Open tubular columns preparation

Open tubular microcolumns also have been developed, with internal diameters of 1-50 pm and lengths of approximately 1 m. These columns, which contain no packing material, may be capable of obtaining column efficiencies of up to 1 million theoretical plates.The development of open tubular columns, however, has been limited by the difficulty of preparing columns with internal diameters less than 10 pm. 

Porous-layer- open tubular (PLOT) and support-coated open tubular (SCOT) columns are prepared by extending the inner surface area of the capillary tube. A layer of particles can be deposited on the surface or the column wall can be chemically treated to create a porous adsorbent layer. Obviously some of the wall-modified open tubular columns discussed in section 2.3.3 could be... 

Before discussing column preparation procedures a few comments on nomenclature are in order. Open tubular columns are also widely known as capillary columns. The characteristic feature of these columns is their openness, which provides an unrestricted gas path through the column. Thus open tubular colximn rather than capillary column is a more apt description. However, both descriptions appear frequently in the literature and can be emsidered interchangeable. The type of columns discussed so far are also known as wall-coated open tubular columns (WCOT). Here the liquid phase is deposited directly onto the column wall without the inclusion of any additive that might be considered as... 

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... 

The first chiral phases introduced for gas chromatography were either amino acid esters, dipeptide, diamide or carbonyl-bis(amino acid ester) phases [721,724,756-758]. In general, these phases exhitdted poor thermal stability and are infrequently used today. Real interest and progress in chiral separations resulted from the preparation of diamide phases grafted onto a polysiloxane backbone. These phases were thermally stable and could be used to prepare efficient open tubular columns [734,756,758-762]. These phases are prepared from commercially available poly(cyano-propylmethyldimethylsiloxanes) or poly (cyanopropylmethylphenyl-... 

Crego, A. L., Diez-Masa, J. C., and Dabrio, M. V., Preparation of open tubular columns for reversed-phase liquid chromatography, Anal. Chem., 65, 1615, 1993. 

Onuska and Terry [14] have described a method for the determination of chlorinated benzenes in bottom sediment deposits. Sample preparation methods using Soxhlet extraction, ultrasonic extraction or steam distillation were compared. The chlorinated benzenes were characterized by open tubular column gas chromatography with electron capture detection. In recovery studies using sediments with different organic matter contents, the steam distillation method was the most efficient. Detection limits were in the range 0.4-10pg kgy1. 

Chiral SFC can be performed in open tubular [41,42], and packed column [43,44] modes. Packed column SFC can be further categorized into analytical, semipreparative, and preparative SFC [7, 8], Packed column SFC is more suitable for fast separations than open tubular column SFC, since a packed column generally provides low mass transfer resistance and high selectivity [45, 46], Packed column SFC also provides high sample loading capacity [27,47], which can increase sensitivity. Only packed column SFC is suitable for preparative-scale enantioseparation. This chapter will focus on chiral separation using packed column SFC in the analytical scale. 

Packed columns, being easier to prepare than semi-packed columns, offer a more feasible way to avoid many of the problems of open tubular columns while still retaining the advantages of... 

Dhanesar, S.C., Coddens, M.E., and Poole, C.R, Surface roughening by sodium chloride deposition for the preparation of organic molten salt open tubular columns, /. Chromatogr. Sci., 23,320-324,1985. 

In gas chromatography, we have a choice of using open tubular columns or packed columns. For similar analysis times, open tubular columns provide higher resolution and increased sensitivity to small quantities of analyte. Open tubular columns have small sample capacity, so they are not useful for preparative separations. 

The possible use of open tubular columns (OTC) was first suggested by Martin in 1956 but it wasn t until two years later that Golay published the theoretical and practical results for their use. Over the years two excellent books have been published on their preparation and application (24,25). 

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