Modern sample preparation for chromatography
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Elsevier
2015
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| 008 | 141208s2015 xx ad|| |||| 00||| eng d | ||
| 015 | |a GBB4C2562 |2 dnb | ||
| 020 | |a 9780444543196 |c (hbk.) £130.00 |9 978-0-444-54319-6 | ||
| 035 | |a (OCoLC)904553317 | ||
| 035 | |a (DE-599)BVBBV042228355 | ||
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| 100 | 1 | |a Moldoveanu, Serban C. |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a Modern sample preparation for chromatography |c Serban Moldoveanu ; Victor David |
| 264 | 1 | |a Amsterdam [u.a.] |b Elsevier |c 2015 | |
| 300 | |a XII, 453 S. |b Ill., graph. Darst. |c 24 cm | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 650 | 4 | |a Chromatographic analysis | |
| 650 | 4 | |a Sample preparation (Chemistry) | |
| 700 | 1 | |a David, Victor |d 1955- |e Verfasser |0 (DE-588)1029787433 |4 aut | |
| 856 | 4 | 2 | |m HBZ Datenaustausch |q application/pdf |u http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=027666708&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |3 Inhaltsverzeichnis |
| 943 | 1 | |a oai:aleph.bib-bvb.de:BVB01-027666708 | |
Datensatz im Suchindex
| DE-19_call_number | 1801/VG 5170 M717 |
|---|---|
| DE-19_location | 85 |
| DE-BY-UBM_katkey | 5099624 |
| DE-BY-UBM_media_number | 41621342290012 |
| _version_ | 1823055627633557504 |
| adam_text | Titel: Modern sample preparation for chromatography
Autor: Moldoveanu, Serban C
Jahr: 2015
Contents
Preface xi
_I_
GENERAL CONCEPTS IN
SAMPLE PREPARATION
1. Preliminaries to Sample Preparation 3
1.1 Collection of Information and Planning
for a Chromatographic Analysis 3
General Comments 3
Chromatographic Core Analysis 4
Collection of Information Regarding the Analysis 4
Planning the Analysis 7
1.2 The Evaluation of Analytical Data 8
General Aspects 8
Precision and Accuracy in Quantitative Chemical
Analysis 9
Propagation of Uncertainty 13
Comparison of Two Procedures Regarding Accuracy 14
Comparison of Two Procedures Regarding Precision 16
Sensitivity and Limit of Detection 16
Practical LOD and LOQ (PLOD and PLOQ) 21
Validation of an Analytical Method 21
1.3 Sampling 23
General Comments 23
Sampling Techniques 24
Proper Sampling 25
Some Comments on Sampling of Cases 28
Some Comments on Sampling of Liquids 29
Some Comments on Sampling of Solids 30
Some Comments on Sampling of Mixed-Phase
Materials 30
Some Comments on Handling, Preservation,
and Storage of Samples 30
References 31
2. The Role of Sample Preparation 33
2.1 Routine Manipulations of the Sample 34
General Comments 34
Weighing 34
Volume Measuring 34
Mixing and Dilution 34
Heating and Cooling 34
Other Routine Sample Manipulation 34
Preservation of Sample Integrity during Processing 35
2.2 Preliminary Processing of the Sample 35
General Comments 35
Sample Homogenization 35
Adjustment of Water Content in Samples (Drying) 36
Sample Dissolution 36
Resampling for Further Reduction of Sample Size 37
2.3 Sample Cleanup and Fractionation 37
General Comments 37
Cleanup and Fractionation Procedures 38
Analyte Recovery during Sample Cleanup 39
2.4 Concentration of the Sample 40
General Comments 40
Enrichment Factor 40
2.5 Chemical Modifications of the Sample 42
General Comments 42
Chemical Changes for Sample Dissolution 43
Chemical Changes for Cleanup and Fractionation Purposes 43
Chemical Modification for the Enhancement of Detection 43
Chemical Modification for Enhancing the Separation
in Core Chromatography 44
