GOST 6689.22-92

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  ГОСТ 6689.22-92

GOST 6689.22−92 Nickel, alloys Nickel and copper-Nickel. Methods for determination of tin

GOST 6689.22−92

Group B59

STATE STANDARD OF THE USSR

NICKEL, ALLOYS NICKEL AND COPPER-NICKEL

Methods for determination of tin

Nickel, nickel and copper-nickel alloys. Methods for the determination of tin

AXTU 1709

Date of introduction 1993−01−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR

DEVELOPERS

V. N. Fedorov, Y. M. Leybov, Boris Krasnov, A. N. Bulanova, L. V. Morea, A. I. Vorobyov

2. APPROVED AND promulgated by the Decree of Committee of standardization and Metrology of the USSR from 18.02.92 N 167

3. REPLACE GOST 6689.22−80

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS:

This standard specifies the extraction-photometric (with mass fraction of tin from 0.0005 to 0.15%), photometric (with mass fraction of tin from 0.01 to 0.25%) and atomic absorption (at a mass fraction of tin from 0.01 to 0.25%) methods for determination of tin in Nickel, Nickel and copper-Nickel alloys according to GOST 492* and GOST 19241.
______________
* On the territory of the Russian Federation GOST 492−2006. — Note the manufacturer’s database.

1. GENERAL REQUIREMENTS

General requirements for methods of analysis GOST 25086 with the addition of a GOST 6689.1 in sect.1.

2. EXTRACTION-PHOTOMETRIC METHOD FOR THE DETERMINATION OF TIN

2.1. The essence of the method

The method is based on measuring the optical density of the solution complex compounds of tin with quercetin extracted -butyl alcohol from hydrochloric acid solution containing thiourea to eliminate the influence of copper and iron.

2.2. Apparatus, reagents and solutions

Photoelectrocolorimeter or spectrophotometer.

Hydrochloric acid according to GOST 3118 and diluted 1:4 and 1:10.

Hydrogen peroxide according to GOST 10929, 30% solution.

Ammonia water according to GOST 3760, diluted 1:1.

Thiourea according to GOST 6344, solution 100 g/DM.

Sodium chloride according to GOST 4233.

Sodium sulfate according to GOST 4166.

-butyl alcohol according to GOST 6006.

Quercetin, a solution of 4 g/DMin -butyl alcohol.

Tin stamps O1 according to GOST 860.

Standard solutions of tin

Solution a: 0.1 g of tin are placed in a conical flask with a capacity of 100 cm, add 1 g of sodium chloride, 100 CCof concentrated hydrochloric acid, 1 cmof hydrogen peroxide and heated at 60−70 °C. By the end of the dissolution, the temperature was raised to 80 °C. the Solution was cooled, transferred into a measuring flask with volume capacity of 1000 cmand topped to the mark with hydrochloric acid (1:10).

1 cmof the solution contains 0.0001 g of tin.

Solution B: 25 cmsolution And transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with hydrochloric acid (1:10).

1 cmof solution B contains 0,00001 g tin. Solution B is prepared on the day prima

tion.

2.3. Analysis

2.3.1. A portion of the alloy (see table.1) is placed in a beaker with a capacity of 250 cm, add 5 g of sodium chloride, 20 cmof concentrated hydrochloric acid and dropwise 7−10 cmof hydrogen peroxide, cover with a watch glass, a glass or plastic plate and dissolved by heating.

Table 1

Glass or plate and the side of the Cup then rinsed with water and the solution is evaporated to a volume of 2−4 cm. The solution was cooled, transferred to a separatory funnel with a capacity of 100 cm, neutralized dropwise with ammonia until slightly alkaline medium on the paper of the Congo. Add 5 cmof hydrochloric acid (1:4), 20 cmof a solution of thiourea and dilute with water to 50 cm. Add 25 cmof a solution of quercetin -butyl alcohol and vigorously stirred 5 min. After phase separation, the lower aqueous layer discarded, and the organic layer is poured into a dry beaker with a capacity of 50 cmcontaining 0.2−0.5 g of anhydrous sodium sulfate and, after 5 min, measure the optical density of the solution in a cuvette with a thickness of the light absorbing layer 1 cm at a photoelectrocolorimeter with a blue or purple filter or on a spectrophotometer at 440 nm. Solution comparison is the solution of the quercetin -butyl Speer

those.

