Chromatography groups

Gas-liquid chromatography Group contribution method of predicting GLC... 

Attendance at meetings of local chromatography groups (such as... 

Marini-Bettolo, B.G. and Caggiano, E., Paper chromatography and electrophoresis of tertiary bases, a symposium organized by the Chromatography Group of the Czechoslovak Chemical Society at Liblice Czech., June 23, 1961, p. 91 Chem Abs., 60, 838d, 1964. 

In the late 1990s he was involved in the installation and commissioning of process scale HPLC at Zeneca Pharmaceuticals. During 18 years with CRB, ICI, Zeneca and Avecia he was instrumental in establishing the technique of preparative HPLC within the company and served 11 years as the secretary of the company s Process Scale Chromatography Group. 

Table 6.1. Anions determined by ion chromatography (Grouped according to general type).

Thin-Layer and Column Chromatography Group Separation of Steroids as Tri-methylsilyl Ethers. Isolation for GLC Analysis of Pregnanediol and Estriol in Pregnancy Urine Anal. Biochem. 19(2) 234-242 (1967) ... 

The Use of GLC Coupled with Electron Capture to Determine Trace Levsls of Drugs in Biological Fluids 5th Annual Winter Mtg., Chicago Gas Chromatography Group, Chicago, 111., January 1969... 

Sephadex A trade name for an insoluble hydrophilic substance prepared by cross-linking dextran, and used in gel filtration. It can also be linked to acidic or basic groups for ion exchange or to alkanes for the chromatography of lipophilic compounds. 

Hydrocarbon groups (FIA method) NF M 07-024 ISO/DIS 3837 ASTM D 1319 Chromatography on silica gel with fluorescent indicators... 

The 1,6-difunctional hydroxyketone given below contains an octyl chain at the keto group and two chiral centers at C-2 and C-3 (G. Magnusson, 1977). In the first step of the antithesis of this molecule it is best to disconnect the octyl chain and to transform the chiral residue into a cyclic synthon simultaneously. Since we know that ketones can be produced from add derivatives by alkylation (see p. 45ff,), an obvious precursor would be a seven-membered lactone ring, which is opened in synthesis by octyl anion at low temperature. The lactone in turn can be transformed into cis-2,3-dimethyicyclohexanone, which is available by FGI from (2,3-cis)-2,3-dimethylcyclohexanol. The latter can be separated from the commercial ds-trans mixture, e.g. by distillation or chromatography. 

The protecting groups are also used to solubilize synthetic intermediates in organic solvents, e.g. methylene chloride. Chromatography is then possible on a larger scale, since silica gel can be used as adsorbent. Six synthetic strategies have been developed (H. Kdster, 1979) ... 

Glycosidic thiol groups can be introduced into glycosyl bromides by successive reactions with thiourea and aqueous sodium disulfite (D. Horton, 1963 M. Cemy, 1961, 1963). Such thiols are excellent nucleophiles in weakly basic media and add to electrophilic double bonds, e.g., of maleic esters, to give Michael adducts in high yields. Several chiral amphiphiles have thus been prepared without any need for chromatography (J.-H. Fuhrhop, 1986 A). 

A large number of variously 2-, 4-, and 5-substituted thiazoles with alkyl, aryl, hydroxy, methylthio, mercapto, halo, and nitro groups have been analyzed by thin-layer chromatography on silica and alumina by the Stahl s technique (167, 170, 172). Among the many systems recommended for the elution of these compounds are the following ... 

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. 

In reverse-phase chromatography, which is the more commonly encountered form of HPLC, the stationary phase is nonpolar and the mobile phase is polar. The most common nonpolar stationary phases use an organochlorosilane for which the R group is an -octyl (Cg) or -octyldecyl (Cig) hydrocarbon chain. Most reverse-phase separations are carried out using a buffered aqueous solution as a polar mobile phase. Because the silica substrate is subject to hydrolysis in basic solutions, the pH of the mobile phase must be less than 7.5. 

The following experiments may he used to illustrate the application of chromatography and electrophoresis to a number of different types of samples. Experiments are grouped by the type of technique, and each is briefly annotated. 

Polyester composition can be determined by hydrolytic depolymerization followed by gas chromatography (28) to analyze for monomers, comonomers, oligomers, and other components including side-reaction products (ie, DEG, vinyl groups, aldehydes), plasticizers, and finishes. Mass spectroscopy and infrared spectroscopy can provide valuable composition information, including end group analysis (47,101,102). X-ray fluorescence is commonly used to determine metals content of polymers, from sources including catalysts, delusterants, or tracer materials added for fiber identification purposes (28,102,103). 

The separation of the polysaccharide components utilizes their different solubUities, polar groups, extents of branching, molecular weights, and molecular flexibUities and may be accompUshed batchwise or with easUy automated column techniques such as column or high performance Uquid chromatography. These procedures have been summarized in several reviews (3,141—143). 

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