GOST 19863.10-91

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  ГОСТ 19863.10-91

GOST 19863.10−91 Alloy of titanium. Methods for determination of tin

GOST 19863.10−91

Group B59

STATE STANDARD OF THE USSR

ALLOYS OF TITANIUM

Methods for determination of tin

Titanium alloys.
Methods for the determination of tin

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 5.05.91 N 625

3. REPLACE GOST 19863.10−80

4. The frequency of inspection — 5 years

5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

This standard establishes titrimetric (mass fraction in from 0.5 to 6.0%) and atomic absorption (at a mass fraction of from 0.5 to 6.0%) methods for determination of tin.

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. TITRIMETRIC METHOD FOR DETERMINATION OF TIN

2.1. The essence of the method

The method is based on dissolving the samples in hydrochloric acid, the recovery of tin to the divalent phosphonoacetate sodium in the presence of a catalyst of monovalent mercury chloride and the titration of tin with a solution of iodine in presence of starch as indicator.

2.2. Apparatus, reagents and solutions

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

Sodium posterolaterally 1-water according to GOST 200, a solution of 400 g/DM.

The monovalent mercury chloride (calomel).

Potassium iodide according to GOST 4232.

Iodine GOST 4159.

The iodine solution 0,025 mol/l: 40 g of potassium iodide were placed in a glass with a capacity of 400 cm, and dissolved in 200 cmof water. Then added 6.4 g of iodine, mix thoroughly until complete dissolution, was poured into a measuring flask with a capacity of 2,000 cm, made up to the mark with water and mix.

The solution is allowed to stand for 2−3 days, after which the set mass concentration.

Titan according to GOST 17746* stamps TG-100.
_______________
* On the territory of the Russian Federation GOST 17746−96, here and hereafter. — Note the manufacturer’s database.

Tin GOST 860 stamps O1.

A standard solution of tin, 1 g of tin is placed in a conical flask with a capacity of 250 cm, flow 50 cmof hydrochloric acid, cover with a funnel or watch glass and dissolved by heating without bringing the solution to boiling.

The flask with the solution cooled in running water 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 tin.

The soluble starch according to GOST 10163, solution 2 g/DM. The solution is prepared before use.

To establish the mass concentration of iodine solution on the tin () into three conical flasks with a capacity of 500 cmis placed 0.5 g of titanium, poured on 80 cmof a solution of hydrochloric acid, cover with a funnel or watch glass and dissolved by heating, maintaining a constant volume of the same solution of hydrochloric acid. In cooled to 50−60 °C the solution is poured 10 cmof a standard solution of tin, 40 cmof a hydrochloric acid solution, 8 cmmortar phosphonoacetate sodium, add 0.02 g of calomel, made up with water to 200 cmand mixed.

The flask is stoppered with reverse air refrigerator with a length of 80 cm, and the solution slowly heated to boiling and boiled for 15 min.

The flask with the solution cooled in running water to room temperature, poured 100 cmof water 5 cm ofstarch solution and titrated solution of iodine to a sharp change purple color of the solution in dark blue.

The mass concentration of iodine solution on the tin () in g/cmis calculated by the formula

, (1)

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

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

 — the volume of iodine solution consumed for titration, sm.

2.3. Analysis

A sample of alloy weighing 0.5 g is placed in a conical flask with a capacity of 500 cm, 80 cm pour thehydrochloric acid solution, cover with a funnel or watch glass and dissolved by heating, maintaining a constant volume of the same solution of hydrochloric acid.

In cooled to 50−60 °C the solution was poured 40 cmof a hydrochloric acid solution, 8 cmmortar phosphonoacetate sodium, add 0.02 g of calomel, made up with water to 200 cmand mixed.

The flask is stoppered with reverse air refrigerator with a length of 80 cm, and the solution slowly heated to boiling and boiled for 15 min.

The flask with the solution cooled in running water to room temperature, poured 100 cmof water 5 cm ofstarch solution and titrated solution of iodine to a sharp change purple color of the solution in dark blue

.

2.4. Processing of the results

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

, (2)

where is the volume of iodine solution consumed for titration, cm;

 — established mass concentration of iodine solution on the tin, g/cm;

 — weight of sample in aliquote part of the solution,

2.4.2. Discrepancies in the results must not exceed the values given in table.1.

Table 1

3. ATOMIC ABSORPTION METHOD FOR DETERMINATION OF TIN

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 tin at a wavelength of 286,3 nm in a flame acetylene-nitrous oxide.

3.2. Apparatus, reagents and solutions

Spectrophotometer of atomic absorption with a radiation source for tin.

Acetylene according to GOST 5457.

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

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.

Titanium sponge according to GOST 17746 grade TG-100.

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.

Tin GOST 860 stamps O1.

A standard solution of tin — according to claim 2.2.

1 cmof the solution contains 0,001

g tin.

3.3. Analysis

3.3.1. A portion of the sample weight in accordance with table.2 is placed in a conical flask 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 2

After dissolution of the sample add 3−5 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, add 2 cmof hydrochloric acid of 1:1, 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.

3.3.3. Construction of calibration curve

3.3.3.1. When the mass fraction of tin from 0.5 to 2.0%

Five volumetric flasks with a capacity of 100 cmpoured in 25 cmof a solution of titanium And four of them measure 2,5; 5,0; 7,5; 10,0 cmstandard solution of tin, which corresponds to RUB 0.0025; to 0.005; 0,0075; 0.01 g of tin.

3.3.3.2. When the mass fraction of tin of more than 2.0 to 6.0%

In six volumetric flasks with a capacity of 100 cmpoured in 25 cmof a solution of titanium Used, five of them measure 5,0; 7,5; 10,0; 12,5; 15,0 cmstandard solution of tin, which corresponds to 0,005; 0,0075; 0,01; of 0.0125; 0.015 g of tin.

3.3.4. The solutions in the flasks prepared according to claim.3.3.3.1, 3.3.3.2, 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 into the flame of acetylene — nitrous oxide (recovery) and measure the atomic absorption of tin at a wavelength of 286,3 nm.

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

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

, (3)

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

 — mass concentration of tin 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.3.

Table 3