Summary
TMS derivatives of ethoxylates and proproxylates were separated with high resolution, on standard bore and 2 mm packed columns, using both UV and FID detection. A methyl silicone column was found to dramatically decrease retention and allow the elution of heavier oligomers, compared to C18 or C8. Standard bore columns eliminated pre-column splits, and allowed full loop injections. Reproducibility for individual homologs was found to be 0.2–0.3% in retention time and 0.85 to 1.3% in area, over 10 consecutive automated injections.
The UV data was found to be equivalent to “corrected” FID data. Switching to the UV detector at 191 nm, eliminated any need for a fixed restrictor. Slow and fast program rates were shown to provide equivalent mass distribution information.
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Berger, T.A., Todd, B.S. Packed column supercritical fluid chromatography of oligoethers using pure carbon dioxide with flame ionization and ultraviolet detection. Chromatographia 54, 777–781 (2001). https://doi.org/10.1007/BF02492498
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DOI: https://doi.org/10.1007/BF02492498