the world leader in serving science plot gc columns and applications bonded traceplot columns
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The world leader in serving science
PLOT GC Columns and Applications
Bonded TracePLOT Columns
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PLOT Columns - Introduction
Porous Layer Open Tubular (PLOT) GC Columns are made by coating a layer of small particles on the inside wall of capillary tubing.
Conventional capillary columns (WCOT, Wall Coated Open Tubular) are made by coating a layer of “liquid” phase on the inside wall of capillary tubing.
PLOT columns are the best choice for analysis of highly volatile compounds such as permanent gases, solvents, and volatile petrochemicals such as refinery gases
PLOT phases:
Phases:TG-BOND Alumina (Na2SO4)TG-BOND Alumina (KCl)TG-BOND Msieve 5ATG-BOND QTG-BOND Q+TG-BOND STG-BOND U
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PLOT – Phase Polarity
TracePLOT Column Phase Polarity Maximum Operating Temperature
TG-BOND Alumina (Na2SO4)Na2SO4 Deactivated Aluminium Oxide Non-Polar 200°C
TG-BOND Alumina (KCl)KCl Deactivated Aluminium Oxide Non-Polar 200°C
TR-BOND Msieve 5AMolecular Sieve (5A) Non-Polar 300°C
TG-BOND Q100% divinylbenzene Non-Polar 280°C / 300°C
TG-BOND Q+Porous divinyl benzene polymer Mid-Polarity 250°C
TG-BOND SDivinylbenzene 4-vinylpyridine Mid-Polarity 250°C
TG-BOND UDivinylbenzene ethylene glycol / dimethylacrylate Polar 190°C
Increasing Polarity
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PLOT – Column Stability
“Modern” PLOT columns are engineered to provide stability and reproducibility:
Reproducibility
• Using advances in technology PLOT column manufacturers are able to accurately control the process used to create the particles, enabling reproducible production of small particles with uniform diameter and pore size.
Stability
• All of the particles are bonded to the tubing and/or to other particles, reducing particle generation. This reduces or eliminates detector spiking and changes in the flow characteristics through the column.
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PLOT – Capillary Tubing
• Polyimide coating provides strength, flexibility and protection from stress corrosion caused by exposure to moisture
• Fused silica tubing
• Control of the Fused Silica dimensions is imperative to the performance of the GC column
• ID• OD• Shape
• Surface Activity
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Solvent Mixture (TG-BOND Q) Argon in Air (TG-BOND Msieve 5A) Gas Standard (H2,O2,N2,CH4,CO) (TG-BOND Msieve 5A)
Hydrocarbons C1-C4 (TG-BOND Alumina Na2SO4)
Hydrocarbons C1-C4 (TG-BOND Alumina KCl)
Application Focus: Refinery Gas Sample (TG-BOND Alumina Na2SO4, Alumina KCl, Q+)
PLOT – Applications
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PLOT – Solvent Mixture
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(1) Methanol(2) Ethanol(3) Acetonitrile(4) Acetone(5) Dichloromethane(6) 1,1,1-Trichloroethene(7) Nitromethane(8) Trans-1,2-Dichloroethene(9) Cis-1,2-Dichloroethene(10) Tetrahydrofuran(11) Ethyl acetate(12) 1,2-Dichloroethane(13) n-Hexane(14) 1,1,1-trichloroethane(15) Benzene(16) Trichloroethylene(17) 1,4-Dioxane(18) 2-Hexanone(19) Pyridine(20) N,N-Dimethylformamide(21) n-Heptane(22) Methycyclohexane(23) Toluene(24) DMSO(25) Chlorobenzene(26) N,N-Dimethylacetamide(27) Ethylbenzene(28) m-Xylene(29) p-Xylene(30) o-Xylene(31) Ethylene glycol 34.21min.
