SU1684638A1 - Method of quantitative determination of polyethylene polyamine - Google Patents

Abstract

The invention relates to analytical chemistry, and specifically to methods for the quantitative determination of polyethylene polyamine. The purpose of the invention is to increase the sensitivity and simplify the method. The method consists in dissolving a sample containing 2.5-38 µg of polyethylene polyamine in 3-5 ml of water, adding to the solution 6 1СГ5 mol of N-phenylsulfonyl-1,4-naphthohino: imine at room temperature. Then the solution is diluted with acetone to a concentration of 0.1-1.5 µg / mg and photometrically at a wavelength of 90 nm in cuvettes with an optical path length of 3 cm. 4 tab.

Description

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The invention relates to analytical chemistry, in particular to methods for the quantitative determination of polyethylene polyamine, used in industry as an antifoam and splash-catch, galvanizing electrolyte.

The purpose of the invention is to increase the sensitivity and simplify the quantitative determination method.

PRI me R 1. Quantitative determination of polyethylene polyamine in substance. The exact weight of the analyte (0.015-0.025 g) is dissolved in water in a 200 ml volumetric flask and adjusted to the mark with water. 5 ml of the resulting solution is placed in a 50 ml volumetric flask and diluted with water to the mark. 3 ml of the resulting dilution is placed in a 25 ml volumetric flask, 6 ml of a 0.3% acetone solution is added.

M-phenylsulfonyl-1,4-naphthoquinone imine and diluted with acetone to the mark. In parallel, the experiment was carried out with 3 ml of a 0.001% solution of polyethylene polyamine (standard) and the control. The measurement of the optical density of the colored solutions is carried out using a photoelectrocolorimeter at 490 nm in cuvettes with a layer thickness of 3 cm. The content of polyethylene polyamine is determined by the formula

g c-0 2

With% TZGLR

where D is the optical density of the measured solution;

Do is the optical density of the standard solution;

p - weight, g;

2 - the estimated coefficient taking into account the dilution and concentration of the standard solution

About 00

N

Os 00 00

The results of quantitative determination are given in Table. one.

The cuvette length is limited to 3 cm, since when measuring the optical density at a light path length of 5 cm, due to the colored control, the sensitivity of the photoelectric colorimeter is insufficient to calibrate the instrument to O optical density.

The concentration limits within which the observance of the law of absorption is observed lie in the range of 0.1-1.5 µg in 1 ml of the photometric solution. This corresponds to a concentration range of 2.5-38 μg in the sample to be analyzed.

The effect of the amount of reagent on the value of optical density is given in Table. 2

As follows from the table. 2, a rational excess of reagent is 6 ml of a 0.3% aqueous solution (6-10 mol), since a further increase in the amount of reagent does not cause an increase in optical density.

The amount of water in the photometric solution should not exceed 6 ml, since this leads to a significant decrease in the optical density (Table 3) and, consequently, the sensitivity of the method.

PRI mme R 2. Determination of polyethylene-polyamine in industrial wastewater.

To the analyzed sample of water (250 ml) add 2 ml of 0.1N. hydrochloric acid solution and evaporated to a volume of 4-5 ml. The resulting solution was transferred to a 25 ml volumetric flask, and 6 ml of a 0.3% solution of M-phenylsulfonyl-1,4-naphthoquinone imine in acetone and acetone were added.

3

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The tone is adjusted to the mark. In parallel, the experiment was carried out with 1 ml of a 0.001% solution of polyethylene polyamine and a control. The measurement of the optical density of the colored solutions is carried out using a photoelectrocolorimeter at 490 nm in cuvettes with a layer thickness of 3 cm. The content of polyethylene polyamine is calculated by the formula

S. mg / l-2.

where D is the optical density of the test solution:

Do is the optical density of the standard solution;

0.04 is a conversion factor taking into account the dilution, weighed amount and concentration of the standard solution.

The results of the determination are given in

table.4.

Claims (1)

The invention of the method of quantitative determination of polyethylene polyamine, which consists in dissolving a sample, is introduced into a solution. the color reagent is diluted with an organic solvent and the resulting solution is photometric, characterized in that, in order to increase the sensitivity and simplify the process, the sample containing 2.5-38 µg of the test substance is dissolved in 3-5 ml of water, injected into the resulting solution b -10 mol of the color reagent M-phenylsulfonyl-1,4-naphthoquinone imine at room temperature, diluted with acetone to a concentration of 0, 1-1,5 µg / ml and photometrically at a wavelength of 490 nm in cuvettes with an optical path length of 3 cm. Hitch,% 1.0 2.0 zo 4.05,06,07,08,0 Table 4