The GC Column - Agilent

1 How to Choose the Correct Type and DimensionSimon JonesApplication EngineerThe GC ColumnThings to TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected?

2 What is the sample Matrix?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected? What is the sample Matrix? Can we do sample clean up?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected? What is the sample Matrix? Can we do sample clean up? Is it an established method?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected?

3 What is the sample Matrix? Can we do sample clean up? Is it an established method?--EPA, ASTM, USPG roup/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected? What is the sample Matrix? Can we do sample clean up? Is it an established method?--EPA, ASTM, USP What do we Know about the analytes?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected? What is the sample Matrix? Can we do sample clean up? Is it an established method?

4 --EPA, ASTM, USP What do we Know about the analytes? What else MAY be present in the sample?Group/Presentation TitleAgilent RestrictedPage 2 Things to Is it Volatile enough to chromatograph by GC? Is it a Gas or a Liquid? How are we getting the Sample Injected? What is the sample Matrix? Can we do sample clean up? Is it an established method?--EPA, ASTM, USP What do we Know about the analytes? What else MAY be present in the sample?Group/Presentation TitleAgilent RestrictedPage 2 Group/Presentation TitleAgilent RestrictedPage 3 CAPILLARY Column TYPESL iquid PhaseCarrier GasPorous Layer Open Tube (PLOT)Wall Coated Open Tube (WCOT)

5 Solid ParticlesCarrier GasPacked ColumnsPacked Column Designs and Materials1950 Introduction with the first gas chromatographsPacked Column AnatomyPacked columns 1 12 m length Internal Diameter 4mm Tubing Stainless Steel, UltimetalTMSS, Glass, Nickel, PTFEP acked Column AnatomyPacked columns 1 12 m length Internal Diameter 4mm Tubing Stainless Steel, UltimetalTMSS, Glass, Nickel, PTFE Packing Coated packing Inert, solid support (diatomaceous earth) coated with liquid stationary phase ( OV-1, SE-30, Carbowax 20M, FFAP) Porous packing Porous polymers (PoraPak Q, N, HayeSep Q, R, S, etc.) Porous carbons (Carboxens, Carbosieves, Carbotraps)Packed Column AnatomyPacked columns 1 12 m length Internal Diameter 4mm Tubing Stainless Steel, UltimetalTMSS, Glass, Nickel, PTFE Packing Coated packing Inert, solid support (diatomaceous earth) coated with liquid stationary phase ( OV-1, SE-30, Carbowax 20M, FFAP) Porous packing Porous polymers (PoraPak Q, N, HayeSep Q, R, S, etc.)

6 Porous carbons (Carboxens, Carbosieves, Carbotraps)WCOT CapillaryPacked Column AnatomyPacked columns 1 12 m length Internal Diameter 4mm Tubing Stainless Steel, UltimetalTMSS, Glass, Nickel, PTFE Packing Coated packing Inert, solid support (diatomaceous earth) coated with liquid stationary phase ( OV-1, SE-30, Carbowax 20M, FFAP) Porous packing Porous polymers (PoraPak Q, N, HayeSep Q, R, S, etc.) Porous carbons (Carboxens, Carbosieves, Carbotraps)WCOT CapillaryPLOT CapillaryGroup/Presentation TitleAgilent RestrictedPage 6 STATIONARY PHASE POLYMERSSiRROSiRROSiRRSiRROnmOSiRRnSilox aneSiarylene backboneR=methyl, phenyl, cyanopropyl, trifluoropropylOHCH2CH2O nPolyethylene GlycolStationary Phase% Substitution --polysiloxanesGroup/Presentation TitleAgilent RestrictedPage 7% = # of sites on silicon atoms occupiedBalance is methylOSiRRnSiloxaneR=methyl, phenyl, cyanopropyl, trifluoropropylStationary PhasePoly(ethylene) GlycolGroup/Presentation TitleAgilent RestrictedPage 8100% PEG (DB-WAX)

