GOST 6689.21-92
GOST 6689.21−92 Nickel, alloys Nickel and copper-Nickel. Methods for determination of titanium
GOST 6689.21−92
Group B59
STATE STANDARD OF THE USSR
NICKEL, ALLOYS NICKEL AND COPPER-NICKEL
Methods for determination of titanium
Nickel, nickel and copper-nickel alloys. Methods for the determination of titanium
AXTU 1709
Date of introduction 1993−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR
DEVELOPERS
V. N. Fedorov, Y. M. Leybov, Boris Krasnov, A. N. Bulanova, L. V. Morea, A. I. Vorobyov
2. APPROVED AND promulgated by the Decree of Committee of standardization and Metrology of the USSR from
3. REPLACE GOST 6689.21−80
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
The number of the paragraph, subparagraph, section |
| GOST 8.315−91 |
2.4.3; 4.4.3 |
| GOST 199−78 |
3.2 |
| GOST 492−73 |
Chapeau |
| GOST 859−78 |
4.2 |
| GOST 3118−77 |
3.2 |
| GOST 4204−77 |
2.2; 3.2; 4.2 |
| GOST 4461−76 |
2.2; 3.2; 4.2 |
| GOST 6552−80 |
2.2 |
| GOST 6689.1−91* |
Sec. 1 |
| GOST 10484−78 |
2.2, 3.2, 4.2 |
| GOST 10929−76 |
2.2 |
| GOST 25086−87 |
Sec. 1, 2.4.3, 4.4.3 |
________________
* Probably a mistake of the original. Should read GOST 6689.1−92. — Note the manufacturer’s database.
This standard sets the photometric and atomic absorption methods for the determination of titanium (with a mass fraction of titanium from 0.05 to 0.4%) in copper-Nickel alloys according to GOST 492*.
________________
* On the territory of the Russian Federation GOST 492−2006. — Note the manufacturer’s database.
1. GENERAL REQUIREMENTS
General requirements for method of analysis according to GOST 25086 with the addition of sec. 1 GOST 6689.1.
2. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM WITH HYDROGEN PEROXIDE
2.1. The essence of the method
The method is based on the formation of titanium in sulfuric acid medium with hydrogen peroxide in the orange-yellow complex, and measuring the optical density of the resulting solution.
2.2. 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.
Hydrogen peroxide according to GOST 10929.
Titanium metal with a titanium content not less than 99.5%.
Potassium titanium fluoride.
A standard solution of titanium And
Of metal titanium solution is prepared of 0.2 g of the titanium is dissolved by heating in 100 cmof sulphuric acid (1:4). Then when boiling, oxidize titanium, adding dropwise nitric acid to the bleaching solution. The solution was boiled for 2−3 min, cooled, transferred to a volumetric flask with a capacity of 500 cm
and topped to the mark with water.
1 cmof a solution containing 0.0004 g of titanium.
Fluoride potassium titanium solution is prepared: 1,002 g of the drug is placed in a platinum Cup, dissolved in 10 cmof sulphuric acid (1:1) and evaporated to obtain a wet residue, which is dissolved in 50 cm
of sulphuric acid (1:4). The solution was transferred to a volumetric flask with a capacity of 500 cm
, add 50 cm
of sulphuric acid (1:4) and top up with water to the mark.
1 cmof solution A contains 0.0004 g Titan
.
2.3. Analysis
2.3.1. A sample of alloy weighing 0.5 g is placed in a platinum Cup, add 10 cmof nitrogen and 1 cm
hydrofluoric acid and dissolved by heating. To the solution was added 20 cm
of sulphuric acid (1:1) and evaporated until a white smoke of sulfuric acid. After cooling, the residue is dissolved in water, transferred to a volumetric flask with a capacity of 100 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 solution on a photoelectrocolorimeter with a blue filter or on a spectrophotometer at 410 nm in a cuvette with the thickness of the light absorbing layer 1 see Solution comparison is the same solution, but without adding hydrogen peroxide.
2.3.2. Construction of calibration curve
In a volumetric flask with a capacity of 100 cmadd 0,5; 1,0; 2,0; 3,0; 4,0; 5,0 and 6.0 cm
of a standard solution of titanium 25 cm
of sulphuric acid (1:4), 5 cm
of phosphoric acid, 1 cm
of hydrogen peroxide and then filled to the mark with water. Then do as mentioned in paragraph
2.4. Processing of the results
2.4.1. 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,
2.4.2. Discrepancies in the results of three parallel definitions of d (indicator of convergence) and the results of the two analyses D (a measure of reproducibility) shall not exceed the values of permissible differences given in the table.
| Mass fraction of titanium, % | The allowable divergence, % | |
| d |
D | |
| From 0.05 to 0.2 incl. |
0,01 | 0,01 |
| SV. 0,2 «0,4 « |
0,02 | 0,03 |
2.4.3. Control of accuracy of analysis results is carried out according to State standard samples (GSO) or industry standard sample (CCA), or by standard samples of the enterprise (SOP) of copper-Nickel alloys, approved under GOST 8.315*, or supplements method, or the comparison of the results obtained by atomic absorption method in accordance with GOST 25086.
________________
* On the territory of the Russian Federation GOST 8.315−97, here and hereafter. — Note the manufacturer’s database.
3. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM WITH DIANTIPYRYLMETHANE
3.1. The essence of the method
The method is based on the formation of the titanium complex with diantipyrylmethane, painted in Golden yellow color, and measuring the optical density of the resulting solution.
