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CHROMATOGRAPHY tips?
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(/)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.

GC(/c/gc) Defectivedetectorboard ConsultGCmanufacturer.

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.

Syringes(/g/syringes) Contaminatedcolumn Bakeoutthecolumn.Cutofffirst10cmofcolumn.Ifitdoesnothelp,replacethe

column.
Agilentsyringes
(/c/agilentsyringes) ColumninsertedtoofatintotheflameofFID, Reinstallthecolumn.Besuretoinsertthecolumnintothedetectorexactlythecorrect
NPDorFPDdetectors distancespecifiedintheinstrumentmanual.
CTCsyringes(/c/ctc
syringes) Contaminateddetector Cleanthedetectorifpossible.

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

NEWS Possiblecause Suggestions

Baselinewanderingmaybecausedbychangesinenvironmental Trytocorrelatethewanderingwithenvironmentalparameters.Ifa
Chroms conditionssuchastemperatureorlinevoltage correlationisobserved,youwillknowwhattodo.
LikePage InadequatetemperaturecontrolCheckifvariationscanbe Measuredetectortemperature.
correlatedwithchangesinthebaselineposition.

Bethefirstofyour Wanderingwhileusingisothermalconditionsmaybedueto Changethecarriergasorthegaspurificationtraps.

friendstolikethis contaminatedcarriergas

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

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