A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems:
Saved in:
| Main Author: | |
|---|---|
| Format: | Book |
| Language: | German |
| Published: |
Heidelberg
Hüthig
1995
|
| Edition: | 2nd, enl. and rev. ed. |
| Series: | Chromatographic methods
|
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Physical Description: | XX, 323 S. graph. Darst. |
| ISBN: | 3778523198 |
Staff View
MARC
| LEADER | 00000nam a2200000 c 4500 | ||
|---|---|---|---|
| 001 | BV010157703 | ||
| 003 | DE-604 | ||
| 005 | 19951117 | ||
| 007 | t | ||
| 008 | 950418s1995 gw d||| |||| 00||| ger d | ||
| 016 | 7 | |a 944135617 |2 DE-101 | |
| 020 | |a 3778523198 |c kart. : DM 98.00, ca. sfr 100.00 |9 3-7785-2319-8 | ||
| 035 | |a (OCoLC)246719087 | ||
| 035 | |a (DE-599)BVBBV010157703 | ||
| 040 | |a DE-604 |b ger |e rakddb | ||
| 041 | 0 | |a ger | |
| 044 | |a gw |c DE | ||
| 049 | |a DE-355 | ||
| 050 | 0 | |a QD79.C45 | |
| 082 | 0 | |a 543/.0896 |2 21 | |
| 084 | |a VG 7400 |0 (DE-625)147205:253 |2 rvk | ||
| 100 | 1 | |a Rood, Dean |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |c by Dean Rood |
| 250 | |a 2nd, enl. and rev. ed. | ||
| 264 | 1 | |a Heidelberg |b Hüthig |c 1995 | |
| 300 | |a XX, 323 S. |b graph. Darst. | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 490 | 0 | |a Chromatographic methods | |
| 650 | 4 | |a Gas chromatography | |
| 650 | 4 | |a Gas chromatography |x Instruments |x Maintenance and repair | |
| 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 |
| 650 | 0 | 7 | |a Fehlersuche |0 (DE-588)4016615-6 |2 gnd |9 rswk-swf |
| 689 | 0 | 0 | |a Glaskapillargaschromatographie |0 (DE-588)4157443-6 |D s |
| 689 | 0 | |5 DE-604 | |
| 689 | 1 | 0 | |a Kapillargaschromatographie |0 (DE-588)4252082-4 |D s |
| 689 | 1 | 1 | |a Fehlersuche |0 (DE-588)4016615-6 |D s |
| 689 | 1 | |8 1\p |5 DE-604 | |
| 856 | 4 | 2 | |m DNB Datenaustausch |q application/pdf |u http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=006747625&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |3 Inhaltsverzeichnis |
| 883 | 1 | |8 1\p |a cgwrk |d 20201028 |q DE-101 |u https://d-nb.info/provenance/plan#cgwrk | |
| 943 | 1 | |a oai:aleph.bib-bvb.de:BVB01-006747625 | |
Record in the Search Index
| _version_ | 1807505851030700032 |
|---|---|
| adam_text |
IX
TABLE
OF
CONTENTS
INTENTIONS
AND
INTRODUCTION
1
1
INTRODUCTION
TO
CAPILLARY
GAS
CHROMATOGRAPHY
1.1
A
BRIEF
AND
SIMPLE
INTRODUCTION
TO
GAS
CHROMATOGRAPHY
3
1.1.1
WHAT
IS
GAS
CHROMATOGRAPHY?
3
1.1.2
WHAT
TYPES
OF
COMPOUNDS
ARE
SUITABLE
FOR
GC
ANALYSIS?
3
1.1.3
THE
BASIC
PARTS
OF
A
GAS
CHROMATOGRAPH
4
1.1.3.1
GAS
SUPPLY
AND
FLOW
CONTROLLERS
5
1.1.3.2
INJECTOR
5
1.1.3.3
CAPILLARY
COLUMN
AND
OVEN 6
1.1.3.4
DETECTOR
6
1.1.3.5
RECORDING
DEVICE 6
1.1.4
THE
CHROMATOGRAM
7
1.2
LIMITATIONS
AND
CAUTIONS
8
1.3
THE
MECHANISM
OF
COMPOUND
SEPARATION
9
1.3.1
A
VERY
SIMPLE
DESCRIPTION
OF
THE
CHROMATOGRAPHIC
PROCESS
10
1.3.2
A
DETAILED
DESCRIPTION
OF
THE
CHROMATOGRAPHIC
PROCESS
11
1.4
FACTORS
AFFECTING
SEPARATION
13
1.4.1
STATIONARY
PHASE
13
1.4.2
COMPOUND
STRUCTURE
15
1.4.3
COLUMN
TEMPERATURE
15
1.5
A
FEW
FINAL
COMMENTS
15
X
2
BASIC
BUT
ESSENTIAL
DEFINITIONS
AND
EQUATIONS
2.1
WHY
BOTHER?
