SU1293647A1 - Method of determining water microquantities in organic solvents - Google Patents

Abstract

The invention relates to the field of analytical chemistry, namely, to methods for the spectrophotometric determination of water in organic solutions x, and can be used in the analysis of both solvents and materials that are soluble in them, and allows for an increase in the sensitivity of the analysis. Three samples are taken (10 ml samples of acetone, 10 samples of acetone solution are added to each sample, for example, N-triphenylmethyl-2 perchlorate (p-dimethylaminostyryl) quinolini with a concentration of 2-10 mg / l, stirred at room temperature. Found, optical densities or absorption intensities at a depth of 325 and calculate the arithmetic average of three measurements (32100), using which the concentration of water is determined by the hydrolysis of the injected salt using a calibration graph. The sensitivity of the analysis increases to 2-10 mg / l. with (L Is9 (UD CO O 4ik.

Description

1129

The invention relates to analytical chemistry, namely, methods for determining the amount of water in organic solvents by adding colored compounds to change the absorption rate and can be used in the analysis of both solvent and substances dissolved in them.

The purpose of the invention is to increase the sensitivity of the analysis.

Used colored salts are given in table, 1,

Example 1 A series of acetone solutions were prepared containing water from 0.1 to 0.0001% by weight by mixing calculated amounts of anhydrous acetone and acetone containing

0.1 wt.% Water. Anhydrous acetone was obtained by drying and distilling acetone with an analytical grade. In the acetone solutions obtained, the corresponding reagents were dissolved (Table 2) and optical densities (e) were measured in the region of the absorption maxima. From the change in optical density by 0.0, the minimum detectable concentrations of water were determined.

Example 2, analogously to example 1, a series of dichloroethane solutions was prepared. The reagents are dissolved in them.

I-Xantil-2 (p-dimethylaminosthenyl) quinolini perchlorate

I-Thioxantil-2 (p-dimethylamino styryl) quinolini perchlorate

N-Triphenylmethyl-2 (p-dimethylaminostyryl) quinolini

M-Xantil-4- (p-dimethylaminosthenyl) quinolini perchlorate

I-Thioxantil-4 (p-dimethylamino styryl) quinolini perchlorate

2

and optical densities were measured as in Example 1.

The results of spectrophotometric determination of water by various reagents in solvents are presented in Table 2.

As can be seen from the table, the sensitivity of the proposed reagents is 1–2 orders of magnitude. It takes an equal amount of time (about 5 minutes) to determine the water with all the reagents listed using spectrophotometric method.

Claims (1)

Invention Formula The method of determining the microscopic amounts of water in organic solvents, including the introduction of organic colored compounds and the subsequent quantitative registration of changes in the intensity of absorption, characterized in that, in order to increase the sensitivity of the analysis, colored salts of Ht (xanthyl, thioxantil, triphenyl) are used as organic compounds - Tyl-) quinolini or acridinium containing a p-dimethylaminostrym group,., Table 1 Malinova 525 30900 P 525 . 26600 525 32,000 Rozova 550 21,000 550 19,000 N-xantil-9 (p-dimethylamino styryl) acridinium perchlorate N-Thiok Santil-9- (p-dimethylaminostyryl) acridine perchlorate Diazokhin (2) Trans-azobenzene + (3) 540 0.1 0.1 410 0.02 0.02 Editor V. Kovtun Compiled by G. Tsoy Tehred A. Kravchuk Order 380/49 Circulation 777 VNIIPI USSR State Committee for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5 Production and printing company, Uzhgorod, st. Project, 4 Continuation of table 1 Syn 616 18700 eleven 616 17100 table 2 0.02 0.02 Corrector T. Kolb Subscription