GOST 25278.9-82
GOST 25278.9−82 Alloys and alloys of rare metals. Methods for the determination of titanium (with Amendments No. 1, 2)
GOST 25278.9−82
Group B59
STATE STANDARD OF THE USSR
ALLOYS AND ALLOYS OF RARE METALS
Methods for determination of titanium
Alloys and foundry alloys of rare metals. Methods for determination of titanium
AXTU 1709
Valid from 01.07.83
to 01.07.93*
_______________________________
* Expiration removed
according to the Protocol of the Intergovernmental Council
for standardization, Metrology and certification
(IUS N 2, 1993). — Note the manufacturer’s database.
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
Yu. A. Karpov, E. G. Nembrini, V. G., Miscreants, G. N. Andrianov, E. S. Danilin, M. A. Desyatkova L. I. Kirsanova, T. M. Malyutina, Y. F. Markov, V. M. Mikhailov, L. A. Nikitina, L. G. Obruchkova, N. Rasnitsyn, N. Suvorova, L. N. Filimonov
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 26.05.82 N 2120.
3. The period of examination — 1993
The frequency of inspection is 5 years.
4. INTRODUCED FOR THE FIRST TIME.
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
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|
The designation of the reference document referenced
|
Item number
|
GOST 3118−77
|
2.1, 3.1
|
GOST 4204−77
|
2.1, 3.1
|
GOST 5817−77
|
2.1, 3.1
|
GOST 7172−76
|
2.1
|
GOST 26473.0−85
|
1.1
|
6. Validity extended until 01.01.93 by the Resolution of Gosstandart of the USSR from 29.10.87 N 4096
7. REPRINT (November 1988) with amendment No. 1, approved in October 1987 (ICS 1−88).
The Change No. 2 adopted by the Interstate Council for standardization, Metrology and certification (Protocol No. 12, 21.11.97). The state developed by Russia. By the resolution of Gosstandart of Russia dated 06.04.98 No. 107 enacted in the territory of the Russian Federation with 01.07.98
Change No. 2 made by the manufacturer of the database in the text IUS N 6, 1998
This standard specifies two methods for determination of titanium:
photometric (from 1% to 20%) for alloys (ligatures) based on Zirconia containing not more than 30% of niobium, and vanadium-based alloys containing not more than 10% chromium;
differential photometric (40 to 50%) for binary alloys niobium-titanium; (20 to 80%) for binary alloy gallium-titanium.
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis and security requirements — according to GOST 26473.0−85.
(Changed edition, Rev. N 1).
2. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM
The method is based on formation of colored complex compounds of titanium with diantipyrylmethane in tartrate-hydrochloric acid (1.2 mol/l
by hydrochloric acid) solution. Hydrolysis of niobium to prevent the introduction of tartaric acid. Vanadium (IV), iron (II), zirconium definition, do not interfere.
2.1. Apparatus, reagents and solutions
Photoelectrocolorimeter FEK-56 or similar device.
Muffle furnace with thermostat providing temperatures up to 1000 °C.
Analytical scale.
Libra technical.
Tile electric.
Bath water.
The quartz crucibles high capacity of 40 cm.
Volumetric flasks with a capacity of 50, 100, and 1000 cm.
Pipettes without division into 5, 10 and 15 cm.
Burettes capacity 10 cm.
Measuring beakers with a capacity of 25 and 500 cm.
Potassium preservatory according to GOST 7172−76.
Sulfuric acid GOST 4204−77 and diluted 1:1.
Tartaric acid according to GOST 5817−77, a solution of 150 g/DM.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
Ascorbic acid.
Diantipyrylmethane, solution 20 g/l: 20 g of reagent was dissolved in a mixture consisting of 300 cmof water, 60 cmof sulphuric acid (1:1) and 2.0 g of ascorbic acid, stirring well to dissolve the reagent. The solution was transferred to volumetric flask with a capacity of 1 DM, adjusted to the mark with water and mix. (If the standing of the solution emits crystals of the reagent, the solution is slightly heated to their dissolution).
The titanium metal containing not less than 99.9% titanium in the form of small chips.