2.3.2. Construction of calibration curve

In a separating funnel with a capacity of 100 cmadministered 1,0; 3,0; 5,0; 7,0; 10,0; 15,0 cmstandard solution B tin. The solutions were neutralized with ammonia to slightly alkaline environment in the Congo paper, add 5 cmof hydrochloric acid (1:4) and further analysis are as indicated in claim 2.3.1.

2.4. Processing of the results

2.4.1. Mass fraction of tin () in percent is calculated by the formula

,

where  — weight of tin, was found in the calibration schedule g;

 — the weight of the portion,

2.4.2. Discrepancies in the results of three parallel measurements (rate of convergence) and the results of the two tests (index of reproducibility) shall not exceed the values allowable differences specified in table.2.

Table 2

2.4.3. Control of accuracy of analysis results is carried out according to State standard samples (GSO) or industry standard sample (CCA), or by standard samples of the enterprise (SOP) of Nickel, Nickel and copper-Nickel alloys, approved under GOST 8.315*, or by additives or by comparing the results of photometric, atomic absorption or polarographic (GOST 6689.16) methods in accordance with GOST 25086.
______________
* On the territory of the Russian Federation GOST 8.315−97, here and hereafter. — Note the manufacturer’s database.

3. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TIN

3.1. The essence of the method

The method is based on measuring the optical density of the colored complex compounds of tin with phenylfluorone in the presence of ascorbic and citric acids, masking iron and antimony, respectively, after prior separation of the tin by the coprecipitation with manganese dioxide.

3.2. Apparatus, reagents and solutions

Photoelectrocolorimeter or spectrophotometer.

Nitric acid according to GOST 4461, diluted 1:1 and solution 2 mol/DM.

Sulfuric acid according to GOST 4204, and diluted 1:1 and 1:4 solution of 2.5 mol/DM.

Hydrofluoric acid according to GOST 10484.

Ascorbic acid according to normative-technical documentation, solution 20 g/l, freshly prepared.

Citric acid according to GOST 3652, a solution of 200 g/DM, freshly prepared.

Ammonia water according to GOST 3760.

Manganese nitrate according to GOST 6203, a solution of 50 g/DM.

Potassium permanganate according to GOST 20490, a solution of 10 g/DM.

Hydrogen peroxide according to GOST 10929.

Acetone GOST 2768.

The technical rectified ethyl alcohol according to GOST 18300.

Gelatin food according to GOST 11293*, a solution of 10 g/DM, freshly prepared.
______________
* On the territory of the Russian Federation GOST 11293−89. — Note the manufacturer’s database.

Phenylfluorone, an alcoholic solution of 0.5 g/l; 0.05 g phenylfluorene dissolved by heating in 50 cmof ethyl alcohol, adding 1 cmof sulfuric acid (1:1). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with ethyl alcohol and store in a dark place.

Tin GOST 860 with a mass fraction of tin is not less than 99.9%.

Standard solutions of tin

Solution a: 0.1 g of tin are dissolved in 10 cmof concentrated sulfuric acid, the solution was cooled, transferred to a measuring flask with volume capacity of 1000 cm, made up to the mark of 2.5 mol/DMsulfuric acid solution and stirred.

1 cmof the solution contains 0.0001 g of tin.

Solution B: 25 cmsolution And placed in a volumetric flask with a capacity of 250 cm, made up to the mark of 2.5 mol/DMsulfuric acid solution and stirred.

1 cmof solution B contains 0,0

0001 g tin.

