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CONTACTS(/I/CONTACTINFO)
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(/i/gc
troubleshooting/g
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greatservice,qualityproducts
andtips?
troubleshooting/g
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and
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CHROMATOGRAPHY tips?
and
troubleshooting/g
(/i/gc
(/)Chromatography(/s/chromatography)Hintsandtips(/g/hintsandtips)GCtroubleshooting(/c/gctroubleshooting)GC
(/S/CHROMATOGRAPHY) troubleshooting
lang=CZ)
tips?
and
troubleshooting/g
GC/MSTOF(/g/timeof
lang=SK)
flightgcms) GCtroubleshooting tips?
and
GC/MS/MS(/g/triple lang=BG)
tips?
quadrupole) Prevention lang=RU)
Glossary(/g/glossaryin
chromatography) ManyGCproblemscanbepreventedifthecolumnisproperlyinstalledandGCismaintainedroutinely.Forexample,replacingseptaor
lineratregularintervalsandkeepingtheinjectoranddetectorcleanandwellmaintainedshoudsolvemanyproblems.Regularpreventive
Hintsandtips(/g/hints
maintenancedependsonparticularmodelofGCandyoushouldconsultrequiredoperationsintheoperator'sandservicemanuals.
andtips)
Fortheproblemidentificationwerecommendtouseelectronicflowmeterandleakdetector.
DynamicHeadspace
(/c/dynamicheadspace)
Baselineproblems
GCcolumnconditioning
(/c/gccolumn
conditioning) Baselineproblemscouldbedividedinto5categories:drift,noise,offset,spikingandwander.
GCcolumninstallation Driftmeansslowbaselinemovementinonedirection
(/c/gccolumninstallation) Noiseisrapidandrandommovementofthebaselineposition
GCliners(/c/gcliners) Offsetissuddenunexplainedchangeofthebaselineposition
GCseptaselection(/c/gc Spikingispresentedbypeakswithnowidth,eitherpositiveornegative
septaselection) Wanderislowfrequencynoise
GCtroubleshooting(/c/gc
troubleshooting) Downwarddrift
Hintsandtipsoverview
(/c/hintsandtips
overview)
Possiblecause Suggestions
Downwarddriftforafewminutesis Increasetheoventemperaturetoclosetothemaximumcontinuousoperatingtemperaturefor
HPLCtroubleshooting
normalafterinstallinganewcolumn thecolumn.Maintainthetemperatureuntilflatbaselineisobserved.Ifthedetectorsignaldoes
(/c/hplctroubleshooting)
notdropin10minutes,immediatelycoolthecolumnandcheckforleaks.
Chiralcolumnhandling
Unequilibrateddetector Allowsufficienttimefortemperatureequilibrationofthedetector.
(/c/chiralcolumnuse)
Kinetexandorg.solvents Downwarddriftisfrequentlyduetothe Cleanoutcontamination.
(/c/kinetexandorg "backout"ofcontaminantsfromthe
detectororotherpartsoftheGC
solvents)
Linearvelocitysettings
(/c/linearvelocitysettings) Upwarddrift
Signal:noiseincreacein
GC(/c/signalnoise Possiblecause Suggestions
increaceingc)
Damagetothestationaryphaseof Determinethecauseofthedamage.Itmaybeduetoimpuritiesinthecarriergasortoexcessive
Siltekdeactivation theGCcolumn temperatures.Replacecolumn.
(/c/siltekdeactivation)
Driftingasflowrates Cleanorreplacefloworpressureregulator(s).Adjustpressure.
Syringecare(/c/syringe
care)
Thermaldesorption Noise
(/c/thermaldesorption)
Thermaldesorption Possiblecause Suggestions
sorbents(/c/TDsorbents)
Thecolumnmaybeinsertedtoofarintotheflameof Reinstallthecolumn.Besuretoinsertthecolumnintothedetectorexactlythe
Troubleshooting anFID,NPDorFPDdetector correctdistancespecifiedintheinstrumentmanual.
(/c/troubleshooting)
AnairleakcanresultinnoiseinECDandTCD Eliminatetheleak.
PreparativeHPLC detectors
(/g/preparativehplc) Incorrectcombustiongasesorflowratescangenerate Besureyuorgasesarethepropergrade,aswellascleananddry.Resetthe
noisinFID,NPDorFPDdetectors. flowratesofthegasestotheirpropervalues.
