1、Fundamentals of Gas Chromatography,On the Agilent Web http:/lfs- Sept 27, 2001,Fundamentals of Gas Chromatography Components of a GC System,Pneumatic Fundamentals Recommended GC Carrier/Makeup Gas Plumbing,Moisture Trap P/N 5060-9084,Indicating O2 Trap P/N 3150-0528,1/8” Copper Tubing P/N 5180-4196,
2、Gas Purity 99.9995% Minimum Purity,NO LEAKS!,Fundamentals of Gas Chromatography Definitions:,Solubility - Volatile - Vaporize - Separate - Detect - Identify - Qualitative - What is it? Measure - Quantitative - How much?,Carb and Choke Cleaner Comprised of: Acetone, Xylene, Toluene, Propane, Isobutan
3、e, n-Butane Carburetor deposits 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/SPLITLE
4、SS CAPILLARY INLET Capillary Column Stationary Phases,Sample Analysis by Gas Chromatography,Liquid sample is pipetted into a sample vial,Various GC samples,Solids - Headspace,Liquids - Syringe/Injection Port,Gas - Gas Sampling Valve,Liquids - are typically injected by syringe - 1-3 microliters,TANK
5、PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,BASIC GC Component Identification,SEPTUM,GLASS LINER,COLUMN FERRULE GRAPHITE/VESPEL,COLUMN,LIQUID PHASE,SYRINGE,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE
6、 300 O C (20 O C above highest temperature in the oven program),COLUMN OVEN TEMPERATURE PROGRAMMED 50O TO 200O C,DETECTOR,CARRIER GAS Helium,NEXT,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJEC
7、TION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Ready for Sample Injection,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT P
8、RESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Syringe inserted into Injection Port,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PR
9、ESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Plunger depressed - Sample Injected,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,28? PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRE
10、SSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Sample Vaporized Pressure Pulse? Solvent Vapor Volume?,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO I
11、NJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Sample is Swept into the Column by the Carrier Gas,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROP
12、ORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Sample Condenses at the head of the Column - Solvent moves quickly away from sample components.,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLE
13、R,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS,BASIC GC Sample Condenses at the head of the Column - Solvent moves quickly away from sample components,TANK PRIMARY PRESSURE
14、- 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 50O C,DETECTOR,CARRIER GAS Helium,BASIC GC Solvent is detected,Thermal Conductivity Detector The
15、 TCD Filament temperature increases in the presence of non-helium sample - the filament resistance increases with temperature. This is measured as peak area or height and is reported by the GC Data System,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTI
16、ON PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 75O C,DETECTOR,CARRIER GAS,BASIC GC Oven Temperature Program Begins Sample components start to dissolve in and out of the liquid phase - the lighter components move thro
17、ugh the column more quickly - retention in the column is based on: Boiling Point Molecular Weight Solubility in the liquid phase,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSUR
18、E,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 100O C,DETECTOR,CARRIER GAS,BASIC GC Peaks continue to separate. Separation is a function of: Carrier Gas flow rateLinear velocity Column Length Thickness of Liquid Phase Oven Temperature Program,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100
19、PSI,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 125O C,DETECTOR,CARRIER GAS,BASIC GC First Peak elutes and is detected,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI
20、,PRESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 175O C,DETECTOR,CARRIER GAS,BASIC GC Second Peak elutes and is detected,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,P
21、RESSURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE 200O C,DETECTOR,CARRIER GAS,BASIC GC Third Peak elutes and is detected,TANK PRIMARY PRESSURE - 2000 PSI SECONDARY - 100 PSI,PRES
22、SURE OR FLOW CONTROLLER,25 PSI,INJECTION PORT TEMPERATURE 250OC,COLUMN FLOW PROPORTIONAL TO INJECTION PORT PRESSURE,DETECTOR TEMPERATURE 300 O C,COLUMN OVEN TEMPERATURE PROGRAMMED 50O TO 250O C,DETECTOR,DETECTOR,CARRIER GAS,BASIC GC - Detector Selectivity Sample - 200 PPM C14, 1 PPM Lindane,C14,Lind
23、ane,NOTE: The ECD and TCD are NON-Destructive Detectors!,6850/90 - SPLIT/SPLITLESS CAPILLARY INLET Pressure/Flow/Vapor Volume Calculator,6850/90 - SPLIT/SPLITLESS CAPILLARY INLET Column Flow Setting,Optimum Linear Velocity,6850/90 - SPLIT/SPLITLESS CAPILLARY INLET Partial Liner Selection,LINER PART
24、# ID/VOLUME GLASS WOOL DEACTIVATED TYPICAL APPLICATION,5062-3587 4mm/900uL YES YES Splitless - best for fast injection,5181-3316 4mm/900uL NO YES Splitless,5181-8818 2mm/250uL NO YES Splitless - slow inject/small vapor volumes,18740-80200 1.5mm/140uL NO NO Splitless - slow inject/small vapor volumes
25、,5181-3315 4mm/800uL NO YES Splitless - Volatile solvents/fast inject,5183-4647 4mm/800uL YES YES Split - Fast inject/high precision/low discrimination,19251-60540 4mm/900uL YES NO Split - Fast injection,18740-60840 4mm/800uL YES NO Split - Slow injection,All liners are borosilicate glass except 5181-8818, which is quartz.,5062-3587 and 5183-4647 are the liners currently used for 6850/90 OQ/PV procedures.,.,
