Waters Autospec Premier

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5-14 Calibrating the instrument

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Copyright Notice2
Trademarks2
Customer Comments3
Contacting Waters4
Safety Considerations4
Considerations Specific to the Autospec Premier5
Solvent Leakage Hazard5
Flammable Solvents Hazard6
Pinch Hazard7
High Temperature Hazard8
High Voltage Hazard8
Hazards Associated with Removing an Instrument from Service9
High Magnetic Field Hazard10
Safety Advisories10
Operating this Instrument11
Applicable Symbols11
Intended Use of the Autospec Premier11
Calibrating12
Quality-Control12
ISM Classification12
ISM Classification: ISM Group 1 Class a12
EC Authorized Representative13
Table of Contents15
Instrument Description26
Sample Inlet27
GC Sample Introduction27
Probe Sample Introduction28
Vacuum System28
Masslynx Control System29
Controls and Connections on the Front of the Instrument30
A.C. Distribution Panel30
Status Switch Panel32
Controls and Connections on the Top of the Instrument34
Probe Cooling Water Connections34
Gas Flow Valves34
Controls and Connections on the Rear of the Instrument35
Cooling Water Connections36
Magnet Power Connection37
Electrical Power Outlets38
Vacuum Connections39
Gas Inlet Panel40
Soft-Vent Control Panel41
EPC Power Switch42
Tuning the Instrument43
Low Resolution Tuning53
High Resolution Tuning55
Additional Notes Concerning Manual Instrument Tuning60
Ion Energy60
Alpha Slit61
Z4 Restrictor61
Using the Autotune Facility61
Scanning Techniques65
Function Lists and the MS Method Editor65
The MS Method Editor Toolbar67
The Masslynx Experiment File68
Editing the Function List69
Setting the Maximum Retention Time70
Setting up Scanning Functions71
Magnet Scan Function71
Voltage Scan Function74
B/E (Product Ion) Function76
B2/E (Precursor Ion) Function79
Constant Neutral Loss (CNL) Function82
MIKES Scan Function85
NRMS Scan Function86
SIR Function Editors88
The Voltage SIR Function Editor89
The SIR Mass Dialog Box93
The MRM Function Editor94
The MRM Mass Dialog Box97
Example of VSIR Experiment Set up98
Introduction98
Creating the VSIR Function99
Example of MRM Experiment Set up103
Creating the MRM Function103
Applying an Inter-Scan Current in FI Ionization Mode107
Acquiring Data110
Starting Data Acquisition111
Starting Multiple-Sample Data Acquisition from the Masslynx Window113
Automatic Quantification of the Sample List117
Stopping Data Acquisition119
Pausing Data Acquisition120
Monitoring Data Acquisition120
Viewing the Status of an Acquisition120
Viewing a Chromatogram in Real-Time121
Viewing a Spectrum in Real-Time121
Acquiring Analog Data122
Calibrating the Instrument126
Calibration Files126
Calibrating the Instrument for SIR Experiments126
Calibrating the Instrument for MIKES and NRMS Experiments129
Calibrating the Instrument for Scanning Experiments129
Manually Correcting a Calibration131
Editing the Calibration Parameters133
Saving a Calibration136
Applying the Calibration136
Associating a Calibration File with an Experiment137
Inlets and Probes140
The GC Interface140
Installing the GC Column141
Required Materials141
The Solids Sample Introduction Probe142
Making the Probe Cooling Water Connections143
Fitting the Probe Tip to the Probe144
Loading Sample into the Sample Cup144
Fitting the Sample Cup to the Probe Tip146
Removing the Sample Cup from the Probe Tip147
Inserting the Solids Sample Introduction Probe in the Ion Source147
Removing the Probe from the Ion Source151
Ramping the Probe Temperature152
The Probe Control Dialog Box's Options Tab152
The Probe Control Dialog Box's Ramps Tab154
The Probe Control Dialog Box's Control Tab156
Routine Maintenance159
Maintenance Schedule159
Safety and Handling160
Vacuum Pump Maintenance161
GC Interface Maintenance161
Source Maintenance163
Inner Source Chamber Assembly Maintenance164
Required Materials167
Withdrawing the Inner Source Chamber Assembly from the Source168
Removing the Chamber Assembly from the Source Handle172
Disassembling the Chamber Assembly173
Cleaning Ion Burn from the Inner Source Chamber Assembly Components179
Ultrasonically Cleaning the Chamber Assembly Components181
Assembling the Inner Source Chamber Assembly182
Fitting the Inner Source Chamber Assembly to the Source Handle190
Inserting the Inner Source Chamber Assembly into the Outer Source191
Degassing the Ion Source Assembly195
Outer Source Maintenance196
Required Materials197
Removing the Outer Source Assembly from the Instrument198
Disassembling the Outer Source200
