GOST 12227.1-76
GOST 12227.1−76 Rhodium. Gravimetric method for determination of loss of mass on ignition (with Amendments No. 1, 2, 3)
GOST 12227.1−76
Group B59
STATE STANDARD OF THE USSR
RHODIUM
Gravimetric method for determination of loss on heating
Rodium. Gravimetric method for determination of mass loss on ignition*
AXTU 1709**
________________
* The name of the standard. Changed the wording, Rev. N 2, 3.
** Added, Rev. N 2.
Date of introduction 1978−01−01
The decision of the State Committee of standards of Ministerial Council of the USSR from July 23, 1976 N 1774, the validity period is set from
_______________
* Expiration removed Protocol from MGS
REPLACE GOST 12227−66 in part of sec. 3
MADE: the Change in N 1, approved and put into effect Постановлениеv of Gosstandart of the USSR dated
Change N 1, 2, 3 are made by the manufacturer of the database in the text IUS N 4, 1982; IUS N 10, 1987; IUS N 9, 1993
This standard applies to rhodium and sets gravimetric method for determination of loss of mass on ignition.
The method is based on determining the mass fraction of volatile impurities by difference the mass of the sample analyzed before calcination and after calcination.
(Changed edition, Rev. N 2, 3).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 22864−83.
(Changed edition, Rev. N 2).
2. APPARATUS, MATERIALS AND REAGENTS
Furnace for calcination at temperatures up to 1200 °C.
Platinum crucibles N 100−7 according to GOST 6563−75.
From Kipp apparatus for generating hydrogen.
Gaseous carbon dioxide according to GOST 8050−85.
Crucibles porcelain No. 4, GOST 9147−80.
Sulfuric acid according to GOST 4204−77.
Analytical scale.
Desiccator, according to GOST 25336−82.
Marble.
(Changed edition, Rev. N 1, 2, 3).
3. ANALYSIS
3.1. Clean platinum crucible placed in a porcelain crucible, calcined in a furnace for 10 min at 900−1000 °C in a current of hydrogen. After calcination, the crucible is removed from furnace and cooled in a current of carbon dioxide for 5−10 min, then transferred to desiccator, cooled and weighed on an analytical balance. After that it is weighed 5.0 g of the analyzed metal.
The crucible with metal and placed in a porcelain crucible and calcined for 20−25 min at 900−1000 °C in a current of hydrogen. After calcination the platinum crucible is removed from furnace without turning off the current of hydrogen. Include current of carbon dioxide and 3−5 with shut off the current of hydrogen. Cool platinum crucible in a current of carbon dioxide 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.
The difference between the mass of the crucible with the metal before calcination and after calcination and reconstruction gives the mass loss during annealing in the sample.
(Changed edition, Rev. N 1, 2, 3).
3.2. Before analysis it is necessary to test the apparatus for leaks Kippa and hydrogen purity after displacement of air from the apparatus Kippa current of hydrogen.
4. PROCESSING OF THE RESULTS
4.1. The mass fraction of the mass loss on ignition () 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. Permissible differences between results of the analysis should not exceed 0,005% for the mass concentration of the mass loss during annealing up to 0.02% and 0.01% when the mass fraction of loss on heating from 0.02 to 0.05%.
4.1, 4.2. (Changed edition, Rev. N 2, 3).
The electronic text of the document
prepared by JSC «Code» and checked by:
the official publication of the
M.: Publishing house of standards, 1976
