Support-coated open tube column

Rasmussen [82] describes a gas chromatographic analysis and a method for data interpretation that he has successfully used to identify crude oil and bunker fuel spills. Samples were analysed using a Dexsil-300 support coated open tube (SCOT) column and a flame ionisation detector. The high-resolution chromatogram was mathematically treated to give GC patterns that were a characteristic of the oil and were relatively unaffected by moderate weathering. He compiled the GC patterns of 20 crude oils. Rasmussen [82] uses metal and sulfur determinations and infrared spectroscopy to complement the capillary gas chromatographic technique. 

Rasmussen [495] has described gas chromatography methods for the identification of hydrocarbon oil spills. The spill samples are analysed on a 30.5m Dexsil-300 support coated open tube (SCOT) column to obtain maximum resolution. 

Open tubular columns are simply capillary tubes in which the inside of the column wall is used as the support for the liquid phase. These wall-coated open tubular columns (WCOT) have the stationary phase distributed in the form of a thin film on the inside surface of the open capillary tube, the walls thus serving as the support. In order to reduce the thickness of the liquid phase film, a porous layer may be formed on the inside wall of the capillary tubing and then coated with the liquid phase to produce a support-coated open tubular column (SCOT). Porous-layer open tubular colunms (PLOT) are similar to SCOT colunms, the difference being that in the former, the stationary phase is deposited on fine crystalline particles or glass powder which is adsorbed onto the walls of the tube. In both cases, the available surface area of the wall is increased, and allows an increased amount of liquid phase to be accommodated in the same length and diameter of tubing. The whisker-walled (WW) colunm consists of whiskers chemically etched on the surface of the wall, which also result in a significant increase in the available surface area. Wall-coated, porous-layer, and support-coated capillary columns are all available as whisker-walled, i.e., WWCOT, WWPLOT, and WWSCOT, respectively. 

Open tubular, or capillary, columns are of two basic typos wall-coated open tubular (W( OT) and support-coated open tubular (SCOT) columns. Wall-coated columns are simply capillary tubes coated with a thin layer of the stationary phase. In support-coated open tubular columns, the inner surface of the capillary is lined with a thin film (—.30 pm) of a support material, such as diatomaceous earth. This type of column holds several times as much stationary phase as docs a wall-coated column and thus has a greater sample capacity. Generally, the efficiency of a SCOT column is less than that of a WCOT column but significantly greater than that of a packed column. 

An alternative method for resolving di Bcultly separable combinations (for example, 2,3-di-O-methylrhamnitol and 2,3,4,6-tetra-O-methylglu-citol acetates) is to use a support-coated, open tube (SCOT column) but these are commercially available for only a restricted number of instruments. ... 

The other types of capillary columns are shown in Figure 6.3, the SCOT or support-coated open tubular column, on the left, and the PLOT or porous layer open tubular column, on the right. SCOT columns contain an adsorbed layer of very small solid support (such as Celite ) coated with a liquid phase. SCOT columns can hold more liquid phase, and have a higher sample capacity than the thin films common to the early WCOT columns. However, with the introduction of cross-linking techniques, stable thick films are possible for WCOT columns, and the need for SCOT columns has disappeared. A few SCOT columns are still commercially available but only in stainless steel tubing. 

Open tubular or capillary columns have open unrestricted path for the gas within the column. These columns are about 15-30 meters in length with an inside diameter of about 0.25 mm. The inner wall of these columns is coated with the liquid stationary phase to about 1 m in thickness. The open tubular columns are of two kinds. One is known as the wall coated open tubular column [WCOT) in which the liquid phase is coated on the column wall. These columns have limited sample capacity and are unsuitable for large-scale separations. The second type is known as support coated open tubular columns (SCOT). In these columns a porous layer is formed on the inside wall of the tubing. The porous layer can either be formed by chemical treatment of the inner wall or is deposited on the inner wall. The support is coated in such a way that the inherent property of the capillary columns, i.e., the unrestricted gas flow is retained. The inert porous layer is then impregnated with the liquid stationary phase. These columns have a higher sample capacity. 

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... 

For a period of time, OT columns that had characteristics intermediate between those of WCOT and packed columns were popular. There were two types, but they were similar. Support coated open tubular (SCOT) columns had a thin layer of solid support coated on the inside wall of a capillary tube of larger diameter than that used for WCOT columns. This layer was coated with stationary liquid similar to packed columns. Porous layer open tubular (PLOT) columns were similar but made differently for example, the solid support was added while the capillary tube was being drawn. With a few exceptions, SCOT and PLOT columns are no longer popular because wide diameter WCOT fused silica columns are as good, more stable (no layer to flake off), and easier to use. Subsequent discussion will be restricted to WCOT columns. 

There are two general types of GC column packed and capillary (also known as open tubular). Packed columns contain a finely divided, inert, solid support material (commonly based on diatomaceous earth) coated with a viscous liquid stationary phase. Most packed columns are 1.5-lOm in length and have an internal diameter of 2-4mm. The original glass capillary columns had an internal diameter of a few tenths of a millimeter and were also one of two types, wall-coated open tubular (WCOT) and support-coated open tubular (SCOT). WCOT columns consist of a capillary tube whose walls are coated with liquid stationary phase. In SCOT columns the inner wall of the capillary is lined with a thin layer of support material such as diatomaceous earth, onto which the stationary phase has been adsorbed. Both of these types of capillary column provide greater separation efficiency than packed columns, but since 1979 they have... 

