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Countercurrent extraction of sparingly soluble gases for membrane introduction mass spectrometry.

Membrane introduction mass spectrometry has been applied to inert gas measurements in blood and tissue, but gases with low blood solubility are associated with reduced sensitivity. Countercurrent extraction of inert gases from a blood sample into a water carrier phase has the potential to extract most of the gas sample while avoiding dependence of signal on blood solubility. We present the design of a membrane countercurrent exchange (CCE) device coupled with a conventional direct insertion membrane probe to measure partial pressure of low solubility inert gases in aqueous samples. A mathematical model of steady-state membrane CCB predicts that countercurrent extraction with appropriate selection of carrier and sample flow rates can provide a mass spectrometer signal nearly independent of variations in solubility over a specified range, while retaining a linear response to changes in gas partial pressure over several orders of magnitude. Experimental data are presented for sulfur hexafluoride and krypton in water samples. Optimal performance is dependent on adequate equilibration between the sample and carrier streams, and the large resistance to diffusion in the aqueous phase for insoluble gases presents a substantial challenge to the application of this principle.

Animals↗
PubMed2005

Alkane effect in the Arizona liquid systems used in countercurrent chromatography.

Countercurrent chromatography (CCC) is a separation technique that uses a biphasic liquid system; one liquid phase is the mobile phase, the other liquid phase is the stationary phase. Selection of the appropriate liquid system can be a problem in CCC, since it is necessary to select both the "column" and the mobile phase at the same time as the first is completely dependent on the second. A range of systems with various proportions of solvents were developed to ease this choice; 23 variations of the heptane/ethyl acetate/methanol/water biphasic liquid system were labeled A to Z. This range proved to be extremely useful and became the popular Arizona (AZ) liquid system. However, authors often replace the heptane with hexane. In this work, the chemical compositions of the upper phases and the lower phases of 55 Arizona systems made with various alkanes (pentane, hexane, heptane, isooctane and cyclohexane) were determined by gas chromatography and Karl Fischer titration. The test mixture separated consisted of five steroid compounds. The lower phases were found to have similar compositions when different alkanes were used, but the upper phases were found to change. Exchanging heptane for hexane or isooctane produced minimal changes in the CCC chromatogram, while changing the proportions of the solvents resulted in an exponential change in the retention volumes. The high density of cyclohexane made liquid stationary phase retention difficult. All Arizona systems equilibrated within 30 min, but were not stable: water slowly hydrolyzed the ethyl acetate (as shown by a continuous decrease in the pH of the lower aqueous phase), especially in the water-rich systems (early alphabet letters).

Acetates↗