GOST 12228.2-78
GOST 12228.2−78 Ruthenium. Method for the determination of volatile impurities (with Change No. 1)
GOST 12228.2−78
Group B59
INTERSTATE STANDARD
RUTHENIUM
Method for the determination of volatile impurities
Ruthenium.
Method of volatile additions determination
AXTU 1709
Date of introduction 1980−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
A. K., Dementieva, I., Karshakevich
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. REPLACE GOST 12228−66 in section 3
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Section number, paragraph |
| GOST 6563−75 | 2 |
| GOST 8050−85 | 2 |
| GOST 9147−80 | 2 |
| GOST 22864−83 | 1.1 |
| GOST 25336−82 | 2 |
5. Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization, Metrology and certification (ICS 4−94)
6. The re-release (January, 1999) with amendment No. 1, approved in may 1989 (IUS 8−89)
This standard specifies a gravimetric method for the determination of volatile impurities.
The method is based on determining the content of volatile impurities by difference the mass of the sample analyzed before calcination and after calcination.
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 22864.
2. EQUIPMENT
Furnace for calcination at 1200 °C.
Platinum crucibles with lids N 100−7 according to GOST 6563.
From Kipp apparatus for generating hydrogen.
Crucibles porcelain low N 4 according to GOST 9147.
Analytical scale.
Desiccator, according to GOST 25336.
Gaseous carbon dioxide according to GOST 8050.
(Changed edition, Rev. N 1).
3. ANALYSIS
3.1. Clean platinum crucible placed in a porcelain crucible and calcined in a furnace for 10 min at 900−1000 °C in a current of hydrogen.
After calcination, the crucible is removed from furnace without turning off the current of hydrogen. Off the current of carbon dioxide and 3−5 with shut off the current of hydrogen, after 10−15 minutes the crucible was transferred to a desiccator, cooled to a temperature of (23±4) °C and determine the mass of the crucible. After that it is weighed 5.0 g of the analyzed metal.
The crucible with the metal cover, placed in a porcelain crucible and calcined for 20−25 min at 900−1000 °C in a current of hydrogen. After calcination porcelain crucible with platinum are removed from the oven without interrupting the current of hydrogen, turn on the flow of carbon dioxide and 3−5 with shut off the current of hydrogen, to extinguish the flame, and again turn on the flow of hydrogen. Cool platinum crucible with the analyzed metal in a current of carbon dioxide and hydrogen to a temperature of (23±4) °C, after which it is transferred into the desiccator. A platinum crucible is weighed on an analytical balance. After weighing, the crucible is again placed in a porcelain crucible and calcined under the same conditions for 10−15 min Platinum crucible after cooling is again weighed. This operation is repeated until obtaining constant weight of the platinum crucible.
Platinum crucible after calcination and between subsequent operations are stored in a desiccator.
The difference between the mass of the crucible with the metal before calcination and after calcination and reconstruction gives the mass of volatile impurities in the sample.
(Changed edition, Rev. N 1).
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of volatile impurities () in percent is calculated by the formula
where the difference in mass of the crucible with the metal before calcination and after calcination and recovery, g;
— weight of metal,
4.2. Allowable absolute differences between the parallel results should not exceed 0,005% for the mass concentration of volatile impurities to 0.02% and 0.01% for the mass concentration of volatile impurities from 0.02 to 0.05%.
