Column, capillary characteristics

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... 

In 1957 Golay published his ideas for using columns that were not packed but were open tubes.2 These tubes had to have small inside diameters so they became known as capillary columns, but the name open tubular (OT) columns is more descriptive and preferred. These two types of column necessitate slightly different chromatographic instruments, but the discussion that follows will attempt to integrate them together for simplicity of presentation. In the United States, packed columns were much more widely used than OT columns until recently consequently many laboratories have packed column instruments that, since they will not accept OT columns without modification, are still in use even though OT columns would be preferable for many of their separations. Conversion kits and columns with characteristics intermediate between the two extremes are currently popular. 

Based on their constructional features, GC columns can be divided into three main groups packed columns, capillary (open tubular) columns, and porous-layer open tubular columns. Their basic geometrical characteristics are shown in Fig. 7. 

Table 4.23 shows the main characteristics of advanced GC. The use of FID coupled to a high-efficiency capillary column is sufficient to perform routine additive analysis in the 20 ppm concentration range in solution. With adjustment of injection volume in an on-column injector the detection levels surpass... 

Principles and Characteristics Thermospray ionisation (TSP) involves introduction of a relatively high flow (0.2-2mLmin ) of solvent into the ion source of a mass spectrometer, and is therefore suitable as an interface for HPLC-MS, using standard bore columns. A vaporiser probe (essentially a resistively heated capillary tube of about 100 xm i.d.) acts as a transfer line for taking solvent and solute into the source. The source is heated to prevent condensation of the solvent, and the temperature of the capillary is chosen so as to ensure vaporisation of the solvent. In this way, a vapour jet is generated, which contains small, electrically charged droplets if the solvent is at least partially aqueous and... 

Principles and Characteristics Although early published methods using SPE for sample preparation avoided use of GC because of the reported lack of cleanliness of the extraction device, SPE-GC is now a mature technique. Off-line SPE-GC is well documented [62,63] but less attractive, mainly in terms of analyte detectability (only an aliquot of the extract is injected into the chromatograph), precision, miniaturisation and automation, and solvent consumption. The interface of SPE with GC consists of a transfer capillary introduced into a retention gap via an on-column injector. Automated SPE may be interfaced to GC-MS using a PTV injector for large-volume injection [64]. LVI actually is the basic and critical step in any SPE-to-GC transfer of analytes. Suitable solvents for LVI-GC include pentane, hexane, methyl- and ethylacetate, and diethyl or methyl-f-butyl ether. Large-volume PTV permits injection of some 100 iL of sample extract, a 100-fold increase compared to conventional GC injection. Consequently, detection limits can be improved by a factor of 100, without... 

Principles and Characteristics As mentioned already (Section 3.5.2) solid-phase microextraction involves the use of a micro-fibre which is exposed to the analyte(s) for a prespecified time. GC-MS is an ideal detector after SPME extraction/injection for both qualitative and quantitative analysis. For SPME-GC analysis, the fibre is forced into the chromatography capillary injector, where the entire extraction is desorbed. A high linear flow-rate of the carrier gas along the fibre is essential to ensure complete desorption of the analytes. Because no solvent is injected, and the analytes are rapidly desorbed on to the column, minimum detection limits are improved and resolution is maintained. Online coupling of conventional fibre-based SPME coupled with GC is now becoming routine. Automated SPME takes the sample directly from bottle to gas chromatograph. Split/splitless, on-column and PTV injection are compatible with SPME. SPME can also be used very effectively for sample introduction to fast GC systems, provided that a dedicated injector is used for this purpose [69,70],... 

NMR spectroscopy is essential for the structure determination of carotenoid isomers because the TI-NMR signals of the olefinic range are characteristic for the arrangement of the isomers. The stereoisomers of astaxanthin, as shown in Figure 4.16, can be separated on a shape-selective C30 capillary column with methanol under isocratic conditions. 

Possible differences are also well illustrated by 3-thio- and 3-methyl-thiohex-anols and their esters (Table 1). Among these compounds, there is a tendency for the (R) enantiomers to have a typical, fruity aroma. However, for 3-methylthiohexanol (an aroma component of yellow passion fruit) this situation is reversed the (S) enantiomer had the characteristic fruity aroma ( exotisch, fruchtig ).52 For the separation of enantiomers of odorous compounds, enan-tioselective GLC with chiral stationary phases, and MGDC techniques using a conventional capillary column and an enantioselective column are commonly used.53... 

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. 

For each of the analytical problems below, choose the following characteristics of a gas chromatograph that will solve the problem packed or capillary column, inlet, column dimensions and detector. Justify your choice of each. You may need to use additional sources from the bibliography or references. 

Cryofocusing traps are often used to interface purge and trap concentrators to gas chromatographs with capillary columns. The enhanced performance characteristics of the design provide a significant improvement over previous systems. The use of a sophisticated cyrotrap with a thermal gradient ensures that the sample will be trapped and injected with high efficiency. 

CEC is often inappropriately presented as a hybrid method that combines the capillary column format and electroosmotic flow employed in high-performance capillary electrophoresis with the use of a solid stationary phase and a separation mechanism, based on specific interactions of solutes with the stationary phase, characteristic of HPLC. Therefore CEC is most commonly implemented by means typical of both HPLC (packed columns) and CE (use of electrophoretic instrumentation). To date, both columns and instrumentation developed specifically for CEC remain scarce. 

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