SU395752A1 - METHOD OF QUANTITATIVE DETERMINATION OF SUBSTITUTED HYDRAZINES - Google Patents

Description

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This invention relates to spectrophotometric methods for the metric determination of meshed hydrazines in the presence of hydrazine.

A known method for the quantitative determination of substituted hydrazines, based on spec. OctophotometrO; in a colored compound formed by substituted hydrazine and acetone from l-dimethyl minobenzaldehyde in Presence of alkali.

One: to this method it is impossible to determine the substituted hydrazines in the presence of hydrazine, which often accompanies them as an impurity and replaces the spectrophotometric determination of the substituted hydrazines, as it gives the same color reactions.

In order to POSSIBILITY to determine the substituted hydrazine in the presence of hydrazia, it is not necessary to preliminarily add a solution of dinitrobeisoyl chloride in benzene to the sample of the analyte, followed by treatment of the obtained compound with alkali and water and separation of the benzene layer.

The result of diitrobenzoate of a mixture of substituted hydrazine and hydrazine was carried out with an excess of reagent in an alkaline medium. The derivatives of the substituted hydrazine are then formed and then the benzene is extracted from the reaction mass, and the hydrazine derivative is not removed by benzene, it remains in the aqueous alkaline medium and thus does not interfere with the further spectrophotometric determination of the dinitro derivative of the substituted hydrazine in the benzene extract using a color acetone and a slide. Yanovsky).

Method of determination

substituted g and d r and z and n about IB

in the presence of hydrazine.

A few milliliters of a solution containing 2-10 mol of substituted hydrazine and a few milliliters of a solution containing 3-10 hydrazine are placed in a 50 ml volumetric flask, and 3 ml of reagent solution (200 mg of 3,5 or 2,4 diiitrobenzoyl chloride in 100 ml of absolute benzene), 1 ml of a 0.2 M solution of NaOH and shake for 1 hour on an electric pump. Then, 20 ml of 2 M NaOH solution is added to the mixture (to remove excess reagent) and shaken for another 30 minutes, after which they are poured into a flask of distilled water so that the benzene layer rises to the flask. 1 ml of the benzene layer is pipetted into a 10 ml ml flask, 2-3 ml of an alcohol-acetone mixture (1: 1) is divided, 0.4 ml of 2M XaOI is added, and the mixture is made up to the same alcohol-acetone mixture. The solution is thoroughly mixed and after 3 minutes, measure 3

They are painted in bird color of colored RastiBopoB on FEC-M with a green light filter (if Z.b-dinitrobenzoyl chloride is green) or with a blue filter (if 1 is 2,4-dinitrobenzoylchloro / D), in 1 cm long, using as a comparison solution WATU.

In parallel, lead deaf onyt. According to the obtained values of optical 1step, with the help of the calibration graph,

the concentration of the substituted hydrazine in the test solution. Calibration graphs are based on pure individual substituted hydrazines, using the same procedure. The method is simple and precise, discharges the substituted hydrazines, in the presence of a 10-: fold excess hydrazine. Relative method error.

The results of determination of substituted hydrazines in the presence of hydrazine are presented in the table.

PREDIT METALSH

The method of quantitative determination of substituted hydrazines. By means of spectrophotometry of the short compound, obtained by P) and the interaction of dinitrol-soluble one-time mixed hydrazine with acetone in the presence of alkali, characterized in that

the possibility of detecting the substituted hydrazine in the presence of lidrazine, previously, a solution of dinitrobenzoyl chloride in benzene is added to the sample of the analyte, followed by treatment of the resulting compound with water and water and separation of the benzene layer.