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Tables of Contents for A Practical Guide to the Care, Maintenance, and Troubleshooting of Capillary Gas Chromatographic Systems
Chapter/Section Title
Page #
Page Count
Intentions and Introduction
1
2
Introduction to Capillary Gas Chromatography
A Brief and Simple Introduction to Gas Chromatography
3
5
What is Gas Chromatography?
3
1
What Types of Compounds are Suitable for GC Analysis?
3
1
The Basic Parts of a Gas Chromatograph
4
1
Gas Supply and Flow Controllers
5
1
Injector
5
1
Capillary Column and Oven
6
1
Detector
6
1
Recording Device
6
1
The Chromatogram
7
1
Limitations and Cautions
8
1
The Mechanism of Compound Separation
9
4
A Very Simple Description of the Chromatographic Process
10
1
A Detailed Description of the Chromatographic Process
11
2
Factors Affecting Separation
13
2
Stationary Phase
13
2
Compound Structure
15
1
Column Temperature
15
1
A Few Final Comments
15
2
Basic Definitions and Equations
Why Bother?
17
1
Peak Shapes
17
2
Peak Width (W)
17
1
Peak Symmetry
18
1
Retention
19
3
Retention Time (tr)
19
1
Adjusted Retention Time (tr")
19
1
Partition Radio (k)
20
1
Retention Index (I)
21
1
Phase Radio (β)
22
1
Distribution Constant (KD)
23
3
KD and Column Dimensions
25
1
KD and Column Temperature
25
1
Column Efficiency
26
4
Number of Theoretical Plates (n)
26
1
Height Equivalent to a Theoretical Plate (h)
27
1
Effective Theoretical Plates (N) and Plate Heights (H)
27
1
Precautions When Using Theoretical Plates
27
3
Coating Efficiency (CE%)
30
1
Separation Factor (α)
31
1
Resolution (R)
32
2
Trennzahl (TZ)
34
1
Column Capacity
35
2
Capillary GC Columns: Tubing
Fused Silica Capillary Columns
37
1
Fused Silica Tubing
37
2
Outer Coating
39
1
Other Tubing Materials
40
2
Capillary GC Columns: Stationary Phases
Stationary Phases
42
1
Types of Stationary Phases
43
5
Polysiloxanes or Silicones
43
2
Low Bleed Stationary Phases
45
1
Polyethylene Glycols
46
1
Porous Layer Stationary Phases
47
1
Characteristics of Stationary Phases
48
8
Bonded and Cross-linked Stationary Phases
48
1
Stationary Phase Polarity
49
1
Stationary Phase Selectivity
50
1
Stationary Phase Interactions
51
1
Dispersion Interaction
51
1
Dipole Interaction
52
2
Hydrogen Bonding Interaction
54
1
When There Are Multiple Interactions
55
1
Stationary Phase Equivalencies
56
1
Column Temperature Limits
56
2
Column Bleed
58
4
What Is Column Bleed?
58
2
Measuring Column Bleed
60
1
Sensitivity Considerations
60
1
Detector Considerations
61
1
Minimizing Column Bleed
62
1
Selecting Stationary Phases
62
2
Capillary GC Columns: Dimensions
Introduction
64
1
Column Length
64
5
Length and Efficiency/Resolution
65
1
Length and Retention
66
1
Length and Pressure
66
2
Length and Bleed
68
1
Length and Cost
68
1
Selecting Column Length
68
1
Column Diameter
69
6
Diameter and Efficiency/Resolution
69
1
Diameter and Retention
70
1
Diameter and Pressure
70
2
Diameter and Bleed
72
1
Diameter and Capacity
72
1
Diameter and Carrier Gas Volume
73
1
Diameter and Injector Efficiency
74
1
Diameter and Breakage
74
1
Diameter and Column Cost
74
1
Selecting Column Diameter
75
1
Column Film Thickness
75
5
Film Thickness and Retention
75
2
Film Thickness and Efficiency/Resolution
77
1
Film Thickness and Capacity
78
1
Film Thickness and Bleed
79
1
Film Thickness and Inertness
80
1
Selecting Column Film Thickness
80
1
Manipulating Multiple Column Dimensions
80
3
Carrier Gas
Carrier Gas and Capillary Columns
83
1
Linear Velocity versus Flow Rate
83
1
Van Deemter Curves
83
2
Carrier Gases Measurements
85
6
Average Linear Velocity
85
3
Flow Rate
88
2
Converting Average Linear Velocities and Flow Rates
90
1
Carrier Gas Selection
91
5
Nitrogen
91
2
Helium
93
1
Hydrogen
93
3
Recommended Linear Velocities
96
1
Gas Purities
97
3
Common Carrier Gas Problems
100
2
Injectors
Introduction
102
1
The Basics of Vaporization Injectors
103
6
Injector Temperature
104
1
Speed of Sample Transfer
105
1
Backflash
105
2
Discrimination
107
2
Split Injectors
109
9
Description
109
1
Split Ratio
110
3
Septum Purge for Split Injectors
113
1
Split Injector Liners
114
2
Column Position in Split Injectors
116
1
Other Aspects of Split Injectors
116
1
Common Problems with Split Injectors
117
1
Splitless Injectors
118