Disassembling the Re-Entrant Coupling Mechanism214
Disassembling the Probe Contact Assembly214
Disassembling the Inner Source Contact Support Assembly216
Disassembling the Ion Chamber218
Disassembling the Contact Rail Assemblies220
Cleaning Ion Burn from the Outer Source Assembly Components222
Ultrasonically Cleaning the Outer Source Assembly Components223
Assembling the Re-Entrant Coupling Mechanism224
Assembling the Probe Contact Assembly224
Assembling the Inner Source Contact Support Assembly225
Assembling the Ion Chamber226
Assembling the Contact Rail Assemblies230
Assembling the Outer Source Assembly231
Fitting the Outer Source Assembly to the Instrument237
Changing an Analyzer Ion Gauge238
Measuring EI Sensitivity from the Solids Probe240
Troubleshooting247
Spare Parts247
Safety and Handling247
System Troubleshooting248
Component Hardware Troubleshooting248
Poor Peak Shape252
Contacting Waters252
A Safety Advisories254
Warning Symbols254
Task-Specific Hazard Warnings254
Warnings that Apply to Particular Instruments, Instrument Components, and Sample Types255
Burst Warning255
Mass Spectrometer Flammable Solvents Warning255
Mass Spectrometer Shock Hazard256
Biohazard Warning256
Chemical Hazard Warning257
Caution Symbol257
Warnings that Apply to All Waters Instruments257
Electrical and Handling Symbols260
Electrical Symbols260
Handling Symbols261
Preventing Contamination263
Items Exposed to Solvent263
Solvents Used to Prepare Mobile Phases265
Starting up the Instrument267
Shutting down the Instrument272
D the Masslynx Tune Window275
Opening the Masslynx Tune Window275
The Tune Window File Menu276
The Tune Window Edit Menu277
The Tune Window Ion Mode Menu277
The Tune Window Vacuum Menu278
Monitoring the Instrument Vacuum278
Controlling and Monitoring the Vacuum Pumps279
Controlling Flight Tube Baking283
The Tune Window Inlet Menu285
The Tune Window Options Menu285
Controlling the Display of Readback Windows286
Viewing the Status of the Current Scan286
Setting up the Instrument287
The Instrument Setup Dialog Box's Magnet Tab287
The Magnet Constant Utility Dialog Box288
The Instrument Setup Dialog Box's Limits Tab290
The Instrument Setup Dialog Box's y Focus Tab291
The Instrument Set up Dialog Box Slits Tab293
To Perform an Experiment Calibration294
The Select Peaks of Interest Dialog Box297
Verifying VSIR Experimental Resolution298
Ramping the Probe Temperature300
The Linked Scanning Utility300
Configuring the Magnet and MIKES and NMRS Options302
Viewing the Status Of, and Rebooting, the Instrument's Embedded PC302
Selecting the Instrument Name302
Customizing the Tune Window303
The Tune Window Toolbar303
The Tune Window Tuning Controls305
The Source Tab305
The EI Source Tab Parameters306
The CI Source Tab Parameters307
The LSIMS Source Tab Parameters308
The FI Source Tab Parameters309
The Lenses 1 Tab Parameters (for Analyzer Intensity310
The Lenses 2 Tab Parameters (for Analyzer Resolution311
The Inlets Tab312
The AGHIS Tab Parameters314
The Tune Window Instrument Controls315
The Control 1 Tab Parameters315
Specifying the Accelerating V Value316
The Control 2 Tab Parameters and Controls317
The Vacuum Tab318
The Linked Scanning Tab319
The MIKES And/Or NRMS Tab320
The Tune Window Peak Display321
Customizing the Peak Display321
Opening the Peak Display Menu321
Customizing the Colors and Numbers of Displayed Traces322
Customizing the Peak Trace Line Appearance323
Customizing the Peak Intensity Display323
Customizing the Tune Window Peak Display Toolbar324
Overview329
Editing a Calibration Reference File329
Calibration Reference Files330
F Performance Specifications and File Types334
Performance Specifications334
File Types334
Electron Impact (EI) Ionization335
Chemical Ionization336
Autospec Functionality336
Source Assembly337
Source Focus 1 and Focus 2 Lenses337
Beam Center Lens337
Z Deflect 1 Lens337
First Field-Free Region Gas Cell337
Source Slit339
Y Deflect 1 Lens339
Alpha Slit339
Y Focus Lens339
First ESA Assembly (ESA 1339
Z Focus 2 Lens Assembly339
Z Deflect 2 Lens340
Z Focus 2 Lens340
Rotate 2 Lens340
Curve 2 Lens340
Magnet340
Z Focus 3 Lens Assembly340
Curve 3 Lens340
Rotate 3 Lens341
Z Deflect 3 Lens341
Z Focus 3 Lens341
NRMS Gas Cell (Optional341
MIKES Gas Cell (Optional341
MIKES Slit (Optional341
Second ESA Assembly (ESA 2341
Collector Slit Plate Assembly342
Z Restrictor 4 Plate342
Rotate 4 Lens342
Collector Slit342
Dual Ion Detector343
H File Types346
File Types346

Waters Autospec Premier - Page 138

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