3.3. Analysis

3.3.1. For alloys with a mass fraction of silicon to 0.05%

A portion of the alloy (see table.3) is placed in a beaker with a capacity of 250 cm, and dissolved in 10 cmof nitric acid (1:1) under heating. Nitrogen oxides are removed by boiling, the solution is diluted with water to a volume of 50 cm. Add 5 cmof a solution of nitrate of manganese (at a mass proportion of manganese in the alloy, a 2% solution of nitrate of manganese to add should not), the solution is neutralized with ammonia until the appearance of the precipitate copper hydroxide, adding 24 cmof nitric acid (1:1) and water to a volume of 90 cm. The solution is heated to boiling, add 10 cmof a solution of potassium permanganate, and boil for 2 min. after 30 min the precipitate was filtered off on a tight filter and washed the beaker and the precipitate 8−10 times with hot 1 mol/DMnitric acid until the disappearance of the blue color formed of copper nitrate. The deployed filter is washed with water in a glass, which conducted the deposition. The filter is washed with 10 cmof hot sulfuric acid solution (1:4) containing few drops of hydrogen peroxide solution and then with water.

Table 3

The washed filter is discarded, the filtrate is evaporated to release white smoke of sulfuric acid. To the cooled residue is added with mass fraction of tin from 0.01% to 0.12% — 20 cm, while the mass fraction of tin in excess of 0.12% and up to 50 cmof 2.5 mol/DMsolution of sulphuric acid and the solution transferred to an appropriate volumetric flask (see table 3), made up to the mark with water and mix.

Aliquot part of the solution (see table.3) is placed in a volumetric flask with a capacity of 25 cm, add the specified volume of 2.5 mol/DMsolution of sulphuric acid (see table.3) alternately, mixing after addition of each reagent, add 2cmof a solution of ascorbic acid 5 cmof the citric acid solution, 1 cmof solution of gelatin, 3 cmof acetone, 2 cmof mortar phenylfluorone, made up to the mark with water and mix. After 30 min measure optical density of solution on a photoelectrocolorimeter with a yellow green filter or on spectrophotometer at 510 nm in a cuvette with the thickness of the light absorbing layer 1 see Solution comparison is the solution of the control op

it.

3.3.2. For alloys with a mass fraction of silicon in excess of 0.05%

A portion of the alloy (see table.3) is placed in a platinum Cup and dissolved in 10 cmof nitric acid (1:1) and 2−3 cmhydrofluoric acid when heated.

After dissolution, add 10 cmsulphuric acid (1:1) and the solution was evaporated until a white smoke of sulfuric acid. The residue is cooled, rinse the walls of the Cup with water and evaporated again until a white smoke of sulfuric acid. The residue is cooled, the walls of the Cup should be rinsed with 20 cmof water, heat the solution transferred to a beaker with a capacity of 250 cm, top up with water to a volume of 50 cm, add 5 cmof a solution of manganese nitrate and further analysis is carried out as specified in clause 3.3.1

.

3.3.1. Construction of calibration curve

In seven of eight glasses with a capacity of 50 cmplaced 1,0; 2,0; 3,0; 4,0; 5,0; 6,0 and 7.0 cmstandard solution B tin, the solutions were evaporated to dryness and cooled. All glasses add 2.5 cmto 2.5 mol/DMsolution of sulphuric acid, heat the solution, add 2 cmof ascorbic acid solution, cooled and further analysis are as indicated in claim 3.3.1.

Solution comparison is the solution not containing the tin. According to the obtained results build a calibration curve.

3.4. Processing of the results

3.4.1. Mass fraction of tin () in percent is calculated by the formula

,

where  — weight of tin, was found in the calibration schedule g;

 — the weight of the portion corresponding to aliquote part of the solution,

3.4.2. Discrepancies in the results of three parallel measurements (rate of convergence) and the results of the two tests (index of reproducibility) shall not exceed the values of permissible differences given in table.2.

3.4.3. Control of accuracy of analysis results is carried out as specified in clause 2.4.3.

4. ATOMIC ABSORPTION METHOD FOR DETERMINATION OF TIN

4.1. The essence of the method

The method is based on measuring the absorption of light by atoms of tin, formed during the introduction of the analyzed solution in the flame acetylene-air or acetylene-nitrous oxide, after a preliminary separation of the tin by the coprecipitation with manganese dioxide.

4.2. Apparatus, reagents and solutions

Atomic absorption spectrometer with a radiation source for tin.

Nitric acid according to GOST 4461, diluted 1:1 and a solution of 1.5 mol/DM.

Hydrochloric acid according to GOST 3118, solution 1 mol/DM.