17
2.2
PEAK
SHAPES
17
2.2.1
PEAK
WIDTH
(W)
17
2.2.2
PEAK
SYMMETRY
18
2.3
RETENTION
19
2.3.1
RETENTION
TIME
(T,)
19
2.3.2
ADJUSTED
RETENTION
TIME
(V)
19
2.3.3
PARTITION
RATIO
(K)
20
2.3.4
RETENTION
INDEX
(I)
21
2.4
PHASE
RATIO
(P)
22
2.5
DISTRIBUTION
CONSTANT
(K
D
)
23
2.5.1
K
D
AND
COLUMN
DIMENSIONS
25
2.5.2
K
D
AND
COLUMN
TEMPERATURE
25
2.6
COLUMN
EFFICIENCY
26
2.6.1
NUMBER
OF
THEORETICAL
PLATES
(N)
26
2.6.2
HEIGHT
EQUIVALENT
TO
A
THEORETICAL
PLATE
(H)
27
2.6.3
EFFECTIVE
THEORETICAL
PLATES
(N)
AND
PLATE
HEIGHTS
(H)
27
2.6.4
PRECAUTIONS
WHEN
USING
THEORETICAL
PLATES
27
2.7
COATING
EFFICIENCY
(CE%) 30
2.8
SEPARATION
FACTOR
(A)
31
2.9
RESOLUTION
(R)
32
2.10
TRENNZAHL
(TZ) 34
2.11
COLUMN
CAPACITY
35
3
CAPILLARY
GC
COLUMNS:
TUBING
3.1
FUSED
SILICA
CAPILLARY
COLUMNS
37
3.2
FUSED
SILICA
TUBING
37
3.3
OUTER
COATING
39
3.4
OTHER
TUBING
MATERIALS
40
4
CAPILLARY
GC
COLUMNS:
STATIONARY
PHASES
4.1
STATIONARY
PHASES
42
4.2
TYPES
OF
STATIONARY
PHASES
43
4.2.1
POLYSILOXANES
OR
SILICONES
43
XI
4.2.2
POLYETHYLENE
GLYCOLS
45
4.2.3
POROUS
LAYER
STATIONARY
PHASES
46
4.3
CHARACTERISTICS
OF
STATIONARY
PHASES
47
4.3.1
BONDED
AND
CROSS-LINKED
STATIONARY
PHASES
47
4.3.2
STATIONARY
PHASE
POLARITY
48
4.3.3
STATIONARY
PHASE
SELECTIVITY 50
4.3.4
STATIONARY
PHASE
INTERACTIONS
50
4.3.4.1
DISPERSION
INTERACTION 50
4.3.4.2
DIPOLE
INTERACTION
52
4.3.4.3
HYDROGEN
BONDING
INTERACTION
53
4.3.4.4
WHEN
THERE
ARE
MULTIPLE
INTERACTIONS
54
4.4
STATIONARY
PHASE
EQUIVALENCIES
55
4.5
COLUMN
TEMPERATURE
LIMITS
56
4.6
COLUMN
BLEED
57
4.6.1
WHAT
IS
COLUMN
BLEED?
