Agilent GC-MSD ChemStation and Instrument Operation

仪器资料 · 发表于 2017-9-18 14:37:45

Volume 1
G1701DA Version D.02.00
Course Number H4043A
Student Manual

内容目录：
MS BASICS AND HARDWARE CONFIGURATION............................................................ 1
WHAT YOU WILL LEARN ........................................................................................................ 2
GC DETECTORS ...................................................................................................................... 3
COMPARISON OF GC DETECTORS............................................................................................. 5
FUNCTIONAL COMPONENTS OF THE MS ................................................................................... 6
INTERFACING THE GC AND MS................................................................................................ 7
INTERFACE OVERVIEW ............................................................................................................ 8
VACUUM PUMPS ................................................................................................................... 10
TURBO PUMP ........................................................................................................................ 11
REASONS FOR VACUUM IN MS............................................................................................... 12
ELECTRON IONIZATION (EI)................................................................................................... 13
POSITIVE CHEMICAL IONIZATION (PCI).................................................................................. 15
NEGATIVE CHEMICAL IONIZATION (NCI) ............................................................................... 16
HOW DOES A QUADRUPOLE MASS FILTER WORK? ................................................................. 18
MASS FILTER FUNCTION........................................................................................................ 19
X-RAY LENS/ELECTRON MULTIPLIER DETECTOR................................................................... 20
HIGH ENERGY DYNODE/ELECTRON MULTIPLIER DETECTOR................................................... 21
A TYPICAL MASS SPECTRUM................................................................................................. 23
SYSTEM HARDWARE OVERVIEW (LANED)............................................................................. 24
BOOTP SOFTWARE................................................................................................................. 25
NETWORKING MSD LOCAL CONTROL PANEL......................................................................... 26
GC-MS CONFIGURATION ...................................................................................................... 28
MS CONFIGURATION............................................................................................................. 29
MS OPTIONS AND DC POLARITY CONFIGURATION ................................................................. 30
GC CONFIGURATION ............................................................................................................. 31
DATA ANALYSIS CONFIGURATION ......................................................................................... 32
NETWORKING INFORMATION ................................................................................................. 34
LAB EXERCISE: MSD INSTRUMENT CONFIGURATION.............................................. 35
INSTRUMENT/SYSTEM CONFIGURATION ................................................................................. 36
MS TUNING........................................................................................................................... 43
WHAT YOU WILL LEARN ...................................................................................................... 44
WHAT DOES TUNING DO? ..................................................................................................... 45
PFTBA - THE TUNING STANDARD ......................................................................................... 46
TUNING PARAMETERS - EI..................................................................................................... 47
PARAMETER RAMPS .............................................................................................................. 49
AMUGAIN AND OFFSET ....................................................................................................... 50
HOW DO AMUGAIN AND OFFSET AFFECT PEAK WIDTHS? .................................................... 51
MASS AXIS CALIBRATION ..................................................................................................... 52
METHODS OF TUNING............................................................................................................ 53
WHY STANDARD SPECTRA TUNE? ......................................................................................... 55
STANDARD SPECTRA TUNE FLOW CHART .............................................................................. 56
STANDARD SPECTRA TUNE REPORT....................................................................................... 57
AUTOTUNE ........................................................................................................................... 60
AUTOTUNE VERSUS STANDARD SPECTRA TUNE...................................................................... 62
AUTOTUNE REPORT............................................................................................................... 63
QUICK TUNE ......................................................................................................................... 66
TARGET TUNE....................................................................................................................... 67
MANUAL TUNE ..................................................................................................................... 68
PERFORMING A MANUAL TUNE.............................................................................................. 69
PERFORMING A MANUAL TUNE (CONTINUED)......................................................................... 70
LAB EXERCISE: TUNING THE MSD................................................................................. 71
TYPES OF TUNE..................................................................................................................... 72
AUTOTUNING THE MSD........................................................................................................ 73
INTERACTIVE (MANUAL) TUNING .......................................................................................... 75
DATA ACQUISITION........................................................................................................... 77
WHAT YOU WILL LEARN ...................................................................................................... 78
WHAT IS A METHOD? ............................................................................................................ 79
SCAN ACQUISITION PRINCIPLES............................................................................................. 80
MASS SPECTRAL DATA IS THREE-DIMENSIONAL .................................................................... 81
TOTAL ION CHROMATOGRAM (TIC)....................................................................................... 82
TIC (CONTINUED) ................................................................................................................. 83
MASS PEAK DETECTION ........................................................................................................ 84
MASS PEAK DETECTION (CONTINUED) ................................................................................... 85
THRESHOLD .......................................................................................................................... 86
THE DIGITAL SCANNING PROCESS ......................................................................................... 87
SPECTRAL TILTING - NUMBER OF SCANS................................................................................ 89
SPECTRAL TILTING - NUMBER OF SCANS (CONTINUED) ........................................................... 90
SPECTRAL TILTING - NUMBER OF SCANS (CONTINUED) ........................................................... 91
SPECTRAL TILTING - NUMBER OF SCANS (CONTINUED) ........................................................... 92
SPECTRAL INTEGRITY............................................................................................................ 93
SELECTED ION MONITORING (SIM) PRINCIPLES ..................................................................... 94
SELECTED ION MONITORING (SIM)........................................................................................ 95
SIM VERSUS SCAN .............................................................................................................. 96
SETTING UP SIM ACQUISITION.............................................................................................. 97
SIM EXPERIMENT ................................................................................................................. 98
COMPARISON OF EXACT AND INTEGER MASS RATIOS ........................................................... 100
9-CARBOXYTHC TMS DERIVATIVE PEAK RATIOS............................................................... 101
SAMPLE RUNS..................................................................................................................... 102