Column: TracePLOT TG-BOND Q 30m x 0.32mm x 10µm
Part Number: 26004-6030Temperature: 100ºC to 240ºC at 5ºC/minute (10 minute hold)Detector Type: FIDCarrier Gas: HeFlow Rate: 1.5 mL/minInjection Volume: 1.0 µLInjection Mode: Split, 220°C
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TRACE GC-TCDArgon
PLOT – Argon in Air
1. Argon 2. Oxygen3. Nitrogen
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3 Column: TracePLOT TG-BOND MSieve 5A 30m x 0.53mm x 50µm
Part Number: 26003-6100
Temperature: 27ºC Isothermal
Detector Type: TCD
Carrier Gas: He
Flow Rate: 4.0 mL/min
Injection Volume: 1.0 µL
Injection Mode: Split (15:1), 100°C
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200TRACE GC-TCDScottGasMix
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PLOT – Standard Gas Mix
1. Hydrogen2. Oxygen 3. Nitrogen4. Methane 5. Carbon Monoxide
Column: TracePLOT TG-BOND MSieve 5A 30m x 0.53mm x 50µm
Part Number: 26003-6100
Temperature: 120ºC Isothermal
Detector Type: TCD
Carrier Gas: He
Flow Rate: 5.0 mL/min
Injection Volume: 1.0 µL
Injection Mode: Split (12:1), 150°C
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PLOT – C1-C4 Hydrocarbons
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Column: TracePLOT TG-BOND Alumina (Na2SO4) 30m x 0.53mm x 10µm
Part Number: 26001-6080
Temperature: 40ºC (1.0 minute hold)
Ramp 1: To 200ºC at 10ºC/minute (10 minute hold)
Detector Type: FID
Carrier Gas: He
Flow Rate: 40.0 mL/min
Injection Volume: 100 µL
Injection Mode: Splitless, 180°C
1. Methane 2. Ethane3. Ethylene 4. Propane 5. Propylene6. n-Butane7. Acetylene8. Propyne
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PLOT – C1-C4 Hydrocarbons
Column: TracePLOT TG-BOND Alumina (KCl) 30m x 0.53mm x 10µm
Part Number: 26002-6080
Temperature: 40ºC (1.0 minute hold)
Ramp 1: To 200ºC at 10ºC/minute (10 minute hold)
Detector Type: FID
Carrier Gas: He
Flow Rate: 40.0 mL/min
Injection Volume: 100 µL
Injection Mode: Splitless, 180°C
1. Methane 2. Ethane3. Ethylene 4. Propane 5. Propylene6. n-Butane7. Acetylene8. Propyne
Note: Change in elution order for peaks 6 & 7
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PLOT - Refinery Gas Analysis
Porous Layer Open Tubular (PLOT) columns are well suited for the analysis of light hydrocarbons such as those found in refinery gases. These highly selective columns are capable of separating low molecular weight hydrocarbons at above ambient temperatures and the columns can then be programmed to higher temperatures to elute higher boiling compounds. The differences in selectivity of several types of PLOT columns is demonstrated by the differences in the separation of light hydrocarbons in a refinery gas sample.
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PLOT - Refinery Gas Analysis-Alumina
PLOT Alumina Columns
• Alumina is often used for the analysis of volatile hydrocarbons due to its selectivity which provides baseline resolution of most isomers at above ambient temperatures. The highly retentive nature of alumina requires that the surface be deactivated with inorganic salts such as sodium sulfate (Na2SO4) or potassium chloride (KCl) to control retention.
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PLOT - Alumina Na2SO4
Instrument – Thermo Scientific TRACE GC Ultra
Column: TracePLOT TG-BOND Alumina Na2SO4, 30m x 0.53mm ID x 20umSample – Refinery Gas #5 Injection – 10l (manual-syringe)Split injectionSplit flow - 52mL/min (Split ratio 13:1)
Liner – 3mm FocusLiner, straight, no glass
woolInjector Temperature - 200°CCarrier Gas – Helium, Constant Flow at 4.0mL/minuteOven Program - 50°C (2 min) - 200°C (3min) at 10°C/min Detection – FID 250°C.
FIGURE 1. TracePLOT™ TG-BOND Alumina Na2SO4- Refinery Gas
1. Methane2. Ethane3. Ethylene4. Propane5. Propylene6. Isobutane7. n-Butane
8. Propadiene9. Acetylene
10. trans-2-Butene11. 1-Butene12. Isobutylene13. cis-2-Butene14. Isopentane
15. n-Pentane16. 1,3-Butadiene17. trans-2-Pentene18. 2-Methyl-2-butene19. 1-Pentene20. cis-2-Pentene
Instrument – Thermo Scientific TRACE GC Ultra
Column: TracePLOT TG-BOND Alumina Na2SO4, 30m x 0.53mm ID x 20umSample – Refinery Gas #5 Injection – 10l (manual-syringe)Split injectionSplit flow - 52mL/min (Split ratio 13:1)
Liner – 3mm FocusLiner, straight, no glass
woolInjector Temperature - 200°CCarrier Gas – Helium, Constant Flow at 4.0mL/minuteOven Program - 50°C (2 min) - 200°C (3min) at 10°C/min Detection – FID 250°C.
FIGURE 1. TracePLOT™ TG-BOND Alumina Na2SO4- Refinery Gas
1. Methane2. Ethane3. Ethylene4. Propane5. Propylene6. Isobutane7. n-Butane
8. Propadiene9. Acetylene
10. trans-2-Butene11. 1-Butene12. Isobutylene13. cis-2-Butene14. Isopentane
15. n-Pentane16. 1,3-Butadiene17. trans-2-Pentene18. 2-Methyl-2-butene19. 1-Pentene20. cis-2-Pentene
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PLOT - Alumina KCl
FIGURE 2. TracePLOT TG-BOND Alumina KCl - Refinery Gas
Instrument – TRACE™ GC Ultra
Column: TracePLOT TG-BOND Alumina KCl,30m x 0.53mm ID x 20umSample – Refinery Gas #5 Injection – 10l (manual-syringe)Split injectionSplit flow - 52mL/min (Split ratio 13:1)Liner – 3mm FocusLiner, straight, no glass woolInjector Temperature - 200°CCarrier Gas – Helium, Constant Flow at 4.0mL/minuteOven Program - 50°C (2 min)-200°C (3min) at 10°C/min Detection – FID 250°C.