Two types of columns were employed by Veening et al. One was a 6-ft (or 12-ft) length of borosilicate glass tubing, 2mm i.d., packed with 100-120 mesh Gas Chrom-Q coated with 3.6% SE-30 the second column consisted of a 100-ft x 0.5mm i.d. stainless steel, support coated open tubular (SCOT) column coated with m-bis(m-phen-oxyphenoxy) benzene and Apiezon L (Perkin-Elmer). The injection block for the SCOT column was equipped with a split ratio restrictor of 1 4. The hydrogen flow rate was 24ml/min while that of air was 300ml /min. 

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. 

An open-tubular column is a capillary bonded with a wall-supported stationary phase that can be a coated polymer, bonded molecular monolayer, or a synthesized porous layer network. The inner diameters of open-tubular CEC columns should be less than 25 pm that is less than the inner diameters of packed columns. The surface area of fused silica tubing is much less than that of porous packing materials. As a result, the phase ratio and, hence, the sample capacity for open-tubular columns are much less than those for packed columns. The small sample capacity makes it difficult to detect trace analytes. 

The stationary phase can be a liquid or a solid. If it is a liquid, it can be coated directly on the inside walls of a capillary tube (column), or it can be coated on an inert solid support and be handled like a solid. In effect, then, there are three stationary phase configurations in the first type, a solid (with or without stationary liquid) is packed into a column in the second type, a solid is coated on the surface of a flat, plane material like glass (TLC), and in the third type, a liquid is coated on the inside wall of an open tube (OT). 

The stationary liquid phase is coated on a solid support and packed into a column (packed column GC), or it is coated on the wall of an open tube (WCOT), as has been discussed. The higher efficiency of OT columns has reduced the necessity for many selective liquids, and the number of OT columns necessary to analyze for all types of analytes is smaller than for packed columns. 

The pioneering gas-liquid chromatographic studies in the early 1950s were carried out on packed columns in which the stationary phase was a thin film of liquid retained by adsorption on the surface of a finely divided, inert solid support. From theoretical studies made during this early period, it became apparent that unpacked columns having inside diameters of a few tenths of a millimeter could provide separations that were superior to those of packed columns in both speed and column efficiency. In such capillary columns, the stationary phase was a film of liquid a few tenths of a micrometer thick that uniformly coated the interior of capillary tubing. In the late 1950s, such open tubular columns were constructed the predicted... 

The heart of the chromatograph is the column the first ones were metal tubes packed with inert supports on which stationary liquids were coated. Today, the most popular columns are made of fused silica and are open tubes (OT) with capillary dimensions. The stationary liquid phase is coated on the inside surface of the capillary wall. The two types are shown in... 

In GLC the stationary phase is a liquid acting as a solvent for the substances (.solutes) to be separated. The liquid can be distributed in the form of a thin film on the surface of a solid support, which is then packed in a tube (packed column GC. PCGC) or on the wall of an open tube or capillary column (capillary GC, CGC). The term WCOT (wall-coated open tubular) is u.sed only for capillary columns coated with a thin film of a liquid. In GLC the separation is based on partition of the components between the two phases, the stationary phase and the mobile phase, hence the term partition chromatography. This mode of GC is the most popular and most powerful one. 

Column chromatography is a separation technique in which the stationary bed is within a tube. The particles of the solid stationary phase or the support coated with a liquid stationary phase may fill the whole inside volume of the tube (packed column) or be concentrated on or along the inside tube wall leaving an open, unrestricted path for the mobile phase in the middle part of the tube (open tubular column). Differences in rates of movement through the medium are calculated to different retention times of the sample. 

In GC, we distinguish between separation on packed columns and on capillary columns. Briefly, packed columns have a large inner diameter (2-6 mm) and are filled with an inert support coated with the liquid stationary phase, while capillary columns are open tubes with small inner diameter, the liquid stationary phase coating the inner wall. 

With this method the moving phase is a permanent gas and columns contain either an inert support (e.g. Celite) on whose surface is the stationary liquid phase or else are themselves narrow tubes on whose wall is a thin layer of the stationary phase. The latter are known as wall-coated-open-tubular (WCOT) or capillary columns. Because no inert support is present, the flow of gas is relatively unimpeded and very long thin columns (say 100 m long and only 0.25 mm internal diameter) capable of quite remarkable separations are possible. Columns containing inert support may be either... 

Two types of columns are used. A packed column is one filled with inert, solid particles coated with a liquid stationary phase. Standard tubing is about 0.5 cm in diameter, with lengths ranging from 1 m to 20 m however, columns for large-scale preparative work may be up to 5 cm in diameter and several meters long. Commonly used solid supports are diatomaceous earth, Teflon powder, and glass beads. The stationary liquid must be chosen on the basis of the compounds to be analyzed. A more recently developed and more widely used type of column is the open-tubular or capillary column. This is prepared by coating the inner wall of the column with the stationary liquid phase. The inside diameter of a typical capillary tube is 0.25 mm, and... 

Dynamic in-tube SPME In this system, we assume the use of a piece of fused silica capillary, internally coated with a thin film of extracting phase (a piece of open tubular capillary gas chromatography (GC) column), or that the capillary is packed with extracting phase dispersed on an inert supporting material (a piece of micro-LC capillary column). 

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