GOST 19863.14-91

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  ГОСТ 19863.14-91

GOST 19863.14−91 Alloy of titanium. Methods for determination of copper

GOST 19863.14−91

Group B59

STATE STANDARD OF THE USSR

ALLOYS OF TITANIUM

Methods for determination of copper

Titanium alloys.
Methods for the determination of copper

AXTU 1709

Date of introduction 1992−07−01

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of aviation industry of the USSR

DEVELOPERS

V. G. Davydov, doctor of engineering. Sciences; V. A. Moshkin, PhD. tech. Sciences; G. I. Friedman, PhD. tech. Sciences; L. A. Tenyakova; M. N. Gorlova, PhD. chem. Sciences; L. V. Antonenko, O. L. Sikorska, PhD. chem. Sciences

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 5.05.91 N 626

3. INTRODUCED FOR THE FIRST TIME

4. The frequency of inspection — 5 years

5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

This standard specifies the photometric (with a mass fraction of from 0.01 to 0.4%) and atomic absorption (at a mass fraction of from 0.01 to 5.0%) methods for determination of copper.

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 25086 with the Supplement.

1.1.1. For the results analysis be the arithmetic mean of results of two parallel measurements.

2. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF COPPER

2.1. The essence of the method

The method is based on dissolving the sample in a mixture of hydrochloric and bridgestation acid formation at pH 9 blue complex compound of copper with cuprizone and measuring the optical density of the solution at a wavelength of 595 nm.

2.2. Apparatus, reagents and solutions

Spectrophotometer or photoelectrocolorimeter.

Hydrochloric acid according to GOST 3118 density of 1.19 g/cmand a solution of 2:1.

Nitric acid according to GOST 4461 density of 1,35−1,40 g/cmand a solution of 1:1.

Hydrofluoric acid according to GOST 10484.

Boric acid according to GOST 9656.

Acid bridgestation: 280 cmhydrofluoric acid at a temperature of (10±2) °C add portions 130 g of boric acid and stirred. The solution is prepared and stored in a plastic container.

Sodium hydroxide according to GOST 4328, solutions of 100 g/land 0.5 mol/DM.

Ammonium citrate on the other 6−09−01−768, a solution of 200 g/DM.

The indicator neutral red, a solution of 0.5 g/DM.

Buffer solution of sodium borate, pH 9; 13,45 g of boric acid were placed in a glass with a capacity of 500 cm, 350 cm pouredwater and dissolved by heating. The solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 500 cm, flow 65 cmof sodium hydroxide solution 0.5 mol/DM, made up to the mark with water and mix.

Rectified ethyl alcohol according to GOST 18300, solution 1:1.

Bis-(cyclohexanone)-oxalidaceae (cuprizone) TU 6−09−14−1380, a solution of 5 g/DM*: 0.25 g cuprizone placed in a volumetric flask with a capacity of 50 cm, is dissolved in 40 cmof ethyl alcohol, pour the alcohol solution up to the mark and mix.
_______________
* Consistent with the original. — Note the manufacturer’s database.

Copper according to GOST 859* brand M00.
________________
* On the territory of the Russian Federation GOST 859−2001. Here and hereinafter. — Note the manufacturer’s database.

Standard solutions of copper

Solution a: 0.5 g of copper was placed in a beaker with a capacity of 100 cm, 25 cm pour thenitric acid, first dissolved at room temperature, then heated to dissolve the sample and boil for 2−3 min. the Solution was cooled to room temperature, transferred into a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

1 cmof the solution contains 0.0005 g of copper.

Solution B: 10 cmsolution And transferred with a pipette into a measuring flask with a capacity of 500 cm, made up to the mark with water and mix. The solution is prepared before use.

1 cmof solution B has the 0.00001 g of copper

.

2.3. Analysis

2.3.1. A portion of the sample according to table.1 is placed in a conical flask with a capacity of 100 cm, 30 cm, pour thehydrochloric acid solution, 1.5 cmbridgestation acid and dissolved with moderate heating.

Table 1

The solution was added dropwise nitric acid until the disappearance of the purple color, then in excess of 2−3 drops, boil for 2−3 min, cooled to room temperature, transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix.

2.3.2. Aliquot part of the solution is 5 cm,transferred to a volumetric flask with a capacity of 50 cm, 8 cm pour thesolution of citrate of ammonium, add one drop of neutral red solution from the burette slowly, while stirring, pour the sodium hydroxide solution 100 g/DMuntil the color of indicator from red to pale yellow and 1 cmof sodium hydroxide solution in excess. Pour 5 cmof buffer solution with pH 9, 1 cmof solution cuprizone, made up to the mark with water and mix

.

2.3.3. Optical density of the solution measured after 5 min at a wavelength of 595 nm in a cuvette with a layer thickness fotometricheskogo 50 mm. Solution of comparison is water.

From the optical density of the sample solution and subtract the optical density of the solution in the reference experiment, which is prepared according to claim.2.3.1 and 2.3.2 with all the reagents used in the analysis.

Mass fraction of copper calculated according to the calibration schedule.

2.3.4. Construction of calibration curve

In seven of the eight volumetric flasks with a capacity of 50 cmmeasure 0,2; 0,5; 1,0; 1,5; 2,0; 2,5; 3,0 cmstandard solution B, which corresponds to 0,000002; 0,000005; 0,00001; 0,000015; 0,00002; 0,000025; 0,00003 g of copper, poured at 8−10 cmof water and continue on PP.2.3.2 and 2.3.3. Solution comparison is the solution, in which copper has not been introduced.

According to the obtained values of optical density of the solutions and their corresponding masses of copper to build the calibration graph.