1. Methane2. Ethane3. Ethylene4. Propane5. Propylene6. Acetylene7. Isobutane
15. n-Pentane16. 1,3-Butadiene17. trans-2-Pentene18. 2-Methyl-2-butene19. 1-Pentene20. cis-2-Pentene
8. Propadiene9. n-Butane
10. trans-2-Butene11. 1-Butene12. Isobutylene13. cis-2-Butene14. Isopentane
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PLOT - Refinery Gas Analysis-Alumina Results
PLOT Alumina Columns
• Not shown in these chromatograms, alumina Na2SO4 elutes methyl acetylene (a.k.a. propyne) after 1,3-butadiene, while alumina KCl elutes methyl acetylene before 1,3-butadiene.
• The selectivity and retention of alumina will be affected by water, which can come from impure carrier gas and from samples. Shorter retention times are evidence of exposure to water. If this occurs regenerate the column by conditioning for 30 minutes at 200°C under normal carrier gas flow.
• The upper temperature limit for TracePLOT Alumina columns is 200°C. Irreversible changes to the alumina adsorption properties will occur at higher temperatures.
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PLOT - Refinery Gas Analysis-Porous Polymers
Porous Polymer PLOT Columns
• Porous polymer PLOT columns can also be used for the analysis of the refinery gas sample. TracePLOT TG-BOND Q+ is a porous divinyl benzene homopolymer of intermediate polarity incorporating a lower amount 4-vinyl pyridine into the polymer.
• Note: Porous Polymer PLOT columns can tolerate water.
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PLOT – Refinery Gas Analysis-Porous Polymer
Instrument – TRACE GC Ultra
Column: TracePLOT TG-BOND Q+, 30m x 0.53mm ID x 20umSample – Refinery Gas #5 Injection – 10l (manual-syringe)Split injectionSplit flow - 52mL/min (Split ratio 13:1)Liner – 3mm FocusLiner, straight, no glass woolInjector Temperature - 200°CCarrier Gas – Helium, Constant Flow at 4.0mL/minuteOven Program - 50°C (2 min) - 200°C (3min) at 10°C/min Detection – FID 250°C
FIGURE 3. TraceGOLD TG-BOND Q+ - Refinery Gas
1. Methane2. Ethylene 3. Acetylene 4. Ethane5. Propylene6. Propane7. Propadiene
15. Isopentane16. 1-Pentene 17. trans-2-Pentene18. n-Pentane19. cis-2-Pentene20. 2-Methyl-2-butene
8. Isobutane9. Isobutylene
10. 1-Butene 11. 1,3-Butadiene 12. n-Butane13. cis-2-Butene14. trans-2-Butene
Instrument – TRACE GC Ultra
Column: TracePLOT TG-BOND Q+, 30m x 0.53mm ID x 20umSample – Refinery Gas #5 Injection – 10l (manual-syringe)Split injectionSplit flow - 52mL/min (Split ratio 13:1)Liner – 3mm FocusLiner, straight, no glass woolInjector Temperature - 200°CCarrier Gas – Helium, Constant Flow at 4.0mL/minuteOven Program - 50°C (2 min) - 200°C (3min) at 10°C/min Detection – FID 250°C
FIGURE 3. TraceGOLD TG-BOND Q+ - Refinery Gas
1. Methane2. Ethylene 3. Acetylene 4. Ethane5. Propylene6. Propane7. Propadiene
15. Isopentane16. 1-Pentene 17. trans-2-Pentene18. n-Pentane19. cis-2-Pentene20. 2-Methyl-2-butene
8. Isobutane9. Isobutylene
10. 1-Butene 11. 1,3-Butadiene 12. n-Butane13. cis-2-Butene14. trans-2-Butene
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PLOT - Conclusions
PLOT capillary columns are available in a range of phases from non-polar to polar
PLOT columns give minimal particle generation due to the particle being bonded to the inside of the tubing. This enables greater reproducibility both run to run and column to column.
Separation of saturated, unsaturated and branched chain hydrocarbons such as those found in refinery gases is best accomplished on deactivated alumina PLOT columns.
Porous polymers PLOT columns are useful for analysis of volatile substances such as solvents.
Molecular sieve PLOT columns are useful for the analysis of permanent gases.
For additional information, please visit our Chromatography Resource Centre which can be found at: www.thermoscientific.com/chromatography
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