SU990643A1 - Method for detecting halogenide ions - Google Patents

Description

This invention relates to analytical chemistry, and specifically to methods for determining halide ions.

A known method for the determination of chloride ions, including the introduction of diphenylcarbazide and mercury metal-II solution into the analyzed solution of the organic reagent, forms a colored compound with the reagent, and then photometry the solution fl.

This method is characterized by its low sensitivity (10 μg / ml and low selectivity: ammonium, cobalt, copper, xpoMa (vt) zheleaSSh) ions, lead, zinc, sulfate, etc. interfere with the determination.

The closest in technical essence and the achieved result to the invention is a method for determining fluoride ions, including introducing zryochromo cyanine (and a solution of metal ions - zirconium C1U) into the analyzed solution of an organic reagent, in a medium of 0.8 n. hydrochloric acid and the subsequent photometric measurement of the solution. The reagent is injected to a concentration of 0.18 mg / ml, zirconium solution - to 7.25 µm / mlf2

However, the known method is characterized by a low sensitivity of 210 kg / ml), which leads to the need for pre-concentration.

The purpose of the invention is to increase the sensitivity of the analysis.

This goal is achieved by the fact that in the method for determining halide ions

10 as organic reagent, diantipyryl-3,4-dimethoxyphenylmethane is introduced to a concentration of 0.03-0.09 mg / ml, uranium ions are used as a metal to a concentration of 0.02-3.0 µg / ml, and

15, the reaction is carried out in a 7-11 n medium. sulfuric acid when the solution is irradiated.

Table 1 presents the dependence of the optical density (A) on the concentration of diantipyryl-3,4-dimethoxyphenylmethane С С reagent).

From the data presented in Table 1, it can be seen that the optimal concentration of the reagent in the analyzed solution is 0.03-0.09 mg / ml. Table 2 shows the dependence of the optical density (L) on the concentration of uranium )

From Table 2 it follows that the optimum concentration of uranium ions is 30

L ets 0,02-3,0 mkg / ml. Table 3 presents the dependence of optical density (A) on the concentration of sulfuric acid (). From Table 3 it follows that the optimum acidity of the analyzed solution is 7-il n. for sulfuric acid The solutions are irradiated with ultraviolet light with a wavelength of 300-550 nm. Example. Determination of fluorine in rubber. A portion of finely divided rubber, 1,000 g, is placed in a 100 ml conical flask, 40 ml of bidistilled water is added, which is additionally purified with ion exchangers, the flask is closed with a stopper with an air cooler, and boiled for 30 minutes. After cooling, the solution is filtered into a 50 ml volumetric flask and diluted to the mark with a node. A 10 ml portion of the solution is placed in a 50 ml volumetric flask, 1 ml of uranium salt solution (.VI) containing 130 MKf of uranium Cvl, 0.5 ml of 0.5% ethanolic solution of diantipyryl 1-3, 4 is poured. -dimethoxyphenylmethane, diluted to 50 ivin 9 n. sulfuric acid solution and mix. The solutions are then irradiated in 50 ml beakers with a BW quartz mercury lamp SVD-120-A with nm for 1 hour with constant stirring of the solution, after which the optical density of the solutions is measured on an SF-4A spectrophotometer, nm in a cell with an absorbing thickness 5 cm layer. Fluoride ion content is determined by calibration curve. PRI mme R 2. Determination of fluorine in rubber. The analysis is carried out as in Example 1, but injected into a 50 ml flask with 1 µg uranium tyi) to create a concentration of 0.02 µg / ml, a solution of dantipyryl-3, 4-dimethoxyphenylmethane. To create a concentration of 0.03 mg / mp, diluted to tags 7 n. sulfuric acid and irradiated with a mercury lamp with a. Froze Determination of fluorine in rubber. The analysis is carried out as in Example 1, but injected into a 50 ml flask with 150 µg of uranium (vl) to create a concentration of 3 µg / ml, a solution of diantipyryl-3, 4-imyroxyphenylmethane to create. Neither a concentration of 0.09 mg / ml is diluted to the 11 n mark. sulfuric acid and irradiated with a wavelength of 546 nm. Example4. Determination of chloride in process water. 5 ml of process water are placed in a 50 ml volumetric flask and 1 µg of uranium is added (to create a concentration of 0.02 µg / ml and a solution of diantipyryl-3, 4-dimethoxyphenylmethane to a concentration of 0.03 mg / ml, diluted to the mark 7 with a solution of sulfuric acid and irradiated with a light of a mercury lamp with –405 nm Example 5. Determination of bromide in process water 10 ml of process water are placed in a 50 ml volumetric flask and all reagents are added as described in Example 1. The proposed method of determination halide ion improves sensitivity by 20 0 times x x 10 mcg / ml. Table 1

 mcg / ml 0.01 0.02

0.5750.620 0.630 0.635 0.630 0.635 0.570 35 0.3200.540 A

Claims (2)

Invention Formula The method of determining halide ions, including the introduction into the analyzed solution of organic reagent and the solution of metal ions forming the colored compound with the reagent in an acidic medium and the following Table 2 0.1 0.5 1.5 3.0 3.0 5.0 Table 3 791113 0.610 0.630 0.615 0.550 S9906436 photometry that distinguishes between 7–11 n. of sulfuric acid and irradiation by the fact that, in order to increase the sense of solution, of the analysis, as the sources of information, organic reagent is introduced dianti-taken into account during the examination of "pyryl-3,4-dimethoxyphenyl methane to the Kon- 1. Factory laboratory, 1946, centering 0.03-0.09 ug / ml, and quality 5ts i2, p.161. ve metal - ions of uranium Vl) to 0.02 - 2. Avio €. , 1957, v 29, 3.0 µg / ml, and the reaction was carried out in 1709.