The troubleshooting and maintenance guide for gas chromatographers:
Gespeichert in:
| Vorheriger Titel: | Rood, Dean A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
|---|---|
| 1. Verfasser: | |
| Format: | Buch |
| Sprache: | English |
| Veröffentlicht: |
Weinheim [u.a.]
Wiley-VCH
2007
|
| Ausgabe: | 4., rev. and updated ed. |
| Schlagworte: | |
| Online-Zugang: | Inhaltsverzeichnis |
| Beschreibung: | XVII, 326 S. Ill., graph. Darst. |
| ISBN: | 9783527313730 |
Internformat
MARC
| LEADER | 00000nam a2200000 c 4500 | ||
|---|---|---|---|
| 001 | BV021295510 | ||
| 003 | DE-604 | ||
| 005 | 20131021 | ||
| 007 | t | ||
| 008 | 060117s2007 gw ad|| |||| 00||| eng d | ||
| 020 | |a 9783527313730 |9 978-3-527-31373-0 | ||
| 035 | |a (OCoLC)153538333 | ||
| 035 | |a (DE-599)BVBBV021295510 | ||
| 040 | |a DE-604 |b ger |e rakddb | ||
| 041 | 0 | |a eng | |
| 044 | |a gw |c DE | ||
| 049 | |a DE-91G |a DE-703 |a DE-19 |a DE-634 |a DE-20 |a DE-11 |a DE-858 | ||
| 050 | 0 | |a QD79.C45 | |
| 082 | 0 | |a 543.85 |2 22 | |
| 084 | |a VG 7400 |0 (DE-625)147205:253 |2 rvk | ||
| 084 | |a CHE 234f |2 stub | ||
| 100 | 1 | |a Rood, Dean |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a The troubleshooting and maintenance guide for gas chromatographers |c Dean Rood |
| 250 | |a 4., rev. and updated ed. | ||
| 264 | 1 | |a Weinheim [u.a.] |b Wiley-VCH |c 2007 | |
| 300 | |a XVII, 326 S. |b Ill., graph. Darst. | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 650 | 4 | |a Gas chromatography | |
| 650 | 4 | |a Gas chromatography |x Instruments |x Maintenance and repair | |
| 650 | 0 | 7 | |a Fehlersuche |0 (DE-588)4016615-6 |2 gnd |9 rswk-swf |
| 650 | 0 | 7 | |a Glaskapillargaschromatographie |0 (DE-588)4157443-6 |2 gnd |9 rswk-swf |
| 650 | 0 | 7 | |a Kapillargaschromatographie |0 (DE-588)4252082-4 |2 gnd |9 rswk-swf |
| 689 | 0 | 0 | |a Kapillargaschromatographie |0 (DE-588)4252082-4 |D s |
| 689 | 0 | 1 | |a Fehlersuche |0 (DE-588)4016615-6 |D s |
| 689 | 0 | |8 1\p |5 DE-604 | |
| 689 | 1 | 0 | |a Glaskapillargaschromatographie |0 (DE-588)4157443-6 |D s |
| 689 | 1 | |8 2\p |5 DE-604 | |
| 780 | 0 | 0 | |i Bis 3. Auflage |a Rood, Dean |t A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
| 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=014616279&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |3 Inhaltsverzeichnis |
| 999 | |a oai:aleph.bib-bvb.de:BVB01-014616279 | ||
| 883 | 1 | |8 1\p |a cgwrk |d 20201028 |q DE-101 |u https://d-nb.info/provenance/plan#cgwrk | |
| 883 | 1 | |8 2\p |a cgwrk |d 20201028 |q DE-101 |u https://d-nb.info/provenance/plan#cgwrk | |
Datensatz im Suchindex
| _version_ | 1804135090210471936 |
|---|---|
| adam_text | VII
Contents
Preface V
Intentions and Introduction 1
1 Introduction to Capillary Gas Chromatograph/ 3
1.1 What Is Gas Chromatography? 3
1.2 What Types of Compounds Are Suitable for GC Analysis? 3
1.3 The Basic Parts of a Gas Chromatograph 4
1.3.1 Gas Supply and Flow Controllers 4
1.3.2 Injector 5
1.3.3 Capillary Column and Oven 5
1.3.4 Detector 6
1.3.5 Data System 6
1.4 The Chromatogram 6
1.5 The Mechanism of Compound Separation 8
1.5.1 A Simple Description of the Chromatographie Process 8
1.5.2 A Detailed Description of the Chromatographie Process 9
1.6 Factors Affecting Separation 11
1.6.1 Stationary Phase 11
1.6.2 Compound Structure 12
1.6.3 Column Temperature 12
2 Basic Definitions and Equations 14
2.1 Why Bother? 14
2.2 Peak Shapes 14
2.2.1 Peak Width (W) 14
2.2.2 Peak Symmetry 14
2.3 Retention 16
2.3.1 Retention Time (tr) 16
2.3.2 Adjusted Retention Time ($ 16
2.3.3 Retention Factor (fc) 16
2.3.4 Retention Index (/) 18
2.4 Phase Ratio (ß) 19
2.5 Distribution Constant (Kc) 20
The Troubleshooting and Maintenance Guide for Gas Chromatographers, Fourth Edition. Dean Rood
Copyright © 2007 WILEY-VCH Verlag GmbH Co. KGaA, Weinheim
ISBN: 978-3-527-31373-0
VIII Contents
2.5.1 Kc and Column Dimensions 21
2.5.2 Kc and Column Temperature 21
2.6 Column Efficiency 21
2.6.1 Number of Theoretical Plates (N) 22
2.6.2 Height Equivalent to a Theoretical Plate (H) 22
2.6.3 Effective Theoretical Plates (Neff) and Effective Plate Heights (Heff) 23
2.6 A Precautions When Using Theoretical Plates 23
2.7 Utilization of Theoretical Efficiency (UTE%) 24
2.8 Separation Factor (a) 25
2.9 Resolution (R) 25
2.10 Trennzahl (TZ) 27
2.11 Column Capacity 28
3 Capillary CC Columns: Tubing 30
3.1 Fused Silica Capillary Columns 30
3.2 Fused Silica Tubing 30
3.3 Outer Coating 32
3.4 Other Tubing Materials 32
3.5 Polyimide Fused Silica Tubing Bending Stress 33
4 Capillary GC Columns: Stationary Phases 34
4.1 Stationary Phases 34
4.2 Types of Stationary Phases 35
4.2.1 Polysiloxanes or Silicones 35
4.2.2 Arylene-Modified Polysiloxanes 37
4.2.3 Polyethylene Glycols 37
4.2.4 Porous Layer Stationary Phases 38
4.3 Characteristics of Stationary Phases 39
4.3.1 Bonded and Cross-linked Stationary Phases 39
4.3.2 Stationary Phase Polarity 39
4.3.3 Stationary Phase Selectivity 40
4.4 Stationary Phase Interactions 41
4.4.1 Dispersion Interaction 41
4.4.2 Dipole Interaction 42
4.4.3 Hydrogen Bonding Interaction 43
4.4.4 When There are Multiple Interactions 44
4.5 Stationary Phase Equivalencies 45
4.6 Column Temperature Limits 46
4.7 Column Bleed 47
4.7.1 What is Column Bleed? 47
4.7.2 Measuring Column Bleed 48
4.7.3 Sensitivity Considerations 49
4.7 A Detector Considerations 49
4.7.5 Minimizing Column Bleed 50
4.8 Selecting Stationary Phases 50
Contents IX
5 Capillary CC Columns: Dimensions 53
5.1 Introduction 53
5.2 Column Length 53
5.2.1 Column Length and Efficiency/Resolution 53
5.2.2 Column Length and Retention 57
5.2.3 Column Length and Pressure 57