7 Less stable than polysiloxanesUnique separation characteristicsHOCH2CH2 OHnPoly(Ethylene) GlycolModifiedGroup/Presentation TitleAgilent RestrictedPage 9 Base deactivated (CAM) Acid Modified (DB-FFAP) Extended Temperature RangeWCOT Column Types Mexico 2012 Agilent J&W has over 50 different stationary phase offeringsPLOT columns are primarily, but not exclusively, used for the analysis of gases and low boiling point solutes ( , boiling point of solute is at or below room temperature).PLOT Column Types Agilent J&W PLOT columns begin with the designation of GS (Gas Solid) or HP-PLOT followed by a specific name CP (ChromPack) followed by name 10 stationary phases GS-OxyPLOT/ CP-Lowox GS-Alumina HP-PLOT Al2O3 M HP-PLOT Al2O3 S HP-PLOT Al2O3 KCl / CP-AL2O3/KCl HP-PLOT MoleSieve/ CP-Molsieve5A GS-CarbonPLOT/ CP-CarboBOND HP-PLOT Q / CP PoraBONDQ HP-PLOT U / CP-PoraBONDU GS-GasPro/ CP-SilicaPLOT GS-OxyPLOT: oxygenates HP-PLOT Molesieve: O2, N2, CO, Methane HP-PLOT Alumina and GS-Alumina: complex hydrocarbon gas matrices, ethylene and propylene purity, 1,4-butadiene HP-PLOT Q: freons, sulfides HP-PLOT U.

8 C1 to C7 hydrocarbons, CO2, Polar Hydrocarbons GS-GasPro: freons, sulfurs, inorganic gases GS-CarbonPLOT: inorganic and organic gasesIntegrated Particle Trap PLOT ColumnsGroup/Presentation TitleAgilent RestrictedPage 12 Particle trap is on both ends of the columnOn the front end to help facilitate backflushingwithout blowing particles back into the inlet / valveSpecialty PhasesGroup/Presentation TitleAgilent RestrictedPage 13 columns developed for particular applicationsExamples: DB-UI 8270D, DB-624UI <467>,DB-VRX, DB-MTBE, DB-TPH, DB-ALC1, DB-ALC2, DB-HTSimDis, DB-Dioxin, Select Low Sulfur, CP-Volamine, Select PAH, DB-EUPAH, DB-CLP1 & 2, DB-Select 624 UI 467, CP-LowOx, Select Permanent Inert PhasesGroup/Presentation TitleAgilent RestrictedPage 14DB-1msUIHP-1msUIDB-5msUIHP-5msUIDB-17m sUIDB-624 UIDB-Select 624UI 467DB-WAXUISame Selectivity, more Inertness!

9 Three Types Of Low Bleed PhasesGroup/Presentation TitleAgilent RestrictedPage 15 Phases tailored to mimic currently existing polymersExamples: DB-5ms, DB-35ms, DB-17ms, VF-1701ms New phases unrelated to any previously existing polymersExamples: DB-XLB Optimized manufacturing processesDB-1ms, HP-1ms, HP-5ms, VF-5msSiRROSiRROSiRRSiRROnmSiarylene backboneWhat is Column Bleed??? Back Biting Mechanism of Product FormationGroup/Presentation TitleAgilent RestrictedPage 16+RepeatSiSiSiSiSiSiSiOOOOOOOHCH3CH3CH3 CH3CH3CH3CH3CH3CH3CH3CH3CH3CH3CH3 OHSiSiOSiOSiOCH3CH3CH3CH3CH3CH3CH3CH3 SiOOOCH3H3CH3CH3 CSiSiCH3CH3 OOOOOOSiHOH3 CCH3CH3CH3CH3 SiSiSiSiSiSiCH3CH3CH3CH3CH3CH3CH3CH3CH3 Cyclic products are thermodynamically more stable!

10 DB-5ms StructureGroup/Presentation TitleAgilent RestrictedPage 17CH3 SiSiSiSiOOOODB-5 StructureDB-55% PhenylSiSiSiSiOODB-5ms to match DB-5CH3CH3CH3CH3CH3CH3CH3CH3CH3CH3CH3CH3 DB-35MS VS STANDARD 35% PHENYLB enzo[g,h,i]perylene, 1ngGroup/Presentation TitleAgilent RestrictedMonth ##, 35% PhenylDB-35msGroup/Presentation TitleAgilent RestrictedPage 19 Solid line:DB-5ms 30 m x .25 mm x .25 mmDashed line: DB-5 30 m x .25 mm x .25 mmOven:60oC isothermalCarrier gas: H2at 40 cm/sec1: Ethylbenzene2: m-Xylene3: p-Xylene4: o-XyleneChromatograms are offset on x-axisfor easier viewingWhy is stationary phase type important?Group/Presentation TitleAgilent RestrictedPage 20k2= partition ratio of 2ndpeakk1= partition ratio of 1stpeakInfluence on 12kk= RsNkk=411+ - SelectivityGroup/Presentation TitleAgilent RestrictedPage 21 Relative spacing of the chromatographic peaks The result of all non-polar, polarizable and polar interactions that cause a stationary phase to be more or less retentive to one analytethan anotherOptimizing Selectivity ( )