A standard solution of titanium (spare) containing 1 mg/cmtitanium: 0.1 g of titanium metal is placed in a quartz crucible and fused with 2−4 grams of potassium persulfate in muffle at the temperature of 700−800 °C to produce a clear float. The smelt is dissolved by heating in 20 cmof a solution of tartaric acid, the cooled solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with water.
A solution of titanium (working) containing 100 µg/cmtitanium, is prepared by dilution of a standard solution of water in
10 times.
2.2. Analysis
2.2.1. A portion of the sample weighing 0.1 g was placed in a quartz crucible, add 2−4 g of persulfate potassium, a few drops of concentrated sulphuric acid and fused in a muffle at a temperature of 700−800 °C to obtain a homogeneous melt. The smelt is dissolved by heating in 20 cmof a solution of tartaric acid, the cooled solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix. If the expected titanium content more than 10% of the resulting solution was diluted again: take 10 cmof solution in a volumetric flask with a capacity of 100 cm, add 20 cmof tartaric acid and adjusted to the mark with water.
To determine the Titan select 5, 10 and 15 cmof solution in a volumetric flask with a capacity of 50 cm, add 10 cmof tartaric acid, place the flask in a boiling water bath for 5 min, cooling, and immediately pour 15 cmof the solution diantipyrylmethane 10 cmof hydrochloric acid. The solutions were cooled, adjusted to the mark with water and mix. Measure the optical density of solutions on the photoelectrocolorimeter at 
508 nm in a cuvette with the thickness of the light absorbing layer 30 mm in relation to the zero solution.
Weight titanium find for the calibration graph
the IR.
2.2.2. Construction of calibration curve
In a volumetric flask with a capacity of 50 cmis injected from microburette from 1.0 to 6.0 cmof working solution of titanium at intervals of 1.0 cm. Add 10 cmof tartaric acid, place the flask in a boiling water bath for 5 min and, without cooling, immediately pour the 15 cmsolution diantipyrylmethane and 10 cmof hydrochloric acid. Solutions of cool (first at room temperature for 10−15 minutes, after this time you can cool the solution in cold water, but it is impossible to prevent the sudden cooling solutions), adjusted to the mark with water and mix. In one of the flasks poured all reagents with the exception of titanium (zero solution). Measure the optical density of solutions on the photoelectrocolorimeter at 
508 nm in a cuvette with the thickness of the light absorbing layer 30 mm in relation to the zero solution. According to the obtained results build a calibration curve in the coordinates: the optical density is the mass of titanium. Separate test points of the graph along with the analysis of samples
.
2.3. Processing of the results
2.3.1. Mass fraction of titanium (
) in percent is calculated by the formula
,
where 
is the mass of titanium, was found in the calibration graphics mg;
the capacity of volumetric flasks at the first dilution, cm;
the capacity of the volumetric flask for the second dilution, cm;
— aliquotes volume of the solution taken for dilution, cm;
— aliquotes volume of the solution taken for the determining, cm;
— the weight of the portion of the sample,
G.
2.3.2. Discrepancies between the results of two parallel determinations and the results of the two tests should not exceed the values of permissible differences given in table.1.
Table 1
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|
Mass fraction of titanium, %
|
The allowable divergence, %
|
1,0
|
0,1
|
5,0
|
0,4
|
10,0
|
0,8
|
15,0
|
1,3
|
20,0
|
1,7
|
(Changed edition, Rev. N 1).
3. DIFFERENTIAL PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM IN THE ALLOY NIOBIUM-TITANIUM
______________
* The name of the section. Changed the wording, Rev. N 2.
The method is based on formation of colored complex compounds of titanium with diantipyrylmethane in tartrate-hydrochloric acid (1.2 mol/lby hydrochloric acid) solution. Measurement of optical density of solutions produced relative to the comparison solution containing 2.0 mg of titanium. Hydrolysis of niobium to prevent the introduction of tartaric acid.
3.1. Apparatus, reagents and solutions
The spectrophotometer SF-4A or similar device.
Muffle furnace with thermostat providing temperatures up to 1000 °C.
Analytical scale.
Libra technical.
Tile electric.
Bath water.