5.2.4 Column Length and Bleed 58
5.2.5 Column Length and Cost 58
5.2.6 Selecting Column Length 58
5.3 Column Diameter 59
5.3.1 Column Diameter and Efficiency/Resolution 59
5.3.2 Column Diameter and Retention 62
5.3.3 Column Diameter and Pressure 62
5.3.4 Column Diameter and Bleed 63
5.3.5 Column Diameter and Capacity 63
5.3.6 Column Diameter and Carrier Gas Volume 64
5.3.7 Column Diameter and Injector Efficiency 64
5.3.8 Column Diameter and Breakage 65
5.3.9 Column Diameter and Cost 65
5.3.10 Selecting Column Diameter 65
5.4 Column Film Thickness 66
5.4.1 Column Film Thickness and Retention 66
5.4.2 Column Film Thickness and Efficiency/Resolution 69
5.4.3 Column Film Thickness and Capacity 70
5.4.4 Column Film Thickness and Bleed 71
5.4.5 Column Film Thickness and Inertness 71
5.4.6 Selecting Column Film Thickness 72
5.5 Manipulating Multiple Column Dimensions 72
6 Carrier Gas 74
6.1 Carrier Gas and Capillary Columns 74
6.2 Linear Velocity versus Flow Rate 74
6.3 Controlling the Linear Velocity and Flow Rate 74
6.4 Van Deemter Curves 75
6.5 Carrier Gas Measurements 76
6.5.1 Average Linear Velocity (m) 76
6.5.2 Column Flow Rate 79
6.6 Carrier Gas Selection 80
6.6.1 Nitrogen 80
6.6.2 Helium 80
6.6.3 Hydrogen 82
6.7 Recommended Average Linear Velocities 83
6.8 Gas Purities 86
6.9 Common Carrier Gas Problems 87
XI Contents
7 Injectors 89
7.1 Introduction 89
7.2 The Basics of Vaporization Injectors 89
7.2.1 Injector Temperature 91
7.2.2 Speed of Sample Transfer 91
7.2.3 Injector Backflash 91
7.2.4 Injector Discrimination 94
7.3 Split Injectors 95
7.3.1 Description of a Split Injector 95
7.3.2 Split Ratio 96
7.3.3 Septum Purge for Split Injectors 99
7.3.4 Split Injector Liners 99
7.3.5 Column Position in Split Injectors 101
7.3.6 Common Problems with Split Injectors 102
7.4 Splitless Injectors 102
7 .4.1 Description of a Splitless Injector 102
7.4.2 Selecting Purge Activation Times 105
7.43 Solvent Effect for Splitless Injectors 106
7.4.4 Cold Trapping for Splitless Injectors 108
7.4.5 Septum Purge for Splitless Injectors 108
7.4.6 Splitless Injection Liners 109
7.4.7 Column Position in Splitless Injectors 109
7.4.8 Other Aspects of Splitless Injectors 110
7.4.9 Common Problems with Splitless Injectors 111
7.5 Direct Injectors 112
7.5.1 Description of a Direct Injector 112
7.5.2 Direct Injection Liners 113
7.5.3 Septum Purge for Direct Injectors 115
7.5.4 Column Position in Direct Injectors 115
7.5.5 Other Aspects of Direct Injectors 115
7.5.6 Common Problems with Direct Injectors 116
7.6 Cool On-Column Injectors 117
7.6.1 Description of an On-Column Injector 117
7.6.2 Solvent Effect and Cold Trapping for Cool On-Column Injectors 118
7.6.3 Secondary Cooling 119
7.6.4 Retention Gaps and Cool On-Column Injectors 119
7.6.5 Other Aspects of Cool On-Column Injectors 120
7.6.6 Common Problems With On-Column Injectors 120
7.7 Pressure and Flow Programmable Injectors 121
7.7.1 Description of Programmable Injectors 121
7.7.2 Constant Pressure Mode 122
7.7.3 Constant Flow or Velocity Mode 122
7.7 .4 Pressure Program Mode 123
7.7.5 Pulsed Pressure Mode 124
7.7.6 Gas Saver Mode 125
Contents XI
7.7.7 Other Aspects of Programmable Injectors 125
7.8 Injection Techniques 126
7.8.1 Syringe Filling Techniques 126
7.8.2 Injection Speed 128
7.9 Autosamplers 129
7.10 Injector Septa 131
7.10.1 Introduction 131
7.10.2 Septa Hardness 131
7.10.3 Septa Bleed 131
7.10.4 Handling Septa 133
7.11 Injector Maintenance 134
7.11.1 Cleaning Injectors 134
7.11.2 Injector Traps 135
7.11.3 Cleaning Injector Liners 135
7.11.4 Silylaring Injector Liners 136
8 Detectors 139
8.1 Introduction 139
8.2 Detector Characteristics 139
8.2.1 Detector Dead Volume 139
8.2.2 Detector Makeup or Auxiliary Gas 140
8.2.3 Detector Temperature 141
8.2.4 Detector Sensitivity 142
8.2.5 Detector Selectivity 143
8.2.6 Detector Linear Range 144
8.3 Flame Ionization Detector (FID) 145
8.3.1 FID Principle of Operation 145
8.3.2 FID Gases 146
8.3.3 Column Position in a FID 147
8.3.4 FID Temperature 147
8.3.5 FID Selectivity 147
8.3.6 FID Sensitivity and Linear Range 147
8.3.7 Verifying Flame Ignition of a FID 148
8.3.8 FID Maintenance 148
8.3.9 Common Problems with a FID 149
8.3.9.1 Change in FID Sensitivity 149
8.3.9.2 Difficulty in Lighting the FID Flame 149
8.3.9.3 Peak Shape Problems Attributed to the FID 150
8.3.9.4 Miscellaneous Problems with a FID 150
8.4 Nitrogen-Phosphorus Detector (NPD) 151
8.4.1 NPD Principle of Operation 151
8.4.2 NPD Gases 152
8.4.3 Column Position in a NPD 152
8.4.4 NPD Temperature 153
8.4.5 NPD Selectivity 153
XII Contents
8.4.6 NPD Sensitivity and Linear Range 153
8.4.7 NPD Maintenance 154
8.4.8 Common Problems with a NPD 155
8.4.8.1 Change in NPD Sensitivity 155
8.4.8.2 Peak Shape Problems Attributed to the NPD 155
8.4.8.3 NPD Baseline Problems 156
8.5 Electron Capture Detector (ECD) 157
8.5.1 ECD Principle of Operation 157
8.5.2 ECD Gases 158
8.5.3 Column Position in an ECD 158
8.5.4 ECD Temperature 159
8.5.5 ECD Selectivity 159
8.5.6 ECD Sensitivity and Linear Range 160
8.5.7 ECD Maintenance 160
8.5.8 Common Problems with an ECD 161
8.5.8.1 Change in ECD Sensitivity 161
8.5.8.2 Peak Shape Problems Attributed to the ECD 162
8.5.8.3 ECD Baseline Problems 162
8.5.8.4 Negative Peaks with an ECD 163
8.5.8.5 ECD Linear Range Problems 163
8.5.8.6 Miscellaneous Problems with an ECD 163
8.6 Thermal Conductivity Detector (TCD) 164
8.6.1 TCD Principle of Operation 164
8.6.2 TCD Gases 165
8.6.3 Column Position in a TCD 166
8.6.4 TCD Temperature 166
8.6.5 TCD Selectivity 166
8.6.6 TCD Sensitivity and Linear Range 166
8.6.7 TCD Maintenance 167
8.6.8 Common Problems with a TCD 168
8.6.8.1 Change in TCD Sensitivity 168
