(or How to Retain Your Gases) - Agilent Column... · (or How to Retain Your Gases) Telephone...
Transcript of (or How to Retain Your Gases) - Agilent Column... · (or How to Retain Your Gases) Telephone...
PLOT Column Selection(or How to Retain Your Gases)
Telephone Number: 816-650-0621Chair Person: Lisa Lloyd
Allen K. VickersApplications Engineer ManagerDecember 6, 2000
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WCOT vs. PLOT
Type
WCOT
PLOT
Stationary Phase
Liquid orgum
Solid
ChromatographicProcess
Gas / Liquidpartition
Gas solidadsorption
Stationary Phases
PolysiloxanesPEG
Porous Polymers,Al2O3,
Zeolites, etc.
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Why Use PLOT Columns?
• Enhanced retention
• Enhanced selectivity
• Permit higher initial oven temperatures than WCOT
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PLOT Columns
"Solid"PorousLayer
Fused Silica Tubing
Ideal for the analysis of gases due totheir increased retention (k) and uniqueselectivity (α) compared to WCOT
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Selectivity Interactions in PLOT Phases
Shape / Size Surface
Zeolites Al2O3
Porous Polymers
Bonded Carbon Bonded SilicaMolecular Sieves
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J&W / Agilent PLOT Columns
• GS-Alumina
• HP-PLOT Al2O3 “M”
• HP-PLOT Al2O3 “S”
• HP-PLOT Al2O3 “KCl”
• HP-PLOT MoleSieve
• GS-CarbonPLOT
• HP-PLOT Q
• HP-PLOT U
• GS-GasPro
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Al2O3 PLOT Columns
• GS-Alumina
• HP-PLOT Al2O3 “M”
• HP-PLOT Al2O3 “S”
• HP-PLOT Al2O3 “KCl”
•Different "polarities" due to different salt deactivation treatments
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Surface Interactions in PLOT Columns
• Vapor pressure always plays a leading role in solute interactions
Gas Flow δ- δ- δ+δ+
neutral
+ + + + + + + + + + + + ++ + + + + + + + + + + + +
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Al2O3 PLOT Column Dimensions Available
• “M”, “S” and “KCl”
• all available in 0.25, 0.32 and 0.53 mm ID
• 15, 30 and 50 meter lengths (depending onID)
• GS-Alumina
• available in 0.53 mm ID
• 15, 30 and 50 meter lengths
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Al2O3 Column Considerations
• Will adsorb water and CO2, affecting retention and resolution.
• Recondition at 200°C to restore performance.
• Not recommended for analysis of “polar” compounds such as alcohols,sulfurs, ketones, etc.
• Upper temperature limit of 200ºC
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Molecular Sieve PLOT Columns
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Zeolite "Backbone"
Size Selectivity
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Molecular Sieve PLOT Columns
• 5Å zeolite for the analysis of fixed and permanent gases:
H2, O2, N2, CO, CH4
He, Ne, Ar, Kr, Xe
SF6
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HP-PLOT MoleSieve
• 0.32 and 0.53 mm ID
• 15 and 30 meter lengths
• Both thin and thick films available
• Choose thin film for standard permanent gas analysis
• Choose thick film for resolution of argon from oxygen at 35ºC
• Upper temperature limit of 350ºC
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Molecular Sieve Column Considerations
• Very high retention stationary phase
• Can be easily fouled by high MW hydrocarbons and polarcompounds
• Use pre-column or backflush if necessary
• Will adsorb water and CO2
• Columns can be reconditioned by holding at elevatedtemperature (350ºC) for several hours
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GS-CarbonPLOT
• Monolithic carbon layer
• Unique selectivity
• Phase formed in situ
• No particle generation
• Extended temperature limit of 360ºC
• Not affected by water
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GS-CarbonPLOT Applications
• Light hydrocarbons (C1-C5)
• Synthesis Gas
• H2, CO, CO2, CH4, N2/O2, H2O
• Trace CO, CO2 and acetylene in ethylene streams (simplification ofASTM D2505)
