Supercritical fluid chromatography pressure

Henry, M.C. and Yonker, C.R., Supercritical fluid chromatography, pressurized liquid extraction, and supercritical fluid extraction. Anal. Chem., 78, 390, 2006. 

Supercritical fluid chromatography pressure gradient solvent delivery system Pierce Chemicals Life Science Laboratories Ltd Sedgewick Road Luton... 

The most common mobile phase for supercritical fluid chromatography is CO2. Its low critical temperature, 31 °C, and critical pressure, 72.9 atm, are relatively easy to achieve and maintain. Although supercritical CO2 is a good solvent for nonpolar organics, it is less useful for polar solutes. The addition of an organic modifier, such as methanol, improves the mobile phase s elution strength. Other common mobile phases and their critical temperatures and pressures are listed in Table 12.7. 

The use of separation techniques, such as gel permeation and high pressure Hquid chromatography interfaced with sensitive, silicon-specific aas or ICP detectors, has been particularly advantageous for the analysis of siUcones in environmental extracts (469,483—486). Supercritical fluid chromatography coupled with various detection devices is effective for the separation of siUcone oligomers that have molecular weights less than 3000 Da. Time-of-flight secondary ion mass spectrometry (TOF-sims) is appHcable up to 10,000 Da (487). 

T. L. Chester and J. D. Pinkston, Pressure-regulating fluid interface and phase behavior considerations in the coupling of packed-column supercritical fluid chromatography with low-pressure detectors , ]. Chromatogr. 807 265-273 (1998). 

Supercritical fluid chromatography (SFC) refers to the use of mobile phases at temperatures and pressures above the critical point (supercritical) or just below (sub-critical). SFC shows several features that can be advantageous for its application to large-scale separations [132-135]. One of the most interesting properties of this technique is the low viscosity of the solvents used that, combined with high diffusion coefficients for solutes, leads to a higher efficiency and a shorter analysis time than in HPLC. 

A number of analytical techniques such as FTIR spectroscopy,65-66 13C NMR,67,68 solid-state 13 C NMR,69 GPC or size exclusion chromatography (SEC),67-72 HPLC,73 mass spectrometric analysis,74 differential scanning calorimetry (DSC),67 75 76 and dynamic mechanical analysis (DMA)77 78 have been utilized to characterize resole syntheses and crosslinking reactions. Packed-column supercritical fluid chromatography with a negative-ion atmospheric pressure chemical ionization mass spectrometric detector has also been used to separate and characterize resoles resins.79 This section provides some examples of how these techniques are used in practical applications. 

Supercritical fluid chromatography (SEC) was first reported in 1962, and applications of the technique rapidly increased following the introduction of commercially available instrumentation in the early 1980s due to the ability to determine thermally labile compounds using detection systems more commonly employed with GC. However, few applications of SEC have been published with regard to the determination of triazines. Recently, a chemiluminescence nitrogen detector was used with packed-column SEC and a methanol-modified CO2 mobile phase for the determination of atrazine, simazine, and propazine. Pressure and mobile phase gradients were used to demonstrate the efficacy of fhe fechnique. 

In supercritical fluid chromatography (SFC) the mobile phase is a supercritical fluid, such as carbon dioxide [15]. A supercritical fluid can be created either by heating a gas above its critical temperature or compressing a liquid above its critical pressure. Generally, an SFC system typically has chromatographic equipment similar to a HPLC, but uses GC columns. Both GC and LC detectors are used, thus allowing analysis of samples that cannot be vaporized for analysis by GC, yet cannot be detected with the usual LC detectors, to be both separated and detected using SFC. SFC is also in other... 

Supercritical fluid chromatography employs supercritical fluid instead of gas or liquid to achieve separations. Supercritical fluids generally exist at conditions above atmospheric pressure and at an elevated temperature. As a fluid, the supercritical state generally exhibits properties that are intermediate to the properties of either a gas or a liqiud. Chapter 16 discusses various advantages of SFC over GC and HPLC and also provides some interesting applications. 

The major difference in supercritical fluid chromatography and conventional LC equipment is the pumping systems as well as the safety features installed to maintain higher pressure. Unique SFC equipment differences are ... 

A high-speed injector is required in supercritical fluid chromatography. This is to prevent loss of pressure during the injection process. 

Backstrom B, Cole MD, Carrott MJ, Jones DC, Davidson, G, et al. 1997. A preliminary study of the analysis of Cannabis by supercritical fluid chromatography with atmospheric pressure chemical ionization mass spectroscopic detection. Sci Justice 37 91. 

Finally, supercritical fluid chromatography, in which a supercritical fluid is used as the mobile phase, was introduced by Klesper [164-166]. SFE directly coupled to SFC provides an extremely powerful analytical tool. The efficient, fast and selective extraction capabilities of supercritical fluids allows quantitative extraction and direct transfer of the selected solutes of interest to be accomplished to the column, often without the need for further sample treatment or cleanup. Extraction selectivity is usually achieved by adjusting the pressure of the supercritical fluid at constant temperature or, less often, by changing the temperature of the supercritical fluid at constant pressure. SFE coupled with packed column SFC has found... 

Supercritical fluid chromatography is a form of chromatography in which the system is held near the critical temperature of the mobile phase and pressure utilized to effect solvency and hence migration. 

---