Sulfuric acid according to GOST 4204, diluted 1:1, 1:4, and the solution of 2.5 mol/DM.

Hydrofluoric acid according to GOST 10484.

Ammonia water according to GOST 3760.

Manganese nitrate according to GOST 6203, a solution of 20 g/DM.

Potassium permanganate according to GOST 20490, a solution of 10 g/DM.

Hydrogen peroxide according to GOST 10929.

Tin GOST 860 with a mass fraction of tin is not less than 99.9%.

A standard solution of tin: 0.25 g of tin dissolved by heating in 20 cmof concentrated sulfuric acid, the solution was cooled, transferred to a volumetric flask with a capacity of 500 cmand topped to the mark of 2.5 mol/DMsulfuric acid solution and stirred.

1 cmof the solution contains 0.0005 g olo

VA.

4.3. Analysis

4.3.1. For alloys with a mass fraction of silicon to 0.05%

A portion of the alloy (see table.4) is placed in a beaker with a capacity of 250 cmand dissolved when heated in nitric acid (1:1), to the extent taken in accordance with the indication in table.4.

Table 4

Nitrogen oxides are removed by boiling and the solution diluted with water to a volume of 50 cm. Add 5 cmof manganese nitrate, the solution is neutralized with ammonia until the copper hydroxide, add 18 cmof nitric acid (1:1) and water to a volume of 90 cm. The solution is heated to boiling, add 10 cmof a solution of potassium permanganate, and boil for 2 min. after 30 min the precipitate was filtered off on a tight filter and washed the beaker and the precipitate 4−5 times a hot 1.5 mol/DMsolution of nitric acid. The deployed filter is washed with water in a glass, which conducted the deposition, the filter is washed with 10 cmof hot sulfuric acid solution (1:4) containing few drops of hydrogen peroxide solution and then with water. The washed filter is discarded and the solution was evaporated to wet salts. After cooling, add 8 cm1 mol/DMhydrochloric acid solution, transferred to a volumetric flask with a capacity of 100 cmand topped to the mark of 1 mol/DMhydrochloric acid solution.

Measure the atomic absorption of tin in the flame of acetylene-air or acetylene-nitrous oxide at a wavelength of 286,3 nm 224,6 or in parallel with calibration solvents

Rami.

4.3.2. For alloys with a mass fraction of silicon in excess of 0.05%

A portion of the alloy (see table.4) is placed in a platinum Cup and dissolved when heated in nitric acid (1:1), to the extent taken in accordance with the specified in table.4, and 2 cmhydrofluoric acid.

After dissolution, add 10 cmsulphuric acid (1:1) and the solution was evaporated until a white smoke of sulfuric acid. The residue is cooled, rinse the walls of the Cup with water and evaporated again until a white smoke of sulfuric acid. The residue is cooled, the walls of the Cup should be rinsed with 20 cmof water, heat the solution transferred to a beaker with a capacity of 250 cm, top up with water to a volume of 50 cm, add 5 cmof a solution of manganese nitrate and further analysis is carried out as specified in clause 4.3.1.

4.3.3. Construction of calibration curve

In seven of eight glasses with a capacity of 250 cmis placed 0,4; 1,0; 2,0; 3,0; 4,0; 5,0; 6,0 cmstandard solution of tin. In all the cups add water to a volume of 50 cm, add 5 cmof a solution of manganese nitrate and further analysis is carried out as specified in clause 4.3.1. According to the obtained results build a calibration curve.

4.4. Processing of the results

4.4.1. Mass fraction of tin () in percent is calculated by the formula

,

where is the concentration of tin was found in the calibration schedule, g/cm;

 — the volume of the final solution, cm;

 — the weight of the portion of alloy,

4.4.2. Discrepancies in the results of three parallel measurements (rate of convergence) and the results of the two tests (index of reproducibility) shall not exceed the values of permissible differences given in table.2.

4.4.3. Control of accuracy of analysis results is carried out according to State standard samples (GSO) or industry standard sample (CCA), or by standard samples of the enterprise (SOP) of Nickel, Nickel and copper-Nickel alloys, approved under GOST 8.315, or by a method of additives, or a comparison of the results obtained photometric methods in accordance with GOST 25086.