8.6.8.2 Peak Shape Problems Attributed to the TCD 169
8.6.8.3 TCD Baseline Problems 169
8.6.8.4 Negative Peaks with a TCD 170
8.6.8.5 Short TCD Filament Lifetimes 170
8.7 Flame Photometric Detector (FPD) 170
8.7.1 FPD Principle of Operation 170
8.7.2 FPD Gases 171
8.7.3 Column Position in a FPD 172
8.7.4 FPD Temperature 172
8.7.5 FPD Selectivity 172
8.7.6 FPD Sensitivity and Linear Range 172
8.7.7 Verifying Flame Ignition of a FPD 173
8.7.8 FPD Maintenance 173
8.7.9 Common Problems with a FPD 174
Contents XIII
8.7.9.1 Change in FPD Sensitivity 174
8.7.9.2 Peak Shape Problems Attributed to the FPD 174
8.7.9.3 Loss of FPD Linear Range 175
8.7.9.4 FPD Flame Frequently Goes Out 175
8.7.9.5 Miscellaneous Problems with a FPD 175
8.8 Mass Spectrometers (MS) 175
8.8.1 MS Principle of Operation 175
8.8.2 Mass Spectral Data 177
8.8.3 Other Ionization, Detection and Mass Filtering Modes 178
8.8.4 MS Selectivity 179
8.8.5 MS Sensitivity and Linear Range 179
8.8.6 MS Temperatures 180
8.8.7 Column Position in a MS 181
8.8.8 Carrier Gas Flow Rate Considerations for MS Detectors 181
8.8.9 MS Maintenance 182
8.8.10 Common Problems with a MS 183
8.8.10.1 Change in MS Sensitivity 183
8.8.10.2 Excessive Noise or High Background in a MS 184
8.8.10.3 Leaks in the MS 185
9 Column Installation 286
9.1 Importance of a Properly Installed Column 186
9.2 Installing Fused Silica Capillary Columns 186
9.2.1 Column Installation Steps 186
9.2.2 Cutting Fused Silica Capillary Columns 187
9.2.3 Column Placement in the GC Oven 187
9.2.4 Column Installation in the Injector 188
9.2.5 Turning On and Verifying the Carrier Gas Flow 189
9.2.6 Column Installation in the Detector 189
9.2.7 Verifying Proper Column Installation and Detector Operation 190
9.2.8 Column Conditioning 192
9.2.8.1 What is Column Conditioning? 192
9.2.8.2 Conditioning Temperatures 192
9.2.8.3 Conditioning the Column While Connected to the Detector 192
9.2.8.4 Conditioning the Column While Disconnected from the Detector 194
9.2.9 Setting the Carrier Gas Average Linear Velocity 195
9.2.10 Bleed Test 195
9.2.11 Injecting Column Test Sample 196
9.3 Column Ferrules 198
9.4 Tightening Fittings 199
9.5 Techniques for Measuring Column Insertion Distances 200
9.6 Leak Detection 201
10 Column Test Mixtures 202
10.1 Column Performance Testing 202
XIV Contents
10.2 Column Test Mixture Compounds 203
10.2.1 Hydrocarbons 203
10.2.2 Alcohols 203
10.2.3 Acids and Bases 204
10.2.4 FAMEs 204
10.2.5 Other Compounds 205
10.3 Column Testing Conditions 205
10.3.1 Injectors 205
10.3.2 Detectors 205
10.3.3 Column Temperature 206
10.3.4 Test Sample Concentration 206
10.4 Grob Test 207
10.5 Own Test Mixture 208
10.6 When to Test a Column 209
11 Causes and Prevention of Column Damage 220
11.1 Causes of Column Damage and Performance Degradation 210
11.2 Column Breakage 210
11.2.1 Causes of Column Breakage 210
11.2.2 Symptoms of Column Breakage 211
11.2.3 Prevention of Column Breakage 211
11.2.4 Recovery from Column Breakage 221
11.3 Thermal Damage 212
11.3.1 Causes of Thermal Damage 222
11.3.2 Symptoms of Thermal Damage 222
11.3.3 Prevention of Thermal Damage 213
11.3.4 Recovery from Thermal Damage 223
11.4 Oxygen Damage 213
11.4.1 Causes of Oxygen Damage 213
11.4.2 Symptoms of Oxygen Damage 224
11.4.3 Prevention of Oxygen Damage 214
11.4.4 Recovery from Oxygen Damage 224
11.5 Chemical Damage 214
11.5.1 Causes of Chemical Damage 224
11.5.1.1 Bases 225
11.5.1.2 Acids 225
11.5.1.3 HClandNH4OH 226
11.5.1.4 Organic Solvents and Water 226
11.5.2 Symptoms of Chemical Damage 227
11.5.3 Prevention of Chemical Damage 217
11.5.4 Recovery from Chemical Damage 218
11.6 Column Contamination 228
11.6.1 Causes of Column Contamination 228
11.6.2 Symptoms of Column Contamination 220
11.6.3 Prevention of Column Contamination 222
Contents XV
11.6.4 Recovery from Contamination 221
11.7 Solvent Rinsing Columns 222
11.7.1 Solvent Rinse Kits 222
11.7.2 Solvent Selection, Volumes and Flow Rates 224
11.7.3 Conditioning the Column After Solvent Rinsing 225
11.7.4 Some Solvent Rinsing Considerations 226
11.8 Guard Columns and Retention Gaps 226
11.8.1 Deactivated Fused Silica Tubing 226
11.8.2 Guard Columns 227
11.8.3 Retention Gaps 227
11.8.4 Unions 228
11.9 Packed Injector Liners 230
11.10 Gas Impurity Traps 230
11.11 Column Storage 232
11.12 Column Repair 232
12 Troubleshooting Guidelines, Approaches and Tests 233
12.1 Introduction 233
12.2 Approaches to Solving GC Problems 234
12.2.1 Systematic Approach 234
12.2.2 Checking the Obvious 234
12.2.3 Looking for Changes 235
12.2.4 Looking for Trends, Patterns and Common Characteristics 235
12.2.5 Asking If ...Then ... Questions 236
12.2.6 One Thing at a Time 236
12.2.7 Moving from the General to the Specific 236
12.2.8 Eliminating the Possibilities 237
12.2.9 Divide and Conquer 237
12.3 Troubleshooting Tools 238
12.4 Troubleshooting Tests 239
12.4.1 Jumper Tube Test 239
12.4.2 Condensation Test 240
12.4.3 Check Out Column 240
12.4.4 Column Exchange 241
12.4.5 Static Pressure Check 241
12.4.6 Column Test Samples 242
13 Common Capillary CC Problems and Probable Causes 243
13.1 Using This Troubleshooting Guide 243
13.2 Troubleshooting Checklist and Pre-Work 243
13.3 Baseline Problems 245
13.3.1 Baseline Drift or Wander 245
13.3.2 Noisy Baseline 246
13.3.3 Spikes in the Baseline 246
13.4 Peak Shape Problems 247
XVI Contents
13.4.1 Tailing Peaks 247
13.4.2 Fronting Peaks 249
13.4.3 Extremely Broad or Rounded Peaks 250
13.4.4 Flat Top Peaks 250
13.5 Split Peaks 251
13.6 Negative Peaks 252
13.7 Excessively Broad Solvent Front 253
13.8 Loss of Resolution 254
13.9 Retention Changes 254
13.9.1 Retention Time (tr) Change Only 254
13.9.2 Retention Factor (fe) Change 255
