I am running a high-pressure reaction containing rice straw, methanol, and catalyst to produce lignocellulosic material. The final pressure has a difference of 4-5 bar once the reactor is cooled down. Initially, the reactor is purged with nitrogen. Literature suggests hydrogen is produced due to the presence of catalyst and methanol and solvent and it helps in depolymerization reaction. I want to know if there is any GC method to determine the presence of hydrogen in the residual gas after the reaction is completed? Any other analytical methods? For now, I am just collecting the vent gas in a mylar balloon. Any suggestions would be very helpful.
Should hydrogen be produced, it would also be dissolved in the liquid phase and this is detectable by 1H NMR (characteristic shift around 4.5 ppm) - provided the mixture is not too complex and does not contain paramagnetic compounds.
Burning splint test
A splint is lit and held near the opening of the tube, then the stopper is removed to expose the splint to the gas. If the gas is flammable, the mixture ignites. This test is most commonly used to identify hydrogen, which extinguishes with a distinctive 'squeaky pop' sound.
Hi,
GC-Thermal desorption method will be used to identify and quantify the gases in the sample but need to be careful in carrier gas for run the analysis. Ii am herewith attached reported paper for your perusal, it may useful to you.
Indirect hydrogen analysis by gas chromatography coupled to mass spectrometry (GC-MS). 2013 Aug;48(8):914-8.J Mass Spectrom
doi: 10.1002/jms.3232.
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