CHOOSING SIM IONS........................................................................................................... 103
CHOOSING SIM IONS - COURSE PROBLEM............................................................................ 104
SYNCHRONOUS SIM/SCAN .................................................................................................. 105
LOW OR HIGH MASS RESOLUTION ....................................................................................... 106
SETTING UP DATA ACQUISITION.................................................................................. 107
WHAT YOU WILL LEARN .................................................................................................... 108
VIEWS - INSTRUMENT CONTROL .......................................................................................... 109
VIEWS - DATA ANALYSIS .................................................................................................... 110
EDITING THE METHOD......................................................................................................... 111
METHOD INFORMATION....................................................................................................... 113
INLET AND INJECTION PARAMETERS .................................................................................... 114
INJECTOR CONTROL ............................................................................................................ 115
VALVES .............................................................................................................................. 116
SPLIT INJECTION MODE ....................................................................................................... 117
SPLITLESS INJECTION MODE ................................................................................................ 118
INLETS - SPLIT INJECTION .................................................................................................... 119
INLETS - SPLITLESS INJECTION............................................................................................. 121
INLETS - PULSED SPLITLESS INJECTION ................................................................................ 122
INLETS - PULSED SPLIT INJECTION ....................................................................................... 124
FLOW BURST INJECTION...................................................................................................... 126
COLUMNS ........................................................................................................................... 127
CHANGING COLUMNS.......................................................................................................... 129
ADDING A NEW COLUMN TO THE INVENTORY ...................................................................... 130
INSTALLING THE COLUMN FOR USE ..................................................................................... 132
OVEN ................................................................................................................................. 133
DETECTORS ........................................................................................................................ 135
SIGNALS ............................................................................................................................. 136
AUXILIARY ......................................................................................................................... 137
RUNTIME ............................................................................................................................ 138
OPTIONS ............................................................................................................................. 139
GC REAL TIME PLOT........................................................................................................... 140
MS TUNE FILE .................................................................................................................... 141
MS SCAN MODE ................................................................................................................. 142
MS SCAN PARAMETERS (SCANNING MASS RANGE) ............................................................... 144
MS SCAN PARAMETERS (THRESHOLD & SAMPLING RATES) ................................................... 145
MS SCAN PARAMETERS (PLOTTING) .................................................................................... 146
MS SIMMODE ................................................................................................................... 147
MS SIMMODE (PARAMETERS)............................................................................................ 148
SCAN AND SIMMODE......................................................................................................... 150
TIMED EVENTS.................................................................................................................... 151
SELECT REPORTS ................................................................................................................ 153
SAVING THE METHOD.......................................................................................................... 154
MSMONITORS.................................................................................................................... 155
MONITOR ALARMS.............................................................................................................. 156
RUNNING THE METHOD AND ACQUIRING DATA.................................................................... 157
REAL TIME DISPLAY ........................................................................................................... 159
LAB EXERCISE: LINEAR VELOCITY............................................................................. 161
DETERMINING THE LINEAR VELOCITY ................................................................................. 162
LAB EXERCISE: SCAN DATA ACQUISITION................................................................ 165
EDITING THE ENTIRE METHOD............................................................................................. 166
ACQUIRING DATA ............................................................................................................... 187
REAL TIME DISPLAY FUNCTIONS ......................................................................................... 188
LAB EXERCISE: SIM EXPERIMENT............................................................................... 189
ION SELECTION ................................................................................................................... 190
TUNE.................................................................................................................................. 192
SIM ACQUISITION PARAMETERS.......................................................................................... 193
ACQUIRING DATA ............................................................................................................... 196
DATA ANALYSIS ................................................................................................................. 197
LAB EXERCISE: SIM.......................................................................................................... 199
SIM ACQUISITION PARAMETERS.......................................................................................... 200
ACQUIRING DATA ............................................................................................................... 202
MAINTENANCE.................................................................................................................. 203
WHAT YOU WILL LEARN .................................................................................................... 204
ROUTINE AND PREVENTIVE MAINTENANCE - GAS CHROMATOGRAPH.................................... 205
CAPILLARY DIRECT COLUMN INSTALL................................................................................. 207
ROUTINE AND PREVENTIVE MAINTENANCE -MASS SELECTIVE DETECTOR............................ 209
EARLY MAINTENANCE FEEDBACK ....................................................................................... 210
GENERAL PREVENTIVE HINTS.............................................................................................. 212
TYPICAL GC-MS PROBLEMS ............................................................................................... 213
TROUBLESHOOTING............................................................................................................. 215
MASS PEAKS OF COMMON CONTAMINANTS ......................................................................... 216
TROUBLESHOOTING VACUUM PROBLEMS............................................................................. 217
DIAGNOSTIC VALUE OF MANUAL TUNE ............................................................................... 218
AIR AND WATER CHECK...................................................................................................... 219
IDENTIFYING A DIRTY SOURCE ............................................................................................ 220
DIAGNOSING FROM TUNE REPORTS...................................................................................... 221
DIAGNOSING FROM TUNE REPORTS (CONTINUED)................................................................. 222
AUTOTUNE WORKSHEET..................................................................................................... 224