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GCT Premier
Waters GCT Premier User Manual
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W
aters GCT Premier
Mass S
pectrometer
Operator
’
s Guide
71500109202
/Revision B
Copyr
ight ©
Wa
ters C
orpor
ation 2
006.
All righ
ts
reserved
.
2
Table of Contents
Default Chapter
3
Safety Information
3
Biological Hazard
3
Chemical Hazard
3
High Temperature Hazard
4
High Voltage Hazard
5
Safety Symbols
5
Consignes de Sécurité
6
Généralités
6
Risques Biologiques
6
Risques Chimiques
6
Risques de Brûlure
7
Risques D'électrocution
7
GCT Premier Mass Spectrometer Information
8
Intended Use
8
Calibration
9
Table of Contents
11
1 Instrument Description
24
Introduction
24
Ion Source
25
Electron Ionization/Chemical Ionization (EI/CI) Outer Source Assembly
25
Field Ionization/Field Desorption Ionization (FI/FD) Outer Source Assembly
25
Inner Source Assembly
26
Inlets
28
GC Interface for EI/CI
28
GC Interface for FI/FD
28
Direct Insertion (DI) Probe
28
Direct Chemical Ionization (DCI) Probe
28
Reference Reservoir Inlet
29
Vacuum System
29
Masslynx Control System
30
Controls and Indicators on the Instruments' Front Panel
31
Status Display
31
Controls on the Instruments' Top Panel
33
Controls and Connectors on Instruments' Rear Panel
34
Signal Connections
35
Vacuum and Gas Inlet Connections
40
Gas Inlet Connections
41
EPC Power Switch
42
2 Preparing the Instrument for EI/CI Operation
44
Changing the EI/CI Inner Source Assembly
44
Removing the EI/CI Inner Source
45
Installing the EI/CI Inner Source
46
Changing the EI/CI Outer Source Assembly
48
Removing the EI/CI Outer Source from the Instrument
48
Fitting the EI/CI Outer Source to the Instrument
50
3 Tuning the Instrument
53
Preparing the Instrument for Operation
54
Obtaining an Ion Beam
55
Introducing the Reference Sample
58
Setting up the Instrument Automatically
60
Required Material
60
Tuning the Instrument for EI
71
General Tips for Tuning
75
Tuning the Instrument for Best Resolution in EI
76
Tuning the Instrument for Positive CI
77
Introducing CI Reagent Gas
78
Setting up for CI Tuning
79
Tuning CI Gas Peaks
80
Obtaining a Beam in Positive CI Mode
80
Turning off CI Gas
82
Tuning the Instrument for Negative CI
82
Tuning for Negative CI Mode Operation
83
Obtaining a Beam in Negative CI Mode
84
Turning off CI Gas
85
Preparing for FI Operation
85
Managing Tune Parameters
86
Printing Tune Information
86
Storing Tune Parameters
86
Saving and Recalling Parameter Settings
86
4 Acquiring Data
89
Starting Data Acquisition
90
Starting a Single Sample Acquisition
90
Starting a Multiple-Sample Data Acquisition
93
Setting up an MS Method
93
Adding a Function to the List
94
Modifying an Existing Function in the List
95
Copying an Existing Function in the List
95
Deleting a Function from the List
95
Changing the Order of Functions in the List
96
Saving and Restoring a Function List
96
Selecting the Run Time for the Experiment
97
Setting a Solvent Delay
97
Acquiring Analog Data
98
Setting up an MS Scan
100
Types of Data Acquisition
102
Setting up DRE Mode
103
5 Calibration
107
Calibrating the Instrument
108
Setting up the Instrument for Calibration
108
Lock Mass Correction
109
Using the Calibration Wizard
110
Accepting a Calibration
115
Manually Correcting a Calibration
117
Using Calibrations for Subsequent Acquisitions
121
Using Calibrations
121
Associating a Calibration File with an Acquisition
121
Removing a Calibration File
122
Dynamic External Calibration Temperature Compensation
