GOST 12228.1-78

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  ГОСТ 12228.1-78

GOST 12228.1−78 Ruthenium. Method of spectral analysis (with Amendments No. 1, 2, 3)

GOST 12228.1−78

Group B59

INTERSTATE STANDARD

RUTHENIUM

Method of spectral analysis

Ruthenium. Method of spectral analysis

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. Dementiev, I. I., Karshakevich

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 04.07.78 N 1793

Change No. 3 adopted by the Interstate Council for standardization, Metrology and certification (Protocol No. 10 dated 04.10.96)

Was the Technical Secretariat of MGS N 2252

The adoption voted:

3. REPLACE GOST 12228−66 in part of sec. 2

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

5. Limitation of actions taken by Protocol No. 4−93 of the Interstate Council for standardization, Metrology and certification (ICS 4−94)

6. REPRINT (January 1999) with Amendments No. 1, 2, 3, approved in June 1984, may 1989, February 1997 (IUS 10−84, 8−89, 5−97)


This standard establishes a spectral method for the determination of platinum, palladium, gold, rhodium, Nickel, silicon, iron, aluminum, lead, titanium, osmium, tin (with a mass fraction of from 0.001 to 0.1% each), iridium (with a mass fraction of from 0.005 to 0.1%), copper, magnesium, silver, barium (with a mass fraction of from 0.001 to 0.01% each) in Ruthenia.

The method is based on evaporation of metal from the crater of the graphite electrode arc AC and DC currents.

(Changed edition, Rev. N 3).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 22864.

2. APPARATUS, REAGENTS AND SOLUTIONS

The spectrograph diffraction large dispersion grating of 600 strokes at 1 mm or spectrograph with crossed dispersion of the STE-1.

The generator is activated the arc AC and DC currents.

Microphotometer geregistreerde.

Analytical scale.

Machine bench lathe with a set of tools for sharpening graphite electrodes.

Agate mortar with pestle.

Buxy, desiccators for storage of samples and calibration samples, cuvettes and tweezers for handling dry plates or film.

The spectral graphite electrodes-clean, with a diameter of 6 mm.

Samples of the calibration.

Powder graphite brand OS.H.

Photographic plates spectrographic type of ES sensitivity of 5−10 units, or other contrast materials.

The technical rectified ethyl alcohol according to GOST 18300 to wipe the sealed jars, weights and equipment.

Developer and fixer according to GOST 10691.0, GOST 10691.1. Allowed to use other contrast working developer.

Standard sample composition of ruthenium to verify the correctness of analysis results.

(Changed edition, Rev. N 3).

3. PREPARATION FOR ASSAY

3.1. The sample to be analyzed must be in the form of powder with particle size not exceeding 0.3 mm.

From the analyzed samples are taken weighed 100 mg.

Sample sample standard sample and calibration samples are placed press-fit into the crater of the graphite electrode (diameter 3.5−4.0 mm, depth 2−2,5 mm). The counter serve as graphite rods with a length of 30−50 mm, sharpened to a truncated cone.

3.2. The preparation of calibration samples

Calibration samples for the spectral analysis are prepared by mixing powders of impurities (qualifications hç, size 0.15 mm) with a powder-based ruthenium (mass fraction of ruthenium not lower than 99,98%).

The purity of the ruthenium is determined by the spectrographic method under the same conditions under which to conduct analysis. Impurities that are found in the Ruthenia, determined by the method of additives, and found the mass fraction take into account when producing the calibration samples.

First, prepare the basic pattern from which you select a few samples to check the homogeneity of the distribution of impurities. The sample is diluted with ruthenium to receive a series of six calibration samples in the range of mass fraction from 0.001 to 0.1%.

Allowed the preparation of calibration samples by another method ensuring the specified accuracy of the analysis.

3.1, 3.2. (Changed edition, Rev. N 2).

4. ANALYSIS

4.1. Spectra of calibration samples and samples photographed on the spectrograph under the following conditions: the slot width of 0.015 mm, the light slit being a condenser, DC current 10 A, exposure 60 s. the Interelectrode distance of 2.5 mm shall establish and maintain constant throughout the exposure spectra on the image on the intermediate diaphragm. The electrode with the sample is the anode. In the determination of impurities mass fraction of which: Pt, Fe, Ti — more than 0.01%; Pd, Mg, Si — more than 0,003%; Rh, Ni, Pb, Au, Sn — 0.005%; Ag, Cu, Al — more than 0.001%; Ir — more than 0,025% of the analytical samples are taken weighed 100 mg and triturated with 200 mg of graphite powder for 30 min. Spectra of the calibration samples and the samples photographed in the arc of an alternating current power 7−8 And the exposure is 90 s. For the determination of barium spectra of the calibration samples and samples photographed at a current of 7 A, the exposure 45 C. For the determination of osmium analytical samples are taken weighed 400 mg and thoroughly mixed with 400 mg of copper oxide (CuO) for 30 min. Spectra of the calibration samples and the samples photographed in the arc of AC power And, 8−10, exposure 90 s. the Spectra are photographed on high-contrast photographic materials (plates, film). Photographic plates (film) show for 5 min at developer temperature of 20 °C. Shown photographic plates and films rinsed in water, fixed, washed in running water, dried and photometric.

(Changed edition, Rev. N 3).

5. PROCESSING OF THE RESULTS

5.1. For all contaminants, except barium, the «internal standard» are the lines of ruthenium.

When fotomaterialy lines of impurities take into account the background. The intensity of the background subtracted from the intensity of the analytical lines of impurities with the help of characteristic curve.

Mass share of impurities determined by the method of «three standards».

The wavelengths of the analytical lines and «internal standard» are given in table.1.

Table 1

Calibration graphs constructed in the coordinates: on the horizontal axis — (the logarithm of mass fractions of impurities in the calibration samples), and the y — axis (the logarithm of the ratio of the intensity of the impurity line to the line of «internal standard»). With the help of calibration chart, find the mass fraction of impurities in the analyzed samples.

(Changed edition, Rev. N 3).

5.2. Permissible discrepancies in the results of parallel definitions should not exceed the values given in table.2.

Table 2

(Changed edition, Rev. N 2).