10
Description
118
2
Selecting Purge Activation Times
120
1
Solvent Effect
121
1
Cold Trapping
122
1
Septum Purge for Splitless Injectors
123
1
Splitless Injector Liners
123
1
Column Position in Split Injectors
124
1
Other Aspects of Split Injectors
125
1
Common Problems with Split Injectors
125
3
Megabore Direct Injectors
128
6
Description
128
2
Megabore Direct Injector Liners
130
3
Septum Purge for Megabore Direct Injectors
133
1
Column Position in Megabore Director Injectors
133
1
Other Aspects of Megabore Direct Injectors
134
1
Common Problems with Megabore Direct Injectors
134
1
Specialized Vaporization Injectors
134
4
Pressure Programmable Injectors
135
1
Temperature Programmable Injectors
136
1
Septumless Injectors
137
1
Cool On-Column Injectors
138
5
Description
138
1
Solvent Effect and Cold Trapping for Cool ON-Column Injections
139
1
Secondary Cooling
139
2
Retention Gaps and Cool On-Column Injectors
141
1
Other Aspects of Cool On-Column Injectors
141
1
Common Problems with Cool On-Column Injectors
142
1
Injection Techniques
143
3
Syringe Filling Techniques
143
1
Injection Speed
144
2
Autosamplers
146
2
Injector Septa
148
3
Introduction
148
1
Septa Hardness
148
1
Septa Bleed
148
2
Handling Septa
150
1
Injector Maintenance
151
5
Cleaning Injectors
151
1
Cleaning Injector Liners
152
1
Silylating Injector Liners
153
3
Detectors
Introduction
156
1
Detector Characteristics
156
8
Dead Volume
156
1
Makeup Gas
157
1
Detector Temperature
158
1
Sensitivity
159
2
Selectivity
161
1
Linear Range
162
2
Flame Ionization Detector (FID)
164
6
Principle of Operation
164
1
Gases
165
1
Column Position
165
1
Temperature
165
1
Selectivity
166
1
Sensitivity and Linear Range
166
1
Verifying Flame Ignition
166
1
Maintenance
167
1
Common Problems
167
1
Change in Sensitivity
167
1
Difficulty in Lighting Flame
168
1
Peak Shape Problem Attributed to the Detector
169
1
Miscellaneous
169
1
Nitrogen Phosphorus Detector (NPD)
170
7
Principle of Operation
170
1
Gases
171
1
Column Position
172
1
Temperature
172
1
Selectivity
172
1
Sensitivity and Linear Range
173
1
Maintenance
173
1
Common Problems
174
1
Change in Sensitivity
174
1
Peak Shape Problem Attributed to the Detector
175
1
Baseline Problems
176
1
Electron Capture Detector (ECD)
177
8
Principle of Operation
177
1
Gases
178
1
Column Position
179
1
Temperature
179
1
Selectivity
179
1
Sensitivity and Linear Range
179
2
Maintenance
181
1
Common Problems
182
1
Change in Sensitivity
182
1
Peak Shape Problem Attributed to the Detector
183
1
Baseline Problems
183
1
Negative Peaks
184
1
Linear Range Problems
184
1
Miscellaneous
185
1
Thermal Conductivity Detector (TCD)
185
7
Principle of Operation
185
1
Gases
186
1
Column Position
187
1
Temperature
187
1
Selectivity
188
1
Sensitivity and Linear Range
189
1
Maintenance
189
1
Common Problems
190
1
Change in Sensitivity
190
1
Peak Shape Problem Attributed to the Detector
191
1
Baseline Problems
191
1
Negative Peaks
192
1
Short Filament Lifetimes
192
1
Flame Photometric Detector (FPD)
192
6
Principle of Operation
192
1
Gases
193
1
Column Position
193
1
Temperature
194
1
Selectivity
195
1
Sensitivity and Linear Range
195
1
Verifying Flame Ignition
196
1
Maintenance
196
1
Common Problems
197
1
Change in Sensitivity
197
1
Peak Shape Problem Attributed to the Detector
197
1
Loss of Linear Range
197
1
Flame Goes Out
198
1
Miscellaneous
198
1
Mass Spectrometer (MS)
198
12
Principle of Operation
198
2
Mass Spectra Data
200
1
Other Ionization, Detection and Mass Filtering Modes
201
1
Selectivity
202
1
Sensitivity and Linear Range
203
1
Temperature
204
1
Column Position
204
1
Carrier Gas Flow Rate Considerations
205
1
Maintenance
206
1
Common Problems
207
1
Change in Sensitivity
207
1
Excessive Noise or High Background
208
1
Leaks
208
2
Column Installation
The Importance of a Properly Installed Column
210
1
Installing Fused Silica Capillary Columns
210
13
Column Installation Steps
210
1
Cutting Fused Silica Capillary Columns
211
1
Column Placement in the GC Oven
212
1
Column Installation in the Injector
212
1
Turning On and Verifying the Carrier Gas Flow
213
1
Installation in the Detector
214
1
Verifying Column Installation and Detector Operation
214
2
Column Conditioning
216
1
What is Column Conditioning?
