Book Of LC.docx

Book Of LC.docx

《Book Of LC.docx》由会员分享，可在线阅读，更多相关《Book Of LC.docx（90页珍藏版）》请在冰点文库上搜索。

BookOfLC

TheChrom-EdChromatographySeriesby

Dr.R.P.W.Scott

1.PrinciplesandPracticeofChromatography

Introduction

TheDevelopmentProcess

ChromatographyNomenclature

FactorsControllingRetention

FactorsAffectingtheMagnitudeoftheDistributionCoefficient（K）

MolecularForcesandChromatographicSelectivity

TheControlofChromatographicallyAvailableStationaryPhase（Vs）

PeakDispersioninaChromatographicColumn

TheBasicColumnChromatograph

ThinLayerChromatography

ChromatographyApplications

References

2.GasChromatography

Introduction

TheModernGasChromatograph

GasSupplies

InjectionDevices

GCColumns

TheColumnOvenandTemperatureProgrammer

GCDetectors

DataAcquisitionandProcessing

QuantitativeAnalysis

PreparativeGasChromatography

Applications

References

3.LiquidChromatography

Introduction

TheBasicLiquidChromatograph

ColumnOvens

Detectors

TheUVDetector

TheElectricalConductivityDetectors.

TheFluorescenceDetector

TheRefractiveIndexDetector

TheTridetMultiFunctionalDetector

DataAcquisitionandProcessing

LiquidChromatographyStationaryPhases

MacroporousPolymers

LCMobilePhases

ChiralStationaryPhases

LiquidChromatographyApplications

References

4.GasChromatographyDetectors

Introduction

ClassificationofDetectors

DetectorSpecifications

TheFormofDetectorResponse

TheDynamicRangeoftheDetector

DetectorLinearity

DetectorResponse

DetectorNoise

DetectorSensitivityorMinimumDetectableConcentration

SystemDispersionandSensorDispersion

PeakDispersionfromtheOverallDetectorTimeConstant

PressureSensitivity

FlowSensitivity

TemperatureSensitivity

SummaryofDetectorCriteria

EarlyGasChromatographyDetectors

TheGeneralPropertiesofGCDetectors

TheKatharometerDetector

TheSimpleGasDensityBalance

TheFlameIonizationdetector

TheResponseMechanismoftheFID

TheOperationoftheFID

TheNitrogenPhosphorusDetector（NPD）

TheEmissivityorPhotometricDetector

IonizationDetectors

TheRadioactivityDetector

SomeLessCommonGCDetectors

ClosingNotes

References

5.LiquidChromatographyDetectors

Introduction

DetectorSpecifications

DispersioninDetectorSensors

LCDetectorsBasedonRefractiveIndexMeasurement

TheUVDetectors

TheFluorescenceDetector

TransportDetectors

TheEvaporativeLightScatteringDetector

LiquidLightScatteringDetectors

TheElectricalConductivityDetector

TheElectrochemicalDetector

References

6.PlateTheoryandExtensions

Introduction

ThePlateTheory

TheRetentionVolumeofaSolute

TheConditionsforChromatographicSeparation

TheCapacityRatioofaSolute

TheCompressibilityoftheMobilePhase

TheColumnDeadVolume

ChromatographicDeadVolumes

ExperimentalExaminationofDeadVolumeMeasurement

TheGaussianFormoftheElutionEquation

RetentionMeasurementsonCloseElutingPeaks

QuantitativeAnalysisfromRetentionMeasurements

ColumnEfficiency

ThePositionofthePointsofInflection

ResolvingPowerofaColumn

EffectivePlateNumber

TheSummationofVariances

TheMaximumSampleVolumethatCanBePlacedonaChromatographicColumn

VacancyChromatography

TemperatureChangesDuringthePassageofaSoluteThroughaTheoreticalPlateinGasChromatography

ThePeakCapacityofaChromatographicColumn

References

7.TheMechanismofChromatographicRetention

Introduction

ChromatographicInteractions

MixedPhases

TheAssociationofMethanolwithWater

Solvent/SoluteInteractionswithAdsorbentSurfaces

SoluteStationaryPhaseInteractions

RetentionandExclusion

ChiralChromatography

References

8.TheThermodynamicsofChromatography

ThermodynamicsBasics

TheAnalysisoftheStandardEnergyofDistribution

TheInteractiveEnergyDifferenceBetweenthatofaMethyleneGroupandthatofaMethylGroupwithanAlkaneStationaryPhase

TheThermodynamicAnalysisoftheDispersiveInteractionsthatCanTakePlacebetweenDifferentSolutesandHighMolecularWeigh

InteractionsBetweentheAtomsofHydrogen,Carbon,ChlorineandBromineandanExclusivelyDispersiveStationaryPhase