122
Setting the DXC Drift Value
122
Calibrating the Instrument in CI
124
Calibrating the Instrument in CI+ Mode
124
Manual Calibration
125
Creating a Calibration File
128
Calibrating the Instrument in CI- Mode
131
Calibrating the Instrument in FI/FD Mode
131
6 The GC Interface
134
Installing the GC Interface
135
Determining the Transfer Line Position
135
Reinstallation of the GC Interface
138
Working with the Interface Fitting Tool
138
Installing the GC Column
141
Configuring the GC and Autosampler
143
Removing the GC Interface
143
7 The Direct Insertion Probe
145
Introduction
146
Installing the Probe Insertion Lock
146
Inserting and Removing the DI Probe
148
Loading Sample into the DI Probe
148
Inserting the DI Probe into the Insertion Lock
150
Removing the DI Probe from the Probe Insertion Lock
152
Controlling the DI Probe Temperature
154
Ramping the Probe Temperature Manually
154
Ramping the Probe Temperature Automatically
155
Probe Control Dialog Box Ramps Tab
158
Probe Control Dialog Box
160
Ramping the Probe During a Acquisition
161
8 The Direct Chemical Ionization (DCI) Probe
164
Introduction
164
Installing the Probe Insertion Lock
164
Inserting and Removing the DCI Probe
165
Loading Sample into the DCI Probe
165
Inserting the DCI Probe into the Insertion Lock
166
Removing the DCI Probe from the Probe Insertion Lock
168
Controlling the DCI Probe Current
169
Ramping the Probe Current Manually
169
Ramping the Probe Current Automatically
170
9 FI/FD Operation
171
Introduction
172
Preparing the Instrument for FI/FD Operation
172
Choosing an Emitter for the FI/FD Inner Source
172
Setting-Up for FI/FD Operation
173
Changing the FI/FD Outer Source Assembly
173
Changing the FI/FD Inner Source Assembly
177
Installing the FI/FD Inner Source Direct Insertion Probe Only Flange
179
Changing the FI/FD GC Interface
184
Positioning the GC Column for FI Operation
188
Tuning in FI Mode
190
Introducing the Reference Sample
191
Obtaining a Beam and Tuning in FI Operation
191
General Considerations for Tuning in FI Mode
193
Lens Tuning
193
Setting up and Calibrating the Instrument
194
Instrument Setup in FI Mode
194
Calibrating and Accurate Mass in FI Mode
194
Optimization of FI Calibration
195
Running Samples
196
Running MS Samples in GC FI Mode
196
Using Direct Insertion Probe in FI Mode
196
Tuning in FD Mode
197
Obtaining a Beam in FD Operation
197
Introducing the Sample
198
Calibration and Setup in FD
199
Running an FD Experiment Manually
199
Running an FD Experiment Using the Probe Ramp
200
Loading the FD Inner Source Probe with Sample
202
10 Routine Maintenance
205
Maintenance Schedule
206
Safety and Handling
207
Rotary Pump Oil
208
Oil Quality
208
Oil Color
208
Gas Ballast Control
208
Rotary Pump Maintenance
209
Gas-Ballasting the Rotary Pump
209
Checking the Rotary Pump Oil
210
Changing the Rotary Pump Oil
211
Replacing the Oil Mist and Odor Filter Elements
212
Foreline Trap Maintenance
215
Reference Reservoir Maintenance
220
EI/CI Inner Source Maintenance
222
Cleaning the EI and CI Inner Sources
222
Cleaning the Inner Source Components
224
Cleaning Materials
224
Ultrasonically Cleaning the Inner Source Components
225
Cleaning the Ion Exit Plate
226
Cleaning the Trap and Repeller
227
Renewing the Filament
236
FI/FD Inner Source Maintenance
236
Storing an Emitter
236
Changing an Emitter
237
EI/CI Outer Source Maintenance
239
Cleaning the Collimating Slits
239
Cleaning the Complete Outer Source
241
Assembling the Ion Chamber
245
FI/FD Outer Source Maintenance
246