2.6 Selection of a Sample Preparation Procedure 44
General Comments 44
Development of a Sample Preparation Scheme based on
Preliminary Infonnation 45
V
vi
CONTENTS
2.7 Automation in Sample Preparation 48
General Comments 48
References 49
3. Chromatography as a Core Step
for art Analytical Procedure 51
3.1 Basic Concepts in Chromatography 51
General Comments 51
Common Types of Chromatography 52
Basic Characterization of a Chromatographic Process 53
Qualitative Chromatographic Analysis 58
Quantitative Chromatographic Analysis 59
Selection of the Internal Standards in Chromatographic
Analysis 63
3.2 Overview of GC 63
Retention and Separation Mechanism in GC 63
Typical GC Instrumentation 66
Injection and Injection Port of a GC 67
The Oven of a Gas Chromatograph 70
Chromatographic Columns 71
Detectors in GC 74
The Need for Sample Preparation in GC 76
3.3 Overview of HPLC 77
Retention and Separation Mechanism in LC 77
Typical HPLC Instrumentation 77
Solvent Supply and Pumping System 78
Mobile Phase in HPLC 79
Injectors 79
Chromatographic Column 80
Detectors in HPLC 81
The Need for Sample Preparation in HPLC 83
3.4 Other Chromatography Types Used as Core
Analytical Method 83
General Comments 83
References 84
_II_
MAIN SAMPLE PREPARATION
TECHNIQUES
4. Mechanical Processing in Sample
Preparation 89
4.1 Grinding and Sieving 89
General Comments 89
Particle Size Reduction 89
Sieving 91
4.2 Filtration, Microfiltration, and Ultrafiltration 91
General Aspects 91
Theory of Filtration of Solids from Liquids 93
Filters and Membranes Properties 94
Filters and Membranes Materials 96
Filtering Devices in the Laboratory 97
Continuous Filtration 100
In vivo Application of Ultrafiltration 101
4.3 Centrifugation 101
General Aspects 101
The Use of Centrifugation in Connection with Filtration
and Ultrafiltration 103
References 103
5. Phase Transfer in Sample Preparation 105
5.1 Distillation, Vaporization, and Drying 105
General Comments 105
Gas—Liquid Equilibrium for Two-Component Systems 106
Dependence of Boiling Point on Pressure 111
Distillation 112
Distillation under Vacuum and Centrifugal Force 114
Steam Distillation and Other Distillation Processes 114
Vaporization 116
Drying and Freeze-Drying 117
Cryofocusing 119
5.2 Physical Dissolution, Crystallization, and
Precipitation 120
General Comments 120
Dissolution Process (Physical Dissolution) 120
Hildebrand Solubility Parameter 121
Solubility Based on Octanol/Water Partition Coefficient 124
Solubility of Ionic Compounds 124
Selection of Sample Solvent for Chromatography 126
Crystallization and Precipitation 127
References 129
6. Solvent Extraction 131
6.1 Conventional Liquid—Liquid Extraction 132
General Comments 132
Liquid—Liquid Partition Equilibrium 132
Distribution Coefficient 134
Partition Equilibrium for Ionic Species, Metal Complexes,
and Ion Pairs 134
Elementary Thermodynamic Theory for Solvent Extraction 136
Common LLE Procedures 138
CONTENTS
vii
Quantitation when LLE is Part of Sample Preparation 140
Selection of Solvents for the Extraction Process 141
Miscibility of Solvents 143
Solvent Characterization Based on Octanol/Water Partition
Coefficient 143
Solvent Characterization Based on Liquid—Gas Partition 144
The Influence of pH on Extraction 149
Chemical Modifications that Affect Extraction 153
Nonchemical Factors Affecting Extraction 153
Separation Using LLE 154
6.2 Special LLE Procedures 155
General Comments 155
Single-Drop Microextraction 156
Membrane-Assisted Solvent Extraction 157
Microporous Membrane Liquid—Liquid Extraction 158
Hollow Fiber Liquid-Phase Microextraction 158
