Stationary phase for gas chromatography
(57) Abstract:The invention relates to the field of study physical and chemical properties of substances and relates to gas chromatographic separation of mixtures of organic substances. The essence of the invention: polyoxyethylene (arsenate) formula , where applied as a stationary phase for gas chromatography. Specified stationary phase has a higher selectivity for the separation of alcohols from alkanes and other non-polar or slightly polar organic substances in comparison with the known stationary phases. table 1. The invention relates to research the physical and chemical properties of substances and relates to gas chromatographic separation of mixtures of organic substances, and is intended to be used as a stationary phase polyoxyethylene(arsenate) formula
As-O(CH2CH2O)nAs where n is 5 to 500.Polyoxyethylene(arsenate) is known as biologically active substances.Polyoxyethylene(arsenate) are synthesized as follows. In a flask equipped with nozzle Dean-stark and reflux condenser, is placed 30 g (0.1 mole) of polyethylene glycol (300 M), of 28.4 g (0.2 mol) of arsenic acid, 20 is of benzene (80aboutC). The resulting reaction water Argonauts in the form of azeotrope water benzene in the nozzle Dean-stark. Heating is carried out until the cessation of water allocations. After completion of the reaction the solvent (benzene) argonauta at a residual pressure of 30-40 mm RT.article and heated to 50aboutC.Yield: 54 g (98.5 per cent)
Found, C 30,12; H 6,03; As 26,87.Calculated C 29,70; H 5,72; As 27,15.Polyoxyethylene(arsenate) of different molecular masses are synthesized similarly.The structure of the compounds is confirmed by the method of infrared (IR) spectroscopy. The data of IR spectroscopy,cm-1: (C-O) 1100-1130; (CH2) 1460; (As-OH) 810; (As=O) 960; (As-OH) 2100-2500.Spectra of paramagnetic resonance and nuclear magnetic resonance ineffective.Polyoxyethylene(arsenate) have a higher selectivity for the separation of alcohols from alkanes and other non-polar or slightly polar organic substances in comparison with the known stationary phases, for example with Dionysius(diphenylarsine)butane. Determine the factors polarity x,y according to the ratios of Arsagera.The results determine the values of the chromatographic factors polarity is Yunosti separation of alcohols, which confirms the high value of the factor polarity (y).Moreover, comparative tests of the original polyethylene glycol and polyoxyethylene(arsenate) on temperature (DTA) shows higher thermal stability of the second connection: decomposition temperature, respectively 175 and 210aboutC. The use of polyoxyethylenesorbitan General formula
< / BR>where n 5 500,
as stationary phase for gas chromatographic separation and analysis of hydroxyl-containing organic substances.
FIELD: chromatographic sorbents.
SUBSTANCE: invention relates to chromatographic sorbents, which can be used for analysis and preparative purification of optically active compounds. A novel sorbent for resolution of isomers of optically active compounds is developed containing, as chiral selector, macrocyclic glycopeptide antibiotic eremomycin, vancomycin, ristomycin A, teicoplanine, or their aglycons. Method of immobilization of macrocyclic glycopeptide antibiotics is also developed, which resides in that silica gel in aqueous buffer solution is first treated with 3-glycidoxypropyl(trialkoxy)silane and then, in alkaline aqueous or water-organic solution, above-indicated macrocyclic glycopeptide antibiotic is grafted to epoxy group-modified silica gel.
EFFECT: increased selectivity in enantiomer resolution and simplified preparation procedure.
9 cl, 12 dwg, 5 tbl, 9 ex
SUBSTANCE: specific area of silica surface reaches 300,2/g, porosity - up to 1,1 cm3/g, average pores diameter - 12,0-16,0 nm. For separating and property detection couples of substances and carrier gas are let through chromatography column, filled with silica powder, which is precipitated from hydrothermal solution, with receipt at output of column of sequence of special components, recorded in form of peaks. Absorbent, received on basis of silica, precipitated from hydro-thermal solution, in several cases has better separating ability then traditional absorbents.
EFFECT: higher efficiency.