The quartz crucibles high capacity of 40 cm.
Volumetric flasks with a capacity of 50, 100, and 1000 cm.
Pipettes without dividing by 5 cm.
Burettes capacity 10 cm.
Measuring beakers with a capacity of 25 and 500 cm.
Potassium preservatory according to GOST 7172−76.
Sulfuric acid GOST 4204−77 and diluted 1:1.
Tartaric acid according to GOST 5817−77, a solution of 150 g/DM.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
Ascorbic acid.
Diantipyrylmethane, solution 20 g/l: 20 g of reagent was dissolved in a mixture consisting of 300 cmof water, 60 cmof sulphuric acid (1:1) and 2.0 g of ascorbic acid, stirring well to dissolve the reagent. The solution was transferred to volumetric flask with a capacity of 1 DM, adjusted to the mark with water and mix. (If the standing of the solution emits crystals of the reagent, the solution is slightly heated to their dissolution).
The titanium metal containing not less than 99.9% titanium in the form of small chips.
A standard solution of titanium (spare) containing 1 mg/cmtitanium: 0.1 g of titanium metal is placed in a quartz crucible and fused with 2−4 grams of potassium persulfate in muffle at the temperature of 700−800 °C to produce a clear float. The smelt is dissolved by heating in 20 cmof a solution of tartaric acid, the cooled solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with water.
A solution of titanium (working) containing 200 µg/cmtitanium, is prepared by dilution of a standard solution of water in p
ive times.
3.2. Analysis
3.2.1. A portion of the sample weighing 0.1 g was placed in a quartz crucible, add 2−4 g of persulfate potassium, a few drops of concentrated sulphuric acid and fused in a muffle at a temperature of 700−800 °C to obtain a homogeneous melt. The smelt is dissolved by heating in 20 cmof a solution of tartaric acid, the cooled solution was transferred to volumetric flask with a capacity of 100 cm, adjusted to the mark with water and mix.
For the determination of titanium in a volumetric flask with a capacity of 50 cmtaken 5 cmof a solution containing the 2.1−2.5 mg of titanium, is added 10 cmof tartaric acid, place the flask in a boiling water bath for 5 min, cooling, and immediately pour 15 cmof the solution diantipyrylmethane 10 cmof hydrochloric acid. Solution cool (first at room temperature for 10−15 minutes, after this time you can cool the solution in cold water, as it is impossible to prevent a sharp cooling solutions), adjusted to the mark with water and mix. Measure the optical density of the solution on the spectrophotometer at 
480 nm in a cuvette with the thickness of the light absorbing layer 10 mm relative to the comparison solution containing 2.0 mg of titanium. Weight titanium find for the calibration graph
.
3.2.2. Construction of calibration curve
In a volumetric flask with a capacity of 50 cmimpose a 10 cmworking solution of titanium containing 200 µg/cmtitanium, and then 1,0; 2,0; 3,0; 4,0 and 5,0 cmof working solution of titanium, containing 100 µg/cmof titanium (one of the flasks not go further working solution of titanium, containing 100 µg/cmof titanium), which corresponds to 2,0; 2,1; 2,2; 2,3; 2,4 and 2,5 mg of titanium. Add 10 cmof tartaric acid, place the flask in a boiling water bath for 5 min, cooling, and immediately pour 15 cmof the solution diantipyrylmethane 10 cmof hydrochloric acid. The solution was cooled, adjusted to the mark with water and mix. Measure the optical density of solutions containing 2.1 to 2.5 mg of titanium, with respect to a solution containing 2.0 mg of titanium on the spectrophotometer at 480 nm in a cuvette with the thickness of the light absorbing layer 10 mm. According to the obtained results build a calibration curve in the coordinates: the optical density is the mass of titanium. Separate test points of the graph along with the analysis of the p
Rob.
3.3. Processing of the results
3.3.1. Mass fraction of titanium () in percent is calculated by the formula
,
where is the mass of titanium, was found in the calibration graphics mg;
— capacity volumetric flasks, cm;
— aliquotes volume of the solution taken for the determining, cm;
— the weight of the portion of the sample,
3.3.2. Discrepancies between the results of two parallel determinations and the results of the two tests should not exceed the values of permissible differences given in table.2.