Liquid—Liquid—Liquid Microextraction 158
Dispersive Liquid—Liquid Microextraction 159
Salting-out-Assisted LLE 160
LLE with Low-Temperature Partitioning 160
Cloud Point Extraction 160
Electrochemically Modulated LLE 161
Simultaneous Distillation and Extraction 161
Automation in LLE 162
6.3 Conventional Liquid—Solid Extraction 163
General Comments 163
The Rate of Extraction in LSE 163
Solvents Used in LSE 165
Simple Extraction Conditions 165
Soxhlet Extraction 166
Separation Using LSE 168
6.4 Accelerated Solvent Extraction 169
General Comments 169
Instrumentation in ASF 169
Selection of Parameters for ASF Operations 170
Pressurized Hot Water Extraction 171
6.5 Microwave-Assisted Solvent Extraction 172
General Comments 172
Theory of Microwave Usage 173
Practice of Microwave Extraction 174
6.6 Supercritical Solvent Extraction 176
General Aspects 176
Elementary Theory of SEE 176
Diffusion Coefficients for Supercritical Fluids 178
Steps in the SEE Process 179
Optimization of the Extraction 179
Expansion of Fluid and Collection Process in SEE 181
SEE On-line with Other Chromatographic Techniques 183
6.7 Solvent—Gas Extraction 185
General Aspects 185
Headspace Single-Drop Microextraction
References 185
185
195
7. Solid-Phase Extraction 191
7.1 Conventional Solid-Phase Extraction 192
General Comments 192
Practice of Conventional SPE 193
Quantitation when SPE is Part of Sample Preparation
Equilibrium in SPE 195
Comparison of SPE with Liquid Chromatography 197
Breakthrough Volume in SPE 198
7.2 Materials Used as Solid Phases and Formats 201
General Comments 201
Chemical Nature of Materials Used as SPE Sorbent 202
Physical Properties of Materials Used as SPE Sorbent 217
Formats Used in SPE 218
Parameters Characterizing SPE Performance 221
7.3 Retention and Elution Mechanisms in SPE 222
General Comments 222
Retention and Elution on Hydrophobic Phases 223
Retention and Elution on Polar Phases 225
Retention and Elution on Ion Exchange Phases 225
7.4 Selection of Sorbents in SPE Practice 229
General Comments 229
Nonpolar SPE Sorbents 230
Polar SPE Sorbents 233
Ion Exchange SPE Sorbents 235
Chelating Ion Exchange Resins 240
Affinity and Immunoaffinity Sorbents
Molecular Imprinted SPE 241
Moisture and Particulate Removal SPE
Other Types of Sorbents Used for SPE
Mixed-Mode Sorbents 243
Sorbents Used in Headspace Analysis
240
241
242
244
246
7.5 Solvents Used in SPE
General Comments 246
Sorbent Conditioning 246
Selection of Solvent for Solute Retention 247
Selection of Solvent for Solute Elution 249
viii
CONTENTS
7.6 Optimization of SPE 249
Making the Sample Amenable for SPE 249
Optimization of Sorbents and Solvent Selection 250
7.7 SPE from Headspace 254
General Aspects 254
Basic Theory of Static Headspace Extraction 254
Basic Theory of Dynamic Headspace Extraction 258
Practice of Static Headspace Analysis 259
Practice of Dynamic Headspace Analysis 260
Desorption of the Analytes from the Trap 262
Quantitation in Headspace Techniques 264
Open Tubular Trapping 265
7.8 Solid-Phase Microextraction (SPME) 266
General Comments 266
Basic Theory of the Retention of Analytes on SPME
Fiber 268
Common Coatings for SPME Fibers 270
Desorption of Analytes and Conditioning of the SPME
Fiber 274
Optimization of SPME Analysis 275
Qualitative and Quantitative Analysis with SPME 277
SPME Automation 278
7.9 Special SPE Techniques 278
General Comments 278
Matrix Solid-Phase Dispersion 279
QuEChERS 279
Stir Bar Sotptive Extraction (SBSE) 280
Comments on Automation in SPE 283
References 283
8. Other Sample Preparation Techniques
