Bimodal poly(4-methylstyrene) was freeze dried either from THF solution or from Benzene one. Conditions of freeze drying would not be fulfilled for THF solution with provided equipment, but a trial might have been done. For Benzene, however, freeze drying should've run in a good manner (until almost all the solvent is gone). Is there an easy way to figure out which solvent was used? What comes to mind is NMR, which is, however, usually not a very good technique for very small concentrations (in this case: of THF/Benzene in polymer)...
Vasilii,
I would suggest head space analysis using gas chromatography/mass spectrometry. Warm a sample of your polymer in a vial with a septum and analyse the headspace over the sample on the GC/MS. You can use either a gas syringe or a solid phase microextraction fibre to take the sample.
This approach works for dried paint samples when we are interested in the solvent used in their preparation.
Vasilii,
I would suggest head space analysis using gas chromatography/mass spectrometry. Warm a sample of your polymer in a vial with a septum and analyse the headspace over the sample on the GC/MS. You can use either a gas syringe or a solid phase microextraction fibre to take the sample.
This approach works for dried paint samples when we are interested in the solvent used in their preparation.
In addition, I have seen several cases for which the amount of solvent remained trapped inside the structure, although quite low, was enough for being detected by FT-IR spectroscopy. A few characteristics bands were enough to identify the solvent in which the gel was prepared. You might try this, as it is a fast and easy method.
Alain
Hello
I would agree that GC-MS is the best method, but as Alain Celzard wrote, FT-IR also works. We have successfully used FT-IR to detect residual toluene in solid polystyrene films, in which the fraction of toluene was well below 5%.
Josef
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