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Allen K. Vickers Applications Engineer Manager December 6, 2000

PLOT Column Selection

(or How to Retain Your Gases)

Telephone Number: 816-650-0621 Chair Person: Lisa Lloyd WCOT vs. PLOT

Stationary Chromatographic Stationary Type Phase Process Phases

WCOT Liquid or Gas / Liquid Polysiloxanes gum partition PEG

PLOT Solid Gas solid Porous Polymers,

adsorption Al2O3, Zeolites, etc.

Dial 1-816-650-0621 for e-Seminar Audio Why Use PLOT Columns?

• Enhanced retention • Enhanced selectivity • Permit higher initial oven temperatures than WCOT

Dial 1-816-650-0621 for e-Seminar Audio PLOT Columns

"Solid" Porous Layer Fused Silica Tubing Ideal for the analysis of gases due to their increased retention (k) and unique selectivity (α) compared to WCOT

Dial 1-816-650-0621 for e-Seminar Audio WCOT Analysis

Dial 1-816-650-0621 for e-Seminar Audio PLOT Ethylene Analysis

Dial 1-816-650-0621 for e-Seminar Audio Selectivity Interactions in PLOT Phases

Shape / Size Surface

Zeolites Al2O3 Porous Polymers

Bonded Bonded Silica Molecular Sieves

Dial 1-816-650-0621 for e-Seminar Audio 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

Dial 1-816-650-0621 for e-Seminar Audio 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

Dial 1-816-650-0621 for e-Seminar Audio Surface Interactions in PLOT Columns

+ + + + + + + + + + + + + neutral δ- δ+

Gas Flow δ- δ+

+ +

+ + + + + + + + + + +

• always plays a leading role in solute interactions

Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Propylene Impurities

Dial 1-816-650-0621 for e-Seminar Audio Crude 1,3-

Dial 1-816-650-0621 for e-Seminar Audio Extended HC Mixture

Dial 1-816-650-0621 for e-Seminar Audio 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 on ID)

• GS-Alumina • available in 0.53 mm ID • 15, 30 and 50 meter lengths

Dial 1-816-650-0621 for e-Seminar Audio 0.25 mm ID PLOT Al2O3 “S”

Dial 1-816-650-0621 for e-Seminar Audio Al2O3 Column Considerations

• Will adsorb and CO2, affecting retention and resolution. • Recondition at 200°C to restore performance. • Not recommended for analysis of “polar” compounds such as , sulfurs, ketones, etc. • Upper temperature limit of 200ºC

Dial 1-816-650-0621 for e-Seminar Audio Break Number 1

For Questions and Answers Press *1 on Your Phone to Ask a Question

Dial 1-816-650-0621 for e-Seminar Audio Molecular Sieve PLOT Columns

Size Selectivity

)ORZ

Zeolite "Backbone"

*UDSKLFÃRIÃW\SHÃ.),ÃPROHFXODUÃVLHYH REWDLQHGÃIURPÃWKHÃ,QWHUQDWLRQDOÃ=HROLWH $VVRLFDWLRQÃZHEÃVLWHÃ ZZZL]RRQOLQHRUJ  Dial 1-816-650-0621 for e-Seminar Audio 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

Dial 1-816-650-0621 for e-Seminar Audio Permanent Gases

Dial 1-816-650-0621 for e-Seminar Audio Noble Gases

Dial 1-816-650-0621 for e-Seminar Audio Sulfur Hexafluoride

Dial 1-816-650-0621 for e-Seminar Audio 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 from at 35ºC • Upper temperature limit of 350ºC

Dial 1-816-650-0621 for e-Seminar Audio Molecular Sieve Column Considerations

• Very high retention stationary phase • Can be easily fouled by high MW and polar compounds • Use pre-column or backflush if necessary

• Will adsorb water and CO2 • Columns can be reconditioned by holding at elevated temperature (350ºC) for several hours

Dial 1-816-650-0621 for e-Seminar Audio GS-CarbonPLOT

• Monolithic carbon layer • Unique selectivity • Phase formed in situ • No particle generation • Extended temperature limit of 360ºC • Not affected by water

Dial 1-816-650-0621 for e-Seminar Audio GS-CarbonPLOT Applications

• Light hydrocarbons (C1-C5) • Synthesis Gas

•H2, CO, CO2, CH4, N2/O2, H2O

• Trace CO, CO2 and in ethylene streams (simplification of ASTM D2505)

• Great resolution of air, CO, CO2 and C1-C2 • Light solvents

Dial 1-816-650-0621 for e-Seminar Audio C1 to C3 Hydrocarbons

GS-CarbonPLOT 1. 30 m x 0.32 mm I.D., 1.5 µm 2. Acetylene 7 Carrier: He @ 30 cm/s 3. Ethylene Oven: 125°C for 2 min 125°C to 225°C at 20°/min 4. Ethane Injector: Split 1:20, 250°C 5. Propyne Detector: MSD, SIM 6. Propylene 7. 2

