GOST 12552.2-77

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  ГОСТ 12552.2-77

GOST 12552.2−77 Alloys, platinum-Nickel. Method of spectral analysis (with Change No. 1)

GOST 12552.2−77

Group B59

STATE STANDARD OF THE USSR

ALLOYS, PLATINUM-NICKEL

Method of spectral analysis

Platinum-nickel alloys. Method of spectral of analysis

AXTU 1709*
_____________
* Introduced advanced Edit. N 1.

Valid from 01.01.1979
to 01.01.1984*
_______________________________
* 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 Sverdlovsk factory on processing of nonferrous metals

Director S. G. Gushchin

Heads: V. G. Levin, V. D. Ponomareva

Performers: M. P. Yufa, N. With. Stepanova, N. And. Chentsova, R. M. Bogdanova

INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

Zam. Minister V. S. Ustinov

The draft all-Union scientific research Institute of standardization (VNIIS)

Director A. V. Gichev

APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR of 27 December 1977 N 3069

REPLACE GOST 12552−67 in part of sec. 3

The Change N 1, approved and put into effect by the Decree of the USSR State Committee for standards from 15.06.88 N 1825 from 01.01.89

Change No. 1 made by the manufacturer of the database in the text IUS N 9, 1988


This standard establishes a spectral method for the determination of iridium, palladium, rhodium, gold and iron (when the mass fraction of iridium and rhodium from 0.02 to 0.20%, palladium and gold from 0.005 to 0.10% and iron from 0.01 to 0.10%).

The method is based on measuring the intensity of impurity lines in an arc spectrum. Quantification of the mass fraction of impurities is set by calibration with the test samples in the form of beads of an alloy of platinum-Nickel-silver.

(Changed edition, Rev. N 1).

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 a digit of the same rank as that of the normalized indicator grade composition.

(Added, Rev. N 1).

2. APPARATUS, REAGENTS AND SOLUTIONS

Quartz spectrograph medium dispersion.

The generator is activated the arc AC.

Microphotometer.

Furnace for melting beads.

Graphite crucibles for melting beads.

Laboratory scales lever according to GOST 24104−80*.
_______________
* On the territory of the Russian Federation GOST 24104−2001. — Note the manufacturer’s database.

Silver brand 999,9 according to GOST 6836−80*.
______________
* On the territory of the Russian Federation GOST 6836−2002. — Note the manufacturer’s database.

The control samples.

Clips (electrode holders) with forced cooling.

Photographic plates of the spectral type II sensitivity of 10−15 conventional units.

Three-step attenuator.

The N developer 1 and fixer.

Hydrochloric acid by the GOST 3118−77.

Nitric acid GOST 4461−77.

A mixture of acids, consisting of one volume of nitric acid, four volumes of hydrochloric acid and ten volumes of water.

(Changed edition, Rev. N 1).

3. PREPARATION FOR ASSAY

3.1. To remove surface contamination, the samples are placed in the cups, pour hydrochloric acid diluted 1:1 was boiled for 2 min, washed with water and dried.

3.2. To obtain beads of the control and analyzed samples weighed in the form of strips or chips weighing 1.6 g (two each) are placed in graphite crucibles, add 0.4 g of silver and is melted.

Chilled Wren press press or prokovyvayut to 10 mm in diameter, placed in glasses, pour a mixture of acids is heated to weak staining solution, washed with water and dried.

Flattened kinglet serve as electrodes for analysis.

4. ANALYSIS

Photographing spectra is produced when the width of the slit of a spectrograph 0.015 mm, the distance between the electrodes of the discharge circuit, wherein in each half-cycle of current is one or two digits, and exposure time 30 s. the Samples are installed in the clips, provided with water cooling.

Spectra of the control and analyzed samples photographed through a three-stage attenuator on a photographic plate SP-11. For each sample three get the spectrum.

Photographic plates showing within 3 min when the temperature of the developer of 18−20 °C.

The shown plate is rinsed in water, fixed, washed thoroughly in running water for 10 min, dried and photometric.

5. PROCESSING OF THE RESULTS

5.1. Wavelength of analytical spectral lines are given in table.1.

Table 1

Mass fraction of impurities determined by the method of «three standards» with the objective photoretrieval. The calibration graphs are built for each analyzed element. Y-axis delay value difference pucherani lines of impurities and the main substances, and the horizontal axis — the values of the logarithm of the mass fraction of control samples.

With the help of calibration curve by the known values of the difference of pochernenija find the mass fraction of impurities in the sample.

(Changed edition, Rev. N 1).

5.2. Permissible relative discrepancy between the results of parallel measurements at a confidence probability of 0.95 should not exceed the values given in table.2.

Table 2