Not Involving Chemical Modifications
of the Analyte 287
8.1 Chromatographic Procedures as Preliminary
Separations 287
General Comments 287
Thin Layer Chromatography as Sample Preparation 288
Open-Column Liquid Chromatography 289
Size Exclusion Used in Sample Preparation 290
8.2 Membrane Separations as Sample Preparation
Techniques 295
General Comments 295
Gas Diffusion through Membranes 295
Reverse Osmosis 296
Dialysis 298
Ion-Exchange Membranes 299
8.3 Electroseparations in Sample Preparation 300
General Comments 300
Electrophoretic Techniques 300
Other Electroseparation Techniques 304
8.4 Other Techniques in Sample Preparation 304
General Comments 304
References 304
9. The Role of Derivatization in
Chromatography 307
9.1 Derivatization for Sample Dissolution 308
General Comments 308
Sample Dissolution by pH Change 308
Other Common Dissolution Procedures Using Chemical
Reactions 309
9.2 Improvement of Gas Chromatographic
Analysis by Derivatization 311
General Comments 311
Procedures for Performing Derivatization for GC 312
Derivatization for Making Polar and/or Nonvolatile
Compounds Amenable for GC 313
The Role of Derivatization in the Improvement of
Separation 313
Derivatization for Improving Sensitivity of
Detection 314
Derivatization for Improving Compound
Identification 316
Improvement of Quantitation Accuracy through
Derivatization 318
9.3 Improvement of Liquid Chromatographic Analysis by
Derivatization 319
General Comments 319
Procedures for Performing Derivatization for EC 319
The Role of Derivatization in the Improvement of
Separation 320
The Role of Derivatization in the Improvement of Detection
Sensitivity 320
Improvement of Quantitation Accuracy through
Derivatization 325
CONTENTS
ix
Derivatization for the Improvement of Stability of the
Analyte 325
9.4 Derivatization for Chiral Separations 326
General Comments 326
Separation of Enantiomers on Chiral Stationary
Phases 328
Separation of Diastereoisomers After Derivatization
with Chiral Reagents 328
References 330
10. Chemical Reactions Used
in Derivatizations 333
10.1 Reactions with Formation of Alkyl or Aryl
Derivatives 334
General Comments 334
Alkylation and Arylation Mechanisms 334
Common Alkylation Reagents 337
Artifact Formation in Alkylation Reactions 345
10.2 Reactions with Formation of Silyl Derivatives 347
General Comments 347
Some Aspects of Silylation Mechanism 348
Reagents Used for Silylation 351
Silylation for the Introduction of Groups Other than TMS 362
Artifact Formation in Trimethylsilyl Derivatizations 370
10.3 Derivatives Formation through Acylation
Reactions 374
General Comments 374
Some Aspects Regarding Acylation Mechanism 375
Typical Acylation Reagents 375
Derivatization with Chloroformâtes 380
Derivatization with Sulfonyl Derivatives 384
Derivatization with Isocyanates, Isothiocyanates, Carbonyl
Azides 384
Artifact Formation in Acylation Reactions 384
10.4 Other Derivatization Reactions 385
General Comments 385
Additions to Carbon—Heteroatom Multiple Bonds 385
Derivatization with Formation of Cyclic Compounds 387
Additions to Double Bonds, Oxidation—Reductions, Hydrolysis,
Other Transformations of Reactive Analytes 388
References 388
11. Chemical Degradation of Polymers
for Chromatographic Analysis 393
11.1 Chemical Degradation of Polymeric
Carbohydrates 393
General Comments 393
Polysaccharide Structure 394
Steps in Polysaccharide Analysis 395
Identification of the Constituent Monosaccharides, their n or L
Configuration, and Polymerization Degree 395
Determination of the Position of Glycosidic Linkages 397