13.10 Peak Size Problems 256
13.10.1 No Peaks 256
13.10.2 All Peaks Change in Size 256
13.10.3 Some Peaks Change in Size or Missing Peaks 257
13.11 Extra or Ghost Peaks (Carryover) 258
13.12 Rapid Column Deterioration 259
13.13 Quantitation Problems 260
Appendix A Terms 261
Appendix B Equations 263
Appendix C Mass, Volume and Length Unit Conversions 266
Appendix D Column Bleed Mass Spectra 267
Appendix E The Basics of High Speed GC Using Small Diameter Columns 273
E.I Introduction 273
E.2 Column Considerations 273
E.3 Carrier Gas Considerations 274
E.4 Injector Considerations 275
E.5 Detector and Data System Considerations 276
E.6 GC Oven Considerations 276
E.7 Sample Considerations 277
E.8 An Example of High Speed GC Using a Small Diameter Column 277
E.9 High Speed GC Summary 279
Appendix F Basic Quantitative Capillary CC 280
F.I Intentions 280
F.2 Definitions 280
F.3 Concentration 282
F.3.1 Weight-to-Weight (w/w) and Weight-to-Volume (w/v) 282
F.3.2 Parts per Million (ppm) and Parts per Billion (ppb) 283
F.3.3 Percent (%) 284
Contents XVII
F.3.4 Molarity (M or mM) 284
F.4 Density (p) 285
F.5 Calibration for Quantitative Purposes 286
F.5.1 Single and Multiple Point Calibration 286
F.5.2 Calibration Curves 287
F.6 Quantitation Calculations 289
F.6.1 External Standard 289
F.6.2 Internal Standard 291
F.6.3 Modified Standard Addition 295
F.6.4 Relative Percent 296
F.7 Techniques for Preparation of Analytical Standards for GC 297
F.7.1 Standard Composition Considerations 297
F.7.2 Preparing One Component Standards 299
F.7.2.1 Using a Volumetric Flask 299
F.7.2.2 Using Vials and an Exact Measurement Technique 302
F.7.3 Preparing Multi-Component Standards 304
F.7.3.1 Equal Volume Method 304
F.7.3.2 Equal Concentration Method 306
F.7.3.3 Unequal Volume and Unequal Concentration Method 309
F.7.4 Serial Dilution 311
References 317
Subject Index 319
|
| adam_txt |
VII
Contents
Preface V
Intentions and Introduction 1
1 Introduction to Capillary Gas Chromatograph/ 3
1.1 What Is Gas Chromatography? 3
1.2 What Types of Compounds Are Suitable for GC Analysis? 3
1.3 The Basic Parts of a Gas Chromatograph 4
1.3.1 Gas Supply and Flow Controllers 4
1.3.2 Injector 5
1.3.3 Capillary Column and Oven 5
1.3.4 Detector 6
1.3.5 Data System 6
1.4 The Chromatogram 6
1.5 The Mechanism of Compound Separation 8
1.5.1 A Simple Description of the Chromatographie Process 8
1.5.2 A Detailed Description of the Chromatographie Process 9
1.6 Factors Affecting Separation 11
1.6.1 Stationary Phase 11
1.6.2 Compound Structure 12
1.6.3 Column Temperature 12
2 Basic Definitions and Equations 14
2.1 Why Bother? 14
2.2 Peak Shapes 14
2.2.1 Peak Width (W) 14
2.2.2 Peak Symmetry 14
2.3 Retention 16
2.3.1 Retention Time (tr) 16
2.3.2 Adjusted Retention Time ($ 16
2.3.3 Retention Factor (fc) 16
2.3.4 Retention Index (/) 18
2.4 Phase Ratio (ß) 19
2.5 Distribution Constant (Kc) 20
The Troubleshooting and Maintenance Guide for Gas Chromatographers, Fourth Edition. Dean Rood
Copyright © 2007 WILEY-VCH Verlag GmbH Co. KGaA, Weinheim
ISBN: 978-3-527-31373-0
VIII Contents
2.5.1 Kc and Column Dimensions 21
2.5.2 Kc and Column Temperature 21
2.6 Column Efficiency 21
2.6.1 Number of Theoretical Plates (N) 22
2.6.2 Height Equivalent to a Theoretical Plate (H) 22
2.6.3 Effective Theoretical Plates (Neff) and Effective Plate Heights (Heff) 23
2.6 A Precautions When Using Theoretical Plates 23
2.7 Utilization of Theoretical Efficiency (UTE%) 24
2.8 Separation Factor (a) 25
2.9 Resolution (R) 25
2.10 Trennzahl (TZ) 27
2.11 Column Capacity 28
3 Capillary CC Columns: Tubing 30
3.1 Fused Silica Capillary Columns 30
3.2 Fused Silica Tubing 30
3.3 Outer Coating 32
3.4 Other Tubing Materials 32
3.5 Polyimide Fused Silica Tubing Bending Stress 33
4 Capillary GC Columns: Stationary Phases 34
4.1 Stationary Phases 34
4.2 Types of Stationary Phases 35
4.2.1 Polysiloxanes or Silicones 35
4.2.2 Arylene-Modified Polysiloxanes 37
4.2.3 Polyethylene Glycols 37
4.2.4 Porous Layer Stationary Phases 38
4.3 Characteristics of Stationary Phases 39
4.3.1 Bonded and Cross-linked Stationary Phases 39
4.3.2 Stationary Phase Polarity 39
4.3.3 Stationary Phase Selectivity 40
4.4 Stationary Phase Interactions 41
4.4.1 Dispersion Interaction 41
4.4.2 Dipole Interaction 42
4.4.3 Hydrogen Bonding Interaction 43
4.4.4 When There are Multiple Interactions 44
4.5 Stationary Phase Equivalencies 45
4.6 Column Temperature Limits 46
4.7 Column Bleed 47
4.7.1 What is Column Bleed? 47
4.7.2 Measuring Column Bleed 48
4.7.3 Sensitivity Considerations 49
4.7 A Detector Considerations 49
4.7.5 Minimizing Column Bleed 50
4.8 Selecting Stationary Phases 50
Contents IX
5 Capillary CC Columns: Dimensions 53
5.1 Introduction 53
5.2 Column Length 53
5.2.1 Column Length and Efficiency/Resolution 53
5.2.2 Column Length and Retention 57
5.2.3 Column Length and Pressure 57
5.2.4 Column Length and Bleed 58
5.2.5 Column Length and Cost 58
5.2.6 Selecting Column Length 58
5.3 Column Diameter 59
5.3.1 Column Diameter and Efficiency/Resolution 59
5.3.2 Column Diameter and Retention 62
5.3.3 Column Diameter and Pressure 62
5.3.4 Column Diameter and Bleed 63
5.3.5 Column Diameter and Capacity 63
5.3.6 Column Diameter and Carrier Gas Volume 64
5.3.7 Column Diameter and Injector Efficiency 64
5.3.8 Column Diameter and Breakage 65
5.3.9 Column Diameter and Cost 65
5.3.10 Selecting Column Diameter 65
5.4 Column Film Thickness 66
5.4.1 Column Film Thickness and Retention 66
5.4.2 Column Film Thickness and Efficiency/Resolution 69
5.4.3 Column Film Thickness and Capacity 70
5.4.4 Column Film Thickness and Bleed 71
5.4.5 Column Film Thickness and Inertness 71
