SFC, capillary

Other Chromatographic and Related Techniques. Supercritical fluid chromatography (SFC), capillary electrophoresis (CE), and several related separation techniques are occasionally used in environmental chemical determinations. The CE technique is very... 

A flame ionization detector and MSD were also used for detection of PCBs in SFC. Capillary columns packed with aminosilane-bonded silica and open tubular columns coated with polysiloxane were employed for PCB separation in these works. 

Sample Introduction. The small internal diameters of SFC capillary columns place stringent requirements on saoiple introduction in order to avoid band-broadening due to too large of an injector volume. These requirements have been met using a 0.2- jL internal volume high pressure valve operated in a splitting mode (12). Split ratios of 3 1 to 5 1 are usual. Recently, valves designed specifically for use with capillaries have become available (Valeo Instruments Co., Houston, Texas). These valves offer internal volumes as low as 60-nL and show promise for use in capillary SFC. 

Modern chromatography boasts an impressive range of techniques and instrumentation which to the new practitioner can appear somewhat bewildering. In the past decade alone, a number of techniques have achieved maturity for example, SFC, capillary GC, GC-MS and LC-MS while others such as instrumental TLC and CE offer quite remarkable promise and capability. Over the same period, the established techniques of GC and HPLC have been revolutionised with regards to capability and complexity. 

Chen, E. N. Jr., Drinkwater, D. E., and McCann, J. M., Compositional Analysis of Hydroceffbon Groups in Gasoline-Range Materials by Multidimensional SFC-Capillary GC, Journal of Chromatographic Science, Vol. 33,1995, pp. 353-359. 

GC-SFC Lube oil additives Crude oil, etc. Packed capillary (diol) FID... 

SFC/HPLC (sequential) Polymers Packed capillary (Si02) UV... 

Figure 12.18 LC-SFC analysis of mono- and di-laurates of poly (ethylene glycol) ( = 10) in a surfactant sample (a) normal phase HPLC trace (b) chromatogram obtained without prior fractionation (c) chromatogram of fraction 1 (FI) (d) chromatogram of fraction 2 (F2). LC conditions column (20 cm X 0.25 cm i.d.) packed with Shimpak diol mobile phase, w-hexane/methylene chloride/ethanol (75/25/1) flow rate, 4 p.L/min UV detection at 220 nm. SFC conditions fused-silica capillary column (15 m X 0.1 mm i.d.) with OV-17 (0.25 p.m film thickness) Pressure-programmed at a rate of 10 atm/min from 80 atm to 150 atm, and then at arate of 5 atm/min FID detection. Reprinted with permission from Ref. (23).

An on-line supercritical fluid chromatography-capillary gas chromatography (SFC-GC) technique has been demonstrated for the direct transfer of SFC fractions from a packed column SFC system to a GC system. This technique has been applied in the analysis of industrial samples such as aviation fuel (24). This type of coupled technique is sometimes more advantageous than the traditional LC-GC coupled technique since SFC is compatible with GC, because most supercritical fluids decompress into gases at GC conditions and are not detected by flame-ionization detection. The use of solvent evaporation techniques are not necessary. SFC, in the same way as LC, can be used to preseparate a sample into classes of compounds where the individual components can then be analyzed and quantified by GC. The supercritical fluid sample effluent is decompressed through a restrictor directly into a capillary GC injection port. In addition, this technique allows selective or multi-step heart-cutting of various sample peaks as they elute from the supercritical fluid... 

Figure 12.20 SFC-GC analysis of a sample of aviation fuel (a) SFC separation into two peaks (b and c) coixesponding GC ttaces of the respective peaks (flame-ionization detection used throughout). Reprinted from Journal of High Resolution Chromatography, 10, J. M. Levy et ah, On-line multidimensional supercritical fluid chromatography/capillary gas chromatography , pp. 337-341, 1987, with permission from Wiley-VCH.

Figure 12.23 SFC-SFC analysis, involving a rotaiy valve interface, of a standard coal tar sample (SRM 1597). Two fractions were collected from the first SFC separation (a) and then analyzed simultaneously in the second SFC system (h) cuts a and h are taken between 20.2 and 21.2 min, and 38.7 and 40.2 min, respectively. Peak identification is as follows 1, tii-phenylene 2, chrysene 3, henzo[g/ i]perylene 4, antliracene. Reprinted from Analytical Chemistry, 62, Z. Juvancz et al, Multidimensional packed capillary coupled to open tubular column supercritical fluid chromatography using a valve-switcliing interface , pp. 1384-1388, copyright 1990, with permission from the American Chemical Society.

Figure 12.24 Schematic diagram of the multidimensional packed capillary to open tubular column SFC-SFC system. Reprinted from Analytical Chemistry, 62, Z. Juvancz et al., Multidimensional packed capillary coupled to open tubular column supercritical fluid chromatography using a valve-switching interface , pp. 1384-1388, copyright 1990, with permission from the American Chemical Society.

SFC has been performed with either open capillary columns similar to those used in GC or packed columns transferred from LC, and the instrumentation requirements differ for these two approaches [12]. This chapter will focus on the use of packed column technology because of its dominance in the area of pharmaceutical compound separations. Current commercial instrumentation for packed column SFC utilizes many of the same components as traditional LC instruments, including pumps, injection valves, and detectors. In fact, most modem packed column SFC instm-ments can also be used to perform LC separations, and many of the same stationary phases can be used in both LC and SFC [9]. 

Figure 9.9 Schesatic diagrans of flow-through cell. A, and solvent elimination interfar B, for SFC/FTIR. For A (1) polished stainless steel lig..v.pipe (2) zinc selenide window (3) PTFE spacer (4) viton rubber o-ring (5) graphitized Vespel nicroferrule (6) deactivated fused-silica capillary tubing (7) bolt with Allen nut (8) stainless steel end-fitting and (9) stainless steel body of flow cell.

Cortes, H. J., Campbell, R. M., Himes, R. P., and Pfeiffer, C. D., On-line coupled liquid chromatography and capillary supercritical fluid chromatography large-volume injection system for capillary SFC, ]. Microcol. Sep., 4, 239, 1992. 

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