Deairate your reactor, inject certain volume of H2 into the head-spase by a gas-tight syringe. Analyze your head spase gas. Repeat with different amount of H2. Plot GC peak Surface area versus H2. You get a calibration curve. 

I am agree with Prof. Yurii

Dear Prof. Yurii V Geletti,

Thank you for your valuable information. 

Stander ed gas % (like 5% or 20 % or 99 or etc) is no matter for calibration. 

Different amount of H2 means (volume or % gas).

Looking for your valuable information.

Thanks in advance.

Different amount of H2 means different amounts in moles

Dear Prof. Yurii V Geletti,

Thank you for your valuable information. 

Thanking you,

Dear Rayees Ahmad Rather 

Thank you for your information.

Only one concentration of gas is enough for calibration? or we need to calibrate with different PPM or different concentrations of standard gas. We have 99.99 % pure hydrogen gas how to collect small H2 and inject to GC.

Can you write some information about this.

Thank you. 

Dear D,

Multiple point calibration should be better, especially at low concentration, hard to get line from 0 to 100%.

get a  cylinder  with valve both end, install a pressure gauge (small range) and sampling port between the cylinder and valve. One side, connect to vacuum, empty the cylinder. Fill up the gas with inert gas like nitrogen, read the gauge. then fill up with hydrogen. Using a partial pressure equation, you can get the dilution/mole fraction/concentration for your GC calibration. Good luck

One of the neck of your reactor should have a rubber septa. You can use a gas tight syringe with a volume 0.1-0.2 mL for sampling the head space of your reactor and injection to the GC.  You can use the same syringe or smaller to inject 0.01 -0.1 mL pure H2 into your reactor for calibration. Do multipoint calibration. Use Ar as a carrier  gas in your GC. Your reactor should be deairated and filled with Ar. WE use the same procedure for O2 quantification, see my publications. 

Dear D. Reddy

You can buy small cylinder (canister) with different percentage of hydrogen. For example  5%, 10% and 50% of Hydrogen and remaining volume is your carrier gas. From that you take hydrogen gas, inject into the GC and then make the calibration curve. From the calibration curve  you can find out your unknown samples.

Thillai, can I do the same but for CH4 (and an FID) by diluting a pure gas (Reserach purity ~99.9999%) instead of buying the CH4 at three different concentrations?

Humberto Carvajal-Ortiz ,

Yes, you can do by diluting a pure gas with carrier gas. It could be possible with FID. 

Why did  you switch from H2 to CH4.  Diluting of a gas (mixing of gases) is a very tricky procedure. 

Dear Yurri V Geleti,

Can I please have a look at the your papers that you have mentioned. " WE use the same procedure for O2 quantification, see my publications". 

Thank you

Prof. Yuri V Geletii for being shared valuable information