Carbon silica packings

In his original work, Tswett examined a number of different column packings, but the vast majority of packing materials that are in use in LC today, are based on silica gel. This is true, even for the recently Introduced carbon based packings (2) as they also require silica gel for their fabrication. Without silica gel LC would have a very limited performance and very limited areas of application. Furthermore, until some substance is... 

SFC is a relatively new technique using a silica-packed column in which the mobile phase is a gas, typically carbon dioxide, which has been converted to a supercritical fluid under controlled pressure and temperature. Sample is injected as in a GLC system, carried by the working fluid onto the packed column where separation occurs by either adsorption or partition. The separated components then wash into a high-pressure UV detector flow cell. At... 

The amount of carbon introduced into the stationary phase by the functional group is referred to as the carbon load, and it is measured as a weight percentage of the bulk silica packing. The carbon load is altered by... 

The attachment of particular solute molecules to the surface of the particulate sorption packing material can be achieved by a number of different methods, which are outside the scope of this paper. There are a large number of different sorption materials and complex physical and chemical interactions which must be considered. The most common sorption materials are activated carbon, silica gel, activated alumina, molecular sieves, and ion exchange resins. This chapter deals with the industrial aspects of handling these materials and operating process-scale equipment, but does not look at the choice of sorption material for a particular process. 

The basic concept of a H2 PSA process is relatively simple. The impurities from the H2-containing feed gas mixture are selectively adsorbed on a micro- and meso-porous solid adsorbent (zeolites, activated carbons, silica and alumina gels) at a relatively high pressure by contacting the feed gas with the solid in a packed column of... 

Li, W. Malik, A. Lee, M.L. Fused silica packed capillary columns using carbon dioxide slurries. J. Microcol. Separ. 1994, 6 (6), 557-563. 

Berek, D and Novak, I., Silica gel and carbon column packings in HPLC, Chromato-graphia, 582-590 (1990). 

A new analytical method, pressurized capillary electrochromatography (pCEC) with AD using 1.5 mm reversed phase nonporous silica packed columns has been developed for the rapid separation and determination of four Sudan dyes in hot chili [36]. The influence of several experimental parameters on the retention behavior has been investigated. The electrochemical oxidation of Sudans I-FV separated by pCEC can be reliably monitored with a carbon electrode at 0.95 V (vs. Ag/AgCl). Fast and efficient separation of the analytes was achieved within 7 min by pCEC under the optimum conditions. To evaluate the feasibility and reliability of this method, the proposed pCEC-AD method was further demonstrated with hot chili samples spiked with Sudan dyes. 

Mcntasty el al. [35] and others [13, 36] have measured methane uptakes on zeolites. These materials, such as the 4A, 5A and 13X zeolites, have methane uptakes which are lower than would be predicted using the above relationship. This suggests that either the zeolite cavity is more attractive to 77 K nitrogen than a carbon pore, or methane at 298 K, 3.4 MPa, is attracted more to a carbon pore than a zeolite. The latter proposition is supported by the modeling of Cracknel et al. [37, 38], who show that methane densities in silica cavities will be lower than for the equivalent size parallel slit shaped pore of their model carbon. Results reported by Ventura [39] for silica xerogels lead to a similar conclusion. Thus, porous silica adsorbents with equivalent nitrogen derived micropore volumes to carbons adsorb and deliver less methane. For delivery of 150 V./V a silica based adsorbent would requne a micropore volume in excess of 0.70 ml per ml of packed vessel volume. 

The column was 25 cm long, 4.6 mm I.D. and packed with Partisil 10. It is seen that linear curves were obtained for three different solutes and two different moderators in n-heptane. Scott and Beesley [14] obtained retention data for the two enantiomers, (S) and (R) 4-benzyl-2-oxazolidinone. The column chosen was 25 cm long, 4.6 mm I.D. packed with 5 mm silica particles bonded with the stationary phase Vancomycin (Chirobiotic V provided by Advanced Separations Technology Inc., Whippany, New Jersey). This stationary phase is a macrocyclic glycopeptide Vancomycin that has a molecular weight of 1449.22, and an elemental composition of 54.69% carbon. 

Figure 12.7 Cliromatograms of a polycarbonate sample (a) microcolumn SEC ti ace (b) capillary GC ti ace of inti oduced fractions. SEC conditions fused-silica (30 cm X 250 mm i.d.) packed with PL-GEL (50 A pore size, 5 mm particle diameter) eluent, THE at aElow rate of 2.0ml/min injection size, 200 NL UV detection at 254 nm x represents the polymer additive fraction ti ansfeired to EC system (ca. 6 p-L). GC conditions DB-1 column (15m X 0.25 mm i.d., 0.25 pm film thickness) deactivated fused-silica uncoated inlet (5 m X 0.32 mm i.d.) temperature program, 100 °C for 8 min, rising to 350 °C at a rate of 12°C/min flame ionization detection. Peak identification is as follows 1, 2,4-rert-butylphenol 2, nonylphenol isomers 3, di(4-tert-butylphenyl) carbonate 4, Tinuvin 329 5, solvent impurity 6, Ii gaphos 168 (oxidized). Reprinted with permission from Ref. (14).

Eor plant and soil samples, transfer the carbon tetrachloride solution into a glass column packed with 7g of silica gel samrated in carbon tetrachloride. Rinse... 

Second cleanup Transfer the above carbon tetrachloride solution into a glass column packed with 7 g of silica gel saturated in carbon tetrachloride. Rinse the column, first with 2 mL of carbon tetrachloride and then with 35 mL of hexane-ethyl acetate (17 3, v/v). Elute benfuracarb with 30 mL of the same hexane-ethyl acetate solution. Concentrate the eluate to near dryness by rotary evaporation and prepare the GC/HPLC-ready sample solution by dissolving the residue either in benzene for plant material or in acetonitrile for water and soil. 

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