I was looking for a general HS method for the analysis of fragrences impregnated in paper (such as those free samples in magazines).

I tried just ripping the paper into little pieces and sticking them in the vial, but that didn't work very well. Then I tried adding ethanol to the vial and that seemed to work better, but still didn't give all the anticipated components. I also tried the USP method of 100mg sample + 5 ml H2O + 1 g sodium sulfate and that worked the best so far, but when running a straight perfume sample (just a drop in a HS vial) I get about 2-4 times as many components. Am I just expecting too much? Will I not be able to get all the components out of the paper?

So what I would like are the HS parameters, such as vial equilibration time, temps, etc. as well as how to prepare the sample before analysis. Thanks.

If I was adding a liquid, I would add water with a matrix modifier like the USP method. Organic solvents will likely have too high a vapor pressure when heated. If you are using a liquid you will be dealing with two partition coefficients, paper to liquid, then liquid to headspace.

When you run a drop of perfume in a vial you are basically performing a full evaporation headspace technique, where all the volatiles in the sample are vaporized. This is the approach that I would suggest, where you heat the sample to a high temperature and try to evaporate all the volatiles into the headspace.

I would suggest 200C for 5 to 10 minutes on 200 to 500 mg paper with no added solvent. Pressurize the vials to about 5 psi before sampling to ensure the loop is filled adequately. The only sample prep would be to shred the paper like you are already doing. Recovery may be low, so the hotter the temperature the better, as long as you do not decompose any compounds. Be sure your septa can withstand high temperature without excessive bleed.