Summary
High resolution SFC separations of polysiloxanes using standard bore and 2 mm ID packed columns with pressure and density programming of pure carbon dioxide are demonstrated. Independent control of flow and pressure allowed enhanced resolution, particularly at higher molecular weights, over previous separations. More than 150 individual homologs of dimethylsiloxanes were at least partially resolved, allowing differentiation of molecular weight to over 11,000. Pure carbon dioxide appeared to be capable of eluting molecular weights up to an estimated 25,000.
The maximum molecular weight eluted was further extended by the addition of hexane to carbon dioxide. Detection was performed using both the FID (where possible) and UV at 191 nm. Use of the UV detector eliminated the need for a fixed restrictor required by the FID, which simplified routine use.
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Berger, T.A., Todd, B.S. Packed column supercritical fluid chromatography of polysiloxanes using pure and hexane modified carbon dioxide with flame ionization and ultraviolet detection. Chromatographia 54, 771–775 (2001). https://doi.org/10.1007/BF02492497
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DOI: https://doi.org/10.1007/BF02492497