216
1
Conditioning Temperatures
217
1
Conditioning the Column While Connected to the Detector
217
2
Conditioning the Column While Disconnected from the Detector
219
1
Setting the Carrier Gas Linear Velocity
220
1
Bleed Test
221
1
Injecting Column Test Sample
222
1
Column Ferrules
223
2
Tightening Fittings
225
1
Techniques of Measuring Column Insertion Distances
226
1
Leak Detection
227
1
Column Test Mixtures
Column Performance Testing
228
1
Column Test Mixture Compounds
229
2
Hydrocarbons
229
1
Alcohols
229
1
Acids and Bases
230
1
FAMEs
231
1
Other Compounds
231
1
Column Testing Conditions
231
2
Injectors
231
1
Detectors
231
1
Column Temperature
232
1
Test Sample Concentration
233
1
Grob Test
233
2
Own Test Mixture
235
1
When to Test a Column
236
1
Causes and Prevention of Column Damage
Causes of Column Damage and Performance Degradation
237
1
Column Breakage
237
2
Causes of Column Breakage
237
1
Symptom of Column Breakage
238
1
Prevention of Column Breakage
238
1
Recovery from Column Breakage
239
1
Thermal Damage
239
1
Causes of Thermal Damage
239
1
Symptoms of Thermal Damage
239
1
Prevention of Thermal Damage
240
1
Recovery from Thermal Damage
240
1
Oxygen Damage
240
2
Cause of Oxygen Damage
240
1
Symptoms of Oxygen Damage
241
1
Prevention of Oxygen Damage
241
1
Recovery from Oxygen Damage
241
1
Chemical Damage
242
4
Causes of Chemical Damage
242
1
Bases
242
1
Acids
242
1
HCI and NH4OH
243
1
Organic Solvents and Water
244
1
Symptoms of Chemical Damage
244
1
Prevention of Chemical Damage
245
1
Recovery from Chemical Damage
245
1
Contamination
246
4
Causes of Contamination
246
2
Symptoms of Contamination
248
1
Prevention of Contamination
249
1
Recovery from Contamination
249
1
Solvent Rinsing Columns
250
5
Solvent Rinse Kits
250
2
Solvent Selection, Volumes and Flow Rates
252
2
Conditioning the Column After Solvent Rinsing
254
1
Some Solvent Rising Considerations
255
1
Guard Columns and Retention Gaps
255
4
Deactivated Fused Silica Tubing
255
1
Guard Columns
255
1
Retention Gaps
256
1
Unions
257
2
Packed Injector Liners
259
1
Gas Impurity Traps
260
1
Column Storage
261
1
Column Repair
262
1
Troubleshooting Capillary GC Systems
Introduction
263
1
Approaches to Solving GC Problems
264
4
Systematic Approach
264
1
One Thing At a Time
264
1
Moving from the General to the Specific
264
1
Checking the Obvious
265
1
Looking for Changes
266
1
Eliminating the Possibilities
266
1
Divide and Conquer
267
1
Asking ``If... Then...'' Questions
267
1
Looking for Trends, Patterns and Common Characteristics
268
1
Tool and Useful Items
268
1
Troubleshooting Tests
269
4
Jumper Tube Test
269
1
Condensation Test
270
1
Check Out Column
271
1
Column Exchange
272
1
Column Test Samples
272
1
Static Pressure Test
272
1
Common Problems and Their Causes
273
17
Baseline Drift or Wander
273
1
Noisy Baseline
274
1
Spikes in the Baseline
275
1
Tailing Peaks
276
1
Fronting Peaks
277
1
Extremely Broad or Rounded Peaks
278
1
Split Peaks
279
1
Negative Peaks
280
1
Flat Top Peaks
281
1
Peak Size Problem
281
1
No Peaks
282
1
All Peaks
283
1
Some Peaks
284
1
Retention Time Changes
284
1
Loss of Resolution
285
1
Ghost Peaks or Carryover Problems
286
1
Excessively Broad Solvent Front
287
1
Quantitation Problems
288
1
Rapid Column Deterioration
288
2
Appendix
A Terms and Equations
290
3
A.1 Terms
290
1
A.2 Additional Equations
291
2
B Table of Phase Ratios
293
1
C Temperature Limits
294
1
D Column Bleed Mass Spectra
295
5
E Table of Column Capacities
300
1
F Capillary Injector Designs
301
5
F.1 Flow and Pressure Controllers
301
1
F.2 Back Pressure Regulated Injectors
301
3
F.3 Forward Pressure Regulated Injectors
304
2
References
306
1
Index
307