SU432384A1 - - Google Patents

Description

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The invention relates to stationary liquid phases for gas chromatographic separation of mixtures of hydrocarbons, for example hydrocarbons SB-Ci2, including hydrocarbons of various classes.

It is known to use gas-chromatographic separation of hydrocarbon mixtures as the stationary phase of various complex organic compounds, for example, phosphoric esters.

The known liquid phase has a low separation capacity with respect to hydrocarbon mixtures of a wide composition. Therefore, in practice, two or more chromatographs having columns with different liquid phases are used for gas chromatographic separation of a mixture of hydrocarbons.

The purpose of the invention is to select the liquid phase for gas chromatographic separation of mixtures of hydrocarbons, which has a high separation capacity with respect to mixtures of hydrocarbons of various classes.

According to the invention, alkyl (aryl) -phosphonic acid esters are used as the stationary liquid phase. The proposed liquid phase is applied to an inert or active carrier or to the inner walls of a capillary chromatographic column and is used for gas chromatography.

separation of mixtures of hydrocarbons, when working on different chromatographs and with various detectors.

Example. A-methyl vinylphosphonic acid diphenyl ether (gross formula CisHisPOs, mol. Weight 274, density 1.1661 g / cm.kip. 175-178 ° C, ng 1.5580) is deposited on the chromaton in an amount of 5-25 weight . % by weight of the carrier. Application is carried out in a solvent by evaporation of the latter at a temperature of 40 ° C in a water bath with occasional stirring. Diethyl or petroleum ether in the amount of 15-20 ml per 1 g of solid carrier is used as a solvent. After evaporation of the solvent, the resulting sorbent is loaded into a chromatographic column and subjected to heat treatment at a temperature of 100 ° C in a stream of carrier gas for 3-4 hours. The sorbent thus crawled is used in an UX-2 chromatograph (detector-katharometer, column with a diameter of 4 mm, 2.5 m long, carrier gas — helium, the amount of sample injected is 0.03–0.05 ml) for gas chromatographic separation of an artificial mixture of hydrocarbons Cs-Ci2. Test conditions: column temperature 60 ° C, detector sensitivity 5 mV, carrier gas rate 1240 ml / hour. Under these conditions, the analysis time is 27 minutes.

The results of the analysis are shown on the chromatogram (Fig. 1).

At a column temperature of 85 ° C and a carrier gas rate of 3000 ml / hour, the analysis time is reduced to 8 minutes without deteriorating the separation of the components. The results of the analysis under these conditions are shown in the chromatogram (Fig. 2). Chromatogram peaks correspond to: 1-isonentane, 2 - n-hexane, 3 - n-heptane + cyclohexane, 4 - methylcyclohexane, 5 - n-octane, 6 - benzene, 7 - toluene, 8 - n-decane, 9 - para- and metaxylene, 10 - isopropylbenzene.

It can be seen from the above chromatograms that the separation of complex hydrocarbon mixtures in the proposed stationary liquid phase is good.

Da-methylvinylphosphonic acid diphenyl ester can be easily obtained from ketone, benzene and phosphorus chloride. The high separation efficiency of the stationary liquid phase, the availability of its raw materials allows it to be used for gas chromatographic separation of mixtures of hydrocarbons.

Subject invention

Use of alkyl (aryl) phosphonic acid esters, for example a-methylvinylphosphonic acid diphenyl ester, as the stationary liquid phase for gas chromatographic separation of hydrocarbon mixtures, for example Cg-Ci2 hydrocarbons.

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