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1、氣相層析質譜儀GC/MS,美商亞洲瓦里安科技(股)公司,GC基本原理MS基本原理數據處理 定性&定量MS Tuning 與 日常保養應用,GC基本原理,GC 基本組件,Injector-Capillary InjectorColumn-CapillaryDetector-MassRecorder-Computer,GC 簡圖,Capillary GC Review,Universal or Selective GC Detectors,Universal DetectorsFlame Ionization Detector(FID)for Hydrocarbon Compounds Therm
2、al Conductivity Detector(TCD)Selective DetectorsElectron Capture Detector(ECD)Pulsed Flame Photometric Detector(PFPD)Thermionic Specific Detector(TSD),Information From GC,QualitationRetention TimeSame compound has the same R.T.under the same GC conditions.QuantitationPeak AreaPeak Height,MS基本原理,The
3、Basic Principle of Mass Spectrometry,M,Ionization,Mass Analyzer,Ion Detection,CH3-CH2-CH2-CH3,The Basic Principle of Mass Spectrometry,CH3-CH2-CH2-CH3CH3-CH2-CH2-CH3CH3-CH2-CH2-CH3,-e,m/z 58,m/z 43,m/z 29,Mass Spectrometry,Inlet SystemsGC,LC,Direct Probe Inlet.Ion SourceEI,CIMass AnalyzerMagnetic Se
4、ctor,The Quadrupole Ion Trap.DetectorElectron Multiplier.,Ionization:Electron Impact,M+.,m/z 15,m/z 57,m/z 27,m/z 43,m/z 29,Ionization:Chemical Ionization,CH4+e-CH4+2e-CH4+CH4 CH3+CH5+CH5+M CH4+(MH)+CH4:CI gasM:Analyte,Electron Impact&Chemical Ionization,Mass Analyzer:Magnetic Sector,Mass Analyzer:E
5、xternal Source/Quadrupole,Mass Analyzer:The Quadrupole Ion Trap,Top endcap,Bottom Endcap,Ring Electrode,GC column inlet,Filament assembly,Ion MultiplierDetector,Fo,Ion Detection:Electron Multiplier,Sn/SnO or Pb/PbO doped glass funnel Shower of electrons is released when an ion strikes the wallThe am
6、plified ion current is sent to the electronic circuit and converted to a voltage signal105107gain,Discrete Dynode Electron Multiplier,Ion beam,slit,electrons,To amplifier,Continuous Dynode Electron Multiplier,Cascade of electrons,Resistive conductive surface,To amplifier,-2kV,GC&Mass,When MS Becomes
7、 a GC Detector,GC/MS Can Provide More Information,Retention TimeMass Spectra of Each CompoundLibrary SearchCompound IdentificationStructure InformationQuantitationRTICCQuantitation Ion,數據處理,Data Process,QualitationBackground SubstractIdentification of Coelution PeakLibrary SearchQuantitationBuild Ca
8、libration CurveSample Analysis,定性,Reconstructed Total Ion Current Chromatography,Reconstructed Total Ion Current Chromatography,RTICC&Quantitation Ion,180,109,定性,Background Correction,Background Correction,A,B,A:Before Background CorrectionB:After Background Correction,Identification of Coelution Pe
9、ak,MS Library,Commercial Available Library(70 eV)NISTWiley LibraryWeber Drug and Pesticide LibraryUser LibraryUser Can Create Library by their own MSRequire reliable,tunable MS to produce reproducible Mass Spectra,Library Search Algorithm,Step I:Data Reduction Step II:PresearchStep III:Main Search W
10、ith Full Spectrafit reverse fitpurity,Library Search,Sample,Reference,Difference,Search Result,Compound Identification:Structure Information From MS,Molecular Ion Formation Molecular Fragmentation,C6H5-CH2CH3+e-C6H5-CH2CH3+(m/z 106)+2 e-C6H5-CH2CH3+e-C6H5-CH2+(m/z 91)C6H5-CH2CH3+e-C6H5+(m/z 77),Comp
11、ound Identification,Structure,Mass Spectra,Name,定量,Quantitation:Preparation of Calibration File,Prepare Reference StandardsAcquire Data Files for Each StandardsIdentify Compounds and Retention TimesBuild Calibration FileAdd Points to Calibration FilesExamine and Edit Calibration File,Quantitation,Ex
12、ternal StandardInternal Standard,Quantitation By GC/MS,Single point Calibration,External Standard Quantitation,Internal Standard Quantitation,Compound Table,SatView,Build Compound Table,Compound Table,R.T.Compound NameQuantum Ion,Edit Method,Calibration SetupCompound TableResults Treatment,Calibrati
13、on Curve,Automatic Quantitation-I,A,B,C,D,E,F,A-R.T.B-Compound NameC-CAS NoD-Peak AreaE-ResultF-Fit,Reverse Fit,Purity,Automatic Quantitation-II,MS Tuning 與 日常保養,Tuning,To optimize the sensitivity and resolutionTo adjust the relative ion ratioAutoTune and Manual Tune,Tuning-I(Good Resolution),Tuning
14、-II(Good Resolution),Tuning-III(Bad Resolution),Tuning-IV(Bad Resolution),Tuning-V(Good Ion Ratio),Tuning-VI(Bad Ion Ratio),Tuning Requirements,Easy to Maintain Tool-free Manifold Disassembly,Easy-to-Maintain Mass Analyzer,應用,GC/MS Applications,EnvironmentAir,Water and soil for pesticides,herbicides
15、,semi-volitiles,etc.PharmaceuticalEnantiomers in biologically active compoundsPetroleumCrude oil,gasoline,diesel fuel for PAH,additives,etc.ChemicalRaw material and synthesized compounds for trace impuritiesForensicBlood and urine for drug of abuseFood/FlavorsPesticide in foods,isolation of flavor,etc.University ResearchOrganic synthesis,PAHs in Diesel Fuel,Organophosphorus Pesticides,Pesticide Residues in Agricultural Products,Volatile Organic Compounds in Water,