SU1575106A1 - Method of quantitative determination of sulfaminate-ion in water - Google Patents

Abstract

The invention relates to analytical chemistry, in particular, to a method for the quantitative determination of sulfamine ion in water, and can be used in sanitary laboratories. The purpose of the invention is to increase the sensitivity of the method. The analysis is carried out by acidifying the sample with acetic acid to a pH of 1.8-3.4, boiling for 1.0-2.0 min, followed by cooling, and treatment with acetic acid in a volume ratio of 1: (0.35-0.75) and sodium nitrite , boiling for 5-25 minutes, adding the Griss-Ilosv reagent's acetic acid solution and colorimetrizing the colored solution. The sensitivity of the method is 0.1 mg / l. 4 tab.

Description

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(21) 44A6610 / 23-04

(22) 04/28/88

(46) 06/30/90, Bull. 24

(71) Scientific and Production Association State Institute of Applied Chemistry

(72) V.K.Potrokhov and K.K.Dlimova

(53) 543.42.062 (088.8)

(56) Root K, K. Methods for the determination of organic compounds. Photometric analysis. M .: Himi, 1975, 64-67 „

Koltgof and „M. and draw Volumetric analysis. M .: Goskhimizdat, 1961, with 806.

(54) METHOD FOR QUANTITATIVE DETERMINATION OF SULFAXAT-ION IN WATER

(57) The invention relates to analytical chemistry, in particular to a method for the quantitative determination of sulfamig sodium ion in water, and can be used in sanitary laboratories. The purpose of the invention is to increase the sensitivity of the method. The analysis is carried out by acidifying the sample with acetic acid to a pH of 1.8-3.4, boiling for 1.0-2.0 min, followed by cooling, treatment with acetic acid in a volume ratio of 1: (0.35-0.75) and sodium nitrite , boil for 5–25 min, add an acetic acid solution of the Griess-Nlosva reagent and colorimeter the colored solution. The sensitivity of the method of 0.1 mg / l, a table.

This invention relates to analytical chemistry, in particular to methods for the quantitative determination of sulfamine-ion in aqueous solutions.

The aim of the invention is to increase the sensitivity of the method.

Example I. Analysis of water containing sulfamine-ion.

A 50 ml beaker is filled with 25 ml of the analyzed water, which is acidified with acid to pK 2., boiled for 1 min, after which the sample is transferred to a measuring tube with a capacity of 25 ml, cooled (in a tube with a tap water to 20 ± 2 ° C and the volume in the test tube is made up to the mark with distilled water. The solution is stirred. An aliquot portion of 5 ml is taken and added to the test tube with a capacity of 15-25 ml, and 2 ml of acetic acid are added to substances not less than 99.5% (ratio of water to be analyzed: acetic acid 1; 0.4) and ayut 1 ml of a solution of sodium nitrite (10 g N0)

The sodium nitrite solution is prepared as follows.

A portion of sodium nitrite 0.15 g, weighed to the fourth decimal, is transferred to a 100 ml volumetric flask, made up to the mark with distilled water, and mixed (mixed 1). 1 ml of solution 1 contains 1000 µg of nitrite. 0.5 ml of the solution is diluted with distilled water to 50 ml (solution 2). 1 ml of solution 2 contains 10 µg of nitrite ion,

The resulting solution is stirred and heated in a boiling water bath for 5 minutes, after which the sample cooled.

O5

Clad (under running tap water up to 20 ± 2 ° C), 2 ml of the Griss-Ilosva reagent is added to it, Griris-Ilosva reagent is prepared by mixing I ml of 0.33% sulfanilic acid solution in 10% - a solution of acetic acid and 1 ml of a 0.067% solution of od-naphtylamine in a 10% solution of acetic acid. After 15 min, the optical density is measured (light filter no. 6,). Idle experience

 Take sulfamide-free t-ion water, acidify it with acetic acid to pH 2 and perform all operations as described above.

DV is found and the concentration of sulfaminate-ionar is determined according to the schedule of sulfate-sodium-ion-f (-D1).

