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GOST 1367.8-83

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

INTERSTATE STANDARD

ANTIMONY

Method for the determination of selenium

Antimony. Method for the determination of selenium

AXTU 1709

GOST

1367.8 -8 3

Resolution of the USSR State Committee on standards of 16 December 1983, No. 6013 date of introduction

installed 01.01.85

Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization,

Metrology and certification (ICS 4−94)

This standard specifies a method for the inversion perimentally polarography for

definition of selenium from 210−5 to 810−5% in the antimony brand Swoooop.

The method is based on the allocation of selenium in elemental form on the collector — sulphur and definition

the method of inversion perimentally polarography with accumulation of 0.4 mol/dm3 solution

sulfuric acid in the presence of ions of dichromate and copper (II).

(Changed edition, Rev. No. 1).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis and security requirements — according to GOST 1367.0−83.

2. APPARATUS, REAGENTS AND SOLUTIONS

Polarograph AC type PU-1.

Beakers, glass, laboratory for GOST 25336−82 with a capacity of 50, 100 cm3.

Volumetric flasks according to GOST 1770−74 with a capacity of 100 cm3.

Pipette with divisions for NTD with a capacity of 1, 2, 5 cm3.

The cylinders are graded according to GOST 1770−74 with a capacity of 50 cm3.

Nitric acid of high purity according to GOST 11125−84.

Hydrochloric acid of high purity according to GOST 14261−77 and 3 mol/dm3 and 6 mol/dm3 solutions.

A mixture of concentrated nitric and hydrochloric acids in a ratio of 3:1 (opposite the Royal

vodka).

Orthophosphoric acid according to GOST 6552−80.

Formic acid according to GOST 5848−73.

Bidistilled water (double-distilled water); prepared by distillation of distilled water in kvar

Zevon distillation apparatus.

Sulfuric acid of high purity according to GOST 14262−78 diluted 1:1 and 0.4 mol/dm3 solution.

Hydroxylamine hydrochloride according to GOST 5456−79, the solution with mass fraction 10% in 6 mol/dm3

a solution of hydrochloric acid and a solution with a mass fraction of 5% in 3 mol/dm3 solution of hydrochloric acid.

Chernovetskiy sodium (sodium thiosulfate) according to GOST 27068−86, a solution with a mass

a share of 30%.

Milk of sulphur: to 10 cm3 of solution with a mass fraction of 30% sodium chernovetskogo add

give 2 cm3 of concentrated sulfuric acid immediately before use.

Bromine according to GOST 4109−79.

Official edition Reprinting is prohibited

Edition with amendments No. 1, approved in March 1989 (IUS 6−89).

54

frame construction

GOST 1 367.8−83 C. 2

Potassium dichromate according to GOST 4220−75, a solution with a mass fraction of 5%.

Copper sulfate according to GOST 4165−78, a solution containing 500 µg 1 cm3 of copper.

Selenium on the other 6−09−5358−87.

The standard solutions of selenium.

Solution a: 0.1 g of metallic selenium, is placed in a beaker with a capacity of 100 cm3 and dissolved

when heated in 10 cm3 of reverse Aqua Regia. Then add 5 cm3 of concentrated sulfuric

acid, is evaporated prior to the allocation of steams of sulfuric acid, cooled, poured pedistal

late, boil and cool again. The resulting solution was transferred to volumetric flask with a capacity of

100 cm3, adjusted with double-distilled water to the mark and mix.

1 cm3 of the solution contains 1 mg selenium.

Solution B: 1 cm3 of solution And poured into a measuring flask with a capacity of 100 cm3, poured

0.4 mol/dm3 sulfuric acid solution to the mark and mix; prepared on the day of use.

1 cm3 of solution B contains 0.01 mg of selenium.

(Changed edition, Rev. No. 1).

3. ANALYSIS

3.1. A portion of the antimony brand Swoooop a mass of 1 g was placed in a beaker with a capacity of 100 cm3,

pour 10 cm3 of reverse Aqua Regia, the solution evaporated to almost dryness on a boiling water

bath and spend denitration residue of formic acid. The excess formic acid

removed by evaporation of water. Traces of formic acid do not interfere further.

NIJ. The precipitate is then dissolved in 20 cm3 of a 10% solution of hydroxylamine in 6 mol/dm3 solution

hydrochloric acid, the solution transferred into a test tube and precipitated sulfur. To do this, the test tube with solution

placed in a boiling water bath, add a pipette of 0.5 cm3 of milk and sulphur soak

the solution is evaporated on a water bath for 3 h. During this time, three times add 0.3 cm3 of sulfur milk

after 30 min, 1 HR and end of the experience. The next day the separated precipitate is sulfur-containing

selenium, filtered through a filter with a white ribbon and washed first 7 times 5%

a solution of hydroxylamine hydrochloride in 3 mol/dm3 solution of hydrochloric acid, and then 5 times

the double-distilled water. The precipitate is washed with a jet of double-distilled water in a beaker with a capacity of 50 cm3, add

1 cm3 of nitric acid, 1 cm3 of sulfuric acid (1:1) and 0.5 cm3 of bromine and leave the glass under

watch glass for 30 min. the solution was Then heated in a water bath until distillation of the excess bromine

and removed on the tile before the appearance of sulphuric acid fumes. The contents of the glass

add 5 cm3 of double-distilled water, 0,2 cm3 of solution of potassium dichromate and 0.2 cm3 of solution

sulphate of copper. The solution was adjusted with double-distilled water to a volume of 30 cm3 in a measuring cylinder with

stopper and mix.

3.2. Polarographic solution in the cell with a remote electrode compared mercuriality

tion on the stationary mercury electrode. Mercury in the bottom of the anode compartment is filled with a mixture of

sulfuric acid, phosphoric acid and double-distilled water in the ratio 1:1:2. Droplet size

corresponds to 20 divisions of the clock indicator. The accumulation time 1−3 min at a potential of

the accumulation of minus 0.6 V. At check polarogram use of cathodic voltage scan

tion. The peak potential of -0.8 V. Polarogram of each solution is removed three to four times

in the interval of potentials from minus 0.6 V to minus 1.0 V. the peak Height is measured vertically

drawn through the top of the peak to the intersection with a tangent connecting the bases of the branches

peak. Concentration of selenium in solution was determined by method of additions. With each series of samples

conduct three follow-up experience.

(Changed edition, Rev. No. 1).

4. PROCESSING OF THE RESULTS

4.1. Mass fraction of selenium (X) in percent is calculated by the formula

t \ '

t (N2 — #,) IQ"4 ,

where MX is the mass of selenium in Supplement mcg;

HX — arithmetic average peak height of the sample solution minus the average value

the peak height of control experiments, mm;

55

C. 3 367.8 1 GOST-83

H2 — the mean arithmetic height of the peak of the sample solution with the additive minus the average

the values of the peak height of control experiments, mm (difference between H2 and H1 should be

less I, and no more GIA,);

t — the weight of antimony,

4.2. The difference between the two results of parallel measurements and the difference between two analysis results

at confidence probability P = 0.95 does not exceed the allowable absolute popular

Denia convergence and reproducibility given in the table.

Absolute peppermint allowable difference, %

M associe fraction of selenium, %

the convergence of reproducibility

From 0,000020 to 0,00004 incl.

SV. 0,00004 «0,00008 «

0,000015

0,00002

0,00002

0,00003

(Changed edition, Rev. No. 1)