WCOT

Capillary columns are of two principal types. Wall-coated open tuhular columns (WCOT) contain a thin layer of stationary phase, typically 0.25 pm thick, coated on the capillary s inner wall. In support-coated open tuhular columns (SCOT), a thin layer of a solid support, such as a diatomaceous earth, coated with a liquid stationary phase is attached to the capillary s inner wall. 

Excellent open tubular columns may now be purchased, providing a number of stationary phases of differing polarity on WCOT and SCOT columns, and whose efficiency, greatly improved sample detectability, and thermal stability surpass those exhibited by packed columns their chief disadvantage is that they have a lower sample capacity than packed columns.65,66... 

The catalyst testing was carried out in a gas phase downflow stainless steel tubular reactor with on-line gas analysis using a Model 5890 Hewlett-Packard gas chromatograph (GC) equipped with heated in-line automated Valeo sampling valves and a CP-sD 5 or CP-sil 13 capillary WCOT colunm. GC/MS analyses of condensable products, especially with respect to O-isotopic distribution, was also carried out using a CP-sil 13 capillary column. For analysis of chiral compounds, a Chirasil-CD capillary fused silica column was employed. 

COMPARISON OF WCOT AND MICROPACKED COLUMNS HAVING SIMILAR PHASE RATIOS... 

Wall-jet cell (LC) 589 Watson-Biemann separator (GC/MS) 963 WCOT... 

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... 

Direct Packed, SCOT, large bore WCOT 200 ng per component Direct quantitation Ease of operation High sample capacity Flash vaporisation Decreased resolution (column requirements)... 

Hot splitless WCOT 0.5 ppm (FID) without preconcentration Lower injection temperature than split Trace analysis Handles dirty samples Automation Flash vaporisation Optimisation required (splitless time, oven temperature, solvent) Limited number of solvents ( solvent effect ) Thermal degradation possible Discrimination possible Poor direct quantification Unsuitable for very polar substances... 

Cold splitless WCOT thick film Idem Reproducible and accurate sampling Controlled evaporation No discrimination on basis of b.p. Large volume injection Low detection limits Minimisation of solvent entering column Allows polar solvents Automation Small sample size introduction (<2 xL) Thermal degradation possible (long residence times of components in liner)... 

Solvent venting WCOT 1 ppm (FID) Limitations in solvent detector compatibility... 

WCOT Wall-coated open-tubular column... 

Analysis of reaction products - Liquid reaction products were analyzed by GC using a capillary column CP-Sil-8CB (WCOT Fused Silica - stationary phase 5% phenyl-methyl-polysiloxane, length 50 m, ID 0.32 mm, OD 0.45 mm film... 

Fused silica capillary columns of various internal bores and of lengths in the range 25 to 50 m are mainly employed for analytical separations. A variety of polar and non-polar column types are available including those open tubular types with simple wall coatings (WCOT), those with coatings dispersed on porous solid-supports to increase adsorbent surface area (SCOT) and porous layer open tubular (PLOT) columns. Important stationary phases include polyethylene glycol, dimethylpolysiloxane and different siloxane copolymers. Various sample introduction procedures are employed including ... 

Gas-Liquid Chromatography. In gas-liquid chromatography (GLC) the stationary phase is a liquid. GLC capillary columns are coated internally with a liquid (WCOT columns) stationary phase. As discussed above, in GC the interaction of the sample molecules with the mobile phase is very weak. Therefore, the primary means of creating differential adsorption is through the choice of the particular liquid stationary phase to be used. The basic principle is that analytes selectively interact with stationary phases of similar chemical nature. For example, a mixture of nonpolar components of the same chemical type, such as hydrocarbons in most petroleum fractions, often separates well on a column with a nonpolar stationary phase, while samples with polar or polarizable compounds often resolve well on the more polar and/or polarizable stationary phases. Reference 7 is a metabolomics example of capillary GC-MS. 

Shafer KH, Cooke M, DeRoos F, et al. 1981. WCOT capillary column GC/FT-IR and GC/MS for identifying toxic organic pollutants. Appl Spectroscopy 35 469-472. 

These have now been superseded by capillary columns, which offer greatly improved separation efficiency. Fused silica capillary tubes are used which have internal diameters ranging from 0.1 mm (small bore) to 0.53 mm (large bore) with typical lengths in excess of 20 m. The wall-coated open tubular (WCOT) columns have the internal surface of the tube coated with the liquid (stationary) phase and no particulate supporting medium is required. An alternative form of column is the porous-layer open tubular (PLOT) column, which has an internal coating of an adsorbent such as alumina (aluminium oxide) and various coatings. Microlitre sample volumes are used with these capillary columns and the injection port usually incorporates a stream splitter. 

Flame ionisation. Flame Photometric and Thermionic Detection use a Perkin—Elmer Sigma 1 gas chromatograph, equipped with an S.G.E on-column injector. The column used was a 25 metrex0.31mm I.D. fused silica WCOT capillary coated with BP-1 (S.G.E), a methyl silicone. 

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