GOST 19863.1-91

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  ГОСТ 19863.1-91

GOST 19863.1−91 Alloy of titanium. Methods for determination of aluminium

GOST 19863.1−91

Group B59

STATE STANDARD OF THE USSR

ALLOYS OF TITANIUM

Methods for determination of aluminium

Titanium alloys.
Methods for the determination of aluminium

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; A. I. Korolev, 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 05.05.91 N 625

3. REPLACE GOST 19863.1−80

4. The frequency of inspection — 5 years

5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

This standard specifies the chelatometric (with a mass fraction of from 0.2 to 10.0%) and atomic absorption (at a mass fraction of from 0.1 to 10.0%) methods for determination of aluminium.

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. COMPLEXOMETRICALLY METHOD FOR THE DETERMINATION OF ALUMINUM AFTER SEPARATION OF THE SODIUM HYDROXIDE

2.1. The essence of the method

The method is based on dissolving the sample in sulfuric acid, the separation of aluminium from titanium, manganese and chromium with sodium hydroxide in presence of ferric chloride (III), binding of aluminium by Trilon B titration of the acetic acid and excess Trilon B with zinc eriochrome black T as indicator. The interfering influence of vanadium at a ratio of vanadium and aluminum not more than 1:1 eliminates the introduction of hydrogen peroxide.

2.2. Apparatus, reagents and solutions

Drying oven with thermostat.

a pH meter.

Thermometer liquid-in-glass or mercury up to 100 °C with interval 1 °C.

Filters obestochennye on the other 6−09−1678.

Sulfuric acid according to GOST 4204 density 1.84 g/cmand a solution of 1:2.

Nitric acid according to GOST 4461 density of 1,35−1,40 g/cm.

Hydrochloric acid according to GOST 3118 density of 1.19 g/cmand a solution of 1:1 and 1:4.

Acetic acid according to GOST 61 density of 1.05 g/cm.

Ammonia water according to GOST 3760.

Ammonium acetate according to GOST 3117, a solution of 200 g/DM.

Barium chloride according to GOST 4108, a solution of 100 g/DM.

Sodium hydroxide according to GOST 4328, a solution of 200 g/DMand 200 g of sodium hydroxide dissolved in 800 cmof water. The solution was cooled to room temperature, poured 25 cmof a solution of barium chloride, mix, after one day filtered through a cotton swab or drained by decantation in the flask with a capacity of 1 DMand close the tube with trap for carbon dioxide. The reagent is prepared and stored in a plastic container.

Iron (III) chloride 6-water according to GOST 4147 solution 100 g/l: 100 g of iron (III) chloride is dissolved in 200 cmof a hydrochloric acid solution 1:4, poured 700 cmof water and stirred.

Hydrogen peroxide according to GOST 10929.

Hydroxylamine hydrochloride according to GOST 5456, solution 100 g/DM.

The technical rectified ethyl alcohol according to GOST 18300.

Eriochrome black T, solution 5 g/DM: 0.5 g eriochrome black T was mixed with 4.5 g of hydroxylamine hydrochloride was dissolved in 100 cmof ethanol.

Methyl orange indicator: 0.1 g of the reagent was placed in a conical flask with a capacity of 100 cmand dissolved by heating in 50 cmof water. The solution was cooled to room temperature, pour the 50 cmof water and stirred.

The indicator Congo red: 0.1 g of the reagent dissolved in 100 cmof water at low heat. The solution was cooled to room temperature, pour the 50 cmof water and stirred.

Indicator paper Congo: medium-density filters («white ribbon») is impregnated with a solution of the Congo, dried in a drying Cabinet at a temperature of 100−105 °C, sliced and stored in boxe. The paper is suitable for use within one month.

Salt is the disodium Ethylenediamine — N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652, solution with molar concentration of 0.05 mol/DM: 18,61 g Trilon B dissolved in 200 cmof water, filtered through a medium density filter (white ribbon) in a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

Zinc acetate 2-water according to GOST 5823, solution with molar concentration of 0.05 mol/DM: 11 g of zinc acetate were placed in a measuring flask with volume capacity of 1000 cm, dissolved in 200 cmof water, poured 20 cmof acetic acid, made up to the mark with water and mix.

Aluminium GOST 11069* brand А999.
________________
* On the territory of the Russian Federation GOST 11069−2001. Here and hereinafter. — Note the manufacturer’s database.