5.4.6 Selecting Column Film Thickness 72
5.5 Manipulating Multiple Column Dimensions 72
6 Carrier Gas 74
6.1 Carrier Gas and Capillary Columns 74
6.2 Linear Velocity versus Flow Rate 74
6.3 Controlling the Linear Velocity and Flow Rate 74
6.4 Van Deemter Curves 75
6.5 Carrier Gas Measurements 76
6.5.1 Average Linear Velocity (m) 76
6.5.2 Column Flow Rate 79
6.6 Carrier Gas Selection 80
6.6.1 Nitrogen 80
6.6.2 Helium 80
6.6.3 Hydrogen 82
6.7 Recommended Average Linear Velocities 83
6.8 Gas Purities 86
6.9 Common Carrier Gas Problems 87
XI Contents
7 Injectors 89
7.1 Introduction 89
7.2 The Basics of Vaporization Injectors 89
7.2.1 Injector Temperature 91
7.2.2 Speed of Sample Transfer 91
7.2.3 Injector Backflash 91
7.2.4 Injector Discrimination 94
7.3 Split Injectors 95
7.3.1 Description of a Split Injector 95
7.3.2 Split Ratio 96
7.3.3 Septum Purge for Split Injectors 99
7.3.4 Split Injector Liners 99
7.3.5 Column Position in Split Injectors 101
7.3.6 Common Problems with Split Injectors 102
7.4 Splitless Injectors 102
7'.4.1 Description of a Splitless Injector 102
7.4.2 Selecting Purge Activation Times 105
7.43 Solvent Effect for Splitless Injectors 106
7.4.4 Cold Trapping for Splitless Injectors 108
7.4.5 Septum Purge for Splitless Injectors 108
7.4.6 Splitless Injection Liners 109
7.4.7 Column Position in Splitless Injectors 109
7.4.8 Other Aspects of Splitless Injectors 110
7.4.9 Common Problems with Splitless Injectors 111
7.5 Direct Injectors 112
7.5.1 Description of a Direct Injector 112
7.5.2 Direct Injection Liners 113
7.5.3 Septum Purge for Direct Injectors 115
7.5.4 Column Position in Direct Injectors 115
7.5.5 Other Aspects of Direct Injectors 115
7.5.6 Common Problems with Direct Injectors 116
7.6 Cool On-Column Injectors 117
7.6.1 Description of an On-Column Injector 117
7.6.2 Solvent Effect and Cold Trapping for Cool On-Column Injectors 118
7.6.3 Secondary Cooling 119
7.6.4 Retention Gaps and Cool On-Column Injectors 119
7.6.5 Other Aspects of Cool On-Column Injectors 120
7.6.6 Common Problems With On-Column Injectors 120
7.7 Pressure and Flow Programmable Injectors 121
7.7.1 Description of Programmable Injectors 121
7.7.2 Constant Pressure Mode 122
7.7.3 Constant Flow or Velocity Mode 122
7.7'.4 Pressure Program Mode 123
7.7.5 Pulsed Pressure Mode 124
7.7.6 Gas Saver Mode 125
Contents XI
7.7.7 Other Aspects of Programmable Injectors 125
7.8 Injection Techniques 126
7.8.1 Syringe Filling Techniques 126
7.8.2 Injection Speed 128
7.9 Autosamplers 129
7.10 Injector Septa 131
7.10.1 Introduction 131
7.10.2 Septa Hardness 131
7.10.3 Septa Bleed 131
7.10.4 Handling Septa 133
7.11 Injector Maintenance 134
7.11.1 Cleaning Injectors 134
7.11.2 Injector Traps 135
7.11.3 Cleaning Injector Liners 135
7.11.4 Silylaring Injector Liners 136
8 Detectors 139
8.1 Introduction 139
8.2 Detector Characteristics 139
8.2.1 Detector Dead Volume 139
8.2.2 Detector Makeup or Auxiliary Gas 140
8.2.3 Detector Temperature 141
8.2.4 Detector Sensitivity 142
8.2.5 Detector Selectivity 143
8.2.6 Detector Linear Range 144
8.3 Flame Ionization Detector (FID) 145
8.3.1 FID Principle of Operation 145
8.3.2 FID Gases 146
8.3.3 Column Position in a FID 147
8.3.4 FID Temperature 147
8.3.5 FID Selectivity 147
8.3.6 FID Sensitivity and Linear Range 147
8.3.7 Verifying Flame Ignition of a FID 148
8.3.8 FID Maintenance 148
8.3.9 Common Problems with a FID 149
8.3.9.1 Change in FID Sensitivity 149
8.3.9.2 Difficulty in Lighting the FID Flame 149
8.3.9.3 Peak Shape Problems Attributed to the FID 150
8.3.9.4 Miscellaneous Problems with a FID 150
8.4 Nitrogen-Phosphorus Detector (NPD) 151
8.4.1 NPD Principle of Operation 151
8.4.2 NPD Gases 152
8.4.3 Column Position in a NPD 152
8.4.4 NPD Temperature 153
8.4.5 NPD Selectivity 153
XII Contents
8.4.6 NPD Sensitivity and Linear Range 153
8.4.7 NPD Maintenance 154
8.4.8 Common Problems with a NPD 155
8.4.8.1 Change in NPD Sensitivity 155
8.4.8.2 Peak Shape Problems Attributed to the NPD 155
8.4.8.3 NPD Baseline Problems 156
8.5 Electron Capture Detector (ECD) 157
8.5.1 ECD Principle of Operation 157
8.5.2 ECD Gases 158
8.5.3 Column Position in an ECD 158
8.5.4 ECD Temperature 159
8.5.5 ECD Selectivity 159
8.5.6 ECD Sensitivity and Linear Range 160
8.5.7 ECD Maintenance 160
8.5.8 Common Problems with an ECD 161
8.5.8.1 Change in ECD Sensitivity 161
8.5.8.2 Peak Shape Problems Attributed to the ECD 162
8.5.8.3 ECD Baseline Problems 162
8.5.8.4 Negative Peaks with an ECD 163
8.5.8.5 ECD Linear Range Problems 163
8.5.8.6 Miscellaneous Problems with an ECD 163
8.6 Thermal Conductivity Detector (TCD) 164
8.6.1 TCD Principle of Operation 164
8.6.2 TCD Gases 165
8.6.3 Column Position in a TCD 166
8.6.4 TCD Temperature 166
8.6.5 TCD Selectivity 166
8.6.6 TCD Sensitivity and Linear Range 166
8.6.7 TCD Maintenance 167
8.6.8 Common Problems with a TCD 168
8.6.8.1 Change in TCD Sensitivity 168
8.6.8.2 Peak Shape Problems Attributed to the TCD 169
8.6.8.3 TCD Baseline Problems 169
8.6.8.4 Negative Peaks with a TCD 170
8.6.8.5 Short TCD Filament Lifetimes 170
8.7 Flame Photometric Detector (FPD) 170
8.7.1 FPD Principle of Operation 170
8.7.2 FPD Gases 171
8.7.3 Column Position in a FPD 172
8.7.4 FPD Temperature 172
8.7.5 FPD Selectivity 172
8.7.6 FPD Sensitivity and Linear Range 172
8.7.7 Verifying Flame Ignition of a FPD 173
8.7.8 FPD Maintenance 173
8.7.9 Common Problems with a FPD 174
Contents XIII
8.7.9.1 Change in FPD Sensitivity 174
8.7.9.2 Peak Shape Problems Attributed to the FPD 174
8.7.9.3 Loss of FPD Linear Range 175
8.7.9.4 FPD Flame Frequently Goes Out 175
8.7.9.5 Miscellaneous Problems with a FPD 175
8.8 Mass Spectrometers (MS) 175
8.8.1 MS Principle of Operation 175
