SU1233047A1 - Method of determining osmium - Google Patents

Abstract

The invention relates to analytical chemistry, in particular, to a method for the determination of osmium, and allows an increase in the sensitivity of the analysis and an increase in the range of detectable contents. In a container (E) with 1 µg of osmi, a 2.7 x X M solution of sulphate 1,10-phenanthroline is sequentially introduced. O, 1 M solution of hydrazine hydrochloride, 2.4 M solution of sodium bromide, 1.0 M solution of sodium acetate or potassium until the equilibrium concentration of the solution is 0.03–0.3 M. Set the pH of the medium to 7.5 by adding sodium hydroxide solution followed by dilution with water and stirring. The closed E with the solution is placed in a water bath for 5 hours, cooled with a stream of cold water. The intensity (I) of luminescence at 700 nm was measured on a spectrofluorometer (power of 100 W glow lamps, SZS-10 light filter, monochromat, photomultiplier FZU-79, direct current source B5-24, microammeter F 116/2); according to the slope of the graded graph with the coordinates: And luminescence (relative units) - the concentration of osmi (µg / ml). 1 tab. with (O (L y with so about about 4

Description

The invention relates to an analytical method, namely, the luminescence method for determining osmium, and can be used in various fields of chemical analysis.

The purpose of the invention is to increase the sensitivity and the expansion of the range of defined contents.

Example. Into a test tube with a ground-in stopper, 1 µg of osmium is injected, 2.5 ml of 2.7 x X 10 M solution of sulphate 1,10-α-phenanthroline, 1 ml of a 0.1 M solution of hydrazine hydrochloride, 0.5 ml 2 are added successively. A 4 M solution of sodium bromide, 1 ml of a 1.0 M solution of sodium acetate (or potassium) and 5 solution of sodium hydroxide is used to stop the pH of the medium at 7.5, then the resulting solution is diluted with water to 10 ml and stirred. The tube is closed, placed in a boiling water bath for 5 hours, then cooled under running cold water, and the luminescence intensity of the solution obtained is measured. The sensitivity of the determination is equal to the tangent of the angle of inclination of the calibration curve, in the coordinates: intensity of any incidence, relative units Osmi concentration 5 µg / ml. The table shows the results of studying the effect of sodium acetate (potassium) concentration on the sensitivity of the determination of (H) µg osmi (determination number 5) o

The proposed method is characterized by a low limit, the detection of osmi is 3-10 µg / ml and a large range.

Compiled by GLDToy Techred 0 Gortway

Order 2762/45 Circulation 778 Subscription

VNIIPI USSR State Committee

for inventions and discoveries 113035, Moscow, Zh-35, Raushsk: nab. D. 4/5

. Production and printing company, Uzhgorod, Projecto st., 4

the zone of detectable contents of 3-10 - 15 O µg / 1 sh,

Measurement of the luminescence intensity was carried out at 700 nm using a spectrofluorometer consisting of a 100W stabilized incandescent light bulb with an SZS-10 light filter, a UM-25 photoelectric multiplier UH-25 monochromator and microampere-millivoltmeter Ф 116/2,

Formulas

and 3 o r e te

The method of determining osmium, including the treatment of the analyzed solution, contains halides of ions, 1,10-phenanthroline, hydrazine, subsequent heating in a boiling water bath, and measurement of the luminescence intensity, so as to increase the sensitivity and spread the range of detectable contents, before scrubbing, sodium or potassium acetate is added to the analyzed solution to an equilibrium concentration of 0.03-0.30 M.

30 Concentration of sodium acetate (potassium), M

72 90

95

100 95

82

Proofreader L. Pilipenko

Claims (1)

Formula ^invention; i am 15 A method for determining osmium, including processing an analyte solution containing halide ions, 1,10-phenanthroline, hydrazine, 20 heating it in a boiling water bath and measuring the luminescence intensity, characterized in that, in order to increase sensitivity and expand the range 25 determinable contents, before heating, sodium or potassium acetate is added to the analyzed solution to an equilibrium concentration of 0.03-0.30 M. 72. 90 95 100 95 82