GOST 1367.10-83

• gost-136710-83.pdf (106.00 KiB)
  ГОСТ 1367.10-83

Group B59

INTERSTATE STANDARD

ANTIMONY

GOST

1367.10−83

Method for the determination of sodium

Antimony. Method for the determination of sodium AXTU 1709

1 the Establishment of the USSR State Committee on standards or on 16 December 1983 No. 6013 date of introduction is established 01.01.8 S

(Ogranichenie validity based on a Protocol Nb 4−93 Mipgaitteesar Council, standarten. Metrology and certification (NUS 4−94)

This standard sets flame photometric method for the determination of sodium 5 10^-3 to 2) ⁴ % antimony brand Swoooop.

(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. FLAME PHOTOMETRIC METHOD

The method is based on measuring the intensity of radiation of the resonance lines of sodium in a flame air-propane-butane. Antimony, deformity, distilled in the form of bromides.

2.1. A p p a RA t u RA reagents and solutions

Photometer flame type ФГ1Л-1 or other photometer or spectrophotometer for flame sensitivity to sodium not lower than 0.01 mg/DM³.

Gas propane-butane according to GOST 20448−90.

Kaaba measuring according to GOST 1770−74 capacity of 500 cm³ 1 DM³.

Pipette with divisions for NTD with a capacity of 5 cm³.

Quartz glasses according to GOST 19908 — -90 with a capacity of 50 and 250 cm³.

Quartz tubes according to GOST 19908−90 with a capacity of 10 cm³ calibrated.

Hydrochloric acid of high purity according to GOST 14261−77, diluted 1:1 with bidistillate.

Bromine in GOST 4109−79, double-distilled in quartz apparatus.

Sodium chloride according to GOST 4233−77.

Water pedestrianonly. prepared by the distillation of distilled water in a quartz distillation apparatus.

Standard solutions of sodium.

Solution A; 2.5419 g of sodium chloride was placed in a volumetric flask with a capacity of 1 DM³, pour the water, dissolve and bring to the mark with water and mix.

1 cm³ of the solution contains I mg of sodium.

Solution B: 1 cm³ solution, And transferred to a volumetric flask with a capacity of DM I³, add distilled water to the mark and mix.

1 cm³ of solution contains 1 mg of sodium.

The standard solutions stored in tightly closed glass container.

Solution comparison: graded quartz vials with a capacity of 10 cm' poured consistently 0: 0.4; 0,6; 0.8; 1,0; 1,2 cm³ of a standard solution B, which corresponds to 0; 0,4; 0.6; 0,8; 1.0; 1,2 mcg sodium, made up to the mark with double-distilled water and stirred. Solutions comparison

Official edition Reprinting is prohibited

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

60

GOST 1367.10−83 C. 2

is sprayed into the flame in order of increasing content of sodium. The sodium concentration in the solutions, respectively equal 0; 0.04: 0.06; 0.08; 0,10: 0,12 mcg/cm³.

(Changed edition, Rev. No. 1).

2.2. Analysis

2.2.1. Preparation of samples for analysis

1 g of antimony brand Swoooop placed in a quartz glass with a capacity of 50 cm\ poured 5 cm³ of hydrochloric acid (1:1) and then carefully dropwise (with continuous stirring and cooling) 2 cm' of bromine (reaction goes rapidly). The resulting solution was evaporated with moderate heat to dryness. The dry residue moistened with 2 cm⁵ hydrochloric acid (1:1), washing away its walls of glass, poured 0.5 cm³ of bromine, and the solution again evaporated to dryness. For the complete removal of antimony processing residue with hydrochloric acid and bromine is repeated twice. The residue is moistened with 10−15 drops of hydrochloric acid (1:1), again evaporated to dryness. The dry residue was dissolved with heating in 2 cm³ of hydrochloric acid (1:1). The solution was transferred to quartz graduated test tube with a capacity of 10 cm³, is adjusted bitstream to the mark and mix.

At the same time spend three control experience.

2.2.2. Fotometricheskie

In order to avoid distortion of the results of the analysis it is necessary to exclude contact of all fotomat-reremix solutions with glass and with other sources of sodium ions. This goal should replace the glass parts of the photometer in the path of flow of fluids and aerosol in the flame, quartz or plastic, i.e. of material which can not be a source of sodium ions.

To prepare photometer for determination of sodium according to the instructions supplied with the device.

When operating the photometer and the flicker of the flames thoroughly flush the system device, spraying first with distilled water and then in double-distilled water for several minutes until the photometer reach the minimum (zero) value.

Photometered by the method of limiting solutions.

3. PROCESSING OF THE RESULTS

3.1. The concentration of sodium in the sample solution (_x) is calculated according to the formula

(C,-C,) (O,-O,-O.)

With,+

0,-0,

where C, is the concentration of sodium in the first solution comparisons, µg/cm³;

With₂ — the sodium concentration in the second solution comparison, µg/cm³;

Oh — emission intensity of sodium in the first solution comparison;

0₂ — emission intensity of sodium in the second solution comparison;

About_x — emission intensity of sodium in the sample solution:

About_K — arithmetic average emission intensity in solutions kontrolnyh experiments.

3.2. Mass fraction of sodium (L) in percent is calculated by the formula

S. • V ■ 100

t 1000 — 1000 '

where_x is the concentration of sodium in sample solution, µg/cm³;

To -the volume of the solution of the sample, cm³, t is the weight of antimony,

3.3. The difference between the two results of parallel measurements and the difference of two analysis results with a confidence probability P = 0.95 does not exceed the allowable absolute differences of precision and reproducibility, are given in the table.

Mass fraction of sodium. % Absolute ihoc permitted discrepancy. % СКОДИМОС1И ■SpotAuditor From 0.00005 to 0,00010 ncloc. SV. 0,00010 * 0.00020 * 0,00004 0.00005 0,00005 0,00006

61