4 3

5 6

1

0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50

Dial 1-816-650-0621 for e-Seminar Audio Natural Gas Mixture

GS-CarbonPLOT 1. Methane 30 m x 0.32 mm I.D., 1.5 µm 2. Acetylene Carrier: He @ 30 cm/s 3. Propane Oven: 125°C for 2 min 5 4. iso-Butane 125°C to 350°C at 20°/min 5. n-Butane Injector: Split 1:20, 250°C 3 Detector: MSD, SIM 6. iso-Pentane 7. n-Pentane

4

1 2

7

6

0 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00

Dial 1-816-650-0621 for e-Seminar Audio Permanent Gases Column: GS-CarbonPLOT 30 m x 0.32 mm I.D. x 3.0 µm J&W P/N: 113-3133 Carrier: Helium at 27 cm/sec (calculated off N2 at 35°C) Oven: 35°C isothermal Injector: 185°C, 1:30 split, 250 µL injection volume Detector: TCD, 150°C 1 1. and Oxygen (5% each) 2. (5%) 2 3. Methane (4%) 4. (5%)

3

4

5 2. 0 2. 5 3. 0 3. 5 4. 0 & Dial 1-816-650-0621 for e-Seminar Audio Solvents 1. Chloride GS-CarbonPLOT 2. 30 m x 0.32 mm I.D., 1.5 µm 3. Carbon Disulfide Carrier: He @ 30 cm/s 3 Oven: 125°C for 2 min 4. Ethyl Ether 125°C to 350°C at 20°/min 5. Ethyl Acetate Injector: Split 1:20, 250°C 6. Detector: MSD, SIM

6

5

1

2

4

6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00

Dial 1-816-650-0621 for e-Seminar Audio 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

Dial 1-816-650-0621 for e-Seminar Audio Break Number 2

For Questions and Answers Press *1 on Your Phone to Ask a Question

Dial 1-816-650-0621 for e-Seminar Audio Porous Polymer Phases

• Retention is a combination of size and surface interactions between the analyte and the porous solid phase. • The polymers are generally homopolymers of divinylbenzene and divinyl-styrene.

• N, R, Q, T, U phases

Dial 1-816-650-0621 for e-Seminar Audio Agilent Porous Polymer PLOT Columns

• HP PLOT-Q • Bonded polystyrene-divinylbenzene • HP PLOT-U • Bonded divinylbenzene/ dimethacrylate • More polar than “Q”

Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Natural Gas on HP-PLOT Q

Dial 1-816-650-0621 for e-Seminar Audio HP-PLOT Q Volatile Solvents

Dial 1-816-650-0621 for e-Seminar Audio HP-PLOT Q Consecutive runs for up to 200 headspace injections of mixture. Excellent stability!!

Dial 1-816-650-0621 for e-Seminar Audio HP-PLOT Q After 150 consecutive direct water injections

Dial 1-816-650-0621 for e-Seminar Audio HP-PLOT U Volatile Solvents

Dial 1-816-650-0621 for e-Seminar Audio HP-PLOT U Impurities in

Dial 1-816-650-0621 for e-Seminar Audio HP-PLOT U Volatile Primary Amines

Dial 1-816-650-0621 for e-Seminar Audio 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

Dial 1-816-650-0621 for e-Seminar Audio GS-GasPro

• Silica-based PLOT column • Bonded stationary phase • Unique selectivity • Highly inert to reactive compounds • Retention stability unaffected by water

Dial 1-816-650-0621 for e-Seminar Audio GS-GasPro

• Upper temperature limit of 260º/300ºC • No particle generation • Applications

•CO, CO2

•C1 to C12 hydrocarbons • trace sulfur analysis • hydrides (arsine, , germane, etc.) • halocarbons

• HCl, NH3

Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio Dial 1-816-650-0621 for e-Seminar Audio GS-GasPro Dimensions Available

• Currently only available in 0.32 mm ID • 5, 15, 30 and 60 meter lengths

Dial 1-816-650-0621 for e-Seminar Audio Considerations for PLOT Column 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

Dial 1-816-650-0621 for e-Seminar Audio Considerations for PLOT Column 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

Dial 1-816-650-0621 for e-Seminar Audio Wrap-up E-Seminar Questions

Thank you for attending Agilent e-Seminars. Our e-Seminar schedule is expanding every week. Please check our website frequently at: www.agilent.com

Dial 1-816-650-0621 for e-Seminar Audio