This is sulfamine-ion2, 0 mg / l

Sulfaminate-ion2 found, 0 mg / l

Table 1 shows the results of experiments on the effect of the pH of the solution at the first boiling.

 As can be seen from table 1, the measured error does not exceed 15% in the range of pH 1.8-3.4.

Table 2 shows the results of experiments on the effect of boiling time at PH 2.0.

As can be seen from Table 2, the total error does not exceed 15% in the time interval of the first boiling 1.0-2.0 minutes.

. Table 3 shows the results of experiments on the effect of the volume ratio

Indicators

7 b 8 b3 2 3f5

That's sulph aminate ion.

Note. Boiling time, the ratio is analyzed

 A sample of acetic acid 1: 0.4, second boiling time 5 minutes.

0

analyzed sample: acetic acid.

As can be seen from table 3, the total error does not exceed 15% in the range of volume ratios of the analyzed sample: acetic acid 1: (0.35-0.75).

Table 4 shows the results of experiments on the effect of the second boiling time on the results of experiments.

As can be seen from Table 04, the total error does not exceed 15% in the second boiling time interval of 5-25 minutes.

Ammonium sulfate ions (. Up to 60 mg / l), chlorine ions (up to 350 mg / l) nitrate ions (up to 300 mg / l), iron ions (up to 1 mg / l) „are not detected.

The sensitivity of the method is 0., 1 mg / l, the total error of -15% with a confidence probability of 0.95, which is 20,000 times better than that by a known method (2.0 g / l).

Claims (1)

Invention Formula The method of quantitative determination of sulfamine-ion in water by treating an analyzed sample with nitrite-ion in an acidic medium, which differs - so that, in order to increase the sensitivity of the method, the analyzed sample is acidified with acetic acid to pH 1.8-3.4, t for 1-2 minutes, cooled, treated with an aliquot of the specified acid in a volume ratio of 1: (0.35-0.75 / and sodium nitrite, boiled for 5-25 minutes, add the acetate solution of the Griess-Ilosva reagent followed by colorimetric staining Table 1 five five 0 solution pH 51575106 6 table 2 Indicators Time of the first boiling (P), with AO | 50 G 130 MAO 150 That's sulfamine-ion, mg / l 2.0 2.0 2.0 2.0 2.0 Found sulfamate ion mg / l 1.30 1.70 1.8A 1.70 1.50 Total error, ±% -35.0-15.0 -8.0 -15.0 -25.0 . Note. pH 2.0, the ratio of the analyzed sample: acetic acid 1: 0, A, the second boiling time of 5 minutes Table 3 Indicators The ratio of the analyzed water: acetic acid 1: 0.25 | 1: 0.30 1: 0.35 1: 0.65 1: 0.70 I 1: 0.80 That's sulphamine-, ion, mg / l 2,0 2,0 2,0 2,0 2,0 2,0 2,0 Found sulfamine-ion, mg / l 1.60 1.68 1.84 1.80 2.00 1.0 Total error, ±% -2.0 -16.0 -8.0 -10.0 0.00 -50,0 Note. PH 2.0, first boiling time 1 min, second time 5 min. i Table 4 Indicators Secondary boiling time, min 3.5, 4.0 4.5, | 7.5 8.5 | 10 | 15 20 G 2 1 25 G 28 J30 That's sul-aminate ion, mg / l 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Found sulfamine, mg / l 1.4 1, 6 1.8 2.1 2.04 1.96 1.88 1.88 1.8 1.68 1.6 1.4 Total error, i% -30 -20 -10 +4 +4 +2 -2 -6 -10 -14 -20 -30 Note, the first boiling time is 1 min, the ratio of the analyzed lobic to acetic acid is 1: 0.4 Compiled by S. Khovanska Editor L. Veselovska Tehred M. Didyk Proofreader V. Kabatsy Order 1781 Circulation 512 Subscription V11IIPI State Committee for Inventions and Discoveries at the State Committee on Science and Technology of the USSR 113035, Moscow, Zh-35, Raushsk nab. 4/5 Production and publishing plant Patent, Uzhgorod, st. Gagarin, 101