GOST 19863.15-91
GOST 19863.15−91 Alloy titanium-Nickel. Method of determining titanium
GOST 19863.15−91
Group B59
STATE STANDARD СОЮ3А SSR
ALLOY TITANIUM-NICKEL
Method of determining titanium
Titanium-nickel alloy.
Method for the determination of titanium
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, L. V. Antonenko, A. I. Queen
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
| The designation of the reference document referenced |
Item number |
| GOST 3118−77 |
3 |
| GOST 4165−78 |
3 |
| GOST 4204−77 |
3 |
| GOST 4461−77 |
3 |
| GOST 5456−79 |
3 |
| GOST 6344−73 |
3 |
| GOST 17746−79 |
3 |
| GOST 25086−87 |
1.1 |
| THAT 6−09−3935−74 |
3 |
| THAT 6−09−1678−86 |
3 |
This standard establishes a differential photometric method for the determination of titanium at a mass fraction of from 40.0 to 50.0%.
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 ESSENCE OF THE METHOD
The method is based on dissolving the sample in sulfuric acid, the formation of the orange yellow complex with titanium diantipyrylmethane and measuring the optical density of the solution at a wavelength of 480 nm.
Alikvotnih from different parts of the sample solution determine the content of titanium, Nickel, and iron and copper (atomic absorption method, respectively according to GOST 19863.5−91 and GOST 19863.14−91).
3. APPARATUS, REAGENTS AND SOLUTIONS
Spectrophotometer.
Ashless filters 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/cm, a solution of 1:1.
Hydroxylamine hydrochloride according to GOST 5456, solution 100 g/DM.
Copper (II) sulfate 5-water according to GOST 4165.
Thiourea according to GOST 6344, solution 100 g/DM.
Diantipyrylmethane on the other 6−09−3835.
The mixture of reagents: 40 g diantipyrylmethane, 16 g of thiourea was placed in a conical flask with a capacity of 2000 cm, pour 700−800 cm
of a hydrochloric acid solution and mix by rotating flask until complete dissolution of the reagents, add 6 cm
of solution of copper sulphate, made up to 1000 cm
with hydrochloric acid and stirred.
If necessary, the solution is filtered through a folded filter from filter paper in a dry or slightly warmed flask to avoid crystallization.
The solution is prepared immediately before use.
Titanium sponge according to GOST 17746* stamps TG-100 or titanium ideny.
_______________
* On the territory of the Russian Federation GOST 17746−96. — Note the manufacturer’s database.
Standard solutions of titanium
Solution a: 0.4 g of titanium was placed in a conical flask with a capacity of 250 cmand dissolved by heating in 160 cm
of sulfuric acid solution, maintaining the initial volume with water. After dissolution, add dropwise a solution of hydroxylamine hydrochloride to the disappearance of a purple color and 3−4 drops in excess. The walls of the flask is washed with 50−70 cm
of water, mix the solution and boil for 1−2 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 solution A contains 0.0004 g of titanium.
Solution B: 0.1 g of titanium was placed in a conical flask with a capacity of 250 cm, 160 cm pour the
sulfuric acid solution and the dissolution is carried out as described for solution A.
1 cmof a solution contains 0.0001 g of titanium.
4. ANALYSIS
4.1. A portion of sample weighing 0.25 g was placed in a conical flask with a capacity of 250 cm, flow 40 cm
of sulfuric acid solution and dissolved by heating.
4.1.1. The solution was added dropwise a solution of hydroxylamine hydrochloride to the disappearance of a purple color, 3−4 drops in excess, pour 50 cmof water, mix and boil for 1−2 min.
4.1.2. In the presence of the copper alloy in the solution instead of hydroxylamine hydrochloride is added dropwise nitric acid until the disappearance of the purple color and complete dissolution of copper particles, is then heated to release the white fumes of sulfuric acid, cooled to room temperature, pour the 50 cmof water, mix and boil for 1−2 min.
4.2. The solution obtained according to claim 4.1.1 or claim 4.1.2, transferred to a volumetric flask with a capacity of 250 cm, made up to the mark with water and mix.
Aliquot part of the solution is 4.0 cm, containing 1.6 to 2.0 mg of titanium, is transferred into a volumetric flask with a capacity of 50 cm
.
4.3. To aliquote part of the solution poured 25 cmof a mixture of reagents, made up to the mark with water and mix.
4.4. Optical density of the solution measured after 5 min at a wavelength of 480 nm in cuvettes with a thickness of fotometricheskogo layer of 10 mm, with strictly the same working length.
The comparison solution is a solution containing 1.6 mg titanium in the amount of 50 cm.
Mass fraction of titanium is determined according to the calibration schedule.
4.5. Construction of calibration curve
Five volumetric flasks with a capacity of 50 cm,measure at 4 cm
standard solution And then four of them measure 1,0; 2,0; 3,0; 4,0 cm
standard solution B, which corresponds to 1,6; 1,7; 1,8; 1,9; 2,0 mg of titanium, and then continue on PP.4.3, 4.4.
According to the obtained values of optical density of the solutions and their corresponding masses of the titanium to build the calibration graph.
5. PROCESSING OF THE RESULTS
5.1. Mass fraction of titanium () in percent is calculated by the formula
where is the mass of titanium in the sample solution found by the calibration schedule g;
— weight of sample in aliquote part of the solution,
5.2. The absolute maximum discrepancy should not exceed: results of parallel measurements is 0.3%; the results of the analysis of 0.4%.