A standard solution of aluminium

1 g of aluminum is placed in a conical flask with a capacity of 250 cm, 100 cm pouredhydrochloric acid solution 1:1. The beaker cover watch glass or funnel and dissolve the aluminum when heated in a constant volume of the same solution of hydrochloric acid. The solution was cooled to room temperature, poured into a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

1 cmof the solution contains 0.001 g of aluminium.

To establish the mass concentration of Trilon B in aluminium (a) three conical flasks with a capacity of 250 cmis placed 10 cmto the standard solution of aluminium, poured 20 cmTrilon B, 100 cmof water 5 cmof sodium hydroxide solution, two drops of methyl orange indicator and neutralize with hydrochloric acid 1:1 to the transition of the yellow colour of the indicator to red, then pour 5 cmof hydrochloric acid, boil for 2 min and cooled to room temperature.

The solution is neutralized with ammonia until the color of indicator from red to yellow and add 15−20 drops in excess of, setting a pH value of 9 (you may use universal indicator paper).

The solution is cooled to a temperature of 15−20 °C, pour 10 cmof a solution of acetate of ammonium, eight drops of solution of eriochrome black T and quickly titrated with a solution of acetate of zinc to the transition of the blue color of the solution in red-violet.

Mass concentration of Trilon B for the aluminium (), g/cm, is calculated by the formula

, (1)

where mass concentration of a standard solution of aluminium in g/cm;

 — the volume of a standard solution of aluminum used for the titration, cm;

 — volume of solution Trilon B, used for titration, cm;

 — the volume of solution of acetate of zinc, consumed in the titration, cm;

 — the relation between the solutions of Trilon B and zinc acetate

. (2)

Set the ratio between the solutions of Trilon B and zinc acetate in a conical flask with a capacity of 250 cmis placed 20 cmTrilon B, pour 100 cmof water, two drops of methyl orange indicator, neutralise with hydrochloric acid 1:1 until the color of indicator from yellow to red. Then pour 2 cmof hydrochloric acid, boil for 2 min and cooled to room temperature.

The solution is neutralized with ammonia until the color of indicator from red to yellow and add 15−20 drops in excess of, setting a pH value of 9 (you may use universal indicator paper).

The solution is cooled to a temperature of 15−20 °C, pour 10 cmof a solution of acetate of ammonium, eight drops of solution of eriochrome black T and quickly titrated with a solution of acetate of zinc to the transition of the blue color of the solution in red-violet.

2.3. Analysis

2.3.1. A portion of the sample weight in accordance with table.1 is placed in a conical flask with a capacity of 250 cm, 30 cm, pour thesulfuric acid solution and heated to complete dissolution.

Table 1

The solution was added dropwise nitric acid until the disappearance of violet colour, three drops in excess, is evaporated until the appearance of fumes of sulfuric acid and heating was continued for 3 min. the Solution was cooled to room temperature, pour the 50 cmof water, heated to boiling and boil to dissolve the salts. Then pour 10 cmof a solution of iron (III) chloride and under vigorous stirring the solution was transferred in portions of 10−15 cmin a volumetric flask with a capacity of 250 cm, 90 cm containshot sodium hydroxide solution. The flask is cooled in running water to room temperature, made up to the mark with water and mix.

Sediment is allowed to settle for 15−20 min, the solution was filtered through a filter medium density (white ribbon) in a conical flask with a capacity of 250 cm, discarding the first portions of the filtrate.

2.3.2. Aliquot part of the solution to 100 cmis transferred to a conical flask with a capacity of 250 cm, add two drops of methyl orange indicator and neutralize with hydrochloric acid 1:1 until the color of indicator from yellow to red. Then pour 5 cmof hydrochloric acid, boil for 2 min and cooled the flask to room temperature in running water.

If the alloy contains vanadium, the cooled solution was poured 3 cmof hydrogen peroxide and incubated for 10 min.

Then pour from burette a solution of Trilon B in accordance with table.2, stand 10 min and neutralized with ammonia until the color changes indicator methyl orange from red to yellow.

Table 2

If the alloy contains vanadium in the solution is placed paper of the Congo and carry out the neutralization with ammonia to change its color from blue to red from one drop of ammonia.

Pour 15−20 drops of ammonia in excess, setting pH 9 (you may use universal indicator paper).

