Agilent 7500 Inductively Coupled Plasma Mass Spectrometry英文版_407页.pdf

Agilent 7500 Inductively Coupled Plasma Mass Spectrometry Course Number H8974A ChemStation Revision 01.XX NT Operating System Student Manual Revision 1 Gas Chromatography Liquid Chromatography Mass Spectrometry Capillary ElectrophoresisData Systems Manual Part Number H8974-90000 Printed in the USA January,2001 Agilent 7500 Inductively Coupled Plasma Mass Spectrometry Course Number H8974A ChemStation Revision 01.XX NT Operating System Student Manual Revision 1 ii 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 by Agilent Technologies,Inc.All rights reserved Printed in the United States of America iii Table Of Contents INTRODUCTION:ELEMENTAL ANALYSIS.1 ATOMIC SPECTROMETRY.2 ATOMIC MASS AND WEIGHT.3 ISOTOPES AND ISOBARS.4 ANALYTICAL TECHNIQUES FOR ELEMENTAL ANALYSIS.5 ELEMENTAL ANALYSIS:FAAS.6 ELEMENTAL ANALYSIS:GFAAS.7 ELEMENTAL ANALYSIS:ICP-OES.8 ELEMENTAL ANALYSIS:ICP-MS.9 COMPARISON OF ELEMENTAL TECHNIQUES.10 GRAPHICAL COMPARISON OF ELEMENTAL TECHNIQUES.11 COMPARISON OF THE COMPLEXITY OF MULTI-ELEMENTAL TECHNIQUES.12 USERS/APPLICATIONS OF ICP-MS.13 MULTI-ELEMENTAL ANALYSIS OF METALS.14 INTRODUCTION:INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY.15 WHAT IS ICP-MS?.16 ADVANTAGES OF ICP-MS.17 AGILENT TECHNOLOGIES AND ICP-MS.18 PROCESSES IN ICP-MS.19 OVERVIEW OF AGILENT 7500 FEATURES.20 SCHEMATIC DIAGRAM OF AGILENT 7500A.21 SCHEMATIC DIAGRAM OF AGILENT 7500S.23 ISIS FOR APPLICATION FLEXIBILITY.24 SAMPLE INTRODUCTION.25 AGILENT 7500 SAMPLE INTRODUCTION.26 AUTOSAMPLERS.27 TYPICAL NEBULIZER.28 SPECIALIZED SAMPLE INTRODUCTION SYSTEMS.29 TYPICAL SPRAY CHAMBER DOUBLE PASS.30 DROPLET DISTRIBUTION WITH AND WITHOUT SPRAY CHAMBER.31 NEW DESIGN AGILENT ICP TORCH BOX.32 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY.33 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY(CONTINUED).34 WHY ARGON?.35 DISTRIBUTION OF IONS IN THE PLASMA.36 SAMPLE IONIZATION IN THE PLASMA.37 FULL MASS CONTROL OF ALL GAS FLOWS.38 INTERFACE.39 AGILENT 7500 ION LENS SYSTEM.40 DISTRIBUTION OF IONS AND ELECTRONS AROUND THE INTERFACE.41 ION ENERGY DISTRIBUTION IN THE INTERFACE.42 THE ELECTROSTATIC LENSES.43 WHY“OFF-AXIS”?.44 LOW TRANSMISSION PHOTON STOP SYSTEM.45 AGILENT HIGH TRANSMISSION OFF-AXIS SYSTEM.46 ION FOCUSING NEW OMEGA II LENS.47 FLAT RESPONSE CURVE HIGH SENSITIVITY AT ALL MASSES.48 AGILENT 7500 