GOST 15027.14-77
GOST 15027.14−77 Bronze without tin. Methods for the determination of titanium (with Amendments No. 1, 2)
GOST 15027.14−77
Group B59
INTERSTATE STANDARD
BRONZE WITHOUT TIN
Methods for determination of titanium
Non-tin bronze.
Methods for the determination of titanium
AXTU 1709
Date of introduction 1979−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from
3. REPLACE GOST 15027.14−69
4. The standard fully complies ST SEV 1538−79
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced | Section number, paragraph |
| GOST 859−2001 |
5.2, 6.2 |
| GOST 3118−77 |
5.2 |
| GOST 3760−79 |
5.2 |
| GOST 4204−77 |
2, 5.2 |
| GOST 4461−77 |
2, 5.2, 6.2 |
| GOST 5457−75 |
6.2 |
| GOST 6552−80 |
2 |
| GOST 9293−74 |
6.2 |
| GOST 10484−78 |
2 |
| GOST 10929−76 |
2 |
| GOST 18175−78 |
Chapeau |
| GOST 25086−87 |
1.1, 4.4 |
6. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)
7. EDITION with Amendments No. 1, 2 approved in February 1983, March 1988 (IUS 6−83, 6−88)
This standard sets the photometric and atomic absorption methods for the determination of titanium (with a mass fraction of titanium from 0.05% to 0.3%) in the tin bronze according to GOST 18175.
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 25086 with the addition of sec. 1 GOST 15027.1.
(Changed edition, Rev. N 1).
2A. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM
2A.1. The essence of the method
The method is based on the formation of titanium in sulfuric acid medium with hydrogen peroxide yellow-orange complex and the change in its optical density.
Sec. 2A. (Added, Rev. N 1).
2. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter or spectrophotometer.
Nitric acid according to GOST 4461, diluted 1:1.
Sulfuric acid according to GOST 4204, diluted 1:1 and 1:4.
Hydrofluoric acid according to GOST 10484.
Orthophosphoric acid according to GOST 6552, diluted 1:1.
Hydrogen peroxide according to GOST 10929.
The titanium metal content not less than 99.5% titanium.
Potassium titanium (IV) fluoride.
A standard solution of titanium; is prepared as follows: 0,201 g of titanium metal was dissolved with heating in 100 cmof sulphuric acid, diluted 1:4. Then when boiling, oxidize titanium, adding dropwise nitric acid diluted 1:1, before bleaching solution. The solution was boiled for 2−3 min, cooled, transferred to a volumetric flask with a capacity of 500 cm
, made up to the mark with water and mix.
1 cmof the solution contains 0.4 mg of titanium.
Of potassium titanium fluoride standard solution of titanium prepared as follows: 1,0024 g of potassium titanium (IV) fluoride was evaporated in a platinum Cup with 10 cmof sulphuric acid diluted 1:1, to a moist residue. The contents of the Cup is dissolved in 50 cm
of sulphuric acid, diluted 1:4, poured into a volumetric flask with a capacity of 500 cm
, add 50 cm
of sulphuric acid, diluted 1:4 and dilute to the mark with water.
1 cmof the solution contains 0.4 mg of titanium.
3. ANALYSIS
3.1. A sample of alloy weighing 0.5 g were placed in a glass, pour 10 cmof nitric acid, diluted 1:1 and dissolved by heating. Then add 10 cm
sulphuric acid diluted 1:1, and evaporated to release white smoke of sulfuric acid. After cooling, the residue is dissolved in water, transfer the solution into a volumetric flask with a capacity of 50 cm
, add 5 cm
of phosphoric acid, 1 cm
of hydrogen peroxide, made up to the mark with water, mix and measure optical density of solutions on a photoelectrocolorimeter with a blue color filter at a wavelength of 410−450 nm or on a spectrophotometer at a wavelength of 410 nm in a cuvette length of 1 cm.
Solution comparison is the solution of the analyzed alloy, carried out through all stages of the analysis, but without adding hydrogen peroxide.
3.2. Construction of calibration curve
In a volumetric flask with a capacity of 50 cmconsistently pour 0; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cm
of a standard solution of titanium, is added to 25 cm
of sulphuric acid, diluted 1:4, 5 cm
of phosphoric acid, and 1 cm
of hydrogen peroxide, made up to the mark with water and mix. Further analysis are as indicated in claim 3.1.
Solution comparison is the solution, not containing titanium.
According to the obtained values of optical density calibration curve building.
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 g;
— the weight of the portion,
4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in the table.
| Mass fraction of titanium, % |
|
|
| From 0.05 to 0.15 |
0,01 | 0,02 |
| SV. Of 0.15 «to 0.30 |
0,02 | 0,05 |
(Changed edition, Rev. N 2).
4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in the table.
4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to State standard samples without tin bronzes, certified in the prescribed manner, by comparing the results of analysis of the obtained photometric and atomic absorption methods or by a method of additives in accordance with GOST 25086.
4.3, 4.4. (Added, Rev. N 2).
5. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM IS WITH THE USE OF DIANTIPYRYLMETHANE
5.1. The essence of the method
The method is based on formation of the complex titanium diantipyrylmethane in the medium of 0.5 mol/DMof hydrochloric acid and the measurement of its optical density. The interfering influence of iron can be eliminated by introduction of ascorbic acid.
5.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Nitric acid according to GOST 4461, diluted 1:1.
Hydrochloric acid according to GOST 3118, diluted 1:1.