57
4.6.2
MEASURING
COLUMN
BLEED
59
4.6.3
SENSITIVITY
CONSIDERATIONS
59
4.6.4
DETECTOR
CONSIDERATIONS
60
4.6.5
MINIMIZING
COLUMN
BLEED
61
4.7
SELECTING
STATIONARY
PHASES
61
5
CAPILLARY
GC
COLUMNS:
DIMENSIONS
5.1
INTRODUCTION
64
5.2
COLUMN
LENGTH
64
5.2.1
LENGTH
AND
EFFICIENCY/RESOLUTION
65
5.2.2
LENGTH
AND
RETENTION
66
5.2.3
LENGTH
AND
PRESSURE
66
5.2.4
LENGTH
AND
BLEED
68
5.2.5
LENGTH
AND
COST
68
5.2.6
SELECTING
COLUMN
LENGTH 68
5.3
COLUMN
DIAMETER
69
5.3.1
DIAMETER
AND
EFFICIENCY/RESOLUTION
69
5.3.2
DIAMETER
AND
RETENTION
70
5.3.3
DIAMETER
AND
PRESSURE
70
5.3.4
DIAMETER
AND
BLEED
72
5.3.5
DIAMETER
AND
CAPACITY
72
5.3.6
DIAMETER
AND
CARRIER
GAS
VOLUME
73
5.3.7
DIAMETER
AND
INJECTOR
EFFICIENCY
74
5.3.8
DIAMETER
AND
BREAKAGE
74
XII
5.3.9
DIAMETER
AND
COLUMN
COST
74
5.3.10
SELECTING
COLUMN
DIAMETER
75
5.4
COLUMN
FILM
THICKNESS
75
5.4.1
FILM
THICKNESS
AND
RETENTION
75
5.4.2
FILM
THICKNESS
AND
EFFICIENCY/RESOLUTION
77
5.4.3
FILM
THICKNESS
AND
CAPACITY
78
5.4.4
FILM
THICKNESS
AND
BLEED
79
5.4.5
FILM
THICKNESS
AND
INERTNESS
80
5.4.6
SELECTING
COLUMN
FILM
THICKNESS
80
5.5
MANIPULATING
MULTIPLE
COLUMN
DIMENSIONS
80
6
CARRIER
GASES
6.1
CARRIER
GASES
AND
CAPILLARY
COLUMNS
83
6.2
LINEAR
VELOCITY
VERSUS
FLOW
RATE 83
6.3
VAN
DEEMTER
CURVES
83
6.4
CARRIER
GASES
MEASUREMENTS
85
6.4.1
AVERAGE
LINEAR
VELOCITY
85
6.4.2
FLOW
RATE 88
6.4.3
CONVERTING
AVERAGE
LINEAR
VELOCITIES
AND
FLOW
RATES
90
6.5
CARRIER
GAS SELECTION
91
6.5.1
NITROGEN
91
6.5.2
HELIUM
94
6.5.3
HYDROGEN
94
6.6
RECOMMENDED
LINEAR
VELOCITIES
95
6.7
GAS
PURITIES
99
6.8
COMMON
CARRIER
GAS
PROBLEMS
99
7
OPERATION
AND
MAINTENANCE
OF
INJECTORS
7.1
INTRODUCTION
102
7.2
THE
BASICS
OF
VAPORIZATION
INJECTORS
103
7.2.1
INJECTOR
TEMPERATURE
104
7.2.2
SPEED
OF
SAMPLE
TRANSFER
105
7.2.3
BACKFLASH
105
7.2.4
DISCRIMINATION
107
7.3
SPLIT
INJECTORS
109
7.3.1
DESCRIPTION
109
7.3.2
SPLIT
RATIO
110
XIII
7.3.3
SEPTUM
PURGE
FOR
SPLIT
INJECTORS
113
7.3.4
SPLIT
INJECTOR
LINERS
114
7.3.5
COLUMN
POSITION
IN
SPLIT
INJECTORS
116
7.3.6
OTHER
ASPECTS
OF
SPLIT
INJECTORS
116
7.3.7
COMMON
PROBLEMS
WITH
SPLIT INJECTORS
117
7.4
SPLITLESS
INJECTORS
118
7.4.1
DESCRIPTION
118
7.4.2
SELECTING
PURGE
ACTIVATION
TIMES
120
7.4.3
SOLVENT
EFFECT
121
7.4.4
COLD
TRAPPING
122
7.4.5
SEPTUM
PURGE
FOR
SPLITLESS
INJECTORS
122
7.4.6
SPLITLESS
INJECTOR
LINERS
123
7.4.7
COLUMN
POSITION
IN
SPLITLESS
