Importance of the topic
Permanent gas and light hydrocarbon analysis is crucial in petrochemical, environmental and industrial gas monitoring to ensure product quality, process control and regulatory compliance. Accurate separation of small molecules like hydrogen, oxygen, nitrogen, carbon monoxide, carbon dioxide and light hydrocarbons enables detection of impurities and optimization of manufacturing processes.
Objectives and study overview
This application note introduces Carboxen-based PLOT capillary columns for gas chromatography, focusing on two phases Carboxen-1010 and Carboxen-1006. The document aims to present column preparation, performance parameters and separation capabilities for permanent gases and C1–C4 hydrocarbons following ASTM D3612-96 and related methods.
Methodology and instrumentation
Carboxen PLOT columns are prepared by bonding spherical carbon molecular sieves onto capillary walls using high-temperature resistant adhesive (up to 360 °C). Individual columns are tested for efficiency, inertness and retention. Performance evaluations were conducted on gas chromatographs equipped with thermal conductivity detectors, methanizer-coupled flame ionization detectors and programmed temperature control. Key parameters include:
- Column dimensions: 30 m × 0.53 mm I.D.
- Oven program: 35 °C hold then ramp to 250 °C at 24 °C/min
- Injection: valve at 200 °C, sample volume 10 µL
- Carrier gases: Argon 3.0 mL/min for Carboxen-1010, Helium 10.0 mL/min for Carboxen-1006
Main results and discussion
Carboxen-1010 demonstrated effective separation of permanent gases (H2, O2, N2, CO) and C1 analytes (CH4, CO2) with clear resolution under ASTM D3612 conditions. The hydrophobic surface prevented water-induced shifts, eliminating the need for thermal conditioning. Carboxen-1006 exhibited enhanced kinetics for mixtures including C2–C4 hydrocarbons. Multiporous structure with macro-, meso- and micropores enabled rapid access and separation, including propylene and butane with high peak symmetry and minimal tailing.
Benefits and practical applications
- Robust high-temperature operation ensures compatibility with temperature programming
- Hydrophobic surface stability allows direct analysis of moisture-containing samples
- Wide analyte range from permanent gases to C4 hydrocarbons benefits transformer gas analysis, environmental monitoring and petrochemical quality control
- Single-run multi-component analysis reduces cycle times and carrier gas consumption
Future trends and potential applications
Integration with portable and micro-GC systems is a promising direction for field analysis. Advances in carbon molecular sieve synthesis may yield phases with tailored pore sizes for specific gas families. Coupling PLOT columns with advanced detectors and data analytics will enhance sensitivity and selectivity for trace impurities in emerging energy applications such as hydrogen fuel and biogas.
Conclusion
Carboxen GC PLOT capillary columns offer a versatile and reliable solution for permanent gas and light hydrocarbon separations. Their unique pore architectures and robust bonding technology ensure high efficiency, inertness and water resistance, making them ideal for a variety of analytical challenges in industry and research.
Reference
Supelco Product Information 2003. Carboxen GC PLOT Capillary Columns. Sigma-Aldrich Co.
Content was automatically generated from an orignal PDF document using AI and may contain inaccuracies.
Product Information
595 North Harrison Road
Bellefonte, PA 16823-0048 USA
Telephone 800-247-6628 ● 814-359-3441
Fax 800-447-3044 ● 814-359-3044
email: [email protected]
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sigma-aldrich.com/supelco
Carboxen GC PLOT Capillary Columns
Supelco PLOT Columns
Supelco PLOT columns are an ideal choice for many permanent gases
and light hydrocarbon analyses in the petrochemical industry.
Supelco PLOT columns are prepared using a proprietary patented
adhesive technology that firmly bonds the adsorbent particles to the
wall of the capillary column. The adhesive also bonds the particles to
each other, eliminating particle loss during routine analysis or rapid
temperature programming. A significant feature of the adhesive is its
high temperature limit, greater than 360 °C, which makes the
operating temperature of the column a function of the particles
used, not the adhesive.