Table 2
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Mass fraction of titanium, %
|
The allowable divergence, %
|
40,0
|
1,1
|
45,0
|
1,3 |
50,0
|
1,5
|
(Changed edition, Rev. N 1).
4. DIFFERENTIAL PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM IN THE ALLOYS GALLIUM-TITANIUM
The method is based on formation of colored complex compounds of titanium with hydrogen peroxide in sulfuric acid solution. Measurement of optical density of solutions produced relative to the comparison solution containing 5.0 mg of titanium. Gallium definition does not interfere.
4.1. Apparatus, reagents and solutions
The spectrophotometer SF-26 or similar device
Analytical scale.
Libra technical.
Tile electric.
Conical flasks with a capacity of 100 cm.
Volumetric flasks with a capacity of 50, 100 and 200 cm.
Pipettes with graduation marks at 5 and 10 cm.
Sulfuric acid GOST 4204−77 and diluted 1:1.
Nitric acid GOST 4461−77 and diluted 1:1.
Orthophosphoric acid according to GOST 6552−80.
Hydrogen peroxide according to GOST 10929−76.
Titanium metal according to GOST 19807−91 brand VT1−00.
Standard titanium solution containing 1 mg/cmtitanium: 0.1 g of titanium metal is placed in a conical flask with a capacity of 100 cm, add 10 cmsulphuric acid diluted 1:1, and heated until complete dissolution of the sample, then add a few drops of concentrated nitric acid (to a bleaching solution of titanium) and heating was continued until the appearance of sulphuric acid fumes. In the cooled flask is added 20−30 cmof water, heated to dissolve the salts; the resulting solution was transferred to volumetric flask with a capacity of 100 cm, cooled, adjusted to the mark with water and mix
T.
4.2. Analysis
4.2.1. A portion of the sample weighing 0.1 g was placed in a conical flask with a capacity of 100 cm, pour 5 cmof sulphuric acid diluted 1:1, 10−15 drops of concentrated nitric acid and heated until complete dissolution of the sample and on until sulphuric acid fumes. In the cooled flask is added 20−30 cmof water, heated to dissolve the salts; the resulting solution was transferred to volumetric flask with a capacity of 100 cm, cooled, adjusted to the mark with water and mix.
For the determination of titanium in a volumetric flask with a capacity of 50 cmis taken aliquot part of the obtained solution containing 5−8 mg of titanium, pour 2 cmof phosphoric acid diluted 1:1, 5 cmof hydrogen peroxide, stirring after adding each reagent, adjusted to the mark with water. Measure the optical density of the solution on the spectrophotometer at 410 nm in a cuvette with the thickness of the light absorbing layer 10 mm relative to the comparison solution containing 5.0 mg of titanium.
The mass of the Titan find the schedule for the calibration or using a calibration of factor
M.
4.2.2. Construction of calibration curve
Four volumetric flasks with a capacity of 50 cmeach pipette introduce 5,0; 6,0; 7,0 and 8,0 cmof a solution of titanium, which corresponds to 5,0; 6,0; 7,0 and 8,0 g of titanium, pour 2 cmof phosphoric acid and then act as described in section 4.2.1.
According to the obtained values of optical density and corresponding mass of titanium is to build a calibration curve or calculate the calibration factor according to GOST 26473.0−85, p. 16.
4.3. Processing of the results
4.3.1. Mass fraction of titanium () in percent is calculated by the formula
,
where is the mass of titanium in solution comparisons, mg;
— the optical density of the analyzed solution in relation to solution comparison;
— calibration factor;
— capacity volumetric flasks, cm;
— the weight of the portion of the sample, g;
— volume aliquote part of the solution, cm
.
4.3.2. Discrepancies between the results of two parallel determinations and the results of the two tests should not exceed the permissible differences given in table.3.
Table 3
| |
|
Mass fraction of titanium, %
|
The allowable divergence, %
|
20,0
|
0,4
|
50,0
|
1,1
|
80,0
|
1,8
|
Section 4. (Added, Rev. N 2).
