GOST 1762.4-71
GOST 1762.4−71 Silumin ingots. Methods for the determination of titanium (with Amendments No. 1, 2)
GOST 1762.4−71
Group B59
STATE STANDARD OF THE USSR
SILUMIN IN PIGS
Methods for determination of titanium
Aluminium-silicon alloy ingots.
Methods for determination of titanium
AXTU 1709
Valid from 01.01.73
to 01.07.95*
_______________________________
* Expiration removed
Protocol N 4−93 inter-state Council
for standardization, Metrology and certification.
(IUS N 4, 1994). — Note the CODE.
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
THE DEVELOPERS OF THE STANDARD
A. A. Kostyukov, G. A. Romanov, N. M. Gertseva, A. P. Nechitailov, V. A. Lavrov
2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from
3. The frequency of inspection — 5 years
4. REPLACE GOST 1762−51 (in terms of sec. V)
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced | Item number | |
| GOST 83−79 | Sec. 5 | |
| GOST 1762.0−71 | 1.1 | |
| GOST 1762.2−71 | 3.1 | |
| GOST 3118−77 | Sec. 2, 5 | |
| GOST 4038−79 | Sec. 5 | |
| GOST 4165−78 | Sec. 2 | |
| GOST 4204−77 | Sec. 2, 5 | |
| GOST 4233−77 | Sec. 5 | |
| GOST 4328−77 | Sec. 5 | |
| GOST 4461−77 | Sec. 2, 5 | |
| GOST 5457−75 | Sec. 5 | |
| GOST 7172−76 | Sec. 2 | |
| GOST 9428−73 | Sec. 5 | |
| GOST 10929−76 | Sec. 5 | |
| GOST 11069−74 | Sec. 5 | |
| GOST 19807−74 | Sec. 2, 5 | |
6. Validity extended until
7. The re-release (may 1989) with Amendments No. 1, 2 approved in August 1984, March 1989 (IUS 12−84, 6−89)
This standard sets the photometric method (at a mass fraction of titanium from 0.005 to 0.25%) and atomic absorption method for the determination of titanium (with a mass fraction of titanium from 0.1 to 0.25%).
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 1762.0−71.
PHOTOMETRIC METHOD
The method is based on measuring the optical density of the colored complex compounds of titanium with diantipyrylmethane in the presence of ascorbic acid, which regenerates trivalent iron.
Colored solution photometered at 385 nm.
(Changed edition, Rev. N 2).
2. APPARATUS, REAGENTS AND SOLUTIONS
Type photoelectrocolorimeter FEK-56M, PEC-60, KLF, spectrophotometer type SF-16, SF-26 or similar.
A muffle furnace with thermostatic control, providing heating to 900 °C.
Diantipyrylmethane, a solution with a mass fraction of 5% in a solution with molar concentration of 1 mol/DMhydrochloric acid. If the storage falls a crystalline precipitate, the solution is heated at 40−50 °C to dissolve the precipitate.
Ascorbic acid, freshly prepared solution with a mass fraction of 2%.
Copper sulfate according to GOST 4165−78, a solution with a mass fraction of 5%.
Sulfuric acid GOST 4204−77, diluted 1:1 and 1:2 solution with a mass fraction of 5%.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
Potassium preservatory according to GOST 7172−76.
Nitric acid GOST 4461−77.
Titanium dioxide.
Titanium metal according to GOST 19807−74*.
________________
* Standards 19807−91, here and hereafter. — Note the CODE.
Standard solutions of titanium
Solution A, prepared as follows: 0,1670 g calcined at 900 °C titanium dioxide is fused with twenty times the number peacemaking potassium until a clear melt. The smelt is leached when heated to 100 cmof sulphuric acid diluted 1:1, and translate the solution into a measuring flask with a capacity of 1 DM
. Then pour 100 cm
of sulphuric acid diluted 1:1, made up to the mark with water and stirred or 0,1000 g of titanium dissolved in 15 cm
of sulfuric acid solution 1:2, after dissolution, is oxidized with concentrated nitric acid added dropwise, and the solution evaporated to fumes of sulphuric anhydride. Then dissolve in water, add 100 cm
of sulfuric acid solution 1:1, transferred into a measuring flask with volume capacity of 1000 cm
containing 100 cm
of sulfuric acid solution 1:1 and stirred.