8.8.2 Mass Spectral Data 177
8.8.3 Other Ionization, Detection and Mass Filtering Modes 178
8.8.4 MS Selectivity 179
8.8.5 MS Sensitivity and Linear Range 179
8.8.6 MS Temperatures 180
8.8.7 Column Position in a MS 181
8.8.8 Carrier Gas Flow Rate Considerations for MS Detectors 181
8.8.9 MS Maintenance 182
8.8.10 Common Problems with a MS 183
8.8.10.1 Change in MS Sensitivity 183
8.8.10.2 Excessive Noise or High Background in a MS 184
8.8.10.3 Leaks in the MS 185
9 Column Installation 286
9.1 Importance of a Properly Installed Column 186
9.2 Installing Fused Silica Capillary Columns 186
9.2.1 Column Installation Steps 186
9.2.2 Cutting Fused Silica Capillary Columns 187
9.2.3 Column Placement in the GC Oven 187
9.2.4 Column Installation in the Injector 188
9.2.5 Turning On and Verifying the Carrier Gas Flow 189
9.2.6 Column Installation in the Detector 189
9.2.7 Verifying Proper Column Installation and Detector Operation 190
9.2.8 Column Conditioning 192
9.2.8.1 What is Column Conditioning? 192
9.2.8.2 Conditioning Temperatures 192
9.2.8.3 Conditioning the Column While Connected to the Detector 192
9.2.8.4 Conditioning the Column While Disconnected from the Detector 194
9.2.9 Setting the Carrier Gas Average Linear Velocity 195
9.2.10 Bleed Test 195
9.2.11 Injecting Column Test Sample 196
9.3 Column Ferrules 198
9.4 Tightening Fittings 199
9.5 Techniques for Measuring Column Insertion Distances 200
9.6 Leak Detection 201
10 Column Test Mixtures 202
10.1 Column Performance Testing 202
XIV Contents
10.2 Column Test Mixture Compounds 203
10.2.1 Hydrocarbons 203
10.2.2 Alcohols 203
10.2.3 Acids and Bases 204
10.2.4 FAMEs 204
10.2.5 Other Compounds 205
10.3 Column Testing Conditions 205
10.3.1 Injectors 205
10.3.2 Detectors 205
10.3.3 Column Temperature 206
10.3.4 Test Sample Concentration 206
10.4 Grob Test 207
10.5 Own Test Mixture 208
10.6 When to Test a Column 209
11 Causes and Prevention of Column Damage 220
11.1 Causes of Column Damage and Performance Degradation 210
11.2 Column Breakage 210
11.2.1 Causes of Column Breakage 210
11.2.2 Symptoms of Column Breakage 211
11.2.3 Prevention of Column Breakage 211
11.2.4 Recovery from Column Breakage 221
11.3 Thermal Damage 212
11.3.1 Causes of Thermal Damage 222
11.3.2 Symptoms of Thermal Damage 222
11.3.3 Prevention of Thermal Damage 213
11.3.4 Recovery from Thermal Damage 223
11.4 Oxygen Damage 213
11.4.1 Causes of Oxygen Damage 213
11.4.2 Symptoms of Oxygen Damage 224
11.4.3 Prevention of Oxygen Damage 214
11.4.4 Recovery from Oxygen Damage 224
11.5 Chemical Damage 214
11.5.1 Causes of Chemical Damage 224
11.5.1.1 Bases 225
11.5.1.2 Acids 225
11.5.1.3 HClandNH4OH 226
11.5.1.4 Organic Solvents and Water 226
11.5.2 Symptoms of Chemical Damage 227
11.5.3 Prevention of Chemical Damage 217
11.5.4 Recovery from Chemical Damage 218
11.6 Column Contamination 228
11.6.1 Causes of Column Contamination 228
11.6.2 Symptoms of Column Contamination 220
11.6.3 Prevention of Column Contamination 222
Contents XV
11.6.4 Recovery from Contamination 221
11.7 Solvent Rinsing Columns 222
11.7.1 Solvent Rinse Kits 222
11.7.2 Solvent Selection, Volumes and Flow Rates 224
11.7.3 Conditioning the Column After Solvent Rinsing 225
11.7.4 Some Solvent Rinsing Considerations 226
11.8 Guard Columns and Retention Gaps 226
11.8.1 Deactivated Fused Silica Tubing 226
11.8.2 Guard Columns 227
11.8.3 Retention Gaps 227
11.8.4 Unions 228
11.9 Packed Injector Liners 230
11.10 Gas Impurity Traps 230
11.11 Column Storage 232
11.12 Column Repair 232
12 Troubleshooting Guidelines, Approaches and Tests 233
12.1 Introduction 233
12.2 Approaches to Solving GC Problems 234
12.2.1 Systematic Approach 234
12.2.2 Checking the Obvious 234
12.2.3 Looking for Changes 235
12.2.4 Looking for Trends, Patterns and Common Characteristics 235
12.2.5 Asking "If .Then ." Questions 236
12.2.6 One Thing at a Time 236
12.2.7 Moving from the General to the Specific 236
12.2.8 Eliminating the Possibilities 237
12.2.9 Divide and Conquer 237
12.3 Troubleshooting Tools 238
12.4 Troubleshooting Tests 239
12.4.1 Jumper Tube Test 239
12.4.2 Condensation Test 240
12.4.3 Check Out Column 240
12.4.4 Column Exchange 241
12.4.5 Static Pressure Check 241
12.4.6 Column Test Samples 242
13 Common Capillary CC Problems and Probable Causes 243
13.1 Using This Troubleshooting Guide 243
13.2 Troubleshooting Checklist and Pre-Work 243
13.3 Baseline Problems 245
13.3.1 Baseline Drift or Wander 245
13.3.2 Noisy Baseline 246
13.3.3 Spikes in the Baseline 246
13.4 Peak Shape Problems 247
XVI Contents
13.4.1 Tailing Peaks 247
13.4.2 Fronting Peaks 249
13.4.3 Extremely Broad or Rounded Peaks 250
13.4.4 Flat Top Peaks 250
13.5 Split Peaks 251
13.6 Negative Peaks 252
13.7 Excessively Broad Solvent Front 253
13.8 Loss of Resolution 254
13.9 Retention Changes 254
13.9.1 Retention Time (tr) Change Only 254
13.9.2 Retention Factor (fe) Change 255
13.10 Peak Size Problems 256
13.10.1 No Peaks 256
13.10.2 All Peaks Change in Size 256
13.10.3 Some Peaks Change in Size or Missing Peaks 257
13.11 Extra or Ghost Peaks (Carryover) 258
13.12 Rapid Column Deterioration 259
13.13 Quantitation Problems 260
Appendix A Terms 261
Appendix B Equations 263
Appendix C Mass, Volume and Length Unit Conversions 266
Appendix D Column Bleed Mass Spectra 267
Appendix E The Basics of High Speed GC Using Small Diameter Columns 273
E.I Introduction 273
E.2 Column Considerations 273
E.3 Carrier Gas Considerations 274
E.4 Injector Considerations 275
E.5 Detector and Data System Considerations 276
E.6 GC Oven Considerations 276
E.7 Sample Considerations 277
E.8 An Example of High Speed GC Using a Small Diameter Column 277
E.9 High Speed GC Summary 279