INJECTORS
124
7.4.8
OTHER
ASPECTS
OF
SPLITLESS
INJECTORS
125
7.4.9
COMMON
PROBLEMS
WITH
SPLITLESS
INJECTORS
125
7.5
MEGABORE
DIRECT
INJECTORS
128
7.5.1
DESCRIPTION
128
7.5.2
MEGABORE
DIRECT INJECTOR
LINERS
130
7.5.3
SEPTUM
PURGE
FOR
MEGABORE
DIRECT
INJECTORS
132
7.5.4
COLUMN
POSITION
IN
MEGABORE
DIRECT
INJECTORS
133
7.5.5
OTHER
ASPECTS
OF
MEGABORE
DIRECT
INJECTORS
133
7.5.6
COMMON
PROBLEMS
WITH
MEGABORE
DIRECT
INJECTORS
134
7.6
SPECIALIZED
VAPORIZATION
INJECTORS
134
7.6.1
PRESSURE
PROGRAMMABLE
INJECTORS
134
7.6.2
TEMPERATURE
PROGRAMMABLE
INJECTORS
136
7.6.3
SEPTUMLESS
INJECTORS
137
7.7
COOL
ON-COLUMN
INJECTORS
137
7.7.1
DESCRIPTION
137
7.7.2
SOLVENT
EFFECT
AND
COLD
TRAPPING
FOR
COOL
ON-COLUMN
INJECTIONS
138
7.7.3
SECONDARY
COOLING
140
7.7.4
RETENTION
GAPS
AND
COOL
ON-COLUMN
INJECTORS
140
7.7.5
OTHER
ASPECTS
OF
COOL
ON-COLUMN
INJECTORS
141
7.7.6
COMMON
PROBLEMS
WITH
COOL
ON-COLUMN
INJECTORS
142
7.8
INJECTION
TECHNIQUES
142
7.8.1
SYRINGE
FILLING
TECHNIQUES
142
7.8.2
INJECTION
SPEED
143
7.9
AUTOSAMPLERS
145
7.10
INJECTOR
SEPTA
147
7.10.1
INTRODUCTION
147
7.10.2
SEPTA
HARDNESS
148
XIV
7.10.3
SEPTA
BLEED
148
7.10.4
HANDLING
SEPTA
150
7.11
INJECTOR
MAINTENANCE
151
7.11.1
CLEANING
INJECTORS
151
7.11.2
CLEANING
INJECTOR
LINERS
152
7.11.3
SILYLATING
INJECTOR
LINERS
153
8
OPERATION
AND
MAINTENANCE
OF
DETECTORS
8.1
INTRODUCTION
156
8.2
DETECTOR
CHARACTERISTICS
156
8.2.1
DEAD
VOLUME
156
8.2.2
MAKEUP
GAS
157
8.2.3
DETECTOR
TEMPERATURE
158
8.2.4
SENSITIVITY
159
8.2.5
SELECTIVITY
161
8.2.6
LINEAR
RANGE
162
8.3
FLAME
IONIZATION
DETECTOR
(FID)
164
8.3.1
PRINCIPLE
OF
OPERATION
164
8.3.2
GASES
165
8.3.3
COLUMN
POSITION
165
8.3.4
TEMPERATURE
165
8.3.5
SELECTIVITY
166
8.3.6
SENSITIVITY
AND
LINEAR RANGE
166
8.3.7
VERIFYING
FLAME
IGNITION
166
8.3.8
MAINTENANCE
167
8.3.9
COMMON
PROBLEMS
167
8.3.9.1
CHANGE
IN
SENSITIVITY
167
8.3.9.2
DIFFICULTY
IN
LIGHTING
FLAME
168
8.3.9.3
PEAK
SHAPE
PROBLEM
ATTRIBUTED
TO
THE
DETECTOR
169
8.3.9.4
MISCELLANEOUS
169
8.4
NITROGEN
PHOSPHORUS
DETECTOR
(NPD)
170
8.4.1
PRINCIPLE
OF
OPERATION
170
8.4.2
GASES
171
8.4.3
COLUMN
POSITION
172
8.4.4
TEMPERATURE
172
8.4.5
SELECTIVITY
172
8.4.6
SENSITIVITY
AND
LINEAR
RANGE
173
8.4.7
MAINTENANCE
173
8.4.8
COMMON
PROBLEMS
174
8.4.8.1
CHANGE
IN
SENSITIVITY
174
8.4.8.2
PEAK SHAPE
PROBLEM
ATTRIBUTED
TO
THE
DETECTOR
175
8.4.8.3
BASELINE
PROBLEMS
176
8.5
ELECTRON