1 cmof solution A contains 0.1 mg of titanium.
Solution B is prepared (prior to application) as follows: 25 cmsolution And placed in a volumetric flask with a capacity of 250 cm
, and topped to the mark with a solution with a mass fraction of sulfuric acid 5%.
1 cmof a solution contains 0.01 mg of titanium.
(Changed edition, Rev. N 1, 2).
3. ANALYSIS
3.1. Aliquot part of the solution is 20−50 cm, prepared for determination of Fe (sect.3 GOST 1762.2−71) is placed in a volumetric flask with a capacity of 100 cm
, is diluted with water to 75 cm
, and then poured, with stirring, 5 cm
of sulphuric acid, diluted 1:2, 5 cm
of ascorbic acid solution and two drops of solution of copper sulphate. After 3−4 minutes pour 10 cm
of the solution diantipyrylmethane, made up to the mark with water and mix.
After 30 min, measure the optical density of the solution on the photoelectrocolorimeter or spectrophotometer, given that a maximum of light absorption of solutions corresponds to a wavelength of 385 nm.
Solution comparison is water.
At the same time carry out the blank experiment with the same reagents as in the dissolution tests, carried it through all the stages of the analysis.
Mass fraction of titanium is determined according to the calibration schedule, taking into account the amendment in the reference experiment.
3.2. Construction of calibration curve
In seven volumetric flasks with a capacity of 100 cmpour 0; 0,5; 1,0; 2,0; 4,0; 6,0; 8,0; 12,0 cm
standard solution B, which corresponds to 0; 0,05; 0,01; 0,02; 0,04; 0,06; 0,08; 0,12 mg titanium, add 2 cm
of hydrochloric acid diluted 1:1 and diluted with water to 50 cm
, then all flasks is poured 10 cm
of sulphuric acid, diluted 1:2, and then carry out the analysis as described in section 3.1.
Solution comparison is the solution in which the titanium was not added. According to the obtained values of optical density and known mass of titanium to build the calibration graph.
3.1, 3.2. (Changed edition, Rev. N 1, 2).
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 graphics mg;
— volume of initial solution, cm
;
— aliquota part of the solution, cm
;
— linkage of silumin,
4.2. Allowable absolute differences of the results of the parallel definitions should not exceed the values given in the table.
| Mass fraction of titanium, % | Allowable absolute differences, % | |
| convergence | reproducibility | |
| From 0,005 to 0,010 incl. | 0,003 | 0,005 |
| SV. 0,010 «0,030 « | 0,005 | 0,008 |
| «0,030» 0,100 « | 0,007 | 0,01 |
| «To 0.10» to 0.25 « | 0,01 | 0,02 |
(Changed edition, Rev. N 2).
ATOMIC ABSORPTION METHOD
The method is based on measuring atomic absorption of titanium in flame acetylene-nitrous oxide at a wavelength of 365,4 nm.
5. APPARATUS, REAGENTS AND SOLUTIONS
Atomic absorption spectrometer model Perkin-Elmer, «Saturn» or similar.
Lamp with a hollow cathode, is intended for the determination of titanium.
Acetylene in cylinders technical — GOST 5457−75.
The nitrous oxide.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
Hydrogen peroxide according to GOST 10929−76, a solution with a mass fraction of 3%.
Nickel chloride according to GOST 4038−79, a solution with a mass fraction of 0.2%.
Aluminum brand А999 according to GOST 11069−74*.
________________
* On the territory of the Russian Federation GOST 11069−2001. — Note the CODE.
The solution of aluminum And 20 g/l: 10.0 g of aluminum is placed in a beaker with a capacity of 600 cm
, add 250 cm
of hydrochloric acid diluted 1:1, and dissolved under heating with adding 1 cm
of Nickel chloride. The solution was cooled, transferred to a volumetric flask with a capacity of 500 cm
, is diluted to the mark with water and mix.
