SU783683A1 - Method of producing solid chromatographic substrates - Google Patents

Description

Example 1. To obtain a solid chromatographic carrier, 2 g (22% by weight per raw material) of bbt, -Hoft orthophosphoric acid are taken, 50 ml of ethyl alcohol are added and 9 g of Spherochrome-2 carrier is added to the semi-mixed mixture. (At a temperature, ethyl alcohol is distilled off in a water bath. The carrier is calcined in a muffle furnace for 0.5 h at 8 ° С (heating rate is). The calcined carrier is washed in portions of 25 g with 10% WATER} - with a solution of salt acidic, followed by washing with distilled water to RP 7. The finished product for removing water is held at 100 ° C for 12 hours. Example 2. To obtain a solid chromatographic carrier, take 4 g (40% by weight of the feedstock) of 85% orthophosphorus acid and add 60 ml of ethyl alcohol, then with stirring 10 g of spherochrome-2 carrier is added. At a temperature ethyl alcohol is distilled off in an oil bath. The carrier is calcined in a muffle furnace at a temperature of 2 hours (preheating rate). The calcined carrier is portionwise washed with 20 g of each 20% aqueous hydrochloric acid solution, followed by washing with distilled water to pH 7. The finished product to remove the water is maintained at a temperature of 9 hours. The proposed method was thoroughly tested in laboratory conditions. The obtained solid chromatographic carrier, as shown by experiments, is characterized by significantly higher chromatographic separation parameters than the sorbent obtained by the prototype method. The upper limit for use of polyethylene glycol adipate is 235 ° C. As a result of the tests, the following comparative data were obtained on the height equivalent to one theoretical plate (WETT) and the asymmetry coefficient of the gas chromatographic peaks of valeric and caproic acids, as well as on the adsorption activity (condition, experiment: amount of 10% by weight of solid carrier; column length 1 m; internal diameter 4 mm; column temperature 100 ° C; sample size 1 μl; carrier gas — hydrogen, its flow rate (LO ml / min),

Vyi: ota, equivalent to theoretical plate for valeric acid peak, mm

Adsorption activity determined by the coefficient of asymmetry of valeric acid peak at 1/10 of its height.

The separation ratio of valeric and caproic acids

As experiments have shown, a significant decrease in the adsorption activity of the solid carrier leads to a decrease in the asymmetry of the chromatographic zones, which significantly improves the results of the analysis. A significant decrease in the catalytic activity of the carrier obtained by the proposed method allows the use of stationary liquid phases at higher temperatures, then increasing the temperature range of their application. In the proposed method, the preparation time of the chromatographic carrier is significantly shortened.

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Claims (2)

Invention Formula The method of obtaining a solid chromatographic carrier, INCLUDING the treatment of the silica raw material with ortho-phosphoric acid, followed by calcining the mixture, is from the process and, in order to reduce the catalytic and adsorption activity of the carrier, the treatment with phosphoric acid is performed at a concentration of 20-40% of the weight of silica cheese, and calcining at a temperature of 750 - for 0, h, and the resulting product first laundered 57836b3 water solution of chloride1. Copyright certificateSSSR hydrogen, and then distilled 396624, cl. G 01 S 31/08, 1975. with water to pH 7. Information sources, 2. Patent ORG 1200024, taken into account during examination. 42 i- 4/16, 1966 (prototype).