TheDistributionofStandardEnergyBetweenDifferentTypesofMolecularInteractions

OtherThermodynamicMethodsthatareUsedforStudyingChromatographicSystems

References

9.DispersioninChromatographyColumns

IntroductiontotheRateTheory

TheSummationofVariances

TheAlternativeAxesofaChromatogram

TheRandomWalkModel

DispersionProcessesthattakePlaceinanLCColumn

ResistancetoMassTransferDispersion

EffectofMobilePhaseCompressibilityOntheHETPEquationforaPackedGCColumn

TheVanDeemterEquation

AlternativeEquationsforPeakDispersion

TheGolayEquation

ExperimentalValidationoftheVanDeemterEquation

Summary

References

10.ExtraColumnDispersion

Introduction

SourcesofExtraColumnDispersion

DispersioninContemporaryLCColumns

DispersioninContemporaryGCColumns

MaximumPermissibleExtraColumnDispersion

GCCapillaryColumns

LCSampleValves

DispersioninTubularConduits

LowDispersionConnectingTubes

DispersioninUnionsandStainlessSteelFrits

DispersionintheDetectorSensorVolume

DispersioninDetectorSensorsDuetoNewtonianFlow

ApparentDispersionfromDetectorSensorVolume

DispersionDuetoDetectorElectronicsResponseTime

LowDispersionGradientElutionApparatus

RapidSeparationsEmployingGradientElution

ChromatographicApparatusforTraceAnalysis

TheDeterminationofTraceOrganicMaterialsinWater

TheUseforLowDispersionInstrumentationwithSmallBoreColumnstoObtainUltraHighEfficiencies.

SeparationsonSmallBoreColumns2mLong

References

11.PreparativeChromatography

Introduction

TheLoadingCapacityofaColumn

TheMaximumSampleVolume

SampleVolumeOverload

SampleMassOverload

PreparativeChromatographyApparatus

PackingPreparativeColumns

RecyclingDevelopment

AlternativePreparativeTechniques

RadialFlowChromatography

ThePreparativeSeparationoftheEnantiomersofChlorokynurenine

CriteriafortheSuccessfulOperationofPreparativeChromatographs.

References

PrinciplesandPracticeofChromatography

Introduction

Chromatography,althoughprimarilyaseparationtechnique,ismostlyemployedinchemicalanalysis.Nevertheless,toalimitedextent,itisalsousedforpreparativepurposes,particularlyfortheisolationofrelativelysmallamountsofmaterialsthathavecomparativelyhighintrinsicvalue.Chromatographyisprobablythemostpowerfulandversatiletechniqueavailabletothemodernanalyst.Inasinglestepprocessitcanseparateamixtureintoitsindividualcomponentsandsimultaneouslyprovideanquantitativeestimateofeachconstituent.Samplesmaybegaseous,liquidorsolidinnatureandcanrangeincomplexityfromasimpleblendoftwoentantiomerstoamulticomponentmixturecontainingwidelydifferingchemicalspecies.Furthermore,theanalysiscanbecarriedout,atoneextreme,onaverycostlyandcomplexinstrument,andattheother,onasimple,inexpensivethinlayerplate.

ThefirstscientisttorecognizechromatographyasanefficientmethodofseparationwastheRussianbotanistTswett

（1）,whousedasimpleformofliquid-solidchromatographytoseparateanumberofplantpigments.Thecoloredbandsheproducedontheadsorbentbedevokedthetermchromatographyforthistypeofseparation（colorwriting）.Althoughcolorhaslittletodowithmodernchromatography,thenamehaspersistedand,despiteitsirrelevance,isstillusedforallseparationtechniquesthatemploystheessentialrequisitesforachromatographicseparation,viz.amobilephaseandastationaryphase.

Thetechnique,asdescribedbyTswettwaslargelyignoredforaalongtimeanditwasnotuntilthelate1930sandearly1940sthatMartinandSynge

（2）introducedliquid-liquidchromatographybysupportingthestationaryphase,inthiscasewater,onsilicainapackedbedandusedittoseparatesomeacetylaminoacids.Intheirpaper,theyrecommendedreplacingtheliquidmobilephasebyasuitablegas,asthetransferofsamplebetweenthetwophaseswouldbefaster,andthusprovidemoreefficientseparations.Inthismanner,theconceptofgaschromatographywascreatedbutagain,littlenoticewastakenofthesuggestionanditwaslefttoMartinhimselfandA.T.Jamestobringtheconcepttopracticalrealitynearlyadecadelater.Inthesamepublicationin1941,theessentialrequirementsforHPLC（HighPerformanceLiquidChromatography）wereunambiguouslydefined,

"Thus,thesmallestHETP（thehighestefficiency）shouldbeobtainablebyusingverysmallparticlesandahighpressuredifferenceacrossthecolumn".

Despitehisrecommendations,however,itwasnearlyfourdecadesbeforethisconceptweretakenseriouslyandthepredictedhighefficiencyliquidchromatographycolumnsbecameareality.Bythemid1960sthedevelopmentofallaspectsofchromatographywerevirtuallycompleteandsincethen,despitetheplethoraofpublicationsthathaveappearedonthesubject,thevastmajorityhasdealtwithapplicationsofthetechniqueandonlyaminoritywithfundamentalaspectsofthesubjectandnovelinstrumentationconcepts.

Today,chromatographyisanextremelyversatiletechnique;itcanseparategases,andvolatilesubstancesbyGC,involatilechemicalsandmaterialsofextremelyhighmolecularweight（includingbiopolymers）byLCandifnecessaryveryinexpensivelybyTLC.Allthreetechniques,（GC）,（LC）andTLChavecommonfeaturesthatclassifythemaschromatographysystems.

Chromatographyhasbeendefinedasfollows,

Chromatogra