Materials, capillary column

One of the most important advances in column construction has been the development of open tubular, or capillary columns that contain no packing material (dp = 0). Instead, the interior wall of a capillary column is coated with a thin film of the stationary phase. The absence of packing material means that the mobile phase... 

To minimize the multiple path and mass transfer contributions to plate height (equations 12.23 and 12.26), the packing material should be of as small a diameter as is practical and loaded with a thin film of stationary phase (equation 12.25). Compared with capillary columns, which are discussed in the next section, packed columns can handle larger amounts of sample. Samples of 0.1-10 )J,L are routinely analyzed with a packed column. Column efficiencies are typically several hundred to 2000 plates/m, providing columns with 3000-10,000 theoretical plates. Assuming Wiax/Wiin is approximately 50, a packed column with 10,000 theoretical plates has a peak capacity (equation 12.18) of... 

A capillary column that does not contain a particulate packing material. 

The Liquid Phase. The stationary phase in an open tubular column is generally coated or chemically bonded to the wall of the capillary column in the same way the phase is attached to the support of a packed column. These are called nonbonded and bonded phases, respectively. In capillary columns there is no support material or column packing. 

For capillary columns fused siHca is the material of choice for the column container. It has virtually no impurities (<1 ppm metal oxides) and tends to be quite inert. In addition, fused siHca is relatively easily processed and manufacture of columns from this material is reproducible. In trace analysis, inertness of tubing is an important consideration to prevent all of the tiny amounts of sample from becoming lost through interaction with the wall during an analysis. 

It is clear that the separation ratio is simply the ratio of the distribution coefficients of the two solutes, which only depend on the operating temperature and the nature of the two phases. More importantly, they are independent of the mobile phase flow rate and the phase ratio of the column. This means, for example, that the same separation ratios will be obtained for two solutes chromatographed on either a packed column or a capillary column, providing the temperature is the same and the same phase system is employed. This does, however, assume that there are no exclusion effects from the support or stationary phase. If the support or stationary phase is porous, as, for example, silica gel or silica gel based materials, and a pair of solutes differ in size, then the stationary phase available to one solute may not be available to the other. In which case, unless both stationary phases have exactly the same pore distribution, if separated on another column, the separation ratios may not be the same, even if the same phase system and temperature are employed. This will become more evident when the measurement of dead volume is discussed and the importance of pore distribution is considered. 

Frequently, column problems are caused by the samples that are being analyzed. This type of problem is more likely to occur on capillary columns because of their low capacity for contamination. Contamination results when the sample contains nonvolatile or even semivolatile materials such as salts, sugars, proteins, and so on. Column contamination is more frequently observed with splitless injection because larger amounts of material are being injected on the column. 

The use of SPE with porous materials such as alumina, diatomaceous earth, Horisil and silica for the cleanup of fat-soluble organochlorine pesticides in fatty foods such as meat, flsh, shellfish, milk and vegetable oils has been well documented. The choice of elution solvents is critical because relatively small amounts of lipid in the final extract can cause rapid deterioration of GC capillary columns and also contaminate the gas chromatograph. A number of workers have used a porous material in tandem with Cig to effect an improved cleanup.Di Mucchio employed a multicartridge system comprising Extrelut, silica and Cig to extract organophosphorus pesticides from oils and fatty extracts. Relatively few literature applications include the pyrethroids, but Ramesh and Balasubramanian reported a simple carbon-based SPE method for the analysis of pyrethroids in vegetable oil. 

Fused-silica capillary column, DB-1, 15 m x 0.32-mm i.d., 0.25-p.m film thickness, 100% dimethylpolysiloxane (for plant materials)... 

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