Read h4043a vol1 student.pdf text version

Agilent GC-MSD ChemStation and Instrument Operation

Volume 1 G1701DA Version D.02.00 Course Number H4043A

Student Manual

Agilent GC-MSD ChemStation and Instrument Operation

Volume 1 G1701DA Version D.02.00 Course Number H4043A

Student Manual

Manual Part Number H4043-90000 Printed in the USA August, 2005

Notice

The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental, or consequential damages in connection with the furnishing, performance, or use of this material. No part of this document may be photocopied or reproduced, or translated to another program language without the prior written consent of Agilent Technologies, Inc. Agilent Technologies, Inc 11575 Great Oaks Way Suite 100, MS 304B Alpharetta, GA 30319

© 2000, 2005 by Agilent Technologies, Inc. All rights reserved Printed in the United States of America

ii

Table Of Contents

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 T UNING STANDARD ......................................................................................... 46 TUNING PARAMETERS - EI..................................................................................................... 47 PARAMETER RAMPS .............................................................................................................. 49 AMU GAIN AND OFFSET ....................................................................................................... 50 HOW DO AMU GAIN 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

iii

MANUAL T UNE ..................................................................................................................... 68 PERFORMING A MANUAL T UNE.............................................................................................. 69 PERFORMING A MANUAL T UNE (CONTINUED)......................................................................... 70 LAB EXERCISE: TUNING THE MSD ................................................................................. 71 TYPES OF T UNE ..................................................................................................................... 72 AUTOTUNING THE MSD ........................................................................................................ 73 INTERACTIVE (MANUAL) T UNING .......................................................................................... 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 E XACT 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

iv

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 SIM MODE ................................................................................................................... 147 MS SIM MODE (PARAMETERS)............................................................................................ 148 SCAN AND SIM MODE ......................................................................................................... 150 TIMED EVENTS.................................................................................................................... 151 SELECT REPORTS ................................................................................................................ 153 SAVING THE METHOD.......................................................................................................... 154 MS MONITORS .................................................................................................................... 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 T UNE ............................................................................... 218

v

AIR AND WATER CHECK...................................................................................................... 219 IDENTIFYING A DIRTY SOURCE ............................................................................................ 220 DIAGNOSING FROM T UNE REPORTS ...................................................................................... 221 DIAGNOSING FROM T UNE REPORTS (CONTINUED)................................................................. 222 AUTOTUNE WORKSHEET ..................................................................................................... 224

vi

Information

h4043a vol1 student.pdf

8 pages

Find more like this

Report File (DMCA)

Our content is added by our users. We aim to remove reported files within 1 working day. Please use this link to notify us:

Report this file as copyright or inappropriate

345530


You might also be interested in

BETA
5954-8364_11_29_01