Silica solid adsorbent

A solid-phase extraction in which the solid adsorbent is coated on a fused-silica fiber held within a syringe needle. 

Liquid-solid chromatography (LSC). This process, often termed adsorption chromatography, is based on interactions between the solute and fixed active sites on a finely divided solid adsorbent used as the stationary phase. The adsorbent, which may be packed in a column or spread on a plate, is generally a high surface area, active solid such as alumina, charcoal or silica gel, the last... 

A cleanup procedure is usually carried out to remove co-extracted matrix components that may interfere in the chromatographic analysis or be detrimental to the analytical instrument. The cleanup procedure is dependent on the nature of the analyte, the type of sample to be analyzed, and the selectivity and sensitivity of the analytical instrument used in the analysis. Preliminary purification of the sample extracts prior to chromatographic separation involves liquid-liquid partitioning and/or solid-phase extraction (SPE) using charcoal/Celite, Elorisil, carbon black, silica, or aminopropyl-silica based adsorbents or gel permeation chromatography (GPC). 

Millson [113] investigated components of sewage sludge and found elementary sulphur in the hydrocarbon fractions eluted from liquid adsorption columns. By using a solid adsorbent such as alumina, silica gel, or Florisil, and heptane as eluent, the sulphur could be separated from weakly adsorbed hydrocarbons, e.g. squalene or biphenyl, but not from more strongly adsorbed hydrocarbons such as phenyldodecane. 

In gas-solid chromatography (GSC) the stationary phase is a solid adsorbent, such as silica or alumina. The associated virtues associated therewith, namely, cheapness and longevity, are insufficiently appreciated. The disadvantages, surface heterogeneity and irreproducibility, may be overcome by surface modification or coating with small amounts of liquid to reduce heterogeneity and improve reproducibility 4,15). Porous polymers, for example polystyrene and divinyl benzene, are also available. Molecular sieves, discussed in Chapter 17, are used mainly to separate permanent gases. 

Adsorption is a physical phenomenon in which some components adsorbates) in a fluid (liquid or gas) move to, and accumulate on, the surface of an appropriate solid adsorbent) that is in contact with the fluid. With the use of suitable adsorbents, desired components or contaminants in fluids can be separated. In bioprocesses, the adsorption of a component in a liquid is widely performed by using a variety of adsorbents, including porous charcoal, silica, polysaccharides, and synthetic resins. Such adsorbents of high adsorption capacities usually have very large surface areas per unit volume. The adsorbates in the fluids are adsorbed at the adsorbent surfaces due to van der Waals, electrostatic, biospecific, or other interactions, and thus become separated from the bulk of the fluid. In practice, adsorption can be performed either batchwise in mixing tanks, or continuously in fixed-bed or fluidized-bed adsorbers. In adsorption calculations, both equilibrium relationships and adsorption rates must be considered. 

Figure 19.12. Batch parametric processing of solid-liquid interactions such as adsorption or ion exchange. The bottom reservoir and the bed interstices are filled with the initial concentration before pumping is started, (a) Arrangement of adsorbent bed and upper and lower reservoirs for batch separation, (b) Synchronization of temperature levels and directions of flow (positive upward), (c) Experimental separation of a toluene and n-hcptane liquid mixture with silica gel adsorbent using a batch parametric pump. (Reprinted from Wilhelm, 1968, with permission of the American Chemical Society), (d) Effect of cycle time t on reservoir concentrations of a closed system for an NaCl-H20 solution with an ion retardation resin adsorbent. The column is initially at equilibrium with 0.05M NaCl at 25°C and a = 0.8. The system operates at 5° and 55°C. [Sweed and Gregory, AIChE J. 17, 171 (1971)J.

One of the most common low-temperature methods for removing impurities involves the use of selective solid adsorbents. Such materials as silica gel, carbon, and synthetic zeolites (molecular sieves) are widely used as adsorbents because of their extremely large effective surface areas. Most of the gels and carbons have pores of various sizes in a given sample, but the synthetic zeolites can be manufactured with closely controlled pore size openings ranging from 0.4 to 1.3 nm. This additional selectivity is useful because it permits separation of gases on the basis of molecular size. 

For the samples that will be subjected to other (so-called interactive) LC techniques, the next question involves the nature of the solvent in which the sample has been or can be dissolved. If this is a non-polar solvent, such as n-hexane, then the sample solution is compatible with Normal Phase LC (NPLC), in which mobile phases with a relatively low polarity are used in combination with more polar stationary phases (see section 3.2.3). In this form of chromatography solid adsorbents (such as silica or alumina) may be used as stationary phases (LSC). Alternatively, polar chemically bonded stationary phases may be used (see section 3.2.2). 

The cryogenic air separation process starts with air entering the plant through air filters, where it is compressed and cooled. The air is passed through heat exchangers for further cooling and for removal of water vapor and carbon dioxide by freezing. Solid adsorbents, such as molecular sieves, silicas, and aluminas can also be used to remove the water and carbon dioxide by adsorption before separation of... 

Arosorb A process for extracting aromatic hydrocarbons from refinery streams using a solid adsorbent, either silica gel or activated alumina. Developed by the Sun Oil Company in 1951. California Research Corporation developed a similar process. 

Case 3 involves the use of mobile-phase mixtures B/C, where B and C are polar, but only C can localize. The solvent B can also be a blend of a nonpolar solvent A with a pure solvent B (A/B), in which case we deal with ternary-solvent mobile phases A/B/C. The effect of restricted-access delocalization on values of e in mixtures B/C is illustrated in Fig. 12 (solid circles) for mobile phases composed of acetone (C) and benzene (B), with silica as adsorbent. The open circles are comparative data for acetone/hexane (A/C) mixtures. The same tendency ofec to increase for smaller Oc is found for acetone in mixtures B/C as is found for mixtures A/C. This is further confirmed by the data of Fig. 13, where %tc for several mobile phases B/C (B is benzene, C varying) are plotted versus dc- The precision of these experimental values of is much reduced in the case of mobile phases B/C in comparison to those of type A/C, as can be seen in... 

Fig. 21. Experimental and calculated isotherms for various LSC binary-solvent mobile phases /AB and silica as adsorbent. Solid curves are calculated from present model using parameters of Table I (based on retention data only) points are experimental uptake values from Scott and Kucera (4) and Snyder and Poppe (12). (a) CHCt/hexane (b) benzene/ hexane (c) toluene/hexane (d) ethyl acetate/hexane (e) isopropanol/hexane.

Solid phase extraction. With the availability of pre-prepared cartridges of silica-based adsorbents, the use of solid phase extraction has increased in the last few years although the technique has been in use for many years for the isolation of many biochemicals, e.g. amino acids, catecholamines. In essence it is a version of chromatography conditions for the selective adsorption of the analytes (column, solvent, pH, etc.) are chosen, the sample is applied to a column, washed and the analytes selectively eluted with appropriate solvents. Since the columns are disposable there is no need to worry about protein contamination or infection. The adsorbents available cover an even wider range than HPLC materials since they are not required to withstand high back pressures. It is possible... 

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