PreparativeLC
(/c/preparativelc) Contaminatedinjector Cleaninjector.Replaceinletliner,septaandselas.
SMB(/c/smb) Contaminatedcolumn Bakeoutthecolumn.Cutofffirst10cmofcolumn.Ifitdoesnothelp,replace
thecolumn.
Stationaryphases
(/g/stationaryphases) Defectivedetector Cleanand/orreplacepartsasnecessary.
HPLC(/c/hplc)
MEPS(/c/meps) Offset
Moreabout
chromatography(/c/more Possiblecause Suggestions
aboutchromatography) Offline
SPE(/c/spe) Linevoltagechanges Monitorlinevoltageforcorrelationwithoffset.Ifcorrelationisfound,installvoltage
regulatororensurestablepowersupply.
StationaryPhases
Overview(/c/stationary Poorelectricalchanges Checkelectricalconnections.Tightenanylooseconnections.Cleananydirtyorcorroded
phasesoverview) connections.
UHPLC(/c/uhplc) Contaminatedinjector Cleaninjector.Replaceinletliner,septaandselas.
UHPLC(/g/uhplc)
Spiking
UHPLCindetails
(/c/uhplcindetails)
UHPLCreagents
Possiblecause Suggestions
(/c/uhplcreagents) Electricaldisturbancesenteringthe Trytocorrelatespikeswitheventsinequipmentnearthechromatograph.Periodicityis
chromatographthroughpowercables,even oftenaclue.Turnoffequipmentormoveit.Ifnecessary,installavoltageregulator.
Unitconversions(/g/unit shieldedcables
conversions)
Wander
Contaminatedinjector Cleaninjector.Replaceinletliner,glasswoolandseals.
Contaminatedcolumn Bakeoutthecolumn.Cutofffirst10cmofcolumn.Ifitdoesnothelp,
replacethecolumn.
Chro
mserv
Distortedpeakshapes
is
7hrs
Allpeaksredusedinsize
Restekuvedlna
trhSPMEArrow
novtypSPME,
kterpekonv
tradinSPME
vlkna.Podvejte
Possiblecause Suggestions
Samplevalidity Checktheconcentrationandstabilityofthesample.
Flattenedtoppeaks
Possiblecause Suggestions
Detectoroverload.Thebroadpeaksmayhavearoundedtoporevenvalleys Reducesamplevolume,dilutewithsolventorusehigher
inthetop. splitratio.
Overloadofthesignalprocessingelectronics.Thepeaksareclippedwithflat Attenuatedetectoroutputorreducesampleamount(see
tops. above).
Frontingpeaks
Fronting peaks are usually the result of column overloading. In this case, the effect should be a function of injection volume. Solutions
include reducing the injection volume or using a column with greatr capacity. Columns with larger diameter or thicker stationary phase
coatingsgenerallyhavelargersamplecapacities,however,resolutionmaybereduced.
Ghostpeaks
Possiblecause Suggestions
Offline
Remmantsofprevioussamplesintheinletorcolumn.Ghost Increasethefinaltemperatureandlengthentheruntimetoallowfor
peaksduetoremmantsaremostlikelytooccurwhenincreasing completeelutionofprevioussamples.Ifghostpeakscontinueto
inletorcolumntemperatures. occur,cleantheinlet.Conditionthecolumnattemperaturehigher
thanhasbeenusedbutlowerthanthemaximumcontinuous
operationtemperatureforthecolumn.Cut10cmofftheinletendof
thecolumnand/orrevereseitbeforereconditioningit.Ifitdoesnot
help,replacethecolumn.
Backflashmaycauseremmants.Backflashreferstovapours
fromthesamplewhichexpandtoexceedthevolumeofthe Useseptumpurge
injectorliner.Thesevapoursmaycomeincontactwithcolder Lowerinjectionvolume
spots,suchastheseptumandgasinletsoftheinjector.Less
Enlargeinjectorliner
volatilecomponentsmaycondense.Thesecondensatesmay
Optimizeinjectortemperature
vaporizelaterandinterferewithsubsequentanalyses,sometimes
producing"ghostpeaks". Usepressurepulsedprogram
Bleedfromtheseptumorfragmentsoftheseptumlodgedinthe Cleantheinlet.Replacetheinletliner,glasswoolandseals.
inletorliner.
