Supercritical fluid chromatography/Fourier transform infrared microspectrometry
โ Scribed by Pentoney, S. L. ;Shafer, K. H. ;Griffiths, P. R. ;Fuoco, R.
- Publisher
- John Wiley and Sons
- Year
- 1986
- Tongue
- English
- Weight
- 322 KB
- Volume
- 9
- Category
- Article
- ISSN
- 0935-6304
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โฆ Synopsis
The feasibility of supercritical fluid chromatography/Fourier transform-infrared (SFC/FT-IR) microspectrometry is presented. In this approach to SFC/FT-IR, the chromatographic eluates are aspirated from the restrictor directly onto the surface of a moving window which then passes into the beam focus of an infrared microscope. Because the mobile phase is gaseous at ambient conditions, elimination of the mobile phase is easily accomplished. Detection limits in all interfaces between a chromatograph and an FT-IR spectrometer in which the mobile phase is eliminated are determined in large part by the area over which thesample is deposited. We have shown that SFCeluates can be condensed at ambient temperature into spots of 100 to 200pm in diameter. The microscope interface therefore serves to increase the sensitivity of the SFC/FT-IR measurements of these spots and detection limits in the low nanogram range are possible. Preliminary results obtained before any real attempts were made to optimize the deposition process indicate that identifiablespectra can beobtained in real timeat the50nglevel for chromatographic separations performed with a 100 pm i.d. wall coated open tubular column. Reproducible reconstructed chromatograms are obtained as each deposited eluate travels through the beam focus of the microscope. The concentration profile of deposited peaks was determined by IR measurements performed at 50 pm increments over the width of the peak to ascertain the deposition size. The results described in this paper, while not yet optimized, indicate the great potential of SFC/FT-IR microspectrometry.
๐ SIMILAR VOLUMES
The combination of capillary supercritical fluid chromatography (SFC) and Fourier transform infrared spectrometry (FTIR) is demonstrated using a low-volume (0.8 pL) flow cell capable of withstanding high pressures. The design of the interface is presented, and its effect on peak shape and detector s