEROGENEITY ON THE
PROPERTIES OF CHEMICALLY BONDED PHASES 122
7.4.1 CHEMICAL INTERACTIONS WITH SILANOL GROUPS 122
7.4.2 DEACTIVATION OF SILANOL GROUPS
WITH MOBILE PHASE MODIFIERS 124
X CONTENTS
7.4.3 SHIELDING OF SILANOL GROUPS
BY POLYMER ENCAPSULATION 126
7.5 MACROPOROUS POLYMERIE PACKINGS 127
7.6 COLUMN PACKINGS USED FOR SPECIAL APPLICATIONS 127
7.7 CONCLUSIONS 131
REFERENCES 132
8 ENANTIOMER SEPARATION BY CAPILLARY
SUPERCRITICAL FLUID CHROMATOGRAPHY
MICHAEL SCHLEIMER
AND
VOLKER SCHURIG
134
8.1 INTRODUCTION 134
8.2 GENERAL ASPECTS 135
8.2.1 TFEMPERATURE 135
8.2.2 SPEED OF ANALYSIS AND EFFICIENCY 136
8.2.3 MOBILE PHASE 138
8.2.4 COLUMN LOADABILITY 139
8.3 PACKED COLUMN SFC 140
8.4 OPEN TUBULAER COLUMN SFC 140
8.5 CONCLUSION 146
REFERENCES 149
9 SUPERCRITICAL FLUID CHROMATOGRAPHY/
MASS SPECTROMETRY
J. DAVID PINKSTON .
.
.
' 151
9.1 INTRODUCTION 151
9.2 EARLY INVESTIGATIONS OF SFC/MS 151
9.3 SFC/MS USING DIRECT INTRODUCTION INTERFACES .
.
. 152
9.3.1 FLOW RESTRICTION 153
9.3.2 IONIZATION METHODS 154
9.3.2.1 CHEMICAL IONIZATION 154
9.3.2.2 ELECTRON IONIZATION AND CHARGE EXCHANGE 155
9.3.2.3 SECONDARY ION MASS SPECTROMETRY 156
9.3.3 TYPE OF MASS ANALYZER 157
9.3.3.1 DFI SFC/MS USING QUADRUPOLE
MASS SPECTROMETERS 157
9.3.3.2 DFI SFC/MS USING DOUBLE-FOCUSSING
SECTOR MASS SPECTROMETERS 158
9.3.3.3 DFI SFC/MS USING FOURIER TRANSFORM
MASS SPECTROMETERS 158
9.4 SFC/MS USING HIGH-FLOW-RATE INTERFACES 161
9.4.1 SFC/MS USING THE MOVING BELT INTERFACE 162
9.4.2 SFC/MS USING THE PARTICLE BEAM INTERFACE 163
CONTENTS XI
9.4.3 OFF-LINE SFC/MS 164
9.4.4 SFC/MS USING DIRECT INTRODUCTION
OF SPLIT EFFLUENTS 164
9.4.5 SFC/MS USING POST-EXPANSION SPLITTING 165
9.4.6 SFC/MS USING THE THERMOSPRAY INTERFACE 170
9.5 SUPERCRITICAL FLUID INJECTION/MASS SPECTROMETRY . 172
9.6 CONCLUSION 174
REFERENCES 175
10 SUPERCRITICAL FLUID CHROMATOGRAPHY
WITH FT-IR DETECTION
LARRY
T.
TAYLOR
AND
ELIZABETH
M.
CALVEY 178
10.1 INTRODUCTION 178
10.2 FLOW CELL APPROACH 178
10.3 SOLVENT ELIMINATION APPROACH 184
10.4 SUMMARY 188
REFERENCES 188
11 SUPERSONIC JET SPECTROSCOPY WITH SUPERCRITICAL FLUIDS
CHUNG HANG SIN, STEVEN R
. GOATES, MILTON L
. LEE,
AND
DAVID M
.
LUBMAN
190
11.1 INTRODUCTION 190
11.2 SUPERSONIC JET SPECTROSCOPY 191
11.2.1 PRINCIPLES. OF SUPERSONIC EXPANSIONS 191
11.2.2 SPECTROSCOPIC METHODS FOR DETECTION 192
11.3 HIGH PRESSURE FLUID INJECTION
FOR NONVOLATILE SAMPLES 193
11.3.1 EXPERIMENTAL 193
11.3.2 SUPERCRITICAL FLUID INJECTION 194
11.3.3 HIGH PRESSURE LIQUID INJECTION 196
11.4 SUPERCRITICAL FLUID CHROMATOGRAPHY
AND SUPERSONIC JET SPECTROSCOPY 197
11.4.1 EXPERIMENTAL 198
11.4.2 THE INTERFACES 199
11.5 CONCLUSIONS 202
REFERENCES 202
BASIC REFERENCES ANALYTICAL SCALE SFC/SFE 203
RECOMMENDED LITERATURE 207
SUBJECT INDEX 211 |
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| indexdate | 2024-12-02T09:05:17Z |
| institution | BVB |
| isbn | 3540554203 0387554203 |
| language | English |
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| spelling | Analysis with supercritical fluids extraction and chromatography Bernd Wenclawiak (ed.) Berlin ; Heidelberg ; New York ; London ; Paris ; Tokyo ; Hong Kong ; Barcelona ; Budapest Springer 1992 XIV, 213 S. Ill. txt rdacontent n rdamedia nc rdacarrier Springer laboratory Gas (DE-588)4019320-2 gnd rswk-swf SFC (DE-588)4184106-2 gnd rswk-swf Überkritischer Zustand (DE-588)4186602-2 gnd rswk-swf Destraktion (DE-588)4124778-4 gnd rswk-swf Extraktion (DE-588)4016062-2 gnd rswk-swf Destraktion (DE-588)4124778-4 s DE-604 Gas (DE-588)4019320-2 s Überkritischer Zustand (DE-588)4186602-2 s Extraktion (DE-588)4016062-2 s SFC (DE-588)4184106-2 s Wenclawiak, Bernd edt DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=019107505&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Analysis with supercritical fluids extraction and chromatography Gas (DE-588)4019320-2 gnd SFC (DE-588)4184106-2 gnd Überkritischer Zustand (DE-588)4186602-2 gnd Destraktion (DE-588)4124778-4 gnd Extraktion (DE-588)4016062-2 gnd |
| subject_GND | (DE-588)4019320-2 (DE-588)4184106-2 (DE-588)4186602-2 (DE-588)4124778-4 (DE-588)4016062-2 |
| title | Analysis with supercritical fluids extraction and chromatography |
| title_auth | Analysis with supercritical fluids extraction and chromatography |
| title_exact_search | Analysis with supercritical fluids extraction and chromatography |
| title_full | Analysis with supercritical fluids extraction and chromatography Bernd Wenclawiak (ed.) |
| title_fullStr | Analysis with supercritical fluids extraction and chromatography Bernd Wenclawiak (ed.) |
| title_full_unstemmed | Analysis with supercritical fluids extraction and chromatography Bernd Wenclawiak (ed.) |
| title_short | Analysis with supercritical fluids |
| title_sort | analysis with supercritical fluids extraction and chromatography |
| title_sub | extraction and chromatography |
| topic | Gas (DE-588)4019320-2 gnd SFC (DE-588)4184106-2 gnd Überkritischer Zustand (DE-588)4186602-2 gnd Destraktion (DE-588)4124778-4 gnd Extraktion (DE-588)4016062-2 gnd |
| topic_facet | Gas SFC Überkritischer Zustand Destraktion Extraktion |
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