Appendix F Basic Quantitative Capillary CC 280
F.I Intentions 280
F.2 Definitions 280
F.3 Concentration 282
F.3.1 Weight-to-Weight (w/w) and Weight-to-Volume (w/v) 282
F.3.2 Parts per Million (ppm) and Parts per Billion (ppb) 283
F.3.3 Percent (%) 284
Contents XVII
F.3.4 Molarity (M or mM) 284
F.4 Density (p) 285
F.5 Calibration for Quantitative Purposes 286
F.5.1 Single and Multiple Point Calibration 286
F.5.2 Calibration Curves 287
F.6 Quantitation Calculations 289
F.6.1 External Standard 289
F.6.2 Internal Standard 291
F.6.3 Modified Standard Addition 295
F.6.4 Relative Percent 296
F.7 Techniques for Preparation of Analytical Standards for GC 297
F.7.1 Standard Composition Considerations 297
F.7.2 Preparing One Component Standards 299
F.7.2.1 Using a Volumetric Flask 299
F.7.2.2 Using Vials and an Exact Measurement Technique 302
F.7.3 Preparing Multi-Component Standards 304
F.7.3.1 Equal Volume Method 304
F.7.3.2 Equal Concentration Method 306
F.7.3.3 Unequal Volume and Unequal Concentration Method 309
F.7.4 Serial Dilution 311
References 317
Subject Index 319 |
| any_adam_object | 1 |
| any_adam_object_boolean | 1 |
| author | Rood, Dean |
| author_facet | Rood, Dean |
| author_role | aut |
| author_sort | Rood, Dean |
| author_variant | d r dr |
| building | Verbundindex |
| bvnumber | BV021295510 |
| callnumber-first | Q - Science |
| callnumber-label | QD79 |
| callnumber-raw | QD79.C45 |
| callnumber-search | QD79.C45 |
| callnumber-sort | QD 279 C45 |
| callnumber-subject | QD - Chemistry |
| classification_rvk | VG 7400 |
| classification_tum | CHE 234f |
| ctrlnum | (OCoLC)153538333 (DE-599)BVBBV021295510 |
| dewey-full | 543.85 |
| dewey-hundreds | 500 - Natural sciences and mathematics |
| dewey-ones | 543 - Analytical chemistry |
| dewey-raw | 543.85 |
| dewey-search | 543.85 |
| dewey-sort | 3543.85 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie Chemie |
| discipline_str_mv | Chemie / Pharmazie Chemie |
| edition | 4., rev. and updated ed. |
| format | Book |
| fullrecord | <?xml version="1.0" encoding="UTF-8"?><collection xmlns="http://www.loc.gov/MARC21/slim"><record><leader>02127nam a2200493 c 4500</leader><controlfield tag="001">BV021295510</controlfield><controlfield tag="003">DE-604</controlfield><controlfield tag="005">20131021 </controlfield><controlfield tag="007">t</controlfield><controlfield tag="008">060117s2007 gw ad|| |||| 00||| eng d</controlfield><datafield tag="020" ind1=" " ind2=" "><subfield code="a">9783527313730</subfield><subfield code="9">978-3-527-31373-0</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(OCoLC)153538333</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(DE-599)BVBBV021295510</subfield></datafield><datafield tag="040" ind1=" " ind2=" "><subfield code="a">DE-604</subfield><subfield code="b">ger</subfield><subfield code="e">rakddb</subfield></datafield><datafield tag="041" ind1="0" ind2=" "><subfield code="a">eng</subfield></datafield><datafield tag="044" ind1=" " ind2=" "><subfield code="a">gw</subfield><subfield code="c">DE</subfield></datafield><datafield tag="049" ind1=" " ind2=" "><subfield code="a">DE-91G</subfield><subfield code="a">DE-703</subfield><subfield code="a">DE-19</subfield><subfield code="a">DE-634</subfield><subfield code="a">DE-20</subfield><subfield code="a">DE-11</subfield><subfield code="a">DE-858</subfield></datafield><datafield tag="050" ind1=" " ind2="0"><subfield code="a">QD79.C45</subfield></datafield><datafield tag="082" ind1="0" ind2=" "><subfield code="a">543.85</subfield><subfield code="2">22</subfield></datafield><datafield tag="084" ind1=" " ind2=" "><subfield code="a">VG 7400</subfield><subfield code="0">(DE-625)147205:253</subfield><subfield code="2">rvk</subfield></datafield><datafield tag="084" ind1=" " ind2=" "><subfield code="a">CHE 234f</subfield><subfield code="2">stub</subfield></datafield><datafield tag="100" ind1="1" ind2=" "><subfield code="a">Rood, Dean</subfield><subfield code="e">Verfasser</subfield><subfield code="4">aut</subfield></datafield><datafield tag="245" ind1="1" ind2="0"><subfield code="a">The troubleshooting and maintenance guide for gas chromatographers</subfield><subfield code="c">Dean Rood</subfield></datafield><datafield tag="250" ind1=" " ind2=" "><subfield code="a">4., rev. and updated ed.</subfield></datafield><datafield tag="264" ind1=" " ind2="1"><subfield code="a">Weinheim [u.a.]</subfield><subfield code="b">Wiley-VCH</subfield><subfield code="c">2007</subfield></datafield><datafield tag="300" ind1=" " ind2=" "><subfield code="a">XVII, 326 S.</subfield><subfield code="b">Ill., graph. Darst.</subfield></datafield><datafield tag="336" ind1=" " ind2=" "><subfield code="b">txt</subfield><subfield code="2">rdacontent</subfield></datafield><datafield tag="337" ind1=" " ind2=" "><subfield code="b">n</subfield><subfield code="2">rdamedia</subfield></datafield><datafield tag="338" ind1=" " ind2=" "><subfield code="b">nc</subfield><subfield code="2">rdacarrier</subfield></datafield><datafield tag="650" ind1=" " ind2="4"><subfield code="a">Gas chromatography</subfield></datafield><datafield tag="650" ind1=" " ind2="4"><subfield code="a">Gas chromatography</subfield><subfield code="x">Instruments</subfield><subfield code="x">Maintenance and repair</subfield></datafield><datafield tag="650" ind1="0" ind2="7"><subfield code="a">Fehlersuche</subfield><subfield code="0">(DE-588)4016615-6</subfield><subfield code="2">gnd</subfield><subfield code="9">rswk-swf</subfield></datafield><datafield tag="650" ind1="0" ind2="7"><subfield code="a">Glaskapillargaschromatographie</subfield><subfield code="0">(DE-588)4157443-6</subfield><subfield