Irreproduciblepeakheightsorareas
Possiblecause Suggestions
Inconsistentinjection Developareproducibleinjectiontechnique.Useautosampler.
Distortedpeakshapescanadverselyaffectquantitative Correctanyproblemsthatresultinthedistortionofpeakshape.SeePeak
determinations shapeproblems.
Baselinedisturbances SeeBaselineproblems.
VariationsinGCoperatingparameters Standardizeoperatingparameters.
Negativepeaks
Possiblecause Suggestions
Incorrectpolarityoftherecorder Reversepolarityofrecorderconnections.
Incorrectsetupinthesoftware Setuprightparametersinyourchromatographysoftware.
Samplecompoundhasgreaterthermalconductivity Ifpossible,changecarriergas.Otherwisethereisnotasolution.
thanthecarriergasandyouareusingaTCDor
TCDdetector
Detectoroverloadinelementspecificdetectors Havethecompoundofinterestarriveatthedetectoratadifferenttimefromthe
suchasECD,NPD,FPD,etc.,canproduceboth solventorothercompoundsinhighconcentration.H2producesnegativepeakswith
positiveandnegativepeaks TCD(TCD)andheliumcarriergas.
DirtyECDdetectorcangivenegativepeakaftera CleanorreplacetheECDdetector.
positiveone
Nopeaksatall
Possiblecause Suggestions
Defectivesyringe Tryaneworprovensyringe.
"Blown"septumormassiveleaksattheinlet Findandfixleaks.
Problemswithcarriergasflow Adjustgasflow.Checkthecolumnflowaththecolumnoutletbyimmersionto
methanol.
Brokencolumnorcolumninstalledinthewrongway Replaceorreinstallthecolumn.
Thedetectorisnotfunctioningornotconnectedtothe Ensurethatdetectorisworkingproperly.E.g.:IstheflameinaFIDon?Check
recorderorintegrator. connectiontotheoutputdevice.
Selectivesensitivityloss
Possiblecause Suggestions
Contaminationofcolumnand/orlinercanleadtolossofsensitivity Cleanliner.Bakeoutthecolumnorreplaceit.
foractivecompounds
Injectorleaksreducethepeakheightofthemostvolatile Findandfixanyleaks.
componentsofasamplemorethanlessvolatile
Initialcolumntemperaturetoohighforsplitlessinjectionwhichcan
Possiblecause Initialcolumntemperatureshouldbebelowtheboilingpointofthe
Suggestions
preventrefocusingofsample.Thisaffectsthemorevolatile solvent.Decreasetheinitialcolumntemperatureoruseless
componentsmost. volatilesolvent.
Inletdescrimination.Injectortemperatureistoolow.Latereluting Increaseinjectiontemperature.
andlessvolatilecompoundshavelowresponse.
Offline
Splitpeaks
Possiblepeaks Suggestions
Fluctuationsincolumntemperature Repairtemperaturecontrolsystem
Mixedsamplesolventforsplitlessoroncolumninjections Usesinglesolvent
Whenusinginjectiontechniquesthatrequire"solventeffect"refocusingsuchas Installingaretentiongap(5metersofuncoated
splitlessinjectiion,thesolventmustformacompact,continuousfloodedzoneinthe butdeactivatedcolumn)aheadofthe
column.Ifthesolventdoesnotwetthestationaryphasesufficientlyasmightbethe crhomatographiccolumnmayreduceor
caseformethanolusedwithanonpolarstationaryphase,thesolventfloodedzonemay eliminatethisproblem.
beseveralmeterslongandnotofuniformthickness.Thiswillresultinbroadand
distortedpeaksbecausethesoluteswillnotberefocusedintoanarrowbandnearthe
beginningofthecolumn.
Tailingpeaks
Possiblecause Suggestions
Contaminatedoractiveinjector Cleanorreplaceinjectorliner.Donotuseglasswoolintheliner.Ifnecessary,replacethecolumn.
liner,sealorcolumn
Deadvolumeduetopoorly Confirmbyinjectinginertpeak(methane).Ifittails,columnisnotproperlyinstalled.Reinstallliner
installedlinerorcolumn. andcolumnasnecessary.