The flask with the solution cooled in running water to a temperature of 15−20 °C, pour 10 cmof a solution of acetate of ammonium, eight drops of solution of eriochrome black T and quickly titrated with a solution of acetate of zinc to the transition of the blue color of the solution in red-violet.

2.3.3. Control experience account in the ratio () between the solutions of Trilon B and zinc acetate. To do this in a conical flask with a capacity of 250 cmcarry aliquot part of the solution in the reference experiment 100 cmand continue according to claim 2.3.1.

2.4. Processing of the results

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

, (3)

where  — volume of solution Trilon B, used for titration, cm;

 — the volume of solution of acetate of zinc, consumed in the titration, cm;

 — established mass concentration of the solution Trilon B in aluminium, g/cm;

 — the relation between the solutions of Trilon B and zinc acetate;

 — weight of sample in aliquote part of the solution

G.

2.4.2. Discrepancies in the results must not exceed the values given in table.3.

Table 3

3. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF ALUMINIUM

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 aluminum at a wavelength of 309,3 nm in a flame acetylene — nitrous oxide.

3.2. Apparatus, reagents and solutions

Spectrophotometer of atomic absorption with a radiation source for aluminium.

Acetylene according to GOST 5457.

Nitrous oxide medical.

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

Nitric acid according to GOST 4461 density of 1,35−1,40 g/cm.

Boric acid according to GOST 9656.

Hydrofluoric acid according to GOST 10484.

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

Potassium chloride according to GOST 4234, solution 20 g/DM.

Titanium sponge according to GOST 17746* stamps TG-100.
_______________
* 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 150 cm, 80 cm add asolution of hydrochloric acid 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.

Aluminium GOST 11069 brand А999.

Standard aluminium solution: 1 g of aluminum is placed in a beaker with a capacity of 300 cm, add 100 cmof hydrochloric acid of 1:1, cover with a watch glass and dissolve with a moderate heat, maintaining a constant volume of the same acid solution. The solution is transferred into a measuring flask with volume capacity of 1000 cm, made up to the mark with water and mix.

1 cmstandard solution contains 0.001 g of aluminium.

3.3. Analysis

3.3.1. A portion of the sample weight in accordance with table.4 placed in the glass of glassy carbon with a capacity of 100 cm, flow 20 cmof a hydrochloric acid solution of 2:1, 1 cmbridgestation acid and dissolved with moderate heating.

Table 4

After dissolving the sample, add ten 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.4, a solution of hydrochloric acid 1:1 and a solution of potassium chloride (according to table.4), made up to the mark with water and mix.

3.3.2. The solution in the reference experiment is prepared according to claim 3.3.1, using is sample the sample the sample of titanium sponge.

3.3.3. Construction of calibration curve

3.3.3.1. When the mass fraction of aluminum from 0.1 to 1.0%.

In six volumetric flasks with a capacity of 100 cmis placed 25 cmof a solution of titanium And, in five of them measure 0,5; 1,5; 2,5; 3,5; 5,0 cmstandard solution of aluminium, which corresponds to 0,0005; 0,0015; 0,0025; 0,0035; 0.005 g of aluminum.

3.3.3.2. When the mass fraction of aluminum from 1.0 to 10.0%.

In six volumetric flasks with a capacity of 100 cmplaced at 10 cmof a solution of titanium Used, five of them measure 1,0; 2,5; 5,0; 7,5; 10,0 cmstandard solution of aluminium, which corresponds to 0.001; 0,0025; 0,005; 0,0075; 0.01 g of aluminum.

3.3.3.3. The solutions in the flasks prepared according to claim.3.3.3.1, 3.3.3.2, add 2 cmof hydrochloric acid 1:1, 10 cmpotassium chloride solution, made up to the mark with water and mix.

3.3.4. The sample solution, solution control experience and solutions to build the calibration curve is sprayed into the flame of acetylene-nitrous oxide (recovery) and measure the atomic absorption of aluminum at a wavelength of 309,3 nm. According to the obtained values of atomic absorption and corresponding mass concentrations of aluminium to build a calibration curve in the coordinates «Value of atomic absorption — Mass concentration of aluminium in g/cm».

The mass concentration of aluminium 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 aluminium () in percent is calculated by the formula

, (4)

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

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

 — the volume of the sample solution, cm;

 — weight of sample, g

.

3.4.2. Discrepancies in the results must not exceed the values given in table.5.

Table 5