QUADRUPOLE.49 iv RESOLUTION AND ABUNDANCE SENSITIVITY.50 NEW SIMULTANEOUS DUAL MODE DETECTOR&HIGH SPEED LOG AMPLIFIER TRUE 9 ORDER DYNAMIC RANGE.51 THE DETECTOR.52 INTERFERENCES IN ICP-MS.53 INTERFERENCES IN ICP-MS.54 MASS SPECTROSCOPIC INTERFERENCES.55 ISOBARIC INTERFERENCES.56 POLYATOMIC INTERFERENCES.57 MASS SPECTROSCOPIC INTERFERENCES.58 OPTIMIZING TO MINIMIZE INTERFERENCE FORMATION IN THE PLASMA 1.59 OPTIMIZING TO MINIMIZE INTERFERENCE FORMATION IN THE PLASMA 2.60 OPTIMIZING TO MINIMIZE INTERFERENCE FORMATION IN THE PLASMA 3.61 EFFECT OF PLASMA TEMPERATURE ON DEGREE OF IONIZATION.62 EFFICIENT AEROSOL DECOMPOSITION.63 OXIDES AND DOUBLY CHARGED IONS.64 DEALING WITH MASS SPECTROSCOPIC INTERFERENCES.65 INTERFERENCE EQUATIONS.66 AS INTERFERENCE CORRECTION.67 INTERFERENCE CORRECTION EQUATIONS-AGILENT 7500.68 NON-SPECTROSCOPIC INTERFERENCES.69 EFFECT OF HIGH DISSOLVED SOLIDS.70 FIRST IONIZATION POTENTIAL.71 IONIZATION EFFICIENCY.72 SIGNAL SUPPRESSION.73 MATRIX EFFECTS ON LOW MASS ANALYTE.74 MATRIX EFFECTS ON MEDIUM MASS ANALYTE.75 MATRIX EFFECTS ON HIGH MASS ANALYTE.76 SPACE CHARGE INTERFACE AND LENS REGION.77 IONIZATION SUPPRESSION PLASMA REGION.78 WHAT CAN BE DONE ABOUT MATRIX EFFECTS.79 TUNING THE AGILENT 7500.81 WHY TUNE THE ICP-MS?.82 TUNING PROCEDURE OVERVIEW.83 AGILENT 7500 ICP-MS MANUAL TUNE CHECKLIST 1.84 AGILENT 7500 ICP-MS MANUAL TUNE CHECKLIST 2.85 AUTOTUNE SCREEN.86 AUTOTUNING OF ICP TORCH POSITION AND NEW TARGET TUNE.87 FEATURES OF AUTOTUNE(1).88 FEATURES OF AUTOTUNE(2).89 CHOOSING THE AUTOTUNE MODE.90 BASICS OF THE SOFT EXTRACTION MODE.91 COMPARISON OF EXTRACTION MODES SETTINGS.92 AUTOTUNE-TARGET SETTING.93 TARGET SETTING-RANGE SETTING.94 SENSITIVITY TUNING.95 PEAK SHAPE AND RESOLUTION.96 ABUNDANCE SENSITIVITY.97 QUADRUPOLE MASS FILTER-SCAN LINE.98 DETECTION LIMITS IN NORMAL MODE.99 DETECTION LIMITS IN SOFT EXTRACTION MODE.100 LOW BECS IN SOFT EXTRACTION MODE.101 PULSE/ANALOG(P/A)TUNING.102 v MAINTENANCE OF THE AGILENT 7500.103 MAINTENANCE SCHEDULE.104 RUNNING TIME MAINTENANCE SCREEN.105 EARLY MAINTENANCE FEEDBACK(EMF).106 NORMAL MAINTENANCE OF THE SAMPLE INTRODUCTION SYSTEM.107 OVERNIGHT CLEANING OF THE SAMPLE INTRODUCTION SYSTEM.108 SAMPLE INTRODUCTION MAINTENANCE.109 NEBULIZER CONNECTIONS.110 MAINTENANCE OF A BABINGTON NEBULIZER.111 TORCH MAINTENANCE.112 INTERFACE MAINTENANCE.113 MAINTENANCE OF THE CONES.114 EXTRACTION LENSES MAINTENANCE.115 EXTRACTION