SU714279A1 - Method of quantitative determining of 2,3-dibromopropyonic acid - Google Patents

Description

(54 METHOD OF QUANTITATIVE DETERMINATION 2, 3-DYBROMPROPIONIC ACID

bromopropionic acid, corresponding to 1 ml of 0.1 n. silver nitrate solution g;

V is the volume of silver nitrate, followed by titration of the sample, vmj K is the correction factor to the normality of silver nitric acid solution;

H - a portion of 2,3-dibromopropionic acid, g; V (f - flask volume, ml; VH - pipette volume, ml. Example. About 1 g of technical 2,3-dibromopropionic acid containing acrylic acid as an impurity is placed in a 100 nirt volumetric flask, dissolved in water, and Pipette 10 ml of the solution, transfer to a conical box for iOO, ml, add 10 mp of monoethanolamine, connect the flask to reflux and 15 min. Then wash the liquid and grind it. with distilled water, transfer the contents of the flask to the titration beaker, look with azoic acid and about pH 2-3 on universal indkatornoy paper and add water to a total volume of 150 ml.

Bholduyotuyenny solution to k: o1myatnoy temperature, immerse in it the silver electrode and the electrolytic CL10CH of chlorate-silver. electrode filled with saturated potassium nitrate pactBOgroM connected to a pH meter.

Titrated with 0.1 n. silver nitrate solution: tide near the equivalent point of 0.1 ml. The end of the titration is determined by a sharp jump in the potential in the region of 1.50-250 mV. y: ...;:.; ./.,:. , N, The volume of expenditure YNHGO, on, titryvoy 0,1 n. The silver nitrate yield is calculated using the second derivative method.

The results of the analysis of this sample and two other samples of Technical 2,3-dibromopropionic acid are given in table. one.

Table 1

Continuation of table 1

 „3

 98.22

0.17 98.05 99.10

0.15 98.95

P ra m e R 2. On an analytical balance, weighed mixture, which contains about 1 g of 2,3-dibromopropionic acid and about 0.2 g of acrylic acid.

Saponification and titration are carried out as in example 1.

The results of the determinations are given in table. 2

table 2

Table 3. Measures 3. The results of determination of the content of 2,3-dibromopropion CEC.POTS in a technical product with a different ratio between monoethanolamine and water are given in table. 3

T a b l and c a 3

0.10

98.60

1,0128 98, .50,

0.15

1.0845 98.63 98.78

1.0521 98.80 0.15 98.65 0.17

1,0098 98,58

Claims (2)

98.75. The formula of the invention. The method of quantitative determination of 2,3-dibromopropionic acid by saponification of the analyzed sample in an alkaline medium at boiling with the resulting solution of potentiometric titration with a solution of nitric acid silver, about t and h in order to reduce the time and increase the accuracy of the determination, a mixture of monoethanolamine and water, taken in a volume ratio of 1-252-1, is used as an alkaline medium. Sources of information taken into account in the examination 1. Guben-Weyl. Methods of organic chemistry. M. / Chemistry, 1967, p.52. 2.JuNstuft sEl to the question of the determination of 2,3-dibromopropanoic acid. AnnaEen der Chemie, 1905, 342 (prototype).