GOST 6674.3-96

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  ГОСТ 6674.3-96

GOST 6674.3−96 copper phosphorous Alloys. Method for the determination of antimony

GOST 6674.3−96

Group B59

INTERSTATE STANDARD

COPPER PHOSPHOROUS ALLOYS

Method for the determination of antimony

Copper-phosphorous alloys.
Method for determination of antimony

ISS 77.120.30
AXTU 1709

Date of introduction 2001−07−01

Preface

1 DEVELOPED by the Interstate technical Committee for standardization MTK 107, Donetsk state Institute of non-ferrous metals (Danism)

SUBMITTED to the State Committee of Ukraine for standardization, Metrology and certification

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 10 dated 3 October 1996)

The adoption voted:

3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated December 19, 2000 N 384-St inter-state standard GOST 6674.3−96 introduced directly as state standard of the Russian Federation from July 1, 2001

4 REPLACE GOST 6674.3−74

1 Scope

This standard sets the photometric method for the determination of antimony in its content is from 0.001% to 0.2% copper-phosphorous alloys.

2 Normative references

The present standard features references to the following standards:

GOST 1089−82 Antimony. Specifications

GOST 3118−77 hydrochloric Acid. Specifications

GOST 4197−74 Sodium atomistically. Specifications

GOST 4204−77 sulfuric Acid. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 5789−78 Toluene. Specifications

GOST 6674.0−96 copper phosphorous Alloys. General requirements for methods of analysis

GOST 6691−77 Urea. Specifications

3 General requirements

General requirements — according to GOST 6674.0.

4 the essence of the method

The method is based on extraction of ions of antimony (V) toluene in the form of hexachlorobuta crystal violet and measuring the optical density of the extract at a wavelength of 590 nm.

5 Apparatus, reagents and solutions

Photoelectrocolorimeter.

Nitric acid according to GOST 4461 and diluted 1:1.

Hydrochloric acid according to GOST 3118 and diluted 7:3, 1:1.

Sulfuric acid according to GOST 4204, and diluted 1:1.

Tin dichloride (tin (II) chloride) according to the current normative document, solution 100 g/lin hydrochloric acid, diluted 1:1.

Sodium atomistically (sodium nitrite) according to GOST 4197, solution 100 g/DM.

Carbamide (urea) GOST 6691, saturated solution: 100 g of urea dissolved in 100 cmof hot water.

Crystal violet according to the current normative document, a solution of 2 g/DM.

Toluene according to GOST 5789.

Antimony GOST 1089 brand Su00.

Standard solutions of antimony.

Solution a: 0.1 g of antimony is dissolved by heating in 50 cmof sulfuric acid. The solution was transferred to a volumetric flask with a capacity of 1 DM, made up of 175 cmof sulphuric acid (1:1), cooled, made up to the mark with water and mix.

1 cmof the solution contains 0.0001 g of antimony.

Solution B: 5 cmsolution And placed in a volumetric flask with a capacity of 100 cm, 70 cm pour thehydrochloric acid, dilute to the mark with water and mix.

1 cmof solution B contains 0,000005 g of antimony.

6 analysis

6.1 a sample of alloy weighing 0.5 g were placed in a glass with a capacity of 100 cm, add 10 cmof nitric acid solution and dissolved by heating, covered with a glass watch glass.

The walls of the beaker and the watch glass rinsed with a little water, add 6 cmof sulphuric acid and is evaporated to release the thick white fumes of sulfuric acid. After cooling, the side of the Cup then rinsed with water and the solution is evaporated to dryness. After cooling, add 7 cmof a hydrochloric acid solution (7:3) and gently heated to dissolve the salts.

6.2 When the mass fraction of antimony to 0.005% solution transferred to a separatory funnel with a capacity of 150 cm, the glass is washed with 3 cmof a hydrochloric acid solution (7:3) and bring them the solution volume up to 10 cm.

6.3 If the mass fraction of antimony in excess of 0.005% solution transferred to a volumetric flask with a capacity of 50 cm, washed the walls of the beaker with hydrochloric acid (7:3) and bring to mark with the same acid solution. Aliquot part of the solution, according to table 1 is transferred to a separatory funnel with a capacity of 150 cm, a solution of hydrochloric acid (7:3) in accordance with table 1.


Table 1

6.4 separating funnel Add in 1−2 drops of solution of tin chloride (II), mix and leave for 1 min Then add 1 cmof a solution of sodium nitrite, a funnel closed with a stopper and shake for 2 min. then the tube of the funnel open. After 2 min add 1 cmof a solution of urea and stirred for 30 s. Then add the 68 cmof water, 10 drops of crystal violet solution, mix, add 25 cmof toluene and extracted for 1 min. After phase separation, the lower layer is discarded and the organic layer was filtered through a filter into a cuvette.

6.5 To construct the calibration curve five separatory funnels with a capacity of 150 cm,introduce respectively 1,0; 2,0; 3,0; 4,0 and 5,0 cmstandard solution B and add solution of hydrochloric acid (7:3) to volume of 10 cm. Add 1−2 drops of solution of tin chloride (II), mix and leave for 1 min Then do as described in 6.4.

6.6 Measured optical density of the extracts of solutions of the samples and solutions for constructing the calibration curve on photoelectrocolorimeter at a wavelength of 590 nm.

Solution comparison is water.

7 Processing of results

7.1 Mass percent of antimony , %, is calculated by the formula

, (1)

where is the mass of antimony, was found in the calibration schedule g;

 — the weight of the portion of alloy,

7.2 discrepancies in the results of parallel measurements and the results of the analysis shall not exceed allowable (at confidence probability of 0.95) of the values given in table 2.


Table 2

Percentage