GOST 26473.8-85
GOST 26473.8−85 Alloys and alloys based on vanadium. Method of determining titanium (with Change No. 1)
GOST 26473.8−85
Group B59
STATE STANDARD OF THE USSR
ALLOYS AND MASTER ALLOYS BASED ON VANADIUM
Method of determining titanium
Vanadium base alloys and alloying elements. Method for determination of titanium
AXTU 1709
Valid from 01.07.86
to 01.07.91*
_______________________________
* Expiration removed
by the decree of Gosstandart of the USSR from
(IUS N 8, 1991). — Note the manufacturer’s database.
DEVELOPED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
Yu. A. Karpov, E. G. Nembrini, V. G., Miscreants, V. V. Nedler, V. M. Mikhailov, L. G. Agapova, G. N. Andrianov, A. V. Antonov, V. D. Dozen, M. A. Desyatkova, T. I. Kirillova, L. I. Kirsanov, I. E. Korepin, V. A. Orlova, N. Rasnitsyn, N. Suvorova, N. L. Tomasev, M. W. Schmidt, L. N. Filimonov
INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
Member Of The Board Of A. P. Snurnikov
APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards of 25 March 1985 N 752
The Change N 1, approved and put into effect by the Decree of the USSR State Committee on management of quality and standards from
Change No. 1 made by the manufacturer of the database in the text IUS N 2, 1990
This standard sets the photometric method for the determination of titanium (1 to 25%) in alloys and master alloys based on vanadium, the contents of related components which are shown in table.1.
Table 1
The accompanying component |
Mass fraction, %, not more |
Aluminium |
50 |
Iron |
3 |
Silicon |
1 |
Manganese |
2,5 |
Molybdenum |
20 |
The method is based on formation of yellow complex compound of titanium with diantipyrylmethane in hydrochloric acid solution and fotomaterialy the color of the solution.
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 26473.0−85.
2. APPARATUS, REAGENTS AND SOLUTIONS
Type photoelectrocolorimeter FEK-56.
Analytical scale.
Libra technical.
Muffle furnace with thermostat providing temperatures up to 1000 °C.
Tile electric.
Bath water.
Glasses chemical glass with a capacity of 100, 200 cm.
The quartz Cup with a capacity of 50 cm.
Volumetric flasks with a capacity of 50 and 100 cm.
Measuring beakers with a capacity of 25 and 50 cm.
Pipettes with a capacity of 2 and 5 cmwith divisions.
Microburette with a capacity of 10 cmwith a scale division of 0.02 cm.
Sulfuric acid GOST 4204−77, diluted 1:1.
Nitric acid GOST 4461−77 diluted 1:1.
Hydrochloric acid by the GOST 3118−77, diluted 1:1, 1:9, 1:10.
Ascorbic acid food.
Diantipyrylmethane, solution concentration 20 g/lin hydrochloric acid: 2 g diantipyrylmethane placed in a beaker with a capacity of 200 cm, 30 cm, pour thehydrochloric acid, diluted 1:9, mix, dilute with water to volume of 100 cm, if the solution is colored yellow, add a pinch of spatula of ~0.1 g of ascorbic acid. The solution is prepared the day of use.
Titanium metal according to GOST 19807−74* brand VT1−00.
______________
* On the territory of the Russian Federation GOST 19807−91. — Note the manufacturer’s database.
Potassium preservatory according to GOST 7172−76.
A standard solution of titanium (spare) containing 1 mg/cmtitanium: 0.1 g of titanium metal in the form of a small chip placed in a quartz Cup, add 3 g of potassium peacemaking, 3−4 drops of concentrated sulfuric acid, fused in a muffle furnace at 850−900 °C until a clear melt. The smelt is dissolved by heating in 50 cmof hydrochloric acid diluted 1:1. The solution was transferred to volumetric flask with a capacity of 100 cm, cooled and adjusted to the mark with water.
A solution of titanium (working) containing 0.1 mg/cm(100 g/cm), prepared by dilution of the standard backup solution 10 times with hydrochloric acid diluted 1:10.
3. ANALYSIS
3.1. Sample preparation
A portion of the sample weighing 0.1 g was placed in a beaker with a capacity of 100 cm, flow 10 cmof sulphuric acid diluted 1:1, and 5 cmof nitric acid. Was heated until complete dissolution of the sample, continuing the heating until the appearance of sulphuric acid fumes.
The solution was cooled, gently on the walls of the flask poured 50 cmof water, transfer the solution into a measuring flask with a capacity of 100 cm, cooled and adjusted to the mark with water.
3.2. To perform the assay
For the determination of titanium in a volumetric flask with a capacity of 50 cmpipetted 1−10 cmof sample solution containing 100−600 µg of titanium, poured 10 cmof hydrochloric acid diluted 1:1, 10 cmof water, place the flask in a boiling water bath, heated for 5 min and, without cooling, poured 15 cmsolution diantipyrylmethane. After this solution was cooled to room temperature (avoiding sudden cooling) and adjusted to the mark with water. Measure the optical density of the solution on the photoelectrocolorimeter using a filter with maximum transmittance at a wavelength of ~490 nm and cuvette thickness of the light absorbing layer of 20 mm in relation to the simultaneously cooked «zero» solution containing all reagents except the standard solution of titanium.
Weight titanium find for the calibration schedule.
(Changed edition, Rev. N 1).
3.3. Construction of calibration curve
In a volumetric flask with a capacity of 50 cmis injected from microburette 1,0; 2,0; 3,0; 4,0; 5,0 and 6,0 cmworking standard solution of titanium, which equals 100; 200; 300; 400; 500 and 600 µg of titanium. Pour 10 cmof hydrochloric acid diluted 1:1, and then do as described in claim 3.2.
On the found values of optical density and corresponding mass of titanium is to build a calibration curve.
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of titanium () in percent is calculated by the formula
,
where is the mass of titanium, was found in the calibration schedule, mcg;
— capacity volumetric flasks, cm;
— aliquotes volume of the solution taken for the determining, cm;
— the weight of the portion of the sample,
4.2. The values of permissible differences are listed in table.2.
Table 2
Mass fraction of titanium, % |
Allowable difference, % |
1,0 |
0,1 |
5,0 |
0,4 |
10,0 |
0,6 |
15,0 | 0,7 |
20,0 | 0,9 |
25,0 | 1,0 |
(Changed edition, Rev. N 1).