3.2. Apparatus, reagents and solutions
Photoelectrocolorimeter or spectrophotometer.
Nitric acid according to GOST 4461.
Sulfuric acid according to GOST 4204, diluted 1:1.
Hydrochloric acid according to GOST 3118 and diluted 1:1.
Hydrofluoric acid according to GOST 10484.
Ascorbic acid, a solution of 100 g/DM.
Sodium acetate according to GOST 199, a solution of 500 g/DM.
Diantipyrylmethane, a solution of 10 g/DMof 10 g of reagent was dissolved in 200 cm
of water, add 80 cm
of hydrochloric acid (concentrated), the solution was cooled, transferred to a volumetric flask with a capacity of 1 DM
, made up to the mark with water and mix.
The titanium metal content not less than 99.5% titanium.
Potassium titanium fluoride.
A standard solution of titanium And prepared as described in step 2.2.
A standard solution of titanium, B: 5 cmsolution And placed in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix, cook in day of application.
1 cmof solution B contains 0,00002 g Titus
on.
3.3. Analysis
3.3.1. A sample weighing 5 g was placed in a platinum Cup, add 15 cmof nitric acid (1:1), 2 cm
hydrofluoric acid and dissolved by heating. Then add 10 cm
sulphuric acid (1:1) and the solution was evaporated prior to the allocation of white smoke of sulfuric acid. After cooling, rinse the walls of the Cup with water and re-evaporated prior to the allocation of white smoke of sulfuric acid. After cooling, the residue is dissolved in water, the solution transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
Depending on the mass fraction of titanium selected aliquot part of the solution — 10 cm(0.05 to 0.1%) and 5 cm
(from 0.1 to 0.4%) in a volumetric flask with a capacity of 100 cm
, add 10 cm
of water and set pH=7−8 with a solution of sodium acetate according to universal indicator paper. Then add 10 cm
of hydrochloric acid (1:1), 2.5 cm
of ascorbic acid, 25 cm
diantipyrylmethane, made up to the mark with water and mix. After 40−50 min, measure the optical density
solution on a photoelectrocolorimeter with a blue filter (
ETANA.
3.3.2. Construction of calibration curve
In a volumetric flask with a capacity of 100 cmis placed 1,0; 2,0; 3,0; 4,0 and 5,0 cm
standard solution B titanium, added to 10 cm
of water and set pH=7−8 with a solution of sodium acetate and further receives, as described in Chapter
Solution comparison is the solution, not containing titanium.
3.4. Processing of the results
3.4.1 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 of the sample corresponding to aliquote part of the solution,
3.4.2. Discrepancies in the results of three parallel definitions of d (indicator of convergence) and the results of the two analyses D (a measure of reproducibility) shall not exceed the values of permissible differences given in the table.
3.4.3. Control of accuracy of analysis results is carried out as specified in clause
4. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF TITANIUM
4.1. 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.
4.2. Apparatus, reagents and solutions
Atomic absorption spectrometer with a radiation source for titanium.
Nitric acid according to GOST 4461, diluted 1:1.
Hydrofluoric acid according to GOST 10484.
Sulfuric acid according to GOST 4204, diluted 1:1 and 1:4.
Copper according to GOST 859*.
________________
* On the territory of the Russian Federation GOST 859−2001. — Note the manufacturer’s database.
The copper solution: 10 g of copper was dissolved with heating in 80 cmof nitric acid (1:1). The solution was 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.
The titanium metal.
Standard titanium solution: 0.1 g of titanium was placed in a platinum Cup and dissolved by heating in 20 cmof sulphuric acid (1:4) and 2 cm
hydrofluoric acid. Then add 10 cm
sulphuric acid (1:1) and evaporated until a white smoke of sulfuric acid. Cup cooled and the residue is dissolved in 50 cm
of water when heated. The solution was transferred to a volumetric flask with a capacity of 100 cm
and top up with water to the mark.
1 cmof the solution contains 0.001 g Titus
on.
4.3. Analysis
4.3.1. A portion of the alloy with a mass of 2 g is placed in a platinum Cup and dissolved by heating in 20 cmof nitric acid (1:1) and 2 cm
hydrofluoric acid. Then add 10 cm
sulphuric acid (1:1) and evaporated until a white smoke of sulfuric acid. Cup cooled and the residue is dissolved in 50 cm
of water when heated. The solution was 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 364,3 nm parallel to the calibration solutions.
4.3.2. Construction of calibration curve
Four volumetric flasks with a capacity of 100 cmis placed 1,0; 3,0; 5,0 and 6,0 cm
standard solution titanium, which corresponds to 1,0; 3,0; of 5.0 and 6.0 mg of titanium, poured 20 cm
of standard copper solution and add water to the mark. Measure the atomic absorption of titanium, as specified in clause
4.4. Processing of the results
4.4.1. 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 sample solution, cm
;
— the weight of the portion of the sample,
4.4.2. Discrepancies in the results of three parallel definitions of d (indicator of convergence) and the results of the two analyses D (a measure of reproducibility) shall not exceed the values of permissible differences given in the table.
4.4.3 Control of accuracy of analysis results is carried out according to State standard samples (GSO) or industry standard sample (CCA), or by standard samples of the enterprise (SOP) of copper-Nickel alloys, approved under GOST 8.315, or by a method of additives, or a comparison of the results obtained by the photometric method according to GOST 25086.
