GOST 12554.1-83
GOST 12554.1−83 Alloys of platinum-ruthenium. Method for the determination of ruthenium (Change No. 1)
GOST 12554.1−83
Group B59
STATE STANDARD OF THE USSR
ALLOYS OF PLATINUM-RUTHENIUM
Method for the determination of ruthenium
Platinum-ruthenium alloys. Method for the determination of ruthenium
GST 17 5000
AXTU 1709*
___________________
* Changed the wording, Rev. N 1.
Valid from 01.07.84
to 01.07.89*
_______________________________
* Expiration removed
Protocol N 3−93 Interstate Council
for standardization, Metrology and certification
(IUS No. 5/6, 1993). — Note the manufacturer’s database.
DEVELOPED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
A. A. Kuranov, G. S. HAK, N. With. Stepanova, N. D. Sergienko, T. I. Belyaeva
INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
Member Of The Board Of A. P. Snurnikov
APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards of 25 March 1983 No. 1372
REPLACE GOST 12554−67 in part of sec. 2
The Change N 1, approved and put into effect by the Decree of the USSR State Committee for standards from
Change No. 1 made by the manufacturer of the database in the text IUS N 1, 1989
This standard establishes photocolorimetric method for the determination of ruthenium in platinum-ruthenium alloys (in mass fraction of ruthenium to 12.0%).
The method is based on measuring the light absorption of the colored complex compound of ruthenium with thiourea in hydrochloric acid medium in the presence of platinum.
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 22864−83.
(Changed edition, Rev. N 1).
1.2. The numerical value of the result of the analysis must end with the digit the same category, and permissible differences.
(Added, Rev. N 1).
2. APPARATUS, REAGENTS AND SOLUTIONS
Photoelectrocolorimeter FEK-56M.
Installation for electrolytic dissolution (figure).
1 — glass; 2 — electrolyte solution (6 m solution of hydrochloric acid); 3 — electrodes; 4 — clips (electrode holders)
Electrode holders made of alloy of platinum 25% and iridium.
Transformer.
Laboratory scales General purpose and model according to GOST 24104−80*.
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* On the territory of the Russian Federation GOST 24104−2001. — Note the manufacturer’s database.
Hydrochloric acid by the GOST 3118−77, solutions the concentration of 6 and 0.4 mol/DM.
Thiourea according to GOST 6344−73, solution 1 mol/DM.
Technical ethyl alcohol according to GOST 17299−78.
Volumetric flasks laboratory according to GOST 1770−74, with a capacity of 100, 250 cm.
The glass according to GOST 25336−82 with a capacity of 100, 200 cm.
(Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
The samples analyzed and the standard of the alloy should be in the form of plates with a length of 80 mm, a width of 30−40 mm and a thickness of 0.3 mm. Surface of the plates to remove surface dirt, wipe with alcohol.
As the standard is repeatedly analysed using the gravimetric method, the alloy, similar in content of components to analyze.
Two plates to be analyzed or of standard alloy is weighed, fixed in mounting clips for electrolytic dissolution (see drawing) and immersed in a glass with 200 cmof a solution of concentration of 6 mol/DMof hydrochloric acid. The dissolution of lead with alternating current at a voltage of 12−15 V, current density of 0.65 A/cmfor 20−25 min.
After reconstitution, the current is turned off, Unscrew the plate, washed with water, dried and weighed.
The solutions were analyzed and the standard of alloy transferred to volumetric flasks with a capacity of 250 cm, was adjusted to the mark with water and mix thoroughly.
The mass of the alloy () 1 cmmain solution is calculated by the formula
,
where is the mass of the plates to dissolve, g;
— the mass of the plate after dissolution,
Major solutions to be analyzed and the standard alloy is prepared in 100 cmof dilute solutions with a content of alloy 1·10g/cm. Necessary aliquot part of the basic solution () is calculated by the formula
,
where is the mass of the alloy in 1 cmcore solution,
Designed aliquot part of the basic solution is placed in a volumetric flask with a capacity of 100 cm, adjusted to the mark with a solution of concentration 0.4 mol/DMhydrochloric acid and mix thoroughly.
(Changed edition, Rev. N 1).
4. ANALYSIS
In glasses with a capacity of 100 cmtaking aliquots of 20 cmof dilute solutions to be analyzed and the standard of alloy (which corresponds to the mass of alloy 0.02 g).
In these solutions, add 40 cmof a solution of concentration 0.4 mol/DMhydrochloric acid, 10 cmof a solution of concentration 1 mol/lof thiourea and heated in a water bath at 50−60 °C for 15 min.
The chilled solutions are transferred to volumetric flasks with a capacity of 100 cm, adjusted to the mark with a solution of concentration 0.4 mol/DMhydrochloric acid, mix thoroughly and measure the optical density on the photoelectrocolorimeter at a wavelength of 600 nm in cuvettes with the thickness of the absorbing layer of 5−10 mm compared to the zero solution, which is solution of concentration 0.4 mol/DMhydrochloric acid.
(Changed edition, Rev. N 1).
5. PROCESSING OF THE RESULTS
5.1. Mass fraction of ruthenium () in percent is calculated by the formula
,
where a — optical density of the solution of the analyzed alloy;
— optical density of the solution of standard alloy;
— mass fraction of ruthenium in the solution of standard alloy, %.
5.2. The difference between the highest and lowest results of parallel measurements at a confidence probability of 0.95 does not exceed the absolute value of the admitted differences of 0.20%.
The difference between two results of analysis of the same sample obtained in different laboratories, should not exceed the absolute value of the permissible divergence of 0.32%.
(Changed edition, Rev. N 1).
5.3. Accuracy control in the determination of the mass fraction of ruthenium is playing its mass fraction in the artificial mixtures the chemical composition close to the composition of the analyzed alloy, drawn through the entire course of the analysis.
The sample analysis results are considered accurate if the absolute difference between the largest and smallest values of the mass fraction of ruthenium in synthetic mixtures does not exceed 0,16%.
(Added, Rev. N 1).