GOST 23859.10-79
GOST 23859.10−79 heat-resistant Bronze. Methods for the determination of titanium (with Amendments No. 1, 2)
GOST 23859.10−79
Group B59
INTERSTATE STANDARD
BRONZE HIGH-TEMPERATURE
Methods for determination of titanium
Bronze fire-resistance. Methods for the determination of titanium
AXTU 1709
Date of introduction 1981−01−01
Resolution of the USSR State Committee for standards, dated 16 October 1979, N 3937 time of the introduction set with 01.01.81
Limitation of actions taken by Protocol No. 5−94 of the Interstate Council for standardization, Metrology and certification (ICS 11−12−94)
EDITION with Amendments No. 1, 2 approved in June 1985, March 1990 (IUS 9−85, 7−90).
This standard establishes photometric methods for determination of titanium (with a mass fraction of from 0.02 to 0.09% and from 0.5 to 2%) in high-temperature copper alloys.
(Changed edition, Rev. N 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 25086−87 with the addition of a GOST 23859.1−79, sec. 1.
(Changed edition, Rev. N 2).
THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM WITH HYDROGEN PEROXIDE
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. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter or spectrophotometer.
Nitric acid GOST 4461−77 and diluted 1:1.
Sulfuric acid GOST 4204−77, diluted 1:1 and 1:4.
Hydrochloric acid by the GOST 3118−77.
Orthophosphoric acid according to GOST 6552−80, diluted 1:1.
The mixture of acids to dissolve; mix one volume of concentrated nitric acid and three volumes of concentrated hydrochloric acid.
Hydrogen peroxide (perhydrol) according to GOST 10929−76.
The titanium metal content not less than 99.5% titanium.
Titanium-potassium fluoride.
Standard solutions of titanium.
A. a solution of 0.2 g of titanium metal was dissolved with heating in 100 cmof sulphuric acid, diluted 1:4. Then when boiling oxidize the titanium (III) to titanium (IV) 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.
A standard solution can also be prepared from potassium titanium fluoride. For this 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, and the solution transferred to 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 cm
of solution A contains 0.0004 g of titanium.
Solution B is prepared on the day of application: 25 cmsolution And placed in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix. 1 cm
of a solution contains 0.0001 g of titanium.
Sec. 2. (Changed edition, Rev. N 1).
3. ANALYSIS
3.1. The weight of bronze weighing 0.5 g (when the mass fraction of titanium from 0.02 to 0.09%) and 0.1 g (with mass fraction of titanium from 0.5 to 2%) were placed in a glass with a capacity of 250 cm, poured 10 cm
of the mixture of acids to dissolve and dissolve when heated. Then add 10 cm
sulphuric acid diluted 1:1, and is evaporated until a white smoke of sulfuric acid. After cooling, the residue is dissolved in water, transfer the solution into 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 at 410 nm in a cuvette with a thickness of absorbing layer 1 cm. Solution comparison is the solution of the analyzed alloy, drawn through the entire course of the analysis, but without adding hydrogen peroxide.
3.2. Construction of calibration graphs
3.2.1. When the mass fraction of titanium from 0.02 to 0.09%
In a volumetric flask with a capacity of 100 DMconsistently pour 0; 1,0; 2,0; 3,0; 4,0 and 5,0 cm
standard solution B 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, mix and then do as described in claim 3.1.
Solution comparison is the solution, not containing titanium.
3.1.-3.2.1. (Changed edition, Rev. N 1, 2).
3.2.2. When the mass fraction of titanium from 0.5 to 2%
In a volumetric flask with a capacity of 100 cmconsistently placed 0; 1,0; 2,0; 3,0; 4,0 and 5,0 cm
standard solution And titanium, is added to 25 cm
of sulphuric acid (1:4), 5 cm
of phosphoric acid, and 1 cm
of hydrogen peroxide, made up to the mark with water, mix and then do as described in claim 3.1.
Solution comparison is the solution, not containing titanium.
Note. Phosphoric acid is added in the presence of bronze in the iron mask iron (III).
(Added, Rev. N 2).
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of titanium () in percent is calculated according to the formula
where is the mass of titanium, was found in the calibration schedule g;
— the weight of the portion,
4.2. Discrepancies in the results of three parallel definitions should not exceed the values permitted by the divergence (
the rate of convergence), calculated by the formula:
where — mass fraction of titanium in the alloy, %.