code="2">gnd</subfield><subfield code="9">rswk-swf</subfield></datafield><datafield tag="650" ind1="0" ind2="7"><subfield code="a">Kapillargaschromatographie</subfield><subfield code="0">(DE-588)4252082-4</subfield><subfield code="2">gnd</subfield><subfield code="9">rswk-swf</subfield></datafield><datafield tag="689" ind1="0" ind2="0"><subfield code="a">Kapillargaschromatographie</subfield><subfield code="0">(DE-588)4252082-4</subfield><subfield code="D">s</subfield></datafield><datafield tag="689" ind1="0" ind2="1"><subfield code="a">Fehlersuche</subfield><subfield code="0">(DE-588)4016615-6</subfield><subfield code="D">s</subfield></datafield><datafield tag="689" ind1="0" ind2=" "><subfield code="8">1\p</subfield><subfield code="5">DE-604</subfield></datafield><datafield tag="689" ind1="1" ind2="0"><subfield code="a">Glaskapillargaschromatographie</subfield><subfield code="0">(DE-588)4157443-6</subfield><subfield code="D">s</subfield></datafield><datafield tag="689" ind1="1" ind2=" "><subfield code="8">2\p</subfield><subfield code="5">DE-604</subfield></datafield><datafield tag="780" ind1="0" ind2="0"><subfield code="i">Bis 3. Auflage</subfield><subfield code="a">Rood, Dean</subfield><subfield code="t">A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems</subfield></datafield><datafield tag="856" ind1="4" ind2="2"><subfield code="m">HBZ Datenaustausch</subfield><subfield code="q">application/pdf</subfield><subfield code="u">http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014616279&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA</subfield><subfield code="3">Inhaltsverzeichnis</subfield></datafield><datafield tag="999" ind1=" " ind2=" "><subfield code="a">oai:aleph.bib-bvb.de:BVB01-014616279</subfield></datafield><datafield tag="883" ind1="1" ind2=" "><subfield code="8">1\p</subfield><subfield code="a">cgwrk</subfield><subfield code="d">20201028</subfield><subfield code="q">DE-101</subfield><subfield code="u">https://d-nb.info/provenance/plan#cgwrk</subfield></datafield><datafield tag="883" ind1="1" ind2=" "><subfield code="8">2\p</subfield><subfield code="a">cgwrk</subfield><subfield code="d">20201028</subfield><subfield code="q">DE-101</subfield><subfield code="u">https://d-nb.info/provenance/plan#cgwrk</subfield></datafield></record></collection> |
| id | DE-604.BV021295510 |
| illustrated | Illustrated |
| index_date | 2024-07-02T13:51:04Z |
| indexdate | 2024-07-09T20:34:58Z |
| institution | BVB |
| isbn | 9783527313730 |
| language | English |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-014616279 |
| oclc_num | 153538333 |
| open_access_boolean | |
| owner | DE-91G DE-BY-TUM DE-703 DE-19 DE-BY-UBM DE-634 DE-20 DE-11 DE-858 |
| owner_facet | DE-91G DE-BY-TUM DE-703 DE-19 DE-BY-UBM DE-634 DE-20 DE-11 DE-858 |
| physical | XVII, 326 S. Ill., graph. Darst. |
| publishDate | 2007 |
| publishDateSearch | 2007 |
| publishDateSort | 2007 |
| publisher | Wiley-VCH |
| record_format | marc |
| spelling | Rood, Dean Verfasser aut The troubleshooting and maintenance guide for gas chromatographers Dean Rood 4., rev. and updated ed. Weinheim [u.a.] Wiley-VCH 2007 XVII, 326 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Gas chromatography Gas chromatography Instruments Maintenance and repair Fehlersuche (DE-588)4016615-6 gnd rswk-swf Glaskapillargaschromatographie (DE-588)4157443-6 gnd rswk-swf Kapillargaschromatographie (DE-588)4252082-4 gnd rswk-swf Kapillargaschromatographie (DE-588)4252082-4 s Fehlersuche (DE-588)4016615-6 s 1\p DE-604 Glaskapillargaschromatographie (DE-588)4157443-6 s 2\p DE-604 Bis 3. Auflage Rood, Dean A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems HBZ Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014616279&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk 2\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Rood, Dean The troubleshooting and maintenance guide for gas chromatographers Gas chromatography Gas chromatography Instruments Maintenance and repair Fehlersuche (DE-588)4016615-6 gnd Glaskapillargaschromatographie (DE-588)4157443-6 gnd Kapillargaschromatographie (DE-588)4252082-4 gnd |
| subject_GND | (DE-588)4016615-6 (DE-588)4157443-6 (DE-588)4252082-4 |
| title | The troubleshooting and maintenance guide for gas chromatographers |
| title_auth | The troubleshooting and maintenance guide for gas chromatographers |
| title_exact_search | The troubleshooting and maintenance guide for gas chromatographers |
| title_exact_search_txtP | The troubleshooting and maintenance guide for gas chromatographers |
| title_full | The troubleshooting and maintenance guide for gas chromatographers Dean Rood |
| title_fullStr | The troubleshooting and maintenance guide for gas chromatographers Dean Rood |
| title_full_unstemmed | The troubleshooting and maintenance guide for gas chromatographers Dean Rood |
| title_old | Rood, Dean A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
| title_short | The troubleshooting and maintenance guide for gas chromatographers |
| title_sort | the troubleshooting and maintenance guide for gas chromatographers |
| topic | Gas chromatography Gas chromatography Instruments Maintenance and repair Fehlersuche (DE-588)4016615-6 gnd Glaskapillargaschromatographie (DE-588)4157443-6 gnd Kapillargaschromatographie (DE-588)4252082-4 gnd |
| topic_facet | Gas chromatography Gas chromatography Instruments Maintenance and repair Fehlersuche Glaskapillargaschromatographie Kapillargaschromatographie |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=014616279&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT rooddean thetroubleshootingandmaintenanceguideforgaschromatographers |