SU1193578A1 - Method of determining fraction of total mass of sorbitol in tobacco - Google Patents

Abstract

Method for determination of sorbitol in tobacco, comprising introducing into vodyy sorbitol solution dichromate solution, potassium and sulfuric acid, incubating the mixture, introduction, into a mixture of potassium iodide solution vscherzhivanie mixture in the dark, the titration of the evolved iodine sodium thiosulfate and determining the mass fraction sorbitol count sodium thiosulfate solution spent on titration, characterized in that, in order to determine the accuracy of the mass fraction of sorbitol in tobacco, the aqueous solution of sorbitol and is prepared by extraction of the tobacco sample water containing sorbitol, and passing the extract through a chromatographic column packed with sorbent combined representing the monofunctional a strongly basic anion exchanger §, activated carbon and tselsl methylcelluloses disposed downstream extract.

Description

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The invention relates to the tobacco industry and can be used in the control of the quality of tobacco and smoking articles containing sorbitol.

The purpose of the invention is to improve the accuracy of determining the mass fraction of sorbitol in tobacco.

Example. A sample of tobacco containing sorbitol is subjected to extraction with distilled water. To do this, take a sample of tobacco weighing about 1 g with an error of no more than + 0.0002 g, place it in a glass with a capacity of 100 ml, pour 20 ml of distilled water at a temperature and mix the contents of the glass for 30 minutes. The precipitate is separated from the liquid by centrifugation, washed with 80 ml of distilled water, collecting the washings in-glass with the extract.

In the glass chromatographic column, fitted at the bottom, with a tap and have a diameter of 22 mm and a height of 500 mm, a small amount of glass wool is placed and filled with a suspension of cellulose powder in water containing 15 g of cellulose. After the cellulose is precipitated, the column is filled with an aqueous suspension consisting of 4 g of activated carbon and 8 g of cellulose, and then with a suspension of 6 g of activated carbon in water. In the process of filling the column, a part of the water is drained through the α-tap, however, to prevent the drying of the sorbent layer. The height of the solvent (water) above the sorbent layer must be at least 50 mm. After the carbon layer is deposited, the column is similarly filled with AB-17 anion exchanger in OH form. After the resin has settled, the column is ready for operation.

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Tabachny {|. an extract containing sorbitol is applied to the column and eluted with water. The flow rate of the eluent is controlled by a valve located at the bottom of the column and maintained at a level of 10 drops per minute. The first 100 ml of eluate is discarded, the subsequent 1400 ml are collected in 100 ml portions. Each portion of the eluate is evaporated in a boiling water bath to a volume of 5 ml, cooled, quantitatively transferred with water to a 250 ml conical flask (the volume of the extract after transfer should be

935782

equal to 20 ml), 25 ml of potassium dichromate solution are poured from a burette, 50 ml of concentrated sulfuric acid are poured carefully along the wall,

5 carefully mixing the contents of the flask. After one hour, the solution is transferred to a 250 ml volumetric flask and made up to the mark with water. From the flask take 50 ml of solution for analysis, put it

10 in a conical flask with a glass stopper (flask capacity 250 ml), 150 ml are poured. distilled water, 10 ml of potassium iodide solution, closed with a stopper moistened with a solution of potassium iodide, and placed in that place for 10 minutes. After the time is up, the plug is rinsed with water, collecting the flush water into the flask, and the contents of the flask are titrated with 0.1 N. sodium thiosulfate solution with starch as an indicator of the presence of iodine. The end of the titration is the transition of the color of the solution from blue to emerald green.

In parallel, a blank experiment was conducted using distilled water instead of sorbitol extract. Such a definition is carried out for

30 all 14 portions of the eluate. The results of the analysis are calculated by the formula

(VrViVti-O.OOOt.250.00 H (iOO-W) -0,

X is the mass fraction of sorbitol in the dry matter of tobacco,%;

V - volume 0.1 n. sodium thiosulfate solution spent on the titration of the sample, ml; Vg - volume 0.1 n. solution

sodium thiosulfate spent on titration of the blank solution, ml; 0.0007 - the amount of sorbitol, corresponding to 1 ml

0.1 and. sodium thiosulfate solution, g; 250 is the volume of the oxidized sorbitol solution, ml; K - amendment to the titer of sodium thiosulfate dilution;

H - a hitch of tobacco, besides

for analysis, g; W is tobacco moisture content,%; 3 11935 50 - the volume of the oxidized sorbitol solution, taken for analysis, ml. The data obtained in the analysis. of all .14 servings, add up and get a value of 5.07%. In tobacco, subjected to analysis, 4.90 sorbitel is introduced, thus, the relative analysis error is equal in this particular case + 3.5%, which found-O 78 within the limits of the accuracy of the proposed method ± 5%. Purification of the extract on a combined sorbent removes all the substances oxidizable by potassium bichromate (except sorbitol) from the extract and thus eliminates the uncontrolled interferences of the analysis created by these substances.

Claims (1)

METHOD FOR DETERMINING THE SORBITOL MASS PERFORMANCE IN TOBACCO, which involves adding a solution of potassium dichromate and sulfuric acid to an aqueous solution of sorbitol, adding a solution of potassium iodide to the mixture, keeping the mixture in the dark, titrating the liberated iodine with sodium thiosulfate solution and determining the mass fraction of sorbitol the amount of sodium thiosulfate solution spent on titration, characterized in that, in order to improve the accuracy of determining the mass fraction of sorbitol in tobacco, • an aqueous solution of sorbitol ovyat tobacco by extraction with water sample containing sorbitol, and passing the extract through a chromatographic column filled with the combined sorbent, which is a. strongly basic monofunctional anion exchange resin, activated carbon and cellulose, located along the extract.