Can anyone suggest a GC-MS or HPLC-MS analytical method to identify Acrolein in a solid sample (soluble in ethanol), without any pretreatement of the sample (no purge and trap, no SPME)?
Dear Benedetta,
I found a GC- Headspace method. If you google 5991-8096EN you can find an example method.
No headspace sampler needed. I did this headpace vials and injected manually with a gas tight glass syringe 1mL. I hope this is usefull
Dear Bernard,
thank you very much for your answer.
If I understood well, you finally did a direct injection.. Nevertheless, as I can use a headspace autosampler, do you think this will be better?
I think a Headsspace GC-MS Method with Autosampler ist a good choice.
Acroleine is a volatile compound, so it will be a propper solution.
The only aspect you have to observe ist the sensitivity.
Headspace methodes are not high senstive, so trace concentrations are only availible in SIM Methods.The Equilibrationtimes for solids is also mostly longer then for liquids. If Sensitivity and time is no problem, try it out.
Upgrade of my anwer
I had a look on the Agilent method for Acroleine, the cloumn used in this method is not GC-MS compatible. the phase ist ok and usefull, but the inner diameter is to large and the columne flow ist to high for GC-MS.
You better use the same phase but in a diameter of about or less 0.25 mm ,but,more length maybe 50 m. Your GC-MS will say thank you.
Daer Joachim,
yes, I noticed the "problem" in column diameters.
Nevertheless now my concern is about sample tratement: in HJ Method 679-2013 they use matrix modifiers...do you think it is necessary?
One possibility to increase sensitivity is to use the ethanol extraction and do headspace with the er than ok extract. Other possibility would be pulverize your sample an do headspace then.
if ethanol is used you can add sodium chloride to move the equilibrium to the gas phase
Dear Benedetta, in order to give you a useful answer, I need more informations. Are there any other volatile substances in the sample? What matrix does your sample have? I guess silica nanoparticles. You should definitely avoid reactions with modifiers and your matrix. Do you observe adsorption effects of solvents that you use in your laboratory? Modifiers are usually used for liquid samples (salting out). Unfortunately, this does not work with solids. I agree with Bernhard that a surface enlargement produces higher peak intensities. An increase in the equilibration temperature may also help.
I am currently working on functional textiles with regard to odor components. However, I use an SPME for this. Headspace method. The concentration range is 40 to 400 µg / kg, unfortunately the static headspace does not help here. I also tried to increase the peak intensity with additives, unfortunately without success. I use a VF5-MS as a separation column with the dimensions 30m x 0.25mm x 0.5 µm. Since I have many different applications on my GC-MS, I need a universal column here. In the appendix you will find a chromatogram with various aldehydes, you can see that even universal columns produce acceptable chromatograms.
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