LENSES.116 CLEANING OF THE EINZEL LENS AND OMEGA LENS ASSEMBLY.117 INSTRUMENT SHUTDOWN.118 REMOVAL OF THE EINZEL LENS-OMEGA LENS ASSEMBLY.119 EXPANDED VIEW OF EINZEL LENS-OMEGA LENS ASSEMBLY.120 PLATE BIAS LENS.121 PENNING GAUGE.122 ROTARY PUMP MAINTENANCE.123 CHANGING ROTARY PUMP OIL.124 MAINTENANCE LOGBOOK SETTING.125 MAINTENANCE LOGBOOK.126 SAMPLE INTRODUCTION MAINTENANCE.127 AIR FILTERS MAINTENANCE.128 INSTRUMENT START-UP.129 INTERNAL STANDARDIZATION IN ICP-MS.131 THE ROLE OF INTERNAL STANDARDS.132 HOW THE INTERNAL STANDARDS WORK-1.133 HOW THE INTERNAL STANDARDS WORK-2.134 CHOICE OF THE INTERNAL STANDARD.135 CONCENTRATION OF INTERNAL STANDARDS.136 ON-LINE ADDITION OF INTERNAL STANDARDS.137 SAMPLE PREPARATION TECHNIQUES FOR ICP-MS.139 CONTAMINATION.140 TYPES OF CONTAMINATION.141 CHALLENGES OF TRACE ANALYSIS.142 WHEN A CONTAMINATION CAN OCCUR.143 REAGENTS.144 WATER-MILLIPORE.145 NITRIC ACID.146 SELECTED METHODS OF SAMPLE PREPARATION.147 COMMONLY USED REAGENTS(1).148 COMMONLY USED REAGENTS(2).149 COMMONLY USED REAGENTS(3).150 SEMI-QUANTITATIVE ANALYSIS OF SAMPLES.151 SEMI-QUANTITATIVE ANALYSIS.152 WHAT IS SEMI-QUANTITATIVE ANALYSIS?.153 DATA ACQUISITION.154 METHOD SET-UP FOR SEMI-QUANTITATIVE ANALYSIS.155 PARAMETERS SELECTION-SPECTRUM ACQUISITION.156 vi PARAMETERS SELECTION-SELECTION OF MASSES.157 MORE ACQUISITION PARAMETERS.158 REPORT GENERATION.159 SEMI-QUANT PARAMETERS.160 SEMI-QUANTITATIVE DATA ANALYSIS.161 EDITING PARAMETERS.162 DAILY UPDATE OF THE SEMI-QUANT PARAMETERS.163 INTERNAL STANDARD CORRECTION FOR OFF-LINE INTERNAL STANDARD ADDITION.164 INTERNAL STANDARD CORRECTION FOR ON-LINE INTERNAL STANDARD ADDITION.165 EXAMPLE OF SEMI-QUANT REPORT 1.166 EXAMPLE OF SEMI-QUANT REPORT 2.167 GENERATING A SEMI-QUANT REPORT.168 MANUAL VERIFICATION OF THE DATA.169 QUANTITATIVE ANALYSIS OF SAMPLES.171 WHAT IS QUANTITATIVE ANALYSIS?.172 METHOD SET-UP FOR QUANTITATIVE ANALYSIS.173 STEP ONE:EDITING THE AMU SELECT FILE.174 EDITING A METHOD FOR QUANTITATIVE ANALYSIS.175 METHOD INFORMATION.176 ACQUISITION MODES.177 ACQUISITION PARAMETERS-MULTITUNE METHOD.179 PERIODIC TABLE.180 MASS TABLE.181 PERISTALTIC PUMP PROGRAM.182 RAW DATA CORRECTIONS.183 CONFIGURE REPORTS.184 CALIBRATION.185 CALIBRATION TABLE.186 SAVE THE CALIBRATION AND THE METHOD.187 QUANTITATIVE DATA ANALYSIS.188 STANDARD DATA FILES.189 CALIBRATION CURVES.190 EXAMPLES OF THE CALIBRATION CURVES FOR“EXCLUDED”.191 SIMPLE