SU667875A1

SU667875A1 - Method of quantitative determining of dibutyl phosphoric acid in solutions of tributyl phosphate in synthin

Info

Publication number: SU667875A1
Application number: SU772536204A
Authority: SU
Inventors: Алексей Евгеньевич Клыгин; Нина Степановна Коляда; Сергей Николаевич Федотов
Original assignee: Предприятие П/Я Р-6575
Priority date: 1977-08-01
Filing date: 1977-08-01
Publication date: 1979-06-15

Description

Изобретение-относитс к области aijajinтической химии, а именно, к способам количественного определени дибутилфосфорной кислоты и может быть использовано при контроле технологических процессов.The invention relates to the field of aijajintic chemistry, namely, to methods for the quantitative determination of dibutyl phosphoric acid and can be used in the control of technological processes.

Известен способ количественного определени дибутилфосфорной кислоты, заключающийс -в обработке анализируемой пробы метиленовым синим и хлороформом с последующим фотометрированием полученного раствора хлороформенного экстракта 1.A known method for the quantitative determination of dibutyl phosphoric acid, which consists in the processing of an analyzed sample with methylene blue and chloroform, followed by photometry of the resulting solution of chloroform extract 1.

Недостатком способа вл етс низка чувствительность определени .The disadvantage of this method is low detection sensitivity.

Наиболее близким к описываемому изобретению по технической сущности и достиraeMOiyiy результату вл етс способ количественного определени дибутилфосфорной кислоты в растворах трибутилфосфата в синтине , заключающийс в последов ательной обработке анализируемой пробы раствором сол ной кислоты, насыпхенным этилендиаминтетрауксусной кислотой, этилендиаминтетраацетатом натри и хлороформом, с последующим отделением водного сло и обработкой его феносафранином и хлороформом. The closest to the described invention according to the technical essence and the achievement of the MEOyiy result is a method for quantitative determination of dibutyltooltoccrystrate in tributylphosphate solutions in synthine, consisting in sequential processing of the sample being analyzed with a solution of hydrochloric acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylene diaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetra acetic acid, ethylenediaminetetraacetic acid, ethylenediaminetetraacetate acid and treating it with phenosafranin and chloroform.

отделении хлороформенного сло , добавлении приЭТОМ раствора 2.separation of the chloroform layer, adding at this solution 2.

Недостатком способа вл етс низка точность и плоха воспроизводимость результатов определени в присутствии продуктов сульфировани синтина - алкилсульфокислот и алкилсульфанолов, так как они по своим химическим свойствам близки к дибутилфосфорной кислоте и присутствуют в растворах в количествах соизмеримых с ней.The disadvantage of the method is low accuracy and poor reproducibility of the results of determination in the presence of sulfonation products of sintine - alkyl sulfonic acids and alkyl sulfanols, since their chemical properties are close to dibutyl phosphoric acid and are present in solutions in amounts commensurate with it.

Цель изобретени - повыщение точности и воспроизводимости определени в присутствии продуктов сульфировани синтина.The purpose of the invention is to increase the accuracy and reproducibility of the determination in the presence of sulfinated sintine products.

Поставленна цель достигаетс тем, что анализируемую пробу предварительно обрабатывают хлоридом бари и хлороформом при рН среды 5,45-5,55 с последующим отделением водного сло .The goal is achieved by the fact that the analyzed sample is pretreated with barium chloride and chloroform at a pH of 5.45-5.55, followed by separation of the aqueous layer.

Claims

Example. In a separating funnel with a capacity of 50 ml, 2-10 ml of the sample, 5 ml of distilled water, 2 ml of acetate buffer solution are taken (0.05 M sodium acetate and 0.04 M acetic acid, pH 5.45-5.55) , 1 g of barium chloride, 7 ml of chloroform and shaken for 2 MHff, then the organic phase is discarded, and 0.9 ml of concentrated hydrochloric acid, 10 ml of tributyl phosphate solution in hydrogenated synthine are added to the aqueous and shaken for 2 min., selected by the SHShleafsslaivanii aqueous phase. The organic phase is washed with 20 and 10 ml of OD n. solution of hydrochloric acid, saturated with ethylenediaminetetraacetic acid. To the washed organic phase, 2 ml of acetate buffer solution, 5 ml of distilled water, 7 ml of chloroform are added and shaken for 2 minutes, dropping the organic phase after settling. To the aqueous phase containing DBP is added 25 ml of chloroform, 5 ml of a 0.25 ° / safranin T solution and shaken for 4 minutes. The organic phase is poured into a 25 ml flask, into which 0.8 g of anhydrous sulphate is previously placed, shaken several times until the chloroform extract is completely dehydrated and photometric is measured in a cuvette of 1-2 cm at 539 named: The proposed method is suitable for determining DBP in solutions of different composition in a, containing sulfinated sulfinated products. Detection limit 2-10 M / l dibutyl phosphoric acid. The coefficient of variation does not exceed 5%. To achieve one definition, 40 mnG is required. Thus, the proposed method, pbz vm y-g goluchuyge dosgbvyrye and reproduce the results of the determination of DBF in techno THG vdskyy Gravity; WITH THE PRODUCTION OF SULFIR SHANT SYNTHES; to control the content of DBP in, the process of reprocessing irradiated fuel. According to a known method, the determination of dibutylphosphoric KZhlGgtrayTychey yevoz MOZHNO in the presence of sulfonation products sintin ,. The reliability and reproducibility of the prediaria Mdro 1 "6D is confirmed by the following SchmidtDayNMGtry analysis of a technological solution containing 100 mg / l DBP, 101 ± 2 mg / l (with a reliability of 0.95) was found. The method of the proposed method is 2 times better than that of the known method (the coefficient of the proposed method is 5% and the known method is 10%). The basic technical advantage of the invention over the known method is that it allows the preparation of the results of the determination of DBP in solutions containing the products of sulphonation of syntin. This ensures reliable control of the quality of the extractant in the extraction process and the removal of hydrolysis products. The method of quantitative determination of dibutylphosphoric acid in solutions of tributyl phosphate in synthine by sequential treatment of the analyzed sample with a solution of hydrochloric acid 1, saturated ethylenediaminetetraacetic acid, buffer solution and chloroform, followed by separation of the aqueous layer and processing it with safranine and chloroform by the procedure, chloroform, chloroform, chloroform, chloroform, chloroform and chloroform. sodium sulfate and the spectrophotometer of the solution obtained therewith, which differs from Tiezh, in order to increase NOSTA and reproducibility for determining .in prisutstvyy Syntyna sulfonation products, the analyzed sample is pretreated with barium chloride and chloroform at pH 5, 55, followed by separating the aqueous layer. Sources of information taken by the HEs in their examination 1.Kbrenman IM Methods for the determination of organic compounds. “Himi, M., 1970, p. 226-228.

2. Klygin A.Ye., Bolshakova A.S., Kolya N.S. Extraction-photometric method for determining dibutylphosphoric acid in circulating extractant. - TV Symposium of the Council for Mutual Economic Assistance. Research in the processing of irradiated fuel. 1977, Karlovy Bars.