Raggedcolumnend Scorethetubinglightlywithaceramicscoringwaferorsapphirescriberbeforebreakingit.Examine
theendusingmagnifyingglass.Ifthebreakisnotcleanandtheendsquare,cutthecolumnagain.
Pointtheenddownwhilebreakingitandwhileinstallinganutandferruletopreventfragmentsfrom
enteringthecolumn.Reinstallthecolumn.
Abadmatchbetweenthe Changethestationaryphase.Usuallypolaranalytestailonnopolarcolumns,ordirtycolumns.
polaritiesofthestationaryphase
andthesolvent
Acoldregioninthesampleflow Removeanycoldzonesintheflowpath
path
Debrisinthelinerorcolumn Cleanorreplacetheliner.Cut10cmofftheendofthecolumnandreinstallit.
Injectiontakestoolong. Improveinjectiontechnique.
Splitrationistoolow Increasesplitratiotoatleast20:1
Overloadingtheinlet Decreasethesamplevolumeordilutesample
Sometypesofcompoundssuch Tryamorepolarcolumn.Makeaderivativeofthedsample.
asalcoholicamines,primaryand
secondaryaminesandcarboxylic
acidstendtotail.
Retentiontimeshifts
Possiblecause Suggestions
Changeincolumn CheckGCoventemperature
temperature
Changeingasflowrate Injectadetectableunretainedsamplesuchasmethanetodeterminethelineargasvelocity.Adjustgas
(linearvelocity) pressureorflowtoobtainpropervaluesforyouranalyticalmethod.
Leakintheinjector Checktheseptumfirst.Change,ifnecessary.Findtheleakandfixit.
Changeofsolvent Usethesamesolventforstandardsandsamples.
Contaminatedcolumn Bakeoutthecolumn.Cut10cmofftheendofthecolumn.Ifnecessary,replacethecolumn.
Lossofresolution
Possiblecause Suggestions
Damagetostationaryphaseofcolumn Replacethecolumn.Thisisusuallyindicatedbyexcessivecolumnbleedingorpeaktailing.
Injectorproblems Checkforleaks,inapropriatetemperature,splitration,purgetime,dirtyliner,glasswoolinliner.
Offline
Possiblecause Suggestions
Largeincreaseinsampleconcentration
Dilutesample
Injectless
Usehighersplitratio
Broadsolventfront
Possiblecause Suggestions
Badcolumninstallation Reinstallcolumn
Injectorleak Findandfixleak
Injectionvolumetoolarge Decreasesamplesizeordiluteit
Injectiontemperaturetoolow Increaseinjectiontemperaturesotheentiresampleisvaporized"instantly".Aninjectiontemperature
higherthanthetemperaturelimitofthecolumnwillnotdamagethecolumn.
Splitratioistoolow Increasesplitratio.
Columntemperaturetoolow Increasecolumntemperature(bacarefulonmaximumcolumntemperaturelimit).Usealowerboiling
solvent.
Initialcolumntemperaturetoo Decreasetheinitialcolumntemperature.Usealessvolatilesolventsotheinitialcolumntemperatureis
highforsplitlessinjection belowthesolventboilingpoint.
Purgetimetoolong(splitless Useashorterpurgevalveclosetime.
injection)
Rapidcolumnperformancedegradation
Possible Suggestions
cause
Brokencolumn Replacecolumn.Avoiddamagingthepolyimidecoatingonthecolumn.Avoidetemperaturesabovemaximu
columntemperaturelimit.Avoidabrasionofthecolumn.Remember,evenifthecolumndoesnotbreak
immediately,whenprotectivecoatingisdamagedthecolumnmaypossiblybreakspontaneouslylater.
Columntoohotfor Replacethecolumn.Staybelowlimitsspecifiedforthecolumn.
toolong
Exposureto Findandfixanylieaks.Besurecarriergasissufficientlypure.
oxygen,particularly
atelevated
temperatures
Chemicaldamage Keepinorganicacidsorbasesoutofcolumn.Neutralizesamples.
duetoinorganic
acidsorbases
Contaminationof Preventnonvolatilematerialsfromgettingintocolumn.Forexpample,useaguardcolumn.
thecolumnwith
nonvolatile
materials
Columninstallation
DetailedinformationaboutGCcolumninstallationisavailablehere(/i/capillarygccolumninstallation?lang=EN).
Preventivemaintenance
Injectorcleaning
Detectorcleaning
Offline
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