气相色谱基本原理

1、Fundamentals of Gas ChromatographyOn the Agilent Web http:/lfs- Sept 27, 2001Fundamentals of Gas ChromatographyComponents of a GC SystemPneumatic FundamentalsRecommended GC Carrier/Makeup Gas PlumbingMoisture TrapP/N 5060-9084Indicating O2 TrapP/N 3150-05281/8” Copper TubingP/N 5180-4196Gas Purity 9

2、9.9995%Minimum PurityNO LEAKS!Fundamentals of Gas ChromatographyDefinitions:Solubility -Volatile -Vaporize -Separate -Detect - Identify - Qualitative - What is it?Measure - Quantitative - How much? Carb and Choke CleanerComprised of:Acetone, Xylene, Toluene,Propane, Isobutane, n-ButaneCarburetor dep

3、osits are soluble in these common solvents.Gas Line anti-freeze - Methanol;Water is soluble in methanol - both are polar - In GC or LC polar compounds are separated on polar stationary phases.Engine starting fluid - Ether, a very volatile solvent.6850/90 - SPLIT/SPLITLESS CAPILLARY INLETCapillary Co

4、lumn Stationary PhasesS St ta at ti io on na ar ry y P Ph ha as se es s APPLICATIO N S H P PH ASES PO LARITY TEM P RAN G E am i nes, hydrocarbons, pesti ci des, H P- 1 nonpol ar - 60 to 325 PCBs, phenol s, sul fur com pounds- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

5、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -a

6、l kal oi ds, drugs, FAM Es, H P- 5, H P- 5 M S nonpol ar - 60 to 325/ 300hal ogenated com pounds, - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

7、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -arocl ors, al cohol s, pesti ci des H P 1301 l ow to m i d- pol ar - 20 to 280 , VO As, cop ol ym er - - - - - - - - - - -

8、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

9、- - - - - - - - - - - - - - - - - - - - - - - - - - - - -arocl ors, am i nes, pesti ci des, H P- 35 i nterm edi ate 40 to 320/ 300 pharm aceuti cal s - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

10、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -arocl ors, herbi ci des, pesti ci des, H P- 1701 i nterm edi ate - 20 t

11、o 280TM S sugars - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

12、 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -drugs, gl ycol s, pesti ci des, steroi ds H P- 50+ i nterm edi ate 30 to 280/ 260 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

13、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -FAM Es, al di tol acetates, neutral sterol s

14、H P- 225 i nterm edi ate 40 to 240/ 220 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

15、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -aci ds, al cohol s, al dehydes, H P- FFAP pol ar 60 to 240 FFAP,acryl ates, ketones, ni tri l es - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

16、- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -al cohol s,

17、 free aci ds, arom ati cs, H P- IN N O W ax pol ar 40 to 260/ 240 BP- 20,essenti al oi l s - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

18、 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -sol vents, gl ycol s, al cohol s H P- W ax pol ar 20 to 250/ 230 Sample Analysis by Gas ChromatographyLiquid sample is pipetted into

19、 a sample vialVarious GC samplesSolids - HeadspaceLiquids - Syringe/Injection PortGas - Gas Sampling ValveLiquids - are typically injected by syringe - 1-3 microlitersTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OC BASIC GC Component I

20、dentification SEPTUMGLASS LINERCOLUMN FERRULEGRAPHITE/VESPELCOLUMNLIQUID PHASESYRINGECOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O C(20 O C above highesttemperature in the ovenprogram)COLUMN OVENTEMPERATUREPROGRAMMED 50O TO 200O C DETECTORCARRIER GASHeliumNEXTTANK PRIMA

21、RYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GC Ready for Sample Injection TANK PRIMARYPRESSURE - 2000 PSISECON

22、DARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GC Syringe inserted into Injection Port TANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPR

23、ESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GC Plunger depressed - Sample Injected TANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCON

24、TROLLER28? PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GC Sample Vaporized Pressure Pulse? Solvent Vapor Volume? TANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOW

25、CONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GCSample is Swept into the Column by the Carrier Gas TANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCON

26、TROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GCSample Condenses at the head of the Column - Solvent moves quickly away from sample components. TANK PRIMARYPRESSURE - 2000

27、 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GAS BASIC GCSample Condenses at the head of the Column - Solvent moves quickly away from samp

28、le componentsTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE 50O C DETECTORCARRIER GASHelium BASIC GC Solvent is detectedThermal Conduct

29、ivity DetectorThe TCD Filament temperature increases in the presence of non-heliumsample - the filament resistanceincreases with temperature. This ismeasured as peak area or height and is reported by the GCData SystemTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSII

30、NJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE75O C DETECTORCARRIER GAS BASIC GCOven Temperature Program Begins Sample components start to dissolve in and out of the liquid phase - the lighter components move through t

31、he column more quickly - retention in the column is based on: Boiling Point Molecular Weight Solubility in the liquid phaseTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERA

32、TURE 300 O CCOLUMN OVENTEMPERATURE100O C DETECTORCARRIER GAS BASIC GCPeaks continue to separate. Separation is a function of: Carrier Gas flow rateLinear velocity Column Length Thickness of Liquid Phase Oven Temperature ProgramTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROL

33、LER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE125O C DETECTORCARRIER GAS BASIC GCFirst Peak elutes and is detectedTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPOR

34、TTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE175O C DETECTORCARRIER GAS BASIC GCSecond Peak elutes and is detectedTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCO

35、LUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATURE200O C DETECTORCARRIER GAS BASIC GCThird Peak elutes and is detectedTANK PRIMARYPRESSURE - 2000 PSISECONDARY - 100 PSIPRESSURE OR FLOWCONTROLLER25 PSIINJECTIONPORTTEMPERATURE 250OCCOLUMN FLOWPROPORTIONAL TO INJECTION PORT PRESSUREDETECTORTEMPERATURE 300 O CCOLUMN OVENTEMPERATUREPROGRAMMED 50O TO 250O C DETECTORDETECTORCARRIER GASBASIC GC - Detector SelectivitySample - 200 PPM C14, 1