Packed columns retention

Kovat s retention index (p. 575) liquid-solid adsorption chromatography (p. 590) longitudinal diffusion (p. 560) loop injector (p. 584) mass spectrum (p. 571) mass transfer (p. 561) micellar electrokinetic capillary chromatography (p. 606) micelle (p. 606) mobile phase (p. 546) normal-phase chromatography (p. 580) on-column injection (p. 568) open tubular column (p. 564) packed column (p. 564) peak capacity (p. 554)... 

Bentone-34 has commonly been used in packed columns (138—139). The retention indices of many benzene homologues on squalane have been determined (140). Gas chromatography of C —aromatic compounds using a Ucon B550X-coated capillary column is discussed in Reference 141. A variety of other separation media have also been used, including phthaUc acids (142), Hquid crystals (143), and Werner complexes (144). Gel permeation chromatography of alkylbenzenes and the separation of the Cg aromatics treated with zeofltes ate described in References 145—148. 

The silica dispersion showed the smallest retention volume. It should be noted, however, that the authors reported that the silica dispersion required sonicating for 5 hours before the silica was sufficiently dispersed to be used as "pseudo-solute". The retention volume of the silica dispersion gave the value of the kinetic dead volume, /.e., the volume of the moving portion of the mobile phase. It is clear that the difference between the retention volume of sodium nitroprusside and that of the silica dispersion is very small, and so the sodium nitroprusside can be used to measure the kinetic dead volume of a packed column. From such data, the mean kinetic linear velocity and the kinetic capacity ratio can be calculated for use with the Van Deemter equation [12] or the Golay equation [13]. 

FIGURE 2.13 From measurements of the retention volume, Vr, and the peak width at half peak height, Wr, of a gaussian peak, an estimate of column efficiency N and relative efficiency, HETP, may be calculated. The last figure is for very well packed columns close to 2 X dp. [Reproduced from Sofer and Hagel (1997), with permission.]... 

The nature of the modifier and the modifier concentration impact both retention and selectivity in packed column SFC. SFC offers considerable flexibility in modifier selection because nearly all commonly used organic modifiers, including methanol and acetonitrile, are miscible with CO,. In contrast, methanol and acetonitrile are rarely used as modifiers in normal phase LC because they are immiscible with hexane [68]. 

Prinsloo SM, De Beer P143R. 1985. Gas chromatographic relative retention data for pesticides on nine packed columns I. Organophosphorus pesticides, using flame photometric detection. J Assoc Off Anal Chem 68 1100-1108. 

Under these chromatographic conditions, the CS2 retention time is about 3 min on a fused-silica capillary column and about 2 min on a Teflon Chromosil 330 packed column. 

There are surprisingly few studies of the retention mechanism for open tubular columns but the theory presented for packed columns should be equally applicable. For normal film thicknesses open tubular columns have a large surface area/volume ratio and the contribution of interfacial adsorption to retention should be significant for those solutes that exhibit adsorption tendencies. Interfacial adsorption has been shown to affect the reproducibility of retention for columns prepared with nonpolar phases of different film thicknesses [322-324]. The poor reproducibility of retention index values for columns prepared from polar phases was demonstrated to be c(ue to interfacial... 

Berger [340] has examined the use of pSFC in polymer/additive analysis. As many polymer additives are moderately polar and nonvolatile SFC is an appropriate separation technique at temperatures well below those at which additives decompose [300,341,342], SFC is also a method of choice for additives which hydrolyse easily. Consequently, Raynor et al. [343] and others [284,344] consider that SFC (especially in combination with SFE) is the method of choice for analysing polymer additives as a relatively fast and efficient sample preparation method. Characterisation of product mixtures of nonpolar to moderately polar components encompassing a wide range of molecular masses can be accomplished by cSFC-FID. Unknown polymer additives may be identified quite adequately by means of cSFC-FID by comparison with retention times of standards [343], However, identification by this method tends to be time-consuming and requires that all the candidate compounds are on hand. SFC-FID of some low-to-medium polarity additives on reversed-phase packed columns... 

Particle diameter (packed columns) (dp) Pressure drop increased with smaller particles retention time longer at same inlet pressure Smaller particles sharper peaks... 

In the case of vancomycin [72], an original study was performed to obtain a well-defined stationary phase structure, since it was reasonably assumed that the antibiotic is randomly linked to the silica by one or both of its amino groups, one belonging to the disaccharide portion (primary), and the other one to the heptapeptide core (secondary). Thus, alternate fluorenylmethyloxycarbonyl (FMOC)-amino-protected derivatives were prepared and immobilized in a packed column, and then vancomycin was recovered by cleavage of the protecting groups. The two defined CSPs obtained, when compared with the CSP produced from native randomly linked vancomycin, showed lower retention and enantioselectivity, also if they still separated the same compounds. Thus, no advantages could be found to choose these phases as an alternative to the native vancomycin CSP. 

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