Diatomaceous earth supports

The problem of adsorption of a phenolic alkaloid such as morphine during gas chromatography because of "active sites" on the solid support (diatomaceous earth) has mostly been avoid ed by converting morphine to derivatives such as acetyl, propionyl, fluoroacetyl, fluoro-... 

Solid Support— diatomaceous earth or equivalent nonreactive particulate material. Typical particle size ranges are 60/80 or 80/100 mesh. 

The most widely used particulate support is diatomaceous earth, which is composed of the silica skeletons of diatoms. These particles are quite porous, with surface areas of 0.5-7.5 m /g, which provides ample contact between the mobile phase and stationary phase. When hydrolyzed, the surface of a diatomaceous earth contains silanol groups (-SiOH), providing active sites that absorb solute molecules in gas-solid chromatography. 

More recently, solid supports made from glass beads or fluorocarbon polymers have been introduced. These supports have the advantage of being more inert than diatomaceous earth. 

Capillary columns are of two principal types. Wall-coated open tuhular columns (WCOT) contain a thin layer of stationary phase, typically 0.25 pm thick, coated on the capillary s inner wall. In support-coated open tuhular columns (SCOT), a thin layer of a solid support, such as a diatomaceous earth, coated with a liquid stationary phase is attached to the capillary s inner wall. 

Catalysts. Commercial sulfuric acid catalysts typically consist of vanadium and potassium salts supported on sUica, usually diatomaceous earth (see Diatomite). Catalyst peUets are available in various formulations, shapes, and sizes depending on the manufacturer and the particular converter pass in which they are to be used. A detailed discussion of oxidation catalysts for sulfuric acid production is available (107). 

The active phase, which is soHd at room temperature, is comprised of mixed potassium and sodium vanadates and pyrosulfates, whereas the support is macroporous siUca, usually in the form of 6—12 mm diameter rings or pellets. The patent Hterature describes a number of ways to prepare the catalyst a typical example contains 7 wt % vanadium pentoxide, 8% potassium added as potassium hydroxide or carbonate, 1% sodium, and 78 wt % siUca, added as diatomaceous earth or siUca gel, formed into rings, and calcined in the presence of sulfur dioxide or sulfur trioxide to convert a portion of the alkah metal salts into various pyrosulfates (81,82). 

Once separated, the supports are washed using acid (HCl) and sdanized, ie, treated with dimethyl dichi orosilane [75-78-5] (DMCS), to reduce the polarity. Sdanizing replaces adjacent SiOH groups with nonpolar CH caps. In addition to diatomaceous earths, supports of carbon (qv), halocarbons, eg. Teflon, and glass beads are in use by various chromatographers. 

Diatomaceous earth has been used as a chromatographic support since the inception of gas chromatography. A diverse line of products are available. The high surface area and stmcture of diatomite enables it to carry the Hquid phase while an inert surface prevents interference with partitioning. Properly treated diatomite chromatographic supports make use of all its unique properties (10). 

Polyphosphoric acid supported on diatomaceous earth (p. 342) is a petrochemicals catalyst for the polymerization, alkylation, dehydrogenation, and low-temperature isomerization of hydrocarbons. Phosphoric acid is also used in the production of activated carbon (p. 274). In addition to its massive use in the fertilizer industry (p. 524) free phosphoric acid can be used as a stabilizer for clay soils small additions of H3PO4 under moist conditions gradually leach out A1 and Fe from the clay and these form polymeric phosphates which bind the clay particles together. An allied though more refined use is in the setting of dental cements. 

SFE usually requires pre-extraction manipulation in the form of cryogenic grinding, except in cases where analytes are sorbed only on the surface or outer particle periphery. The optimum particle diameter is about 10-50 p,m. Diatomaceous earth is used extensively in SFE sample preparation procedures. This solid support helps to disperse the sample evenly, allowing the SCF to solvate the analytes of interest efficiently and without interference from moisture. 

In a partition system the stationary phase is a liquid coated onto a solid support (p. 97). Silica gel, kieselguhr (diatomaceous earth) or cellulose powder are the most frequently used. Conditions closely resemble those of counter-current distribution so that in the absence of adsorption by the solid support, solutes move through the system at rates determined by their... 

Several manufacturers introduced products amenable for this solid-supported LLE and for supported liquid extraction (SLE). The most common support material is high-purity diatomaceous earth. Table 1.8 lists some commercial products and their suppliers. The most widely investigated membrane-based format is the supported liquid membrane (SLM) on a polymeric (usually polypropylene) porous hollow fiber. The tubular polypropylene fiber (short length, 5 to 10 cm) is dipped into an organic solvent such as nitrophenyl octylether or 1-octanol so that the liquid diffuses into the pores on the fiber wall. This liquid serves as the extraction solvent when the coated fiber is dipped... 

One advance in the area of LLE is the use of solid supports that facilitate the partitioning of the analyte(s) of interest. LLE extraction methods involving nonpolar matrices often suffer from the formation of emulsions, and using the solid support is a possible solution. In one study, polychlorinated biphenyls, dioxins, and furans were extracted from the lipid fraction of human blood plasma [32], using diatomaceous earth as the solid support. Long glass columns (30 cm) were packed with several layers of Chem-Elut (a Varian product) and sodium chloride. The plasma samples were diluted with water and ethanol and passed over the columns. A mixture of isopropanol and hexane (2 3) was passed over the column and the LLE was performed. It can be concluded that the LLE with the solid support is easier to perform and can be applied to other lipid heavy matrices such as milk [32]. 

The liquid stationary phase in a GLC packed column is adsorbed on the surface of a solid substrate (also called the support). This material must be inert and finely divided (powdered). The typical diameter of a substrate particle is 125 to 250 ft, creating a 60- to 100-mesh material. These particles are of two general types diatomaceous earth and Teflon . Diatomaceous earth, the decayed silica skeletons of algae, is most commonly referred to by the manufacturer s (Johns Manville s) trade name, Chromosorb . Various types of Chromosorb, which have had different pretreatment procedures applied, are available, such as Chromosorb P, Chromosorb W, and Chromosorb 101-104. The nature of the stationary phase as well as the nature of the substrate material are both usually specified in a chromatography literature procedure, and columns are tagged to indicate each of these as well. 

The silica carrier of a sulphuric acid catalyst, which has a relatively low surface area, serves as an inert support for the melt. It must be chemically resistant to the very corrosive pyrosulphate melt and the pore structure of the carrier should be designed for optimum melt distribution and minimum pore diffusion restriction. Diatomaceous earth or synthetic silica may be used as the silica raw material for carrier production. The diatomaceous earth, which is also referred to as diatomite or kieselguhr, is a siliceous, sedimentary rock consisting principally of the fossilised skeletal remains of the diatom, which is a unicellular aquatic plant related to the algae. The supports made from diatomaceous earth, which may be pretreated by calcination or flux-calcination, exhibit bimodal pore size distributions due to the microstructure of the skeletons, cf. Fig. 5. 

Ethylene is compressed to 1000 psi, mixed with water, and heated to 600°E The two reactants, both. in, a vapor phase, are fed down a catalyst-filled reactor. The catalyst is phosphoric acid (H3PO4) absorbed onto a porous inert support (usually diatomaceous earth or silica gel). 

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