CAPTURE
DETECTOR
(ECD)
176
8.5.1
PRINCIPLE
OF
OPERATION
176
8.5.2
GASES
178
8.5.3
COLUMN
POSITION
178
8.5.4
TEMPERATURE
179
8.5.5
SELECTIVITY
179
8.5.6
SENSITIVITY
AND
LINEAR RANGE
179
8.5.7
MAINTENANCE
181
8.5.8
COMMON
PROBLEMS
182
8.5.8.1
CHANGE
IN
SENSITIVITY
182
8.5.S.2
PEAK
SHAPE
PROBLEM
ATTRIBUTED
TO
THE
DETECTOR
182
8.5.8.3
BASELINE
PROBLEMS
183
8.5.8.4
NEGATIVE
PEAKS
183
8.5.8.5
LINEAR
RANGE
PROBLEMS
184
8.5.8.6
MISCELLANEOUS
184
8.6
THERMAL
CONDUCTIVITY
DETECTOR
(TCD)
185
8.6.1
PRINCIPLE
OF
OPERATION
185
8.6.2
GASES
186
8.6.3
COLUMN
POSITION
187
8.6.4
TEMPERATURE
187
8.6.5
SELECTIVITY
187
8.6.6
SENSITIVITY
AND
LINEAR
RANGE
187
8.6.7
MAINTENANCE
188
8.6.8
COMMON
PROBLEMS
189
8.6.8.1
CHANGE
IN
SENSITIVITY
189
8.6.8.2
PEAK SHAPE
PROBLEM
ATTRIBUTED
TO
THE
DETECTOR
190
8.6.8.3
BASELINE
PROBLEMS
190
8.6.8.4
NEGATIVE
PEAKS
191
8.6.8.5
SHORT
FILAMENT
LIFETIMES
191
8.7
FLAME
PHOTOMETRIC
DETECTOR
(FPD)
192
8.7.1
PRINCIPLE
OF
OPERATION
192
8.7.2
GASES
193
8.7.3
COLUMN
POSITION
193
8.7.4
TEMPERATURE
194
8.7.5
SELECTIVITY
194
8.7.6
SENSITIVITY
AND
LINEAR
RANGE
194
8.7.7
VERIFYING
FLAME
IGNITION
195
8.7.8
MAINTENANCE
195
XVI
8.7.9
COMMON
PROBLEMS
196
8.7.9.1
CHANGE
IN
SENSITIVITY
196
8.7.9.2
PEAK
SHAPE
PROBLEM
ATTRIBUTED
TO
THE
DETECTOR
196
8.7.9.3
LOSS
OF
LINEAR
RANGE
197
8.7.9.4
FLAME
GOES
OUT
197
8.7.9.5
MISCELLANEOUS
197
8.8
MASS
SPECTROMETER
(MS)
197
8.8.1
PRINCIPLE
OF
OPERATION
197
8.8.2
MASS
SPECTRAL
DATA
199
8.8.3
OTHER
IONIZATION,
DETECTION
AND
MASS
FILTERING
MODES
201
8.8.4
SELECTIVITY
202
8.8.5
SENSITIVITY
AND
LINEAR
RANGE
202
8.8.6
TEMPERATURE
203
8.8.7
COLUMN
POSITION
204
8.8.8
CARRIER
GAS
FLOW
RATE
CONSIDERATIONS
204
8.8.9
MAINTENANCE
205
8.8.10
COMMON
PROBLEMS
206
8.8.10.1
CHANGE
IN
SENSITIVITY
206
8.8.10.2
EXCESSIVE
NOISE
OR
HIGH
BACKGROUND
207
8.8.10.3
LEAKS
208
9
COLUMN
INSTALLATION
9.1
THE
IMPORTANCE
OF
A
PROPERLY
INSTALLED
COLUMN
210
9.2
INSTALLING
FUSED
SILICA
CAPILLARY
COLUMNS
210
9.2.1
COLUMN
INSTALLATION
STEPS
210
9.2.2
CUTTING
FUSED
SILICA
CAPILLARY
COLUMNS
211
9.2.3
COLUMN
PLACEMENT
IN
THE
GC
OVEN
212
9.2.4
COLUMN
INSTALLATION
IN
THE
INJECTOR
212
9.2.5
TURNING
ON
AND
VERIFYING
THE
CARRIER
GAS
FLOW
213
9.2.6
INSTALLATION
IN
THE
DETECTOR
214
9.2.7
VERIFYING
COLUMN
INSTALLATION
AND
DETECTOR
OPERATION
214
9.2.8
COLUMN
CONDITIONING
216
9.2.8.1
WHAT
IS
COLUMN
CONDITIONING?