Cleaning the Extraction Rods
246
Cleaning the Source Ceramic and Focus Plates
249
Checking for Leaks after Source Maintenance
252
Inspecting the CI Gas Line for Leaks
252
Detector Maintenance
254
Conditioning the Detector
254
Setting the Optimum Gain for the Detector
256
11 Troubleshooting
259
Spare Parts
260
Safety and Handling
260
System Troubleshooting
260
Component Hardware Troubleshooting
261
Contacting Waters
272
A Starting-Up and Shutting-Down the Instrument
276
Starting-Up the Instrument
276
Shutting-Down the Instrument
277
Emergency Instrument Shutdown
277
Temporary Shutdown (Switch to Standby
277
Complete Shutdown
278
B the Masslynx Tune Window
279
Opening the Masslynx Tune Window
280
The Tune Window Toolbar
282
The Tune Window File Menu
283
The Tune Window Ion Mode Menu
285
The Tune Window Vacuum Menu
285
Pumping/Venting the Analyzer
285
Pumping/Venting the Instrument
286
Pumping/Venting the Source
286
Monitoring the Instrument Vacuum
287
The Tune Window Settings Menu
288
Configuring the Tune Setup Parameters
288
Configuring the TDC Settings
289
Low Mass Cut-Off
294
Conditioning the Detector
294
Ramping the Probe Temperature
296
Viewing the Status Of, and Rebooting, the Instrument's Embedded PC
296
Selecting the Instrument Name
296
The Tune Window View Menu
297
Copying an Image of the Peak Display
297
Hide/Display the Tuning Parameters
297
Hide/Display the Engineer Parameters
297
Hide/Display the Multiple Peak Displays
298
The Tune Window Wizards Menu
298
Tuning Using the Instrument Setup Wizard
298
Calibrating the Instrument Using the Calibration Wizard
298
The Tune Window Tuning Controls
299
The Source Tab
299
The Inlet Tab
312
Calibration Tab
316
The Engineer Tab
317
The DRE Tab
321
The Tune Window Peak Display
323
Customizing the Peak Display
323
Setting up Nominal Mass
325
Setting up Resolution for Dead Time Correction Manually
326
Dead Time Correction
327
Effects of Saturation on Peak Shape
329
C Calibration Reference Information
333
Overview
334
Editing a Calibration Reference File
334
Calibration Reference File
334
Heptacosa
334
Heptacosa Negative
335
Tris (Trifluoromethyl) Triazine
335
Perfluorotripentylamine (Fc70_Ei.ref
336
Perfluorotripentylamine (Fc70_Pci+.Ref
336
Heptacosa PCI
337
Perfluorotripentylamine (FC70_NCI-.Ref
337
DRE Calculation Files
338
Perfluorotripentylamine for DRE
338
Heptacosa PCI DRE
339
Metri DRE
339
Heptacosadrepos
339
Heptacosacpfbdreneg.drf
340
Typical Lock Mass Values
340
D External Connections
342
Safety Considerations
342
GCT Premier System External Wiring
343
GCT Premier System Vacuum Connections
344
E Status Display Vacuum LED
346
Vacuum LED: Displays for Normal Instrument Operation
346
Vacuum LED: Displays for Instrument Faults
349
F Performance Specifications
352
Performance Specifications
352
Mass Range
352
Resolution
352
Acquisition Rate
352
GC Sensitivity
352
Mass Accuracy
352
Dynamic Range
353
G Theory and Principles of Operation
355
GCT Premier Functionality
356
Ionization Techniques
357
Electron Impact Ionization
357
Chemical Ionization
358
Negative Chemical Ionization
359
Field Ionization
359
Field Desorption
360
General Considerations for Tuning
360
Low Mass Cut-Off
362
DRE Mode
364
Multiple Peak Stitching
366
Gain Drop Monitoring
367
4
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Waters GCT Premier Specifications
General
Software
MassLynx
Resolution
10, 000 FWHM
Ionization Modes
EI, CI
Mass Accuracy
<5 ppm
Dynamic Range
>4 orders of magnitude
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