Selectivity changes towards steroids in packed column supercritical fluid chromatography (SFC) induced by temperature and pressure variation

Summary Pressure/temperature variation in SFC was shown to influence selectivity towards steroids. Major changes were observed for polar column packings compared to non-polar packings and variation of the amount of modifier showed that this is valid over the whole investigated range. The effect is underlined by a fall in resolution in the low density range (low pressure/high temperature) for polar stationary phases and appears to be significantly larger than for non-polar phases. Major selectivity shifts induced by variation of the physical properties of the mobile phase are considered to be due to the greater effect of polar modifiers on the nature of polar stationary phases than on non-polar phases.     

A new type of two-dimensional packed + capillary column GC system. I. Theory

Summary To match the need of high efficiency capillary column (plate number N₂, Plate height H₂ and carrier gas linear velocity U₂), a new high efficiency packed column (N₁, H₁ and U₁) at high carrier gas velocity with small capacity factor has been developed in the light of theoretical discussion of factors effecting the column efficiency utilization ratio.     

毛细管电色谱中双电层叠加的研究

通过流动相中电解质浓度对毛细管电色谱柱效能的流动相平均线速度的影响，研究了ＣＥＣ中双电层叠加现象。提出选择合适电解质组成的浓度及在制备色谱柱过程中避免细小和破碎的固定相颗粒进入柱中，以有效地减小双电层叠加作用。     

Effect of ionic additives on the elution of sodium aryl sulfonates in supercritical fluid chromatography

Addition of a small amount of polar solvent (i.e., modifier) to CO2 in packed column supercritical fluid chromatography (SFC) has shown major improvements in both polar analyte solubility and interaction of the polar analyte with the stationary phase. Recently, the addition of an ionic component (i.e., additive) to the primary modifier by one of us has been shown to extend even further the application of SFC to polar analytes. In this work, the effect of various ionic additives on the elution of ionic compounds, such as sodium 4-dodecylbenzene sulfonate and sodium 4-octylbenene sulfonate, has been studied. The additives were lithium acetate, ammonium acetate, tetramethylammonium acetate, tetrabutylammonium acetate, and ammonium chloride dissolved in methanol. Three stationary phases with different degrees of deactivation were considered: conventional cyanopropyl, deltabond cyanopropyl, and bare silica. The effect of additive concentration and additive functionality on analyte retention was investigated. Sodium 4-dodecylbenzene sulfonate was successfully eluted using all the additives with good peak shape under isocratic/isobaric/isothermal conditions. Different additives, however, yielded different retention times and in some cases different peak shapes.     

Supercritical fluid chromatography of petroleum products using flameless sulfur chemiluminescence detection

Supercritical fluid chromatography using flameless sulfur chemiluminescence detection has been investigated for the analysis of sulfur compounds in petroleum products. The chromatography and detection system was easy to implement and exhibited good precision, linearity, selectivity, and sensitivity. A minimum detectable limit of 0.3 pg sulfur/s was obtained, and response to sulfur in different sulfur species was nearly equimolar.     

Chiral separations by capillary electromigration techniques in nonaqueous media. II. Enantioselective nonaqueous capillary electrochromatography

A review on the advantages, peculiarities, and the potential of enantioselective capillary electrochromatography (CEC) in nonaqueous media is presented. Some fundamentals on CEC with particular focus on enantioselective CEC are discussed. The strategies, concepts, preferentially utilized chiral selectors and column technologies that have been utilized to succeed in highly efficient enantiomer separations by nonaqueous CEC are described thoroughly.     

Sulfur hexafluoride as a mobile phase for supercritical fluid chromatography

Summary The capabilities of sulfur hexafluoride as a mobile phase for supercritical-fluid chromatography are investigated. An evaluation of its overall utility on the basis of separations of standard aromatic hydrocarbon odel mixtures performed on a variety of bonded-phase, packed columns with UV detection is presented. The dependence of separation performance upon operational parameters is also examined. A comparative evaluation of the chroamtographic properties of supercitrical sulfur hexafluoride and those of supercritical carbon dioxide is developed from these separations under corresponding supercritical state conditions.     

Carbon dioxide supercritical fluid chromatography-Fourier transform infrared spectrometry

Summary The coupling of carbon dioxide supercritical fluid chromatography with Fourier transform infrared spectrometry (SFC-FTIR) is a powerful tool for the separation and on-line identification of non-volatile compounds. The IR transparency of carbon dioxide in the Fermi resonance bands region versus its density has been studied. Functional groups with stretching vibrations outside the transparent window of carbon dioxide are examined. SFC-FTIR separations allow Gram-Schmidt reconstruction chromatograms or IR window chemigrams with high quality spectra to be obtained. This SFC-FTIR lightpipe (flow cell, beam condensing optics, narrow band detector) has allowed detection limits of 250ng for benzonitrile and 70ng for methyl benzoate to be reached. The feasibility of very rapid SFC-FTIR separations is shown along with the subsequent peak spectra.