216
9.2.8.2
CONDITIONING
TEMPERATURES
217
9.2.8.3
CONDITIONING
THE
COLUMN
WHILE
CONNECTED
TO
THE
DETECTOR
217
9.2.8.4
CONDITIONING
THE
COLUMN
WHILE
DISCONNECTED
FROM
THE
DETECTOR
219
9.2.9
SETTING
THE
CARRIER
GAS
LINEAR
VELOCITY
220
XVII
9.2.10
BLEED
TEST
221
9.2.11
INJECTING
COLUMN
TEST
SAMPLE
222
9.3
COLUMN
FERRULES
223
9.4
TIGHTENING
FITTINGS
225
9.5
TECHNIQUES
OF
MEASURING
COLUMN
INSERTION
DISTANCES
225
9.6
LEAK
DETECTION
227
10
COLUMN
TEST
MIXTURES
10.1
COLUMN
PERFORMANCE
TESTING
228
10.2
COLUMN
TEST
MIXTURE
COMPOUNDS
229
10.2.1
HYDROCARBONS
229
10.2.2
ALCOHOLS
229
10.2.3
ACIDS
AND
BASES
230
10.2.4
FAME'S
231
10.2.5
OTHER
COMPOUNDS
231
10.3
COLUMN
TESTING
CONDITIONS
231
10.3.1
INJECTORS
231
10.3.2
DETECTORS
231
10.3.3
COLUMN
TEMPERATURE
232
10.3.4
TEST
SAMPLE
CONCENTRATION
233
10.4
GROB
TEST
233
10.5
OWN
TEST
MIXTURE
235
10.6
WHEN
TO
TEST
A
COLUMN
236
11
CAUSES
AND
PREVENTION
OF
COLUMN
DAMAGE
11.1
CAUSES
OF
COLUMN
DAMAGE
AND
PERFORMANCE
DEGRADATION
237
11.2
COLUMN
BREAKAGE
237
11.2.1
CAUSES
OF
COLUMN
BREAKAGE
237
11.2.2
SYMPTOMS
OF
COLUMN
BREAKAGE
238
11.2.3
PREVENTION
OF
COLUMN
BREAKAGE
238
11.2.4
RECOVERY
FROM
COLUMN
BREAKAGE
239
11.3
THERMAL
DAMAGE
239
11.3.1
CAUSES
OF
THERMAL
DAMAGE
239
11.3.2
SYMPTOMS
OF
THERMAL
DAMAGE
239
11.3.3
PREVENTION
OF
THERMAL
DAMAGE
240
11.3.4
RECOVERY
FROM
THERMAL
DAMAGE
240
11.4
OXYGEN
DAMAGE
240
XVIII
11.4.1
CAUSES
OF
OXYGEN
DAMAGE
240
11.4.2
SYMPTOMS
OF
OXYGEN
DAMAGE
241
11.4.3
PREVENTION
OF
OXYGEN
DAMAGE
241
11.4.4
RECOVERY
FROM
OXYGEN
DAMAGE
241
11.5
CHEMICAL
DAMAGE
242
11.5.1
CAUSES
OF
CHEMICAL
DAMAGE
242
11.5.1.1
BASES
242
11.5.1.2
ACIDS
242
11.5.1.3
HCIANDNFWH
243
11.5.1.4
ORGANIC
SOLVENTS
AND
WATER
244
11.5.2
SYMPTOMS
OF
CHEMICAL
DAMAGE
244
11.5.3
PREVENTION
OF
CHEMICAL
DAMAGE
245
11.5.4
RECOVERY
FROM
CHEMICAL
DAMAGE
245
11.6
CONTAMINATION
246
11.6.1
CAUSES
OF
CONTAMINATION
246
11.6.2
SYMPTOMS
OF
CONTAMINATION
248
11.6.3
PREVENTION
OF
CONTAMINATION
249
11.6.4
RECOVERY
FROM
CONTAMINATION
249
11.7
SOLVENT
RINSING
COLUMNS
250
11.7.1
SOLVENT
RINSE
KITS
250
11.7.2
SOLVENT
SELECTION,
VOLUMES
AND
FLOW
RATES
252
11.7.3
CONDITIONING
THE
COLUMN
AFTER
SOLVENT
RINSING
254
11.7.4
SOME
SOLVENT
RISING
CONSIDERATIONS
255
11.8
GUARD
COLUMNS
AND
RETENTION
GAPS
255
11.8.1
DEACTIVATED
FUSED
SILICA
TUBING
255
11.8.2
GUARD
COLUMNS
255
11.8.3
RETENTION
GAPS
256
11.8.4
UNIONS
257
11.9
PACKED
INJECTOR
LINERS
259
11.10
GAS
IMPURITY
TRAPS
259
11.11
COLUMN
STORAGE
261
11.12
COLUMN
REPAIR
262
12
TROUBLESHOOTING
CAPILLARY
GC
SYSTEMS
12.1
INTRODUCTION
263
12.2
APPROACHES
TO
SOLVING
GC
PROBLEMS
264
12.2.1
SYSTEMATIC
APPROACH
264
12.2.2
ONE
THING
AT
A
TIME
264
12.2.3
MOVING
FROM
THE
GENERAL
TO
THE
SPECIFIC
264
XIX
12.2.4
CHECKING
THE
OBVIOUS
265
12.2.5
LOOKING
FOR
CHANGES
266
12.2.6
ELIMINATING
THE
POSSIBILITIES
266
12.2.7
DIVIDE
AND
CONQUER
267
12.2.8
ASKING
"IF.THEN."
