布鲁克红外光谱仪介绍(英文)

•PARTIchromatographictechniques•I.0IGC-FT-IR(classical)•I.IIPyrolysis(GC)-FTIR,(Pyrolysis-FT-IR)•I.IIIHPLC-FT-IR/GPC-FT-IR•I.IVSFC-FT-IR•I.VTLC-FT-IR•PARTIIthermoanalyticaltechniques•II.0ITG–FT-IR•II.IIDSC–FT-IRHYPHENATEDTECHNIQUESCombinationsrealisedwithIRGC–FT-IRCOUPLINGTECHNIQUESHYPHENATEDTECHNIQUESGaschromatography–Fourier-Transform-Infraredspectroscopy(GC–FT-IR)A587,GC-FT-IRModuleA586,GC-FT-IRModuleFT-IRGCschemeofatypicalGC-FT-IR;consistingof4majorpartsFIDInGC/IR-Interface„light-pipe“IRDetectorGCPCMonitorTerminalFT-IRSpectrometermodulatedIR-beamGaschromatography–Fourier-Transform-Infraredspectroscopy(GC–FT-IR)„Light-pipe“IR-beam„in“IR-beam„out“ParabolicmirrorInletIR-window„makeup“gasCapillarycolumn350030002500200015001000500Points0.0100020004000Wavenumbercm-1100020004000Wavenumbercm-10300t/sec.Sample100020004000Wavenumbercm-1ReferenceGSFTGaschromatography–Fourier-Transform-Infraredspectroscopy(GC–FT-IR)MON-+Gram-Schmidt-ChromatogramcalculationM:basevectorsN:dimensionO:offsetb1,2:basevectorss:samplevectort:Gram-Schmidt-valuesb1b2pt=s-pDimensionOffsetNumberofdatapoints123123Gaschromatography–Fourier-Transform-Infraredspectroscopy(GC–FT-IR)Seconds0501001502002503000.000.100.200.30GramSchmidt3DPlotR112sec.R66sec.R72sec.R89sec.150020002500300035004000150020002500300035004000Wavenumbercm-1TransmittanceSeconds0501001502002503000.000.100.200.30GramSchmidtOH-StrechGS-trace5001000150020002500300035004000Wavenumbercm-10.2AbsorbanceStructuralIsomersOHOHOHOHOHOH1,3-Butanediole1,2-Butanediole5001000150020002500300035004000Wavenumbercm-1OHOHOHOH1,4-ButanedioleOHOH2,3-ButanedioleOHOHStructuralIsomersSENSITIVITY1/11/1010/10Transmittance[%]TransmittanceGC–FT-IRsensitivityIBMA(METHACRYLICACID,ISOBUTYLESTER)5001000150020002500300035004000Wavenumbercm-1GC–FT-IRsensitivityPyrolysis–[Gaschromatography]–Fourier-Transform-Infraredspectroscopy(Pyrolysis-[GC]–FT-IR)PyrolysisGC–FT-IRcarriergasquartzsampletubeandsamplecapillarycolumnsplitventheaterseptumretainerBULKPOLYM.OLIGOMERSMONOMERESLOWMOLEK.WEIGHTMOLECULESTPYRTOPTTPYRTOPTTPYR=TOPTPyrolysisGC–FT-IR450550650750850PyrT/°C100Area%0MONOMERSGASES[CO2/HOH]PyrolysisGC–FT-IRHigh-performance-liquid-chromatography-Fourier-Transform-InfraredspectroscopyHPLC–FT-IRIRbeamIRwindowInletOutletHPLC–FT-IRCyclohexane100µm100015002000250030003500Wavenumbercm-120406080100Transmittance[%]HPLC–FT-IREthylacetate100µm100015002000250030003500Wavenumbercm-120406080100Transmittance[%]blockedareaHPLC–FT-IRGe-diskheatednitrogenheaterLCflowHPLC–FT-IRHPLC–FT-IRZnSewindowIRbeamFlowthroughcellDepositionGe-diskheaterHPLC–FT-IR•FlowCell•Relativelylowsensitivity(mobilephaseabsorption)•DirectDetection•Easeofoperation,lowmaintenance•Cellmustwithstandhighpressure•Selectedapplications•„on-line“processmonitoring•MobilePhaseElimination•Highsensitivity(nomobilephaseabsorption,signalaveraging,smallareadeposition)•Detectiondelayed•Moredifficulttohandle•Depositionproblem•Mobilephaseimpurities•ComplexsampleanalysisHPLC–FT-IRSupercriticalFluidChromatography-Fourier-Transform-InfraredspectroscopySFC–FT-IRTemperature/°CSFC–FT-IR73.05.2-5731Pressure/atm.~~vapourfluidsolidSupercriticalTriplePointPcTcFluidTc(°C)Pc(atm.)ρc(g/ml)CO231.372.90.47N2O36.572.50.45NH3132.5112.50.24n-C5196.633.30.23n-C4152.037.50.23SF645.537.10.74Xe16.658.41.10CCL2F2111.840.70.56CHF325.946.90.52PhysicalparametersofselectedsupercriticalfluidsSFC–FT-IRDensityg/cm3Viscosityg/cmxsec.Diffusivitycm2/sec.GasLiquidSupercriticalFluid10-310-410-110.3-110-25x10-65x10-45x10-4SFC–FT-IRGCHPLClimitationslimitations-Volatility-resolution-thermalstability-detection-viscositySFCcapillarycolumnspackedcolumnsSFC–FT-IRColumnHP1084SFCOvenSFCPumpHeatexchangerBRUKERIFS88FTIRSFCIR-CellUVSpectrometerPressurestabiliserIn/OutSchemeofSFC/FTIRSFC–FT-IRSFC/FT-IR-highpressurecellWindow40mmSFC–FT-IRTABLE:SFC-ApplicationsIndustrial:Syntheticoligomers,polymers/additivesSurfactants(polyglycols)Oligo-,Poly-sacharides,sucrosepolyestersPesticidesIsocyanatesDyesWaxesBiochemical:StereoidsProstaglandinsFattyacids/lipidsAntibioticsDrugsofabuseFossilFuels:Fractionationofpetroleumandcoal-derivedfluidsHydrocarbongroupanalysisSimulateddistillationSFC–FT-IRSyntheticMixtureofAcidicCompounds1.)2-nitrophenol2.)phenylbenzoate3.)phenol4.)salicylicacid5.)3-bomobenzoicacid6.)2-naphthoicacid7.)vitamineA-acid8.)4-nitrophenolSFC–FT-IRSi3µm125x4mmpressuregradient(linear)150-350bar,28bar/minflow:CO2,2ml/minmodifier:40µl/min0.003%citricacidinCH3OHoventemperature:70°Cdetection:UV220nmSFC–FT-IRThinLayerChromatography–Fourier-Transform-InfraredspectroscopyTLC–FT-IRTLC-FTIRThespectrumof1µgofSudanRedGmeasuredbydirecttransmittancethroughaTLCplateconsistingofa100-µmlayerofsilicageldepositedonasheetofsilverchloride.Thedyewasoriginallypresentasa0.1%componentina1-µlspotofasolutioncontainingthreedyes,SudanRedG,IndophenolsBlue,andButterYellow.C.J.PercivalandP.R.Griffiths,Anal.Chem.,47,154(1975)TLC-FTIRIncaseofFresnelreflectionthereflectivit