(Changed edition, Rev. N 2).
4.3. Discrepancies in the results analysis, 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 calculated by the formulas:
where — mass fraction of titanium in the alloy, %.
4.4. Control of accuracy of analysis results is carried out according to State standard samples of heat-resistant (CR) bronze or supplements method, or comparison of the results obtained by atomic absorption method in accordance with GOST 25086−87.
4.3, 4.4. (Changed edition, Rev. N 2).
THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF TITANIUM WITH DIANTIPYRYLMETHANE
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.
5. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter or spectrophotometer.
Nitric acid GOST 4461−77.
Sulfuric acid GOST 4204−77, diluted 1:1 and 1:4.
Hydrochloric acid by the GOST 3118−77.
Hydrofluoric acid according to GOST 10484−78.
Ascorbic acid, a solution of 100 g/DM.
Ammonia water according to GOST 3760−79 and diluted 1:50.
Silver nitrate according to GOST 1277−75, a solution of 4 g/DM.
Ammonium neccersarily according to GOST 20478−75, a solution of 200 g/DM.
Alum iron ammonium on the other 6−09−5359−87, a solution of 50 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 (conc.), 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.
Titanium-potassium fluoride.
Standard titanium solutions A and B prepared as described in sect.2.
A standard solution of titanium In: 5 cmsolution And placed in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and stirred; prepared on the day of application.
1 cmof the solution contains 0,00002 g of titanium.
Sec. 5. (Changed edition, Rev. N 2).
6. ANALYSIS
6.1 the sample of bronze with a weight of 0.5 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. The residue is cooled, rinse the walls of the Cup with water, is dissolved, the solution was transferred to a beaker with a capacity of 300 cm
and dilute with water to 100 cm
. To the solution was added 2 cm
of a solution of silver nitrate, 10 cm
solution naternicola ammonia and the solution was boiled for 30 min. the Solution was cooled, added with 1 cm
of a solution of iron-ammonium alum, precipitated hydroxide of iron and titanium by ammonia solution and the solution is kept at 50−60 °C to coagulate the precipitate for 30 minutes the Precipitate was filtered off on a medium density filter, a glass and the precipitate washed with hot ammonia solution (1:50). The precipitate is dissolved in 20 cm
of sulphuric acid (1:4) glass, which conducted the deposition, the filter is washed with water and repeating the precipitation of the hydroxide, filtering, dissolving the precipitate and washing of the filter. The solution was 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 — 20 cm(from 0.02 to 0.09%) and 10 cm
(0.5 to 2%) in a volumetric flask with a capacity of 100 cm
and set pH=7−8 with aqueous ammonia in universal indicator paper. Then add 10 cm
of hydrochloric acid, 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 of the solution on a photoelectrocolorimeter with a blue filter (
=400 nm), or on the spectrophotometer at 365 nm in a cuvette with a thickness of the absorbing layer 2 see as a solution comparison solution is used in the control
experience.
6.2. Construction of calibration graphs
In a volumetric flask with a capacity of 100 cmplaced 0; 1,0; 2,0; 4,0; 6,0; 8,0 and 10.0 cm
standard solution B titanium or 0; 1,0; 2,0; 3,0; 4,0 and 5,0 cm
standard solution In titanium, added to 10 cm
of hydrochloric acid and then act as described in clause
Sec. 6. (Changed edition, Rev. N 2).
7. PROCESSING OF THE RESULTS
7.1. 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,
7.2. Discrepancies in the results of three parallel definitions should not exceed the values permitted by the divergence (
the rate of convergence), calculated by the formula:
where — mass fraction of titanium in the alloy, %.
7.3. Discrepancies in the results analysis, obtained in two different laboratories or two of the results of analysis obtained in the same laboratory but under different conditions (the rate of convergence) must not exceed the values calculated by the formulas:
where — mass fraction of titanium in the alloy, %.
7.4. Control of accuracy of analysis results is carried out according to State standard samples of heat-resistant (CR) bronze or by a method of additives or preparation* results obtained by atomic absorption method in accordance with GOST 25086−87.
________________
* The text matches the original. — Note the CODE.
7.5. Method is used when the differences in quality assessment of high-temperature bronzes.
Sec. 7. (Added, Rev. N 2).