QUESTIONS
267
12.2.9
LOOKING
FOR
TRENDS,
PATTERNS
AND
COMMON
CHARACTERISTICS
268
12.3
TOOLS
AND
USEFUL
ITEMS
268
12.4
TROUBLESHOOTING
TESTS
269
12.4.1
JUMPER
TUBE
TEST
269
12.4.2
CONDENSATION
TEST
270
12.4.3
CHECK
OUT
COLUMN
271
12.4.4
COLUMN
EXCHANGE
272
12.4.5
COLUMN
TEST
SAMPLES
272
12.4.6
STATIC
PRESSURE
TEST
272
12.5
COMMON
PROBLEMS
AND
THEIR
CAUSES
273
12.5.1
BASELINE
DRIFT
OR
WANDER
273
12.5.2
NOISY
BASELINE
274
12.5.3
SPIKES
IN
THE
BASELINE
275
12.5.4
TAILING
PEAKS
276
12.5.5
FRONTING
PEAKS
277
12.5.6
EXTREMELY
BROAD
OR
ROUNDED
PEAKS
278
12.5.7
SPLIT
PEAKS
279
12.5.8
NEGATIVE
PEAKS
280
12.5.9
FLAT
TOP
PEAKS
281
12.5.10
PEAK
SIZE
PROBLEM
281
12.5.10.1
NO
PEAKS
282
12.5.10.2
ALL
PEAKS
283
12.5.10.3
SOME
PEAKS
284
12.5.11
RETENTION
TIME
CHANGES
284
12.5.12
LOSS
OF
RESOLUTION
285
12.5.13
GHOST
PEAKS
OR
CARRYOVER
PROBLEMS
286
12.5.14
EXCESSIVELY
BROAD
SOLVENT
FRONT
287
12.5.15
QUANTITATION
PROBLEMS
288
12.5.16
RAPID
COLUMN
DETERIORATION
288
XX
APPENDIX
A
TERMS
AND
EQUATIONS
290
A.1
TERMS
290
A.2
ADDITIONAL
EQUATIONS
291
B
TABLE
OF
PHASE
RATIOS
293
C
TEMPERATURE
LIMITS
294
D
COLUMN
BLEED
MASS
SPECTRA
295
E
TABLE
OF
COLUMN
CAPACITIES
300
F
CAPILLARY
INJECTOR
DESIGNS
301
F.1
FLOW
AND
PRESSURE
CONTROLLERS
301
F.2
BACK
PRESSURE
REGULATED
INJECTORS
301
F.3
FORWARD
PRESSURE
REGULATED
INJECTORS
304
REFERENCES
306
INDEX
307 |
| any_adam_object | 1 |
| author | Rood, Dean |
| author_facet | Rood, Dean |
| author_role | aut |
| author_sort | Rood, Dean |
| author_variant | d r dr |
| building | Verbundindex |
| bvnumber | BV010157703 |
| 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 |
| ctrlnum | (OCoLC)246719087 (DE-599)BVBBV010157703 |
| dewey-full | 543/.0896 |
| dewey-hundreds | 500 - Natural sciences and mathematics |
| dewey-ones | 543 - Analytical chemistry |
| dewey-raw | 543/.0896 |
| dewey-search | 543/.0896 |
| dewey-sort | 3543 3896 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie |
| edition | 2nd, enl. and rev. ed. |
| format | Book |
| fullrecord | <?xml version="1.0" encoding="UTF-8"?><collection xmlns="http://www.loc.gov/MARC21/slim"><record><leader>00000nam a2200000 c 4500</leader><controlfield tag="001">BV010157703</controlfield><controlfield tag="003">DE-604</controlfield><controlfield tag="005">19951117</controlfield><controlfield tag="007">t</controlfield><controlfield tag="008">950418s1995 gw d||| |||| 00||| ger d</controlfield><datafield tag="016" ind1="7" ind2=" "><subfield code="a">944135617</subfield><subfield code="2">DE-101</subfield></datafield><datafield tag="020" ind1=" " ind2=" "><subfield code="a">3778523198</subfield><subfield code="c">kart. : DM 98.00, ca. sfr 100.00</subfield><subfield code="9">3-7785-2319-8</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(OCoLC)246719087</subfield></datafield><datafield tag="035" ind1=" " ind2=" "><subfield code="a">(DE-599)BVBBV010157703</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">ger</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-355</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/.0896</subfield><subfield code="2">21</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="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">A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems</subfield><subfield code="c">by Dean Rood</subfield></datafield><datafield tag="250" ind1=" " ind2=" "><subfield code="a">2nd, enl. and rev. ed.</subfield></datafield><datafield tag="264" ind1=" " ind2="1"><subfield code="a">Heidelberg</subfield><subfield code="b">Hüthig</subfield><subfield code="c">1995</subfield></datafield><datafield tag="300" ind1=" " ind2=" "><subfield code="a">XX, 323 S.