SU1354106A1 - Method of quantitative determination of unsaponifiable residue in fats - Google Patents

Abstract

The invention relates to the oil and fat industry. The aim of the invention is to improve accuracy by reducing the loss of unwashed substances and shortening the process time. This is achieved in that the fats are washed with alkali by heating, then the saponified fat is treated with excess hydrochloric acid to form a precipitate, which is then extracted with an organic solvent. Wash the resulting solution containing an unused residue with an aqueous-alcoholic alkali solution to remove free fatty acids, evaporate the solvent, and determine the amount of the substance gravimetrically. 2 tab. CO SP 4

Description

The invention relates to the oil and fat industry and relates to methods for determining the unsaturated residue in fats.

The aim of the invention is to improve accuracy by reducing the loss of unwashed substances and reducing the efficiency of the process.

Example 1. Refined sunflower oil is analyzed. Two 300 mg samples of fat are subjected to alkaline hydrolysis by heating with 3 ml (four times excess) 10% potassium hydroxide for 20 minutes. Dissolve the sample in 10.0 ml of distilled water and add 2.0 ml of 15% hydrochloric acid, resulting in

in solution, lipid flakes of 20 are formed with the known permits.

substances, 10.0 ml of chloroform is added to the sample and the contents are transferred; test tubes. After the sample was settled for 10 minutes, the upper liquid layer was discarded, and the lower layer, which was used, was a solution of unwashed residue and fatty acids in chloroform, washed three times with an equal volume of a mixture of water, potassium (50:50 : 1), as a result, the risk of reducing the method error

Those free fatty acids are transferred to the industrial liquid, while the unsaturated portion remains in the organic solvent layer. This solution was evaporated under vacuum at 60 ° C to a constant weight of the sample, and the mass of the residue obtained was determined to be 2.38 mg in the first sample and 2.10 mg in the second, which was 0.79 and 0.70% unwashed residue in refined vegetable oil. The time spent on the analysis is about 1, 2 hours. The determination error is + 6.8%,

Example 2, Analysis. Expose sea buckthorn oil taken in duplicate 300 mg each. Further determination of the undiluted residue is carried out analogously to Example 1. The weight of the unstained residue of sea buckthorn oil is 7.20 and 6.55 mg, respectively, or 2.40 and 2.18% of the unsaturated residue. The time spent on the analysis is about 1.3 hours. A determination error of + 4.8%.

Example 3, analysis is subjected to freon leaf extract

sea buckthorn Two samples of the extract be-; Root in duplicate 300 mg. Further determination of the unsoiled residue is carried out analogously to Example 1, the weight of the unsoiled residue of the freon leaf extract is 49.8 and 44.9 mg, or 16.18 and 14.94% of the unwashed residue in the samples. The time spent on the analysis is about 1.5 hours. A determination error of + 4.0%,

Simultaneously with the determination of the unwashed residue according to the proposed

the method is determined by a known method. Comparative results of the analyzes are given in Table 1 and 2.

The proposed method compared

Reduce time spent on prod: analysis from 4.5–36 h to 1.2–1.5 h due to the replacement of triple aqueous alkaline emulsion 25 by 1.0–8.0 h for delamination , for a threefold washing of the solution of the analyte from fatty acids for 10-15 minutes (Table 2),

Increase accuracy of determination

9.5-25.0% to 4.0-6.8% (Table 2)

Improve occupational safety and health by reducing the amount of solvent required for

- analysis of one sample from 150 to 10 cm (Table 2), as well as by reducing the time of installation with this solvent during the analysis of one sample, from 1.0-8.0 h to

10-15 min

In the proposed method, after saponification, the aqueous-alkaline solution of saponified fat is treated with an excess of acid, as a result of which the determinable substance (unsaturated residue) together with free fatty acids precipitates, while the water-soluble impurities lead.

to the formation of a stable emulsion, o1: melt in aqueous solution. The aqueous solution is poured off, and the solid precipitate is dissolved in an organic solvent and the solution is washed with a mixture

water, alcohol and alkali, as a result of which the free fatty acids are removed. 1 A solution of the test substance is evaporated to a constant weight and its mass is determined.

1354

Formula 3 inventions

Method for quantitative determination of inalienable residue in fats, including saponification of a sample of fat, extraction with an organic solvent, washing the resulting solution containing the unwashed residue with an aqueous-alcoholic alkali solution to remove free fatty acids, evaporation of solvent and gravimetric refined sunflower oil butter

Sea buckthorn oil

Freon extract of sea buckthorn leaves

Refined DIVNIIPI

Order 5687/39

Random polygons pr-tie, Uzhgorod, st. Project, 4

106

division of the substance, characterized in that, in order to increase accuracy by reducing the loss of unwashed substances and shortening the process, before extracting a sample of saponified fat, it is treated with excess hydrochloric acid, and the resulting precipitate is extracted.

Table 1

0.7.fO, 18 0.75 ± 0.05 2.41 ± 0.23 2.29 ± 0.1

16.3014.02 15.56 ± 0.62

table 2

Circulation. 776Subscribe

Claims (2)

SUMMARY OF THE INVENTION A method for quantitative determination of an unsaponifiable residue in fats, including saponification of a fat sample, extraction with an organic solvent, washing the resulting solution containing an unsaponifiable residue with an aqueous-alcoholic alkali solution to remove free fatty acids, evaporating the solvent and gravimetric determination 106 dividing a substance, characterized in that, in order to increase accuracy by reducing the loss of unsaponifiable substances and shortening the process time, an excess of hydrochloric acid is treated before extraction of the sample of saponified fat, and the resulting precipitate is subjected to extraction. Table 1 Fat sample The amount of unsaponifiable residue,%, by the method famous previous step Refined Sunflower Oil Sea buckthorn oil Sea buckthorn leaf freon extract 0.72 + 0.18 2.41 + 0.23 16.30 + 4.02 0.75 + 0.05 2.29 + 0.11 15.56 + 0.62 table 2 Fat sample Definition error,%, by the method The cost of barter, h, method fiercely Solvent costs, cm, by the method famous proposed famous proposed famous proposed Refined Sunflower Oil 25.0 6.8 4,5 1,2 150 10 Sea buckthorn oil 9.5 4.8 6.0 1.3 150 10 Sea buckthorn leaf freon extract 24.5 4.0 36.0 1,5 150 10 VNIIIPI Order 5687/39 Circulation. 776 Subscription Custom polygr. ave, city of Uzhhorod, st. Project, 4