Packed column, chromatograph

Bruno, T.J., A review of capillary and packed column chromatographs, Sep. Purif. Methods, 29, 27,... 

Packed columns Chromatographic columns packed with porous materials to provide a large surface area for interaction with analytes in the mobile phase. 

Gyllenhaal O, Karlsson A, Vessman J. Applications of packed column SFC in the development of drugs. In Anton K, Berger C, eds. Supercritical Fluid Chromatography with Packed Columns. Chromatographic Science Series. Vol. 75. New York Marcel Dekker, 1984, Chap 9. 

Some means is usually provided to control the carrier gas flow. In a packed column chromatograph, this is usually accomplished with a differential pneumatic flow control valve placed in the gas line upstream of the injection port. 

The same approach was further developed for low-temperature capillary GC coupling and different packed column chromatographic set-ups. ... 

Solid Support for Packed Columns—Chromatographic grade diatomateous earth solid support material within a particle size range of 60 to 100 sieve mesh size is recommended. 

This method uses a short, packed column that generally produces a poor resolution of chromatographic peaks. The liquid-liquid extraction used to extract the trihalomethanes is nonselective. Besides the trihalomethanes, a wide range of nonpolar and polar organic constituents, such as benzene and... 

The specialities of chromatographic behaviour of cypermethrin, permethrin, X-cyhalothrin, deltamethrin and fenvalerate were investigated in this work. Gas chromatographic determination was cai ry out with use of packed column with stationai y phase of different polarity (OV-101, OV-210 OV-17) and capillary and polycapillary columns with non-polai ic stationary phase. Chromatographic peak identification was realized with attraction GC-MS method. 

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. 

In a packed column the HETP depends on the particle diameter and is not related to the column radius. As a result, an expression for the optimum particle diameter is independently derived, and then the column radius determined from the extracolumn dispersion. This is not true for the open tubular column, as the HETP is determined by the column radius. It follows that a converse procedure must be employed. Firstly the optimum column radius is determined and then the maximum extra-column dispersion that the column can tolerate calculated. Thus, with open tubular columns, the chromatographic system, in particular the detector dispersion and the maximum sample volume, is dictated by the column design which, in turn, is governed by the nature of the separation. 

Table 1. Typical Chromatographic Operating Conditions for an LC Packed Column...

The packing method supplied by the manufacturer of the gel filtration medium may need to be revised according to the column being selected. It is therefore important to have an understanding about the basic principles governing the packing of chromatographic beds. 

All packing materials produced at PSS are tested for all relevant properties. This includes physical tests (e.g., pressure stability, temperature stability, permeability, particle size distribution, porosity) as well as chromatographic tests using packed columns (plate count, resolution, peak symmetry, calibration curves). PSS uses inverse SEC methodology (26,27) to determine chromatographic-active sorbent properties such as surface area, pore volume, average pore size, and pore size distribution. Table 9.10 shows details on inverse SEC tests on PSS SDV sorbent as an example. Pig. 9.10 shows the dependence... 

Each of the PLgel individual pore sizes is produced hy suspension polymerization, which yields a fairly diverse range of particle sizes. For optimum performance in a chromatographic column the particle size distribution of the beads should be narrow this is achieved by air classification after the cross-linked beads have been washed and dried thoroughly. Similarly, for consistent column performance, the particle size distribution is critical and is another quality control aspect where both the median particle size and the width of the distribution are specified. The efficiency of the packed column is extremely sensitive to the median particle size, as predicted by the van Deemter equation (4), whereas the width of the particle size distribution can affect column operating pressure and packed bed stability. 

The difference in resolution between LC and SFC can be significant enough to turn a marginal LC separation into a viable chromatographic method in SFC. String-ham et al. reported that packed column SFC yielded satisfactory chiral analysis... 

The submitters mixed active anhydrous silica gel with water (12% v>/w) and stored it in a sealed container for at least 24 hours prior to use. A ratio of 60-80 g. of silica gel per gram of crude product was used for column chromatographic separations, and a column was chosen that would give a 10 1 height diameter ratio of adsorbent. Columns were wet-packed with distilled petroleum ether (b.p. 60-68c), and after the crude product had been applied a step-gradient was run rapidly through 2% vjv ether in petroleum ether, 5% ether, and 10% ether. The column was then eluted with 20% vjv ether in petroleum ether until the bromohydrin acetate was obtained. 

The gas chromatograph is better to be equipped both with a thermal conductivity detector (TCD) and with a flame ionization detector (FID). The latter is extremely useful in the analysis of organic substances at low concentrations. Packed columns are normally used, although capillary columns offer certain advantages in the analysis of a variety of products. Some of the major companies that supply gas chromatographs are ... 

Prinsloo SM, De Beer P143R. 1985. Gas chromatographic relative retention data for pesticides on nine packed columns I. Organophosphorus pesticides, using flame photometric detection. J Assoc Off Anal Chem 68 1100-1108. 

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