</subfield><subfield code="b">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="490" ind1="0" ind2=" "><subfield code="a">Chromatographic methods</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">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="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="689" ind1="0" 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="0" ind2=" "><subfield code="5">DE-604</subfield></datafield><datafield tag="689" ind1="1" 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="1" 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="1" ind2=" "><subfield code="8">1\p</subfield><subfield code="5">DE-604</subfield></datafield><datafield tag="856" ind1="4" ind2="2"><subfield code="m">DNB 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=006747625&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA</subfield><subfield code="3">Inhaltsverzeichnis</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="943" ind1="1" ind2=" "><subfield code="a">oai:aleph.bib-bvb.de:BVB01-006747625</subfield></datafield></record></collection> |
| id | DE-604.BV010157703 |
| illustrated | Illustrated |
| indexdate | 2024-08-16T01:31:46Z |
| institution | BVB |
| isbn | 3778523198 |
| language | German |
| oai_aleph_id | oai:aleph.bib-bvb.de:BVB01-006747625 |
| oclc_num | 246719087 |
| open_access_boolean | |
| owner | DE-355 DE-BY-UBR |
| owner_facet | DE-355 DE-BY-UBR |
| physical | XX, 323 S. graph. Darst. |
| publishDate | 1995 |
| publishDateSearch | 1995 |
| publishDateSort | 1995 |
| publisher | Hüthig |
| record_format | marc |
| series2 | Chromatographic methods |
| spelling | Rood, Dean Verfasser aut A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems by Dean Rood 2nd, enl. and rev. ed. Heidelberg Hüthig 1995 XX, 323 S. graph. Darst. txt rdacontent n rdamedia nc rdacarrier Chromatographic methods Gas chromatography Gas chromatography Instruments Maintenance and repair Glaskapillargaschromatographie (DE-588)4157443-6 gnd rswk-swf Kapillargaschromatographie (DE-588)4252082-4 gnd rswk-swf Fehlersuche (DE-588)4016615-6 gnd rswk-swf Glaskapillargaschromatographie (DE-588)4157443-6 s DE-604 Kapillargaschromatographie (DE-588)4252082-4 s Fehlersuche (DE-588)4016615-6 s 1\p DE-604 DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=006747625&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis 1\p cgwrk 20201028 DE-101 https://d-nb.info/provenance/plan#cgwrk |
| spellingShingle | Rood, Dean A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems Gas chromatography Gas chromatography Instruments Maintenance and repair Glaskapillargaschromatographie (DE-588)4157443-6 gnd Kapillargaschromatographie (DE-588)4252082-4 gnd Fehlersuche (DE-588)4016615-6 gnd |
| subject_GND | (DE-588)4157443-6 (DE-588)4252082-4 (DE-588)4016615-6 |
| title | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
| title_auth | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
| title_exact_search | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
| title_full | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems by Dean Rood |
| title_fullStr | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems by Dean Rood |
| title_full_unstemmed | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems by Dean Rood |
| title_short | A practical guide to the care, maintenance, and troubleshooting of capillary gas chromatographic systems |
| title_sort | a practical guide to the care maintenance and troubleshooting of capillary gas chromatographic systems |
| topic | Gas chromatography Gas chromatography Instruments Maintenance and repair Glaskapillargaschromatographie (DE-588)4157443-6 gnd Kapillargaschromatographie (DE-588)4252082-4 gnd Fehlersuche (DE-588)4016615-6 gnd |
| topic_facet | Gas chromatography Gas chromatography Instruments Maintenance and repair Glaskapillargaschromatographie Kapillargaschromatographie Fehlersuche |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=006747625&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT rooddean apracticalguidetothecaremaintenanceandtroubleshootingofcapillarygaschromatographicsystems |