SEQUENCING(INTELLIGENT SEQUENCING DISABLED).193 SEQUENCING.194 ASX-500 VIAL POSITION NOMENCLATURE.195 SEQUENCING.196 SAMPLE LOG TABLE-SEQUENCE FLOW AND PERIODIC BLOCK.197 SAMPLE LOG TABLE.198 SPECIAL FEATURES-KEYWORDS.199 RUNNING A SEQUENCE.200 CHAINED SEQUENCE.201 CHAINED SEQUENCE.202 METHOD OF STANDARD ADDITIONS(MSA).203 EXTERNAL CALIBRATION.204 PROS AND CONS OF EXTERNAL CALIBRATION.205 METHOD OF STANDARD ADDITION(MSA).206 PROS AND CONS OF METHOD OF STANDARD ADDITIONS.207 DETERMINATION OF URANIUM IN URINE BY MSA.208 CONVERTING FROM MSA TO EXTERNAL CALIBRATION.209 MATRIX-MATCHED URANIUM IN URINE EXTERNAL CALIBRATION.210 OFF-LINE DATA ANALYSIS AND SEQUENCE REPROCESSING.211 vii OFF-LINE DATA ANALYSIS.212 PROCEDURE FOR OFF-LINE DATA ANALYSIS.213 OFF-LINE CALIBRATION REVIEW OF CURRENTLY RUNNING METHOD.214 USING DOLIST FOR OFF-LINE DATA REPROCESSING.215 HOW TO USE DOLIST.216 SELECTING FILES USING DOLIST.217 SEQUENCE-REPROCESSING DATA BATCH.218 SEQUENCE REPROCESSING.219 CUSTOM REPORTS AND DATABASES.221 WHAT YOU WILL LEARN.222 CUSTOM REPORTS AND DATABASES.223 CREATING AND EDITING A REPORT TEMPLATE.224 CUSTOM REPORTS-REPORT WIZARD.225 CUSTOM REPORTS-DRAG AND DROP(1).227 CUSTOM REPORTS-DRAG AND DROP(2).228 FORMATTING CUSTOM REPORTS.229 CUSTOM REPORTS-PRINTING SET-UP.230 CUSTOM REPORTS-SAVING THE TEMPLATE.231 PRINTING CUSTOM REPORTS-INTERACTIVELY.232 PRINTING CUSTOM REPORTS-PRINTING MULTIPLE FILES 1.233 PRINTING CUSTOM REPORTS-PRINTING MULTIPLE FILES 2.234 DATABASES.235 DATABASE WIZARD.236 DATABASE-DRAG AND DROP.237 DATABASE-FORMATTING.238 DATABASE-CHARTS.239 GLOBAL CHART OPTIONS.240 DATABASE-SAVING.242 UPDATING THE DATABASE-INTERACTIVELY.243 UPDATE THE DATABASE-MULTIPLE FILES 1.244 UPDATE THE DATABASE-MULTIPLE FILES 2.245 ISOTOPE RATIO MEASUREMENTS.247 EDITING A METHOD FOR QUANTITATIVE ANALYSIS.248 ACQUISITION MODES.249 ACQUISITION PARAMETERS FOR ISOTOPIC RATIO MEASUREMENTS.251 REPORT SELECTION.252 SETTING PARAMETERS FOR ISOTOPIC RATIOS.253 EXAMPLE OF THE ISOTOPIC RATIO REPORT.254 AGILENT ICP-MS CHEMSTATION AND WINDOWS OVERVIEW.255 THE WINDOWS INTERFACE.256 WINDOWS MENUS.257 USEFUL WINDOWS TIPS.258 MAINTAINING THE COMPUTER SYSTEM.259 WINDOWS NT EXPLORER-ENHANCED FILE MANAGEMENT.260 DIRECTORY STRUCTURE OF THE AGILENT CHEMSTATION.261 FILE NAMING.262 CHEMSTATION FILE EXTENSIONS.263 AN OVERVIEW OF ICP-MS ENVIRONMENTAL APPLICATIONS.265 OPTIMIZING AGILENT 7500 FOR ENVIRONMENTAL