Sulfuric acid according to GOST 4204, diluted 1:1 and 1:5.
Ascorbic acid according to normative-technical documentation, solution 100 g/DM.
Ammonia water according to GOST 3760.
Diantipyrylmethane (CH
N
O
), a solution of 10 g/DM
in the solution of 0.5 mol/DM
hydrochloric acid; prepared as follows: 10 g of drug is dissolved in 200 cm
of water, add 80 cm
of hydrochloric acid diluted 1:1, the solution was cooled and transferred into a measuring flask with volume capacity of 1000 cm
, made up to the mark with water and mix.
Copper metal stamps MO according to the GOST 859.
The copper solution; prepared as follows: 0.5 g of copper is dissolved in 5 cmof nitric acid, diluted 1:1, and remove the oxides of nitrogen by boiling, the solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
Titanium metal with a mass fraction of titanium is not less than 99.5%.
Standard solutions of titanium.
Solution A, prepared as follows: 0,1005 g of titanium dissolved in 20 cmof sulphuric acid diluted 1:1, the solution was cooled, transferred to a measuring flask with volume capacity of 1000 cm
, made up to the mark with sulfuric acid diluted 1:5, and stirred.
1 cmof the solution contains 0.0001 g of titanium.
Solution B is prepared as follows: 10 cmof the solution And transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with sulfuric acid diluted 1:5, and stirred.
1 cmof solution B contains 0,00
001 g of titanium.
5.3. Analysis
5.3.1. A sample of alloy weighing 0.5 g were placed in a glass with a capacity of 250 cm, and dissolved in 5 cm
of nitric acid when heated. Nitrogen oxides are removed by boiling, the solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix. In two volumetric flasks with a capacity of 100 cm
shift 5 cm
of the solution. The solutions were diluted with water to a volume of 20 cm
, neutralized with ammonia until the appearance of blue color complex of copper, then add 10 cm
of hydrochloric acid and 2.5 cm
of a solution of ascorbic acid. To one of flasks add 25 cm
of the solution diantipyrylmethane and both flasks are topped up to the mark with water and mix. After 50 min, measure the optical density of the solution on a photoelectrocolorimeter with a purple filter or on a spectrophotometer at a wavelength of 389 nm in a cuvette length of 1 cm.
Solution comparison is the solution not containing diantipyrylmethane
on.
5.3.2. Construction of calibration curve
In six volumetric flasks with a capacity of 100 cmis placed 5 cm
of a solution of copper, and five of them placed 1,0; 2,0; 4,0; 6,0 and 8,0 cm
standard solution B. the Solutions were diluted with water to a volume of 20 cm
and further analysis is carried out as specified in clause
5.4. Processing of the results
5.4.1. Mass fraction of titanium () in percent is calculated by the formula
where is the mass of titanium, was found in the calibration schedule g;
— the weight of the portion,
5.4.2. The absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in the table.
(Changed edition, Rev. N 2).
5.4.3. The absolute discrepancies of the analysis results obtained in two laboratories, or two analysis results obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in the table.
5.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to claim 4.4.
5.4.3,
6. ATOMIC ABSORPTION METHOD
6.1. The essence of the method
The method is based on measuring the absorption of light by atoms of titanium, formed during the introduction of the analyzed solution in the flame acetylene-nitrous oxide.
6.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for titanium.
Nitric acid according to GOST 4461, diluted 1:1.
Sulfuric acid according to GOST 4204, diluted 1:1, 1:4 and 1:10.
Acetylene according to GOST 5457.
Nitrous oxide according to GOST 9293.
Copper according to the GOST 859.
Standard copper solution: 10 g of copper was dissolved with heating in 80 cmof nitric acid (1:1). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
and top up with water to the mark.
1 cmof the solution contains 0.1 g of copper.
Titanium metal with a mass fraction of titanium is not less than 99.5%.
Standard titanium solution: 0.1 g of titanium dissolved by heating in 50 cmof sulphuric acid (1:4). The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
and then filled to the mark with sulphuric acid (1:10).
1 cmof the solution contains 0.001 g of titanium.
6.3. Analysis
6.3.1. A portion of the sample weighing 3 g was dissolved with heating in 20 cmof nitric acid 1:1, then add 10 cm
sulphuric acid (1:1) and evaporated until a white smoke of sulfuric acid. The solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
and top up with water to the mark. Measure the atomic absorption of titanium in flame acetylene-nitrous oxide at a wavelength of 365,3 nm parallel to the calibration solutions.
6.3.2. Construction of calibration curve
Five volumetric flasks with a capacity of 100 cmis placed 0; 1,5; 3,0; 6,0 and 9,0 cm
standard solution of titanium, is added to 30 cm
of standard copper solution, 10 cm
of sulphuric acid (1:1) and topped to the mark with water. Measure the atomic absorption of titanium, as specified in clause
6.4. Processing of the results
6.4.1. Mass fraction of titanium () in percent is calculated by the formula
where is the concentration of titanium was found in the calibration schedule, g/cm
;
— the volume of the final sample solution, cm
;
— the weight of the portion of the sample,
6.4.2. Allowable absolute discrepancies in the results of parallel measurements (the rate of convergence) must not exceed the permissible values given in the table.
6.4.3. The absolute discrepancies of the analysis results obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (a measure of reproducibility) shall not exceed the values given in the table.
6.4.4. Control of accuracy of analysis results
Control of accuracy of analysis results is carried out according to claim 4.4.
Sec. 6. (Added, Rev. N 2).