2.4. Processing of the results

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

, (1)

where is the mass of copper in the sample solution found by the calibration schedule g;

 — weight of sample in aliquote part of the solution,

2.4.2. Discrepancies in the results must not exceed the values given in table.2.

Table 2

3. ATOMIC ABSORPTION METHOD FOR DETERMINATION OF COPPER

3.1. The essence of the method

The method is based on dissolving the sample in hydrochloric and bridgestation acids and measurement of atomic absorption of copper at a wavelength of 324,8 nm in the flame acetylene-air.

3.2. Apparatus, reagents and solutions

Spectrophotometer of atomic absorption with a radiation source of copper.

Acetylene according to GOST 5457.

Hydrochloric acid according to GOST 3118 density of 1.19 g/cm, mortar is 2:1 and 1:1.

Nitric acid according to GOST 4461 density of 1,35−1,40 g/cmand a solution of 1:1.

Hydrofluoric acid according to GOST 10484.

Boric acid according to GOST 9656.

Acid bridgestation: 280 cmhydrofluoric acid at a temperature of (10±2) °C add portions 130 g of boric acid and stirred. The solution is prepared and stored in a plastic container.

Titanium sponge according to GOST 17746* stamps TG-100.
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* On the territory of the Russian Federation GOST 17746−96. — Note the manufacturer’s database.

Solutions titanium

Solution A, 20 g/DM: 4 g of titanium was placed in a conical flask with a capacity of 250 cm, 160 cm add asolution of hydrochloric acid 2:1, 8 cmbridgestation acid and dissolved with moderate heating. After dissolution of the sample add 2 cmof nitric acid and boil the solution for 1 min. the Solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 200 cm, made up to the mark with water and mix.

Solution B, 10 g/l, 1 g of titanium was placed in a conical flask with a capacity of 250 cm, add 80 cmof a hydrochloric acid solution of 2:1, 4 cmbridgestation acid and dissolved with moderate heating. After dissolution, the sample is added twenty drops of nitric acid and boil the solution for 1 min. the Solution was cooled to room temperature, transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

Copper according to GOST 859 marks M0.

Standard solutions of copper

Solution a: 1 g of copper is dissolved in 20 cmof a solution of nitric acid at a moderate heat. The solution was cooled to room temperature, transferred to a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

1 cmof the solution contains 0.001 g of copper.

Solution B: 10 cmsolution And transferred to a volumetric flask with a capacity of 100 cm, made up to the mark with water and mix.

1 cmof solution B contains

0.0001 g of copper.

3.3. Analysis

3.3.1. A portion of the sample mass according to table.3 is placed in a conical flask with a capacity of 100 cm, add 20 cmof a hydrochloric acid solution of 2:1, 1 cmbridgestation acid and dissolved with moderate heating. After dissolution of the sample add 5−10 drops of nitric acid and boil the solution for 1 min. the Solution was cooled to room temperature, transferred to a volumetric flask with a capacity according to table.3, a solution of hydrochloric acid 1:1 according to table.3, made up to the mark with water and mix.

Table 3

3.3.2. When the mass fraction of copper in excess of 1.0 to 5.0% aliquot part of the solution is equal to 20 cm, taken in a volumetric flask with a capacity of 100 cm, add 2 cmof hydrochloric acid of 1:1, made up to the mark with water and mix.

3.3.3. The solution in the reference experiment is prepared according to claim.3.3.1, 3.3.2.

3.3.4. Construction of calibration curve

3.3.4.1. When the mass fraction of copper from 0.01 to 0.1%

In six volumetric flasks with a capacity of 100 cmpoured in 25 cmof a solution of titanium And, in five of them measure 0,5; 1,5; 3,0; 4,5; 6,0 cmstandard solution B, which corresponds to 0,00005; 0,00015; 0,0003; is 0 00 045; 0.0006 g of copper.

3.3.4.2. When the mass fraction of copper in excess of 0.1 to 1.0%

In six volumetric flasks with a capacity of 100 cmpour 10 cmof a solution of titanium Used, five of them measure 1,0; 2,5; 5,0; 7,5; 10,0 cmstandard solution B, which corresponds to 0,0001; 0,00025; 0,0005; 0,00075; 0.001 g of copper.

3.3.4.3. When the mass fraction of copper in excess of 1.0 to 5.0%

In six volumetric flasks with a capacity of 100 cmpour 2 cmof a solution of titanium Used, five of them measure 2,0; 4,0; 6,0; 8,0; 10,0 cmstandard solution B, which corresponds to 0,0002; 0,0004; about 0.0006; 0.0008 inch; 0.001 g of copper.

3.3.4.4. The solutions in the flasks prepared according to claim.3.3.4.1, 3.3.4.2, 3.3.4.3, add 2 cmof hydrochloric acid 1:1, made up to the mark with water and mix.

3.3.5. The sample solution, solution control experience and solutions to build the calibration curve is sprayed in the flame acetylene-air (oxidative) and measure the atomic absorption of copper at a wavelength of 324,8 nm.

According to the obtained values of atomic absorption and corresponding mass concentrations of copper to build a calibration curve in the coordinates «Value of atomic absorption — Mass concentration of copper, g/cm».

Mass concentration of copper in sample solution and in the solution of control and experience determined by the calibration schedule.

3.4. Processing of the results

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

, (2)

where is the mass concentration of copper in the sample solution found by the calibration schedule, g/cm;

mass concentration of copper in solution in the reference experiment, was found in the calibration schedule, g/cm;

 — the volume of the sample solution, cm;

 — the weight of the portion in the sample solution or in a suitable aliquote part of the sample solution, g

.

3.4.2. Discrepancies in the results must not exceed the values given in table.4.

Table 4