Sodium carbonate according to GOST 83−79.
Silicon dioxide according to GOST 9428−73.
A solution of silicon B, 1 g/DM: 2,14 g of finely crushed in an agate or plexiglass mortar and calcined for one hour at a temperature of 1000 °C silicon dioxide is fused in a platinum crucible with 15 g of sodium carbonate at a temperature of 900 °C to produce a clear float for 15 min.
The smelt is dissolved in water, platinum, silver or Nickel in the Cup when heated. The solution was cooled, transferred into a measuring flask with volume capacity of 1000 cm, is diluted to the mark with water and mix.
Solution store in a plastic container.
Sodium hydroxide according to GOST 4328−77, a solution with a mass fraction of 30%.
Sulfuric acid GOST 4204−77, diluted 1:5.
Sodium chloride according to GOST 4233−77.
A solution of sodium oxide, 100 g/l: 190 g dried at 105 °C for 30 min. sodium chloride dissolved in water. The solution was transferred into a measuring flask with volume capacity of 1000 cm
, adjusted to the mark with water and mix.
Nitric acid GOST 4461−77.
Titanium metal according to GOST 19807−74.
Standard solutions of titanium.
Solution D: 0,500 g of the titanium is dissolved in 50 cmof sulfuric acid solution 1:5, after dissolution, is oxidized with concentrated nitric acid added dropwise, and the solution evaporated to fumes of sulphuric anhydride. Then dissolve in water, add 100 cm
of sulphuric acid diluted 1:1, transferred into a measuring flask with volume capacity of 1000 cm
containing 200 cm
of sulfuric acid solution 1:1, and stirred.
1 cmof solution contains 0.5 mg of titanium.
Solution: pipette take 10 cmof solution D in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix; prepare before use.
1 cmof solution E contains 0.05 mg of titanium.
Methyl orange solution with a mass fraction of 0.1%.
6. ANALYSIS
6.1. Weighed samples of the silumin weighing 0.5 g were placed in a glass with a capacity of 250 cm, flow 20 cm
of the sodium hydroxide solution. At the end of the reaction the solution is heated on a sand bath until complete dissolution of alloy, add approximately 100 cm
of water and to the cooled solution cautiously add 50 cm
of hydrochloric acid. The solution is heated to enlightenment, add 1 cm
of hydrogen peroxide solution and boiled for 3−5 min to destroy the excess peroxide. The cooled solution was transferred to volumetric flask with a capacity of 250 cm, made up to the mark with water and mix. At the same time through all stages of the analysis carried out control experience with the addition of 20 cm
of a solution of aluminium A. Measure the atomic absorption of titanium in the sample solution, the solution in the reference experiment and in solutions, prepared to build a calibration curve at a wavelength of
365,4 nm in a flame nitrous nitrogen-acetylene.
Before determining the focus burner and set the flame height to obtain the maximum value of atomic absorption.
Mass fraction of titanium is determined according to the calibration schedule, which build on every shot
.
6.2. Construction of calibration curve
Four volumetric flasks with a capacity of 250 cmflow sequentially through 12.5 cm
of solution A with 7 cm
of solution, respectively, 0; 10,0; 15,0; 25,0 cm
standard solution E, which corresponds to 0; 0,10; 0,15; 0,25% mass fraction of titanium in the silumin. Adjusted with water to a volume of 100 cm
and slowly in portions, stirring thoroughly, pour 25 cm
of a solution, add 3−4 drops of methyl orange indicator and drop hydrochloric acid diluted 1:1, until the color changes of the indicator in red. Then the solutions in the flasks was adjusted to the mark with water, mix and measure the absorbance of titanium, as specified in clause 6.1.
According to the obtained values of atomic absorption solutions and the known weight fractions of titanium to build the calibration graph.
7. PROCESSING OF THE RESULTS
7.1. Mass fraction of titanium in percent find the calibration schedule, minus the reference experiment.
7.2. Allowable absolute differences of the results of the parallel definitions should not exceed the values given in the table.
Sec. 5−7. (Added, Rev. N 2).
