Question
Asked 16th Aug, 2018

Gas chromatography: components proportion not supposed to vary with oven temperature ?

Hi everyone,
I'm working on a gas chromatograph Clarus 500, with a column able to separate alcohols (Restek RTX 1701, cross-bonded 14% cyanopropylphenyl 86% dimethylpolysiloxane) . I'm analysing a sample of Cetostearyl Alcohol. Theoretical composition is 30% cetyl alcohol C16 / 70% stearyl alcohol. Cetyl alcohol is C16 and stearyl alcohol is C18. So I should obtain those two peaks, with their areas proportional with the proportion of the associated component in the sample.
But there is an unexpected peak between the two peaks. It could be a C17 but I don't know why it should be there. I'm also thinking about a non-linear C18.
The characteristics I have set up are: Injector 1uL/250 degrees - Carrier gas H2 - Flow rate 1mL/min, split ratio 20:1, Oven 40 degrees for 1min, 10 degrees/min, 250 degrees for 3min, Detector FID 250 degrees.
So I find proportions around: 30% cetyl alcohol, 10% unknown peak, 60% stearyl alcohol. Even more strange, these proportions vary when I change the oven temperature. The unknown peak almost disappears.
Thank you for your help, I'm lost with these results!

Most recent answer

Grzegorz Boczkaj
Gdansk University of Technology
Amandine,
thanks for info.
regards,
GB

All Answers (4)

Grzegorz Boczkaj
Gdansk University of Technology
Amandine,
I suggest to increase the injector temp. to 300 deg.C.
Why you use split injection - it can cause discrimination phenomena (lower answer for higher boiling compound).
regards,
G
Mark Krause
Krause Analytical
I agree with the injector temperature increase. I would also increase my split ratio. 20:1 is low for neat components with a 1 uL injection. Higher split flows may help you eliminate the ghosting that you are seeing.
Amandine Colly
Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)
Hi Grzegorz, Hi Mark,
Thank you so much for your answers. My inconsistent results came from my GC that needed to be serviced. Now The results look better. The parameters I have chosen are 50:1 for the split ratio, 300° for the injection and detection, 3mL/min for the flow rate. Oven: 50 to 180° (15°/min) then 180 to 210­° (5°/min).
Apparently, the "C17 peak" is not a ghost, but comes from another compounds. It would be caused by a partial oxidation of one of the components in my sample.
Thank you again,
Amandine
Grzegorz Boczkaj
Gdansk University of Technology
Amandine,
thanks for info.
regards,
GB

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