Type V gel-silica

Type metal, 3 53, 24 798 Type N hydrated lime, 15 29 Type S hydrated lime, 15 29 Type V gel-silica, 23 75-76 Type VI gel-silica, 23 76 Tyrian purple color, 7 332 Tyril, 7 639 D-Tyrosine... 

The formation of silicon-flvxyride bonds on the surface of silica after treatment with hydrogen fluoride was never proven directly. However, there is a pronounced change in the adsorption and wetting properties. The silica becomes hydrophobic as was mentioned in a patent to Kimberlin (279a). Neimark and collaborators (279b) found a type V isotherm in the methanol adsorption on silica gel which had been treated with a solution of SiF in absolute alcohol. Wilska (280) obtained a water-repellent silica when solutions of HaSiPg were precipitated with ammonia. The Si—F bond is hydrolyzed only slowly. A considerable fluorine content of 7-10% F was reported in an older patent (281) for a silica that had been prepared by hydrolysis of SiF. ... 

Types TV and V They are considered to reflect capillary condensation phenomena, i.e., possibility of condensation of gases in minute pores of the adsorbent at pressures even below the saturation pressures of p0 of the gas and may show hysteresis effect. An example of type IV is furnished by adsorption of benzene on silica gel at 50 C and that of type V by adsorption of water vapour on activated charcoal at 100 C. 

Scott and Kucera [4] carried out some experiments that were designed to confirm that the two types of solute/stationary phase interaction, sorption and displacement, did, in fact, occur in chromatographic systems. They dispersed about 10 g of silica gel in a solvent mixture made up of 0.35 %w/v of ethyl acetate in n-heptane. It is seen from the adsorption isotherms shown in Figure 8 that at an ethyl acetate concentration of 0.35%w/v more than 95% of the first layer of ethyl acetate has been formed on the silica gel. In addition, at this solvent composition, very little of the second layer was formed. Consequently, this concentration was chosen to ensure that if significant amounts of ethyl acetate were displaced by the solute, it would be derived from the first layer on the silica and not the less strongly held second layer. 

The chromatographic resolution of bi-naphthol enantiomers was considered for simulation purposes [18]. The chiral stationary phase is 3,5-dinitrobenzoyl phenyl-glycine bonded to silica gel and a mixture of 72 28 (v/v) heptane/isopropanol was used as eluent. The adsorption equilibrium isotherms, measured at 25 °C, are of bi-Langmuir type and were proposed by the Separex group ... 

The separation of bi-naphthol enantiomers can be performed using a Pirkle-type stationary phase, the 3,5-dinitrobenzoyl phenylglycine covalently bonded to silica gel. Eight columns (105 mm length) were packed with particle diameter of 25 0 fiva. The solvent is a 72 28 (v/v) heptane isopropanol mixture. The feed concentration is 2.9 g for each enantiomer. The adsorption equilibrium isotherms were determined by the Separex group and already reported in Equation (28) [33]. 

This means, in practice, that when employing a polar solvent with n-heptane (or any other paraffin for that matter) to reduce the retention, there will be a dramatic reduction in retention over the concentration range of about 0-2%w/v. However, subsequent changes in solute retention with polar solvent concentration will be relatively small. This will be true for any polar solute and was experimentally verified by Scott and Kucera for solutions of ethyl acetate, tetrahydrofuran and n-propanol in n-heptane. The very sensitive relationship between solvent concentration and retention at very low concentrations makes the phase system very difficult to make reproducible. This problem is one of the factors that deter analysts from using silica gel as a stationary phase for the separation of polar solutes. It is very satisfactory, however, for the separation of polarizable and weakly polar substances that can be eluted by paraffin/methylene dichloride or similar types of solvent mixtures. 

TLC Analysis. Samples were examined by TLC using standard procedures. Rf values were determined and compared with those of authentic reference materials. Radioactive components were located by scanning (Vanguard Instrument Corp., North Haven, Conn., Model 885) or by autoradiography (Eastman Kodak, Rochester, N. Y., type AA film). The relative Rf value of DCDD on silica gel plates (Brinkmann Instruments, Inc., Westbury, N. Y., type For,4) when developed with n-hexane dioxane acetic acid, 90 10 4, V/V/V, was 0.90. The observed impurity had a relative Rf value of 0.40. On Brinkmann alumina plates, developed with n-hexane, DCDD had a relative Rf of 0.32. Neither system separated the chlorinated dibenzodioxin isomers. 

Reversed-phase silica gel column Place a cotton wool plug at the bottom of a glass chromatography column. Pack 5 g of reversed-phase silica gel slurried with a solvent mixture of n-hexane-benzene-methanol (80 20 0.4, v/v/v) into the glass column. Place an anhydrous sodium sulfate layer about 1 -cm thick above and below the silica gel bed Bell jar-type filtering apparatus Buchner funnel, 11-cm i.d. 

Many of the chiral molecules containing amide groups were bonded to a solid support for the preparation of CSPs [16-19]. The racemic compounds resolved on these CSPs include a-hydroxycarbonyls, /i-hydroxycarbonyls, amino acids, amino alcohols, amine, and derivatized and underivatized diols. The preliminary chiral diamide phase [(/V-foriuyl-L-valyl)aminopropyl)silica gel] has sufficient separability for racemic /Y-acylatcd a-amino acid esters but not in other types of enantiomer [16]. Most of the eluents used with these CSPs are of normal phase mode, including w-hcxanc, 2-propanol, chlorinated organic solvents, and acetonitrile. 

Types III (e.g. bromine on silica gel at 352 K) and V (e.g. water vapour on charcoal at 373 K) show no rapid initial uptake of gas, and occur when the forces of adsorption in the first monolayer are relatively small. These isotherms are rare. 

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