Supelco PLOT columns are individually tested for efficiency, inert-
ness, and retention. Each column is shipped with a chromatogram
demonstrating column performance that can be expected.
Carboxen Capillary PLOT Columns
Carboxen™ PLOT columns are the appropriate choice for permanent
gas mixtures that include permanent gases and C1 to C3 hydrocar-
bons. Carboxen PLOT column chemistry is based on synthetic,
spherical carbon molecular sieves that are synthesized in-house
under carefully controlled conditions. Each Carboxen has a unique
combination of pore size, pore structure, and surface area. These two
features permit analyte separations not possible with other PLOT
columns.
Carboxen-1010
A larger pore structure (7 Å ) and increased number of pores make
Carboxen-1010 PLOT columns the preferred choice over zeolite Mol
Sieve 5A PLOT columns for effectively separating oxygen, nitrogen,
and larger analytes up to C3. Because the Carboxen surface is
hydrophobic, samples containing water do not cause retention time
shifts, eliminating the need for thermal conditioning as necessary
with Mol Sieve 5A PLOT columns.
Carboxen-1006
Carboxen-1006 has a multiporous pore structure. The presence of
large macropores and mesopores allow for effective access of the
7 Å micropores for fast kinetic applications. This unique pore
structure makes Carboxen 1006 suitable for permanent gases and
light hydrocarbons. The inert surface chemistry makes it an excellent
choice for formalin analyses.
Figure A. Transformer Gas Analysis for ASTM Method D3612-96 on Carboxen-1010 PLOT Column
column:
Carboxen-1010 PLOT, 30 m x 0.53 mm I.D. (25467)
oven:
35 °C (7.5 min.) to 250 °C at 24 °C/min.
inj.:
200 °C
det.:
TCD/methanizer-FID, 230 °C
flow rate:
Argon, 3.0 mL/min.
valve:
150 °C
injection:
10.0 µL valve injection
sample:
500 ppm each, transformer gas for ASTM Method D3612-96
G002209
0
2
4
6
8
1
2 3
10
12
14
16
18
20
4
5
6
7
8
9
Min
1.
Hydrogen
2.
Oxygen
3.
Nitrogen
4.
Carbon monoxide
5.
Methane
6.
Carbon dioxide
7.
Acetylene
8.
Ethylene
9.
Ethane
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sigma-aldrich.com/supelco
Figure B. Permanent Gases with C2 to C4 Hydrocarbons on Carboxen-1006 PLOT Column
column:
Carboxen-1006 PLOT, 30 m x 0.53 mm I.D. (25461)
oven:
35 °C (1.0 min.) to 250 °C at 24 °C/min.
inj.:
200 °C
det.:
TCD, 230 °C
flow rate:
Helium, 10.0 mL/min.
valve:
150 °C
injection:
10.0 µL valve injection
sample:
Permanent gases and C2 to C4 hydrocarbon mix
794-0618
Ordering Information:
Carboxen-1010 PLOT
Dimension
Max. Temp.
Cat. No.
30 m x 0.32 mm I.D.
250 °C
24246
30 m x 0.53 mm I.D.
250 °C
25467
Carboxen-1006 PLOT
Dimension
Max. Temp.
Cat. No.
30 m x 0.32 mm I.D.
250 °C
24241-U
30 m x 0.53 mm I.D.
250 °C
25461
1.
Nitrogen (bulk)
2.
Carbon monoxide (215 ng on column)
3.
Methane (430 ng on column)
4.
Carbon dioxide (215 ng on column)
I.
Water impurity
5.
Acetylene (430 ng on column)
6.
Ethylene (430 ng on column)
7.
Ethane (430 ng on column)
8.
Methyl acetylene (215 ng on column
9.
Propylene (215 ng on column
10.
Propane (215 ng on column)
11.
n-Butane (215 ng on column)
1
2
3
4
5
6
7
8
9
10
11
0
4
8
12
16
Min
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