• Great resolution of air, CO, CO2 and C1-C2 hydrocarbon isomers
• Light solvents
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C1 to C3 Hydrocarbons
0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50
1. Methane2. Acetylene3. Ethylene4. Ethane5. Propyne6. Propylene7. Propane
GS-CarbonPLOT30 m x 0.32 mm I.D., 1.5 µmCarrier: He @ 30 cm/sOven: 125°C for 2 min 125°C to 225°C at 20°/minInjector: Split 1:20, 250°CDetector: MSD, SIM
1
2
34
56
7
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Natural Gas Mixture
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00
1. Methane2. Acetylene3. Propane4. iso-Butane5. n-Butane6. iso-Pentane7. n-Pentane
GS-CarbonPLOT30 m x 0.32 mm I.D., 1.5 µmCarrier: He @ 30 cm/sOven: 125°C for 2 min 125°C to 350°C at 20°/minInjector: Split 1:20, 250°CDetector: MSD, SIM
1 2
3
4
5
6
7
0
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Column: GS-CarbonPLOT 30 m x 0.32 mm I.D. x 3.0 µmJ&W P/N: 113-3133Carrier: Helium at 27 cm/sec (calculated off N2 at 35°C)Oven: 35°C isothermalInjector: 185°C, 1:30 split, 250 µL injection volumeDetector: TCD, 150°C
1. Nitrogen and Oxygen (5% each)2. Carbon monoxide (5%)3. Methane (4%)4. Carbon dioxide (5%)
Permanent Gases
5 2.0 2.5 3.0 3.5 4.0
1
2
4
3
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Solvents
6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00
1. Methylene Chloride 2. Acetone 3. Carbon Disulfide 4. Ethyl Ether 5. Ethyl Acetate 6. Benzene
GS-CarbonPLOT30 m x 0.32 mm I.D., 1.5 µmCarrier: He @ 30 cm/sOven: 125°C for 2 min 125°C to 350°C at 20°/minInjector: Split 1:20, 250°CDetector: MSD, SIM
1
2
3
4
5
6
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GS-CarbonPLOT
• 0.32 and 0.53 mm ID
• 15, 30 and 60 meters
• 0.32 mm ID available in thin and thick film
• Upper temperature limit of 350º/360ºC
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Porous Polymer Phases
• Retention is a combination of size and surface interactionsbetween the analyte and the porous solid phase.
• The polymers are generally homopolymers of divinylbenzeneand divinyl-styrene.
• N, R, Q, T, U phases
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Agilent Porous Polymer PLOT Columns
• HP PLOT-Q
• Bonded polystyrene-divinylbenzene
• HP PLOT-U
• Bonded divinylbenzene/ethylene glycol dimethacrylate
• More polar than “Q”
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HP-PLOT QConsecutive runs for up to 200 headspace injections of alcoholmixture. Excellent stability!!
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Porous Polymer Column Dimensions Available
• Both HP-PLOT Q and HP-PLOT U:
• 0.32 and 0.53 mm ID
• 15 and 30 meter lengths
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GS-GasPro
• Silica-based PLOT column
• Bonded stationary phase
• Unique selectivity
• Highly inert to reactive compounds
• Retention stability unaffected by water
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GS-GasPro
• Upper temperature limit of 260º/300ºC
• No particle generation
• Applications
• CO, CO2
• C1 to C12 hydrocarbons
• trace sulfur analysis
• hydrides (arsine, phosphine, germane, etc.)
• halocarbons
• HCl, NH3
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GS-GasPro Dimensions Available
• Currently only available in 0.32 mm ID
• 5, 15, 30 and 60 meter lengths
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Considerations for PLOTColumn Analysis
• Inlet issues• split versus direct injection• gas sampling valves• low dead volume• column ID and flow rate
• Detector issues• particle generation or “spiking”; particle traps• column ID and flow rate
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Considerations for PLOTColumn Analysis
• Column issues• selectivity• capacity; overloaded peaks• inertness• temperature limits
• Column contamination• efficiency loss; “ghost peaks”; increase in bleed• water, CO2, high molecular weight hydrocarbons?•Carrier gas purifiers