Filling columns

However, where small quantities of liquids are involved, a column filled with glass helices will probably give the best results and the cost will not be unduly high. Rings in stainless steel and other metals can be purchased in sizes from to i. ... 

A chromatographic column filled in three sections with ground sugar, chalk, and alumina. When a petroleum extract of spinach leaves is run onto the top of the column, ihe extract spreads down the column, but not uniformly bands of green chlorophylls stop near the top. yellow xanthophyll further down, and red carotene near the bottom. 

Three-phase fluidized bed reactors are used for the treatment of heavy petroleum fractions at 350 to 600°C (662 to 1,112°F) and 200 atm (2,940 psi). A biological treatment process (Dorr-Oliver Hy-Flo) employs a vertical column filled with sand on which bacderial growth takes place while waste liquid and air are charged. A large interfacial area for reaction is provided, about 33 cmVcm (84 inVirr), so that an 85 to 90 percent BOD removal in 15 min is claimed compared with 6 to 8 h in conventional units. 

Packed-Bed Fixed-Film Systems These systems were originaUy termed anaerobic trickhng filters because the first systems were submerged columns filled with stones run under anaerobic conditions (Fig. 25-57). A wide variety of packed media is now used ranging in size from graniiles 40 mesh to 7.5-cm (3—in) stones. Many systems use open structure plastic packing similar to that used in aerobic trickhng filters. 

We studied conditions for the determination of tiametoxam (TM), the active component of the fungicide Actai a (Syngenta, Switzerland) by the method of thin layer chromatography with use of the Perkin-Elmer liquid chromatograph combined with spectrophotometric detector. The 250 mm-long and 4.6 mm in diameter steel column filled with Silasorb was used. 

It is also preferred where suspended solids create a high pressure drop, or dissolved gases create bubbles in the carbon bed. For a downflow or percolation system, an influent line should be installed at the top of the column, with an effluent at the bottom. To prevent the column from draining during operation, the effluent line from the last column should extend from the bottom of the column to above the top of the column. This will keep the column filled with liquid at all times during operation and prevent siphoning from occurring. 

FIGURE 1.4 Optical micrograph of macroporous chromatographic column materials, (a) Monosized particles of 20 tm. (b) Commercial column filling of 12-28 tm. [Reprinted from T. Ellingsen et al. (1990). Monosized stationary phases for chromatography.7. Chromawgr. 535,147-161 with kind permission from Elsevier Science-NL, Amsterdam, The Netherlands.]... 

In 1993, Jorgenson s group improved upon then earlier reverse phase HPLC-CZE system. Instead of the six-port valve, they used an eight-port electrically actuated valve that utilized two 10-p.L loops. While the effluent from the HPLC column filled one loop, the contents of the other loop were injected onto the CZE capillary. The entii e effluent from the HPLC column was collected and sampled by CZE, making this too a comprehensive technique, this time with enhanced resolving power. Having the two-loop valve made it possible to overlap the CZE runs. The total CZE run time was 15 s, with peaks occurring between 7.5 and 14.8 s. In order to save separation space, an injection was made into the CZE capillary every 7.5s,... 

Stemerding (S16) has reported dispersion measurements in a column filled with 13-mm Raschig rings with water and air in countercurrent flow. The dispersion coefficient was observed to be essentially independent of the water flow rate and dependent on the air flow rate only. For increasing air flow rates, the dispersion coefficient passed through a maximum. 

In a dry, 1-1., two-necked flask, equipped with a mechanical stirrer and a reflux condenser fitted with a drying tube, are placed 17.8 g. (0.100 mole) of anthracene (Note 1), 27.2 g. (0.202 mole) of anhydrous cupric chloride (Note 2), and 500 ml. of carbon tetrachloride (Note 3). The reaction mixture is stirred and heated under reflux for 18-24 hours. The brown cupric chloride is gradually converted to white cuprous chloride, and hydrogen chloride is gradually evolved. At the end of the reaction the cuprous chloride is removed by filtration, and the carbon tetrachloride solution is passed through a 35-mm. chromatographic column filled with 200 g. of alumina (Note 4). The column is eluted with 400 ml. of carbon tetrachloride. The combined eluates are evaporated to dryness to give 19-21 g. (89-99%) of 9-chloroanthracene as a lemon-yellow solid, m.p. 102-104° (Note 5). Crystallization of the product from petroleum ether... 

The ionic or polar substances can be seperated without any reaction on specially treated chromatographic columns and detected refractometrically. This is necessary because alkyl sulfosuccinates show only small absorption in the UV-visible region no sensitive photometric detection can be obtained. Separation problems can arise when common steel columns filled with reverse phase material (or sometimes silica gel) are used. This problem can be solved by adding a suitable counterion (e.g., tetrabutylammonium) to the mobile phase ( ion pair chromatography ). This way it is possible to get good separation performance. For an explanation of separation mechanism see Ref. 65-67. A broad review of the whole method and its possibilities in use is given in an excellent monograph [68]. 

This method requires about 40 g of tobacco which are extracted with ethyl acetate in the presence of ascorbic acid. A trace amount of C-NDELA is added as an internal standard for quantitative analytical work. The filtered extract is concentrated and NDELA is enriched by column chromatography of the concentrate on silica gel. The residues of fractions with p-activity are pooled and redissolved in acetonitrile. Initially, we attempted to separate NDELA on a 3% OV-225 Chromosorb W HP column at 210 C using a GC-TEA system with direct interface similar to the technique developed by Edwards a. for the analysis of NDELA in urine (18). We found this method satisfactory for reference compounds however, it was not useful for an optimal separation of NDELA from the crude concentrate of the tobacco extract (Figure 4). Therefore, we silylated the crude concentrate with BSTFA and an aliquot was analyzed by GC-TEA with direct interface. The chromatographic conditions were 6 ft glass column filled with 3% OV-... 

FIGURE 11.11 (a) Schematic representation of PLC of Heracleum sosnowskyi fruit crude extract, system silanized silica/MeOH + HjO (6 4) (b) rechromatography of fractions I and II from the plate a on Lobar-type column filled with Horisil eluted with 5% MeCN in CHjClj -I- H (7 3) fractions controlled by analytical HPLC in system ClS/MeOH -i- HjO (6 4). For abbreviations, see Figure 11.5. (For details, see Waksmundzka-Hajnos, M. and Wawrzynow-icz, T., /. Planar Chromatogr, 3, 439 141, 1990.)... 

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