Presentation on theme: "Chromatography Integration and Trouble-shooting"— Presentation transcript:
1 Chromatography Integration and Trouble-shooting Presented by: Marlene MooreOctober 2007Advanced Systems, Inc.
2 AgendaProblemsToolsSolutionsAdvanced Systems, Inc.
3 Problems Baseline Disturbances Irregular Peak Shapes, Sizes Retention Time ShiftsLoss of Separation or ResolutionQuantitation DifficultiesRapid Column DeteriorationGhost PeaksBroad Solvent FrontAdvanced Systems, Inc.
4 Baseline Disturbances spikingnoisewanderdriftoffsetAdvanced Systems, Inc.
5 Spiking Particulate Matter Passing Through Detector Loose Connections CablesCircuit boardsAdvanced Systems, Inc.
6 Noise Contaminated Injector/column Physical Defect Detector Defective Detector BoardCarrier Gas Leak at Septum or ColumnFID, NPD, FPDColumn in FlameIncorrect Combustion Gases or Flow Rate/leakECD, TCDAir LeakAdvanced Systems, Inc.
7 Wander Contaminated Carrier Gas Contaminated Gas Chromatograph Isothermal ConditionsContaminated Gas ChromatographPoor Control of Carrier Gas or Detector Gas FlowsPoor Thermal Control of DetectorAdvanced Systems, Inc.
8 Drift Septum Bleed Upward Downward GC or column contamination Damaged stationary phaseDownwardIncomplete conditioning of columnUnequilibrated detectorAdvanced Systems, Inc.
9 Offset Contamination: Column Inserted Into Flame (FID, NPD, FPD) Injector, column, detectorCarrier gas - change/install impurity trapsColumn Inserted Into Flame (FID, NPD, FPD)Malfunctioning or Improperly Set Recording DeviceAdvanced Systems, Inc.
13 No Peaks Plugged Syringe Broken Column Injecting Sample Into Wrong InjectorColumn Installed in Wrong DetectorIntegrator Reading Wrong Signal or Not ConnectedDetector Not onTemperatureOven not heatedColumn temperature too lowInjection port temperature too lowDetector Gases Improperly Set or Not onVery Low or No Carrier Gas FlowAdvanced Systems, Inc.
14 Reduced Peaks Plugged Syringe Change in Injection Technique Large Leak - InjectorSplit Ratio Too HighToo Short of Purge Activation Time for Splitless InjectionsVery High Septum Purge FlowToo Low Injector TemperatureColumn Temperature Too LowSample Components Absorbed by Column or Inlet LinerAdvanced Systems, Inc.
15 Reduced PeaksInitial Temperature Column Too High for Splitless or On-column InjectionsHigh Background Signal -ContaminationExcessive column bleedCheck auto zero function and settingImproperly Operated DetectorsImpurities Carrier Gas or Detector GasDetector Compound MismatchExcessive Attenuated Integrator SignalSample Concentration or Integrity ProblemsAdvanced Systems, Inc.
16 Tailing Peaks Active Injector Liner or Column Contaminated Dead Volume Caused by Poorly Installed Liner, Column or UnionPoorly Cut Column EndPolarity Mismatch - Stationary Phase, Solute or SolventCold Spot in the Flow PathAdvanced Systems, Inc.
17 Tailing Peaks Solid Debris in Liner or Column Poor Injection Technique - Too SlowToo Low of a Split RatioOverloading on a PLOT ColumnDecrease sample amountAmines and carboxylic acids tail on most columnsNeed ph modified stationary phaseSome Peaks Always Exhibit TailingAdvanced Systems, Inc.
18 Rounded or Flat Topped Peaks Overloaded DetectorExceeding Range of IntegratorAdvanced Systems, Inc.
19 Split Peaks Detector Overloaded Poor Injection Technique Poorly Installed Column Into InjectorColumn Temperature FluctuationsCoelution of Two or More CompoundsMixed Sample Solvent for Splitless or On-column Injections.Advanced Systems, Inc.
20 Negative Peaks All Peaks Negative - Polarity Check Connectors TCD - Select PeaksThermal conductivity of compound greater than carrier gasECD - After Positive PeakDirty or old ECD cellAdvanced Systems, Inc.
21 Retention Time Shifts Different Column Temperature Different Carrier Gas Flow or Linear VelocityLeak in Injector - SeptumContaminated ColumnChange in Sample SolventAdvanced Systems, Inc.
22 Loss of Separation/Resolution Contaminated ColumnDamaged Stationary PhaseDifferent Column Temperature, Carrier Flow Rate, ColumnLarge Changes in Sample ConcentrationsImproper Injector OperationAdvanced Systems, Inc.
23 Quantitation Difficulties Injection TechniquesSplit DiscriminationDifferent Purge Activation Time for Splitless InjectionBaseline DisturbancesImproper Integrator SettingsInconsistent Detector Gas Flows or TemperaturesColumn or Liner ActivityAdvanced Systems, Inc.
24 Rapid Column Deterioration Exposure of Column to Air at Elevated TemperaturesExceeding Upper Temperature Limit of ColumnChemical DamageContamination of Column With High Molecular Weight MaterialsColumn BreakageAdvanced Systems, Inc.
25 Ghost Peaks Contamination Septum Bleed Dirty Syringe Sample Too Large InjectorColumnSeptum BleedDirty SyringeSample Too LargePrevious Run Terminated Too SoonBOO!Advanced Systems, Inc.
26 Broad Solvent Front Poorly Installed Column Leak in the Injector Solvent Interacting with DetectorToo LowSplit Ratio (Flow)Injector TemperatureToo Long Purge Activation for Splitless InjectionsLarge Injection VolumeLow Column Temperature and High Boiling SolventHigh Column Temperature and Low Boiling SolventAdvanced Systems, Inc.
28 Tools Flowmeter Syringe (NEW) Methane or Nonretained Compound Septa, Ferrules, Injection Liners (NEW)Leak DetectorColumn Test Mixture (Reference)Checkout ColumnInstrument ManualsAdvanced Systems, Inc.
29 Solutions Quickest Solution ---- Improve Chromatography --- Do Manual Integration ---Get Results out Fast !!NO!WRONG ANSWER!!!Advanced Systems, Inc.
30 Solutions Preventive Maintenance Allow Time for Optimizing System Clean detectorClean injectorClean and repair partsClean and tighten connectionsFollow instrument manual suggestionsAllow Time for Optimizing SystemIntegration parametersProgramsAdvanced Systems, Inc.
31 Does anyone have a question? Where do you document your trouble shooting?Advanced Systems, Inc.