Determination of the Sequence of Monosaccharide
Residues 399
11.2 Chemical Degradation of Proteins 401
General Comments 401
11.3 Chemical Degradation of Other Macromolecular
Compounds 404
General Comments 404
References 408
12. Comments on Sample Preparation in
Chromatography for Different Types of
Materials 411
12.1 Sample Preparation Techniques for the Analysis
of Air, Water, and Soil 412
General Aspects 412
Analysis of Gaseous Samples 413
Basic Operations in Sample Preparation for Water Analysis 413
Extraction of Volatile and Nonvolatile Compounds
from Soil Samples 415
Sample Preparation for the Analysis of Various
Environmental Pollutants 415
12.2 Sample Preparation for the Analysis of
Pharmaceuticals 416
General Aspects 416
Quality Control of Pharmaceuticals 419
Clinical Trials 421
12.3 Sample Preparation for the Analysis of Biological
Samples 421
General Aspects 421
Handling, Preservation, and Storage of Biological
Samples 422
Analysis of Breath Condensate and Volatiles Emitted
from Skin or Bodily Fluids 423
Analysis of Liquid Samples of Biological Origin 424
Analysis of Solid Samples of Biological Origins 430
X
CONTENTS
12.4 Sample Preparation for Food and Agricultural
Products 431
General Aspects 431
Food and Beverage Analysis 432
Agricultural Products 435
12.5 Sample Preparation Related to the Analysis
of Other Materials and/or Processes 435
General Comments 435
Archeological Artifacts 435
Cosmetics 436
Detergents 437
Dyes and Pigments 437
Preservatives 438
Tobacco and Cigarette Smoke 438
References 439
Index 447
|
| any_adam_object | 1 |
| author | Moldoveanu, Serban C. David, Victor 1955- |
| author_GND | (DE-588)1029787433 |
| author_facet | Moldoveanu, Serban C. David, Victor 1955- |
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| discipline | Chemie / Pharmazie |
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| id | DE-604.BV042228355 |
| illustrated | Illustrated |
| indexdate | 2025-02-03T17:41:49Z |
| institution | BVB |
| isbn | 9780444543196 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-027666708 |
| oclc_num | 904553317 |
| open_access_boolean | |
| owner | DE-11 DE-19 DE-BY-UBM |
| owner_facet | DE-11 DE-19 DE-BY-UBM |
| physical | XII, 453 S. Ill., graph. Darst. 24 cm |
| publishDate | 2015 |
| publishDateSearch | 2015 |
| publishDateSort | 2015 |
| publisher | Elsevier |
| record_format | marc |
| spellingShingle | Moldoveanu, Serban C. David, Victor 1955- Modern sample preparation for chromatography Chromatographic analysis Sample preparation (Chemistry) |
| title | Modern sample preparation for chromatography |
| title_auth | Modern sample preparation for chromatography |
| title_exact_search | Modern sample preparation for chromatography |
| title_full | Modern sample preparation for chromatography Serban Moldoveanu ; Victor David |
| title_fullStr | Modern sample preparation for chromatography Serban Moldoveanu ; Victor David |
| title_full_unstemmed | Modern sample preparation for chromatography Serban Moldoveanu ; Victor David |
| title_short | Modern sample preparation for chromatography |
| title_sort | modern sample preparation for chromatography |
| topic | Chromatographic analysis Sample preparation (Chemistry) |
| topic_facet | Chromatographic analysis Sample preparation (Chemistry) |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=027666708&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT moldoveanuserbanc modernsamplepreparationforchromatography AT davidvictor modernsamplepreparationforchromatography |