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Anlaysis of H2, He, CH4, CO2, Ar using TCD

Posted: Tue Apr 25, 2006 4:20 pm
by patelnk
We have Heysep (to separate CO2) and Molsieve 13X (to separate other gases) columns to separate these gases.
Conc. levels are less than 5% for all gases except Ar.
Can anyone please suggest me the best carrier gas to spearate these?
Will helium interfere hydrogen conc. if He is used as carrier?
As nearly 80% is argon, Is argon good choice as carrier gas?
Is there any of these gases poison to these columns?
Thanks,

Re: Anlaysis of H2, He, CH4, CO2, Ar using TCD

Posted: Wed Apr 26, 2006 12:06 pm
by pi3832
We have Heysep (to separate CO2) and Molsieve 13X (to separate other gases) columns to separate these gases.
Conc. levels are less than 5% for all gases except Ar.
Can anyone please suggest me the best carrier gas to spearate these?
Will helium interfere hydrogen conc. if He is used as carrier?
As nearly 80% is argon, Is argon good choice as carrier gas?
Is there any of these gases poison to these columns?
Helium and hydrogen are going to be difficult to separate. You'll need to run at a low flow rate and at near ambient temperatures. If you can easily run sub-ambient, that would be a good thing.

If the CO2 is introduced onto the Molesieve column it can take a long time to elute. If you can use the Hayesep to separate the CO2 from the rest of the sample then have it by-pass the Molesieve, that would also be a good thing.

Running a helium carrier would, obviously, prevent you from quantifying the helium concentration. The 80% argon peak will be so large that it will be hard to quantify it with good repeatability, and it may interfere with other peaks.

Using a carrier that is the same as your balance (a.k.a. matrix) gas is usually the easiest way to go. In this case that's argon. Your sensitivity will be less than with a helium carrier, but if you're looking for components with percent-level concentrations, sensitivity shouldn't be an issue.

Summary:
Argon carrier. Start with low flow and temperature to resolve the helium and hydrogen. Steeply ramp up the temperature and, if possible, the flow, after the helium and hydrogen come off to get off the CO2 in a reasonable time frame.

By chance are you running this on an SRI GC?

analysis

Posted: Wed Apr 26, 2006 2:55 pm
by chromatographer1
Analysis of H2, He, CH4, CO2, Ar using TCD

We have Haysep (to separate CO2) and Molsieve 13X (to separate other
gases) columns to separate these gases less than 5% except Ar.

H2+He require 30ft of 1mm ID Hayesep column at 80°C, less at 20°C.

Can you please send me the chromatographs for these columns with tuned
parameters (temperatures and gas rate)?

Can you please suggest me the best carrier gas to separate these?

Almost any gas will work, but He H2 and N2 are most commonly used, especially to measure He and H2 accurately.

Will helium interfere hydrogen conc. if He is used as carrier?

A problem with linearity and accuracy of H2 measurement exists using He carrier with TCD.

As nearly 80% is argon, Is argon good choice as carrier gas? Yes, but......

Accuracy of H2 measurement using Argon carrier is in doubt.

Is there any of these gases poison to these columns? No.

I would advise you use a pulsed Helium Ionization detector

or

perform dual analysis using He carrier and then N2 carrier for best and accurate results.

Rodney George
Senior Research and Development Scientist
Gas Separations Research
Supelco
595 North Harrison Road
Bellefonte, PA 16823

814-359-5737 voice
814-359-5459 fax
rgeorge@sial.com

Re: Anlaysis of H2, He, CH4, CO2, Ar using TCD

Posted: Thu Apr 27, 2006 4:18 pm
by patelnk
We have Heysep (to separate CO2) and Molsieve 13X (to separate other gases) columns to separate these gases.
Conc. levels are less than 5% for all gases except Ar.
Can anyone please suggest me the best carrier gas to spearate these?
Will helium interfere hydrogen conc. if He is used as carrier?
As nearly 80% is argon, Is argon good choice as carrier gas?
Is there any of these gases poison to these columns?
Helium and hydrogen are going to be difficult to separate. You'll need to run at a low flow rate and at near ambient temperatures. If you can easily run sub-ambient, that would be a good thing.

If the CO2 is introduced onto the Molesieve column it can take a long time to elute. If you can use the Hayesep to separate the CO2 from the rest of the sample then have it by-pass the Molesieve, that would also be a good thing.

Running a helium carrier would, obviously, prevent you from quantifying the helium concentration. The 80% argon peak will be so large that it will be hard to quantify it with good repeatability, and it may interfere with other peaks.

Using a carrier that is the same as your balance (a.k.a. matrix) gas is usually the easiest way to go. In this case that's argon. Your sensitivity will be less than with a helium carrier, but if you're looking for components with percent-level concentrations, sensitivity shouldn't be an issue.

Summary:
Argon carrier. Start with low flow and temperature to resolve the helium and hydrogen. Steeply ramp up the temperature and, if possible, the flow, after the helium and hydrogen come off to get off the CO2 in a reasonable time frame.

By chance are you running this on an SRI GC?
Michael & Rodney,
Thanks for your suggetions,
We run with argon as carrier gas and We are geeting unique peaks of H2, He, CO2 and CH4
We are running this on Parkin Elmer.
Cheers,