SAMPLES ANALYSIS.266 ENVIRONMENTAL TUNING.267 THREE GOALS OF ENVIRONMENTAL TUNING.269 TUNING FLOW CHART.271 viii RECOMMENDATIONS ON INTERFERENCE EQUATIONS.272 MORE INTERFERENCE CORRECTIONS.274 CALIBRATION STANDARDS.276 LINEAR RANGE DETERMINATION.277 INTERFERENCE CHECK SAMPLES.278 TROUBLESHOOTING ENVIRONMENTAL APPLICATIONS 1.279 TROUBLESHOOTING ENVIRONMENTAL APPLICATIONS 2.281 TROUBLESHOOTING ENVIRONMENTAL APPLICATIONS 3.283 TROUBLESHOOTING ENVIRONMENTAL APPLICATIONS 4.285 SEMICONDUCTOR APPLICATIONS OF ICP-MS AND ADVANTAGES OF AGILENT 7500S SYSTEM.287 CHEMICALS AND MATERIALS USED IN SEMICONDUCTOR INDUSTRY.288 METALS ANALYSIS IN THE SEMICONDUCTOR INDUSTRY-CUSTOMER GROUPS AND REQUIREMENTS.289 SHIELDTORCH INTERFACE.290 SHIELDTORCH INTERFACE.291 NORMAL AND“COOL”PLASMAS.292 SHIELD TORCH“COOL PLASMA”.293 SHIELD TORCH INSTALLATION.294 COOL PLASMA TUNING.295 ADVANTAGES OF COOL PLASMA AT HIGHER POWER(900-1100 W).296 ADVANTAGES OF COOL PLASMA AT LOWER POWER(700-800 W).297 DETECTION LIMITS STUDY 1.298 DETECTION LIMITS STUDY 2.299 AUTOMATIC SWITCHING BETWEEN NORMAL AND COOL PLASMA.300 INTELLIGENT SEQUENCE TRAINING TEXT.301 WHAT IS INTELLIGENT SEQUENCE?.302 TYPICAL ANALYTICAL FLOW.303 USING INTELLIGENT SEQUENCING.304 SETTING UP A QC CONFIGURATION.319 LABORATORY 1:AGILENT 7500 CONFIGURATION,STARTUP AND TUNING.327 CONFIGURATION.328 STARTUP AND TUNING.329 AGILENT 7500 STARTUP CHECKLIST.330 SHUTDOWN CHECKLIST.331 LABORATORY 2:AGILENT 7500 ROUTINE MAINTENANCE.333 GENERAL.334 SAMPLE INTRODUCTION.335 INTERFACE.336 NEBULIZER,SPRAY CHAMBER AND TORCH.337 RE-IGNITE THE PLASMA AND CHECK THE TUNE.338 LABORATORY 3:SEMI-QUANTITATIVE ANALYSIS.339 SEMI-QUANTITATIVE ANALYSIS.340 LABORATORY 4:QUANTITATIVE ANALYSIS OF UNKNOWN SAMPLE.341 QUANTITATIVE ANALYSIS.342 APPENDIX 1 GENERAL INFORMATION.343 PROFESSIONAL ORGANIZATIONS.344 JOURNALS.345 SELECTED WEB SITES(1).346 ix SELECTED WEB SITES(2).347 APPENDIX 2 FLOW CHATS.349 MANUAL TUNE TROUBLESHOOTING FLOWCHART 1.350 MANUAL TUNE TROUBLESHOOTING FLOWCHART 2.351 APPENDIX 3 DEALING WITH POLYATOMICS.353 THE PROBLEM.354 STRATEGY#1:(HIGH POWER)COOL PLASMA ANALYSIS.355 COMMERCIALIZATION OF COOL PLASMA ANALYSIS.356 SCHEMATIC OF AGILENT SHIELDTORCH.357 NOT ALL COOL PLASMAS*ARE THE SAME!1.358 NOT ALL COOL PLASMAS*ARE THE SAME!2.359 FE IN 31%H2O2-5 PPT SPIKE RECOVERY.360 SHIELDTORCH TECHNOLOGY ELIMINATES INTERFERENCES BEFORE THEY FORM!.361 CAN HEAVY MATRICES BE