Waters GCT Premier - Calibration

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ix

Calibration

Follow acceptable methods of calibration with pure standards to calibrate. Use

a minimum of five standards to generate a standard curve. The concentration

range should cover the entire range of quality-control samples, typical

specimens, and atypical specimens.

Table of Contents

Default Chapter3
- Safety Information3
- Consignes de Sécurité6
- GCT Premier Mass Spectrometer Information8
1 Instrument Description24
- Introduction24
- Ion Source25
- Inlets28
- Reference Reservoir Inlet29
- Vacuum System29
- Masslynx Control System30
- Controls and Indicators on the Instruments' Front Panel31
  - Status Display31
- Controls on the Instruments' Top Panel33
- Controls and Connectors on Instruments' Rear Panel34
2 Preparing the Instrument for EI/CI Operation44
- Changing the EI/CI Inner Source Assembly44
  - Removing the EI/CI Inner Source45
  - Installing the EI/CI Inner Source46
- Changing the EI/CI Outer Source Assembly48
  - Removing the EI/CI Outer Source from the Instrument48
  - Fitting the EI/CI Outer Source to the Instrument50
3 Tuning the Instrument53
- Preparing the Instrument for Operation54
- Obtaining an Ion Beam55
  - Introducing the Reference Sample58
- Setting up the Instrument Automatically60
  - Required Material60
- Tuning the Instrument for EI71
  - General Tips for Tuning75
- Tuning the Instrument for Best Resolution in EI76
- Tuning the Instrument for Positive CI77
- Tuning the Instrument for Negative CI82
- Preparing for FI Operation85
- Managing Tune Parameters86
4 Acquiring Data89
- Starting Data Acquisition90
  - Starting a Single Sample Acquisition90
  - Starting a Multiple-Sample Data Acquisition93
- Setting up an MS Method93
- Setting up an MS Scan100
  - Types of Data Acquisition102
- Setting up DRE Mode103
5 Calibration107
- Calibrating the Instrument108
  - Setting up the Instrument for Calibration108
  - Lock Mass Correction109
- Using the Calibration Wizard110
  - Accepting a Calibration115
  - Manually Correcting a Calibration117
- Using Calibrations for Subsequent Acquisitions121
- Dynamic External Calibration Temperature Compensation122
  - Setting the DXC Drift Value122
- Calibrating the Instrument in CI124
  - Calibrating the Instrument in CI+ Mode124
- Manual Calibration125
6 The GC Interface134
- Installing the GC Interface135
- Installing the GC Column141
- Configuring the GC and Autosampler143
- Removing the GC Interface143
7 The Direct Insertion Probe145
- Introduction146
- Installing the Probe Insertion Lock146
- Inserting and Removing the DI Probe148
- Controlling the DI Probe Temperature154
8 The Direct Chemical Ionization (DCI) Probe164
- Introduction164
- Installing the Probe Insertion Lock164
- Inserting and Removing the DCI Probe165
- Controlling the DCI Probe Current169
  - Ramping the Probe Current Manually169
  - Ramping the Probe Current Automatically170
9 FI/FD Operation171
- Introduction172
- Preparing the Instrument for FI/FD Operation172
  - Choosing an Emitter for the FI/FD Inner Source172
- Setting-Up for FI/FD Operation173
- Tuning in FI Mode190
  - Introducing the Reference Sample191
  - Obtaining a Beam and Tuning in FI Operation191
- General Considerations for Tuning in FI Mode193
  - Lens Tuning193
- Setting up and Calibrating the Instrument194
- Running Samples196
  - Running MS Samples in GC FI Mode196
  - Using Direct Insertion Probe in FI Mode196
- Tuning in FD Mode197
10 Routine Maintenance205
- Maintenance Schedule206
- Safety and Handling207
- Rotary Pump Oil208
- Rotary Pump Maintenance209
- Foreline Trap Maintenance215
- Reference Reservoir Maintenance220
- EI/CI Inner Source Maintenance222
- FI/FD Inner Source Maintenance236
  - Storing an Emitter236
  - Changing an Emitter237
- EI/CI Outer Source Maintenance239
- FI/FD Outer Source Maintenance246
  - Cleaning the Extraction Rods246
  - Cleaning the Source Ceramic and Focus Plates249
- Checking for Leaks after Source Maintenance252
  - Inspecting the CI Gas Line for Leaks252
- Detector Maintenance254
  - Conditioning the Detector254
  - Setting the Optimum Gain for the Detector256
11 Troubleshooting259
- Spare Parts260
- Safety and Handling260
- System Troubleshooting260
- Component Hardware Troubleshooting261
- Contacting Waters272
A Starting-Up and Shutting-Down the Instrument276
- Starting-Up the Instrument276
- Shutting-Down the Instrument277
B the Masslynx Tune Window279
- Opening the Masslynx Tune Window280
- The Tune Window Toolbar282
- The Tune Window File Menu283
- The Tune Window Ion Mode Menu285
- The Tune Window Vacuum Menu285
- The Tune Window Settings Menu288
- The Tune Window View Menu297
- The Tune Window Wizards Menu298
  - Tuning Using the Instrument Setup Wizard298
  - Calibrating the Instrument Using the Calibration Wizard298
- The Tune Window Tuning Controls299
- The Tune Window Peak Display323
  - Customizing the Peak Display323
- Setting up Nominal Mass325
- Setting up Resolution for Dead Time Correction Manually326
- Dead Time Correction327
- Effects of Saturation on Peak Shape329
C Calibration Reference Information333
- Overview334
- Editing a Calibration Reference File334
- Calibration Reference File334
- Perfluorotripentylamine (FC70_NCI-.Ref337
- DRE Calculation Files338
- Typical Lock Mass Values340
D External Connections342
- Safety Considerations342
- GCT Premier System External Wiring343
- GCT Premier System Vacuum Connections344
E Status Display Vacuum LED346
- Vacuum LED: Displays for Normal Instrument Operation346
- Vacuum LED: Displays for Instrument Faults349
F Performance Specifications352
- Performance Specifications352
- Mass Range352
- Resolution352
- Acquisition Rate352
- GC Sensitivity352
- Mass Accuracy352
- Dynamic Range353
G Theory and Principles of Operation355
- GCT Premier Functionality356
- Ionization Techniques357
General Considerations for Tuning360
Low Mass Cut-Off362
DRE Mode364
Multiple Peak Stitching366
Gain Drop Monitoring367

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