ANALYZED?.362 CR IN UNDILUTED METHANOL.363 EXAMPLE OF HEAVY MATRIX ANALYSIS.364 CALIBRATION FOR 56FE IN 1000 PPM PT.365 CALIBRATION FOR 66ZN IN 1000 PPM PT.366 DETERMINATION OF SE BY HIGH POWER COOL PLASMA.367 SPECTRUM OF 10 PPB SE AND BLANK.368 CALIBRATION FOR 80SE.369 DETECTION LIMITS FOR SE BY COOL PLASMA.370 CURRENT RESEARCH DEVELOPMENTS USING THE SHIELDTORCH.371 AS CALIBRATION IN 10%HCL.372 LOW LEVEL P CALIBRATION.373 LOW LEVEL S CALIBRATION.374 LOW LEVEL SI CALIBRATION.375 STRATEGY#2:RESOLVE THE INTERFERENCES.376 LIMITATIONS OF HR-ICP-MS.377 RESOLUTION VS.SENSITIVITY.378 OTHER FACTS ABOUT HR-ICP-MS 1.379 OTHER FACTS ABOUT HR-ICP-MS 2.380 OTHER FACTS ABOUT HR-ICP-MS 3.381 STRATEGY#3:DISSOCIATE INTERFERENCES WITHIN THE SPECTROMETER.382 PRINCIPLE OF COLLISION TECHNOLOGY.383 SELECTING A GAS PHASE REAGENT.384 OPTIMIZING THE GAS PHASE REAGENT.385 SIDE REACTIONS ARE INEVITABLE!.386 SIDE REACTIONS CREATE NEW INTERFERENCES.387 HYDROCARBONS ARE PARTICULARLY PRONE TO COMPLEX CHEMISTRIES EVEN AT TRACE LEVELS.388 EFFECTS OF SAMPLE MATRIX.389 STRATEGIES TO OVERCOME THE PROBLEM OF SIDE REACTIONS.390 LIMITATION OF SCANNING THE ANALYZER QUAD.391 COLLISION CELLS CAN CREATE INTERFERENCES.392 IN SUMMARY.393 x Introduction:Elemental Analysis Introduction:Elemental Analysis Atomic Spectrometry 2 Atomic Spectrometry Atomic Spectrometry-GroundStateExcitedState-Light of specific characteristic wavelength is absorbed by promoting an electron to a higher energy level(excitation)Light absorption is proportional toelemental concentrationLight of specific wavelengthfrom Hollow Cathode Lamp(HCL)High energy(light and heat)promotes an electron to a higher energy level(excitation).Electron falls back and emits light at characteristic wavelengthLight emission is proportional toelemental concentrationHigh energy(light and heat)ejects electron from shell(ionization).Result is free electron and atom with positive charge(Ion)Ions are extracted and measured directly in mass spectrometerLight and heat energy from high intensity source(plasma)Light and heat energy from high intensity source(flame or plasma)Atomic AbsorptionAtomic EmissionMass Spectrometry Figure 1 Introduction:Elemental Analysis Atomic Mass and Weight 3 Atomic Mass and Weight Atomic Mass and Weight1840 Electrons+-1 Proton1 Neutron+1 Proton+-ElectronProtonNeutronNucleusElectron shell or cloudAtomic number of an element is the number of Proto