GOST 12223.0-76

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  ГОСТ 12223.0-76

BZ 10−96

STATE STANDARD

OF THE USSR

IRIDIA

METHOD OF SPECTRAL ANALYSIS

GOST 12223.0−76

Edition official

IPK PUBLISHING house of STANDARDS Mocca

546.93 UDC:543.42:006.354 Group B59

STATE STANDARD OF THE USSR

IRIDIUM

Method of spectral analysis

Iridium. Method of spectral analysis

GOST

12223.0−76

AXTU 1709

Date of introduction Q1. Q1J8

This standard applies to iridium and sets the spectral method for the determination of the mass fraction of platinum, palladium, rhodium, ruthenium, osmium, gold, silver, lead, titanium, Nickel, silicon, iron, aluminum, tin, copper, magnesium, and barium.

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

Impurities is determined by the mass fraction of from 0.001 to 0.1% of each, magnesium — from 0.0005 to 0.1%.

(Changed edition, Rev. No. 1, 2).

1. GENERAL REQUIREMENTS

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

(Changed edition, Rev. No. 2).

1.2 — 1.4. (Deleted, Rev. No. 2).

1.5. Sample taking with an accuracy of 0.005 g.

(Added, Rev. No. 1).

Official edition Reprinting is prohibited

© Standards publishing house, 1976 © IPK standards Publishing house, 1997 Reprint with Changes

2. APPARATUS, MATERIALS AND REAGENTS

The spectrograph diffraction large dispersion grating of 600 strokes at 1 mm.

The generator is activated the arc AC and DC.

Geregistreerde microphotometer.

Nine-reliever.

Analytical scale.

Electrodes, carbon, spectral-net with a diameter of 6 mm.

Iridium calibration samples for the determination of impurities.

Photographic plates of the spectral type of ES sensitivity of 3−5 relative units (when the mass fraction of iridium less than 99.9%) and graphic arts film FT-41 according to normative-technical documentation with a sensitivity not less than 0.5 units (for the mass concentration of iridium of 99.9% and above).

Dishes, buxy, desiccators for storage of samples and calibration samples, tweezers for handling dry plates or film.

Stand with cover for electrodes.

Table lathe with a set of tools for sharpening graphite electrodes.

Rectified ethyl alcohol according to GOST 5962 to wipe the sealed jars, weights and all equipment.

Film positive-type M3−3-35 sensitivity of 0.7−1.0 units according to GOST 20945.

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

Standard sample of iridium to verify the correctness of analysis results.

Powder high purity graphite brand.

(Changed edition, Rev. No. 1, 2, 3).

3. PREPARATION FOR ASSAY

3.1. The sample to be analyzed must be in the form of chips, ribbons, wire, powder with particle size not exceeding 0.3 mm. From the analyzed samples are taken weighed up to 100 mg.

3.2. Sample sample standard sample and calibration samples are placed in the crater of a thin-walled graphite electrode (diameter 3−3. 5 mm, depth 1.5−2.0 mm). Protivoelektrodom serve graphite rods with a length of 30−50 mm, sharpened to a truncated cone.

(Changed edition, Rev. No. 2).

3.3. Calibration samples for spectral analysis were prepared by mechanical mixing of powders of impurities (mark H. h, the particle size 0.15 mm) with a powder-based — iridium.

The purity of iridium check spectrographic method under the same conditions under which to conduct analysis. Impurities found in iridia, determined by the method of additives, and found concentration into account when producing the calibration samples.

First, prepare the parent sample from which to select a few samples to check the homogeneity of the distribution of impurities. Then the parent sample is diluted with iridium to obtain a series of seven calibration samples in the concentration range from 0.001 to 0.1%.

Allowed the preparation of calibration samples in a different way.

4. ANALYSIS

4.1. Spectra of the calibration samples, the standard sample and the sample photographed on the spectrograph under the following conditions; the width of the slit is 0.015 mm, the illumination slits being a condenser, an arc gap of 2.5 mm, power DC-DC 10 A, exposure 1 min. Electrode include with the sample as the anode.

In the determination of impurities mass fraction of more than 0.01% each, from analytical samples are taken weighed 100 mg and triturated with 200 mg of graphite powder for 30 min. Spectra of the calibration samples, the standard sample and the samples photographed in the arc of an alternating current power And 7−8, the exposure of 60 s. the Interelectrode distance of 2.5 mm adjust in the process of exhibiting spectra in the image on the intermediate diaphragm. To determine the barium spectra of the calibration samples, the standard sample and samples photographed at a current of 9 A (AC). Exposure 90 s.

The spectra are photographed on high-contrast fine-grain photographic plates of type ES or positive film M3−35.

Photographic plates (films) are within 5 min at a temperature of 20 ° C. Shown photographic plates and films rinsed in water, fixed, washed in running water, dried and photometric.

(Changed edition, Rev. No. 2, 3).

4.2. (Deleted, Rev. No. 2)

5. PROCESSING OF THE RESULTS

5.1. 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.

Determination of the mass fractions of all impurities produced by the method of «three standards».

Analytical lines are recommended for the analysis presented in table 1.

Table 1

Calibration graphs constructed in the coordinates: the abscissa shows the lg calibration samples; y-axis

lg-f. With the help of calibration chart, find the mass fraction of EE

impurities in the analyzed samples.

The final result of the analysis be the arithmetic mean of four parallel measurements, the maximum difference between them does not exceed the admissible discrepancy at a confidence probability P = 0,95.

(Changed edition, Rev. No. 1, 2).

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

Table 2

Mass fraction of impurities, %

Allowable difference, %

convergence

reproducibility

SV. Of 0.0005 to 0.001 incl.

0,001

0,004

0,006

0,01

0,02

0,001

0,005

0,008

0,02

0,03

«To 0.001» 0,003 «

"Of 0.003» to 0.01 «

"Is 0.01» to 0.03 «

"0,03» 0,1 «

(Changed edition, Rev. No. 2)

INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

DEVELOPERS

V. A. Korneev; V. E. Avramov, PhD. tech. Sciences; M. A. Gavrilov; A. K. Dementiev, head of the work; I. I., Karshakevich

2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from 23.07.76 No. 1773

3. The frequency of inspection — 5 years

4. REPLACE GOST 12223−66 in part of sec. 1, 2

5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

6. Limitation of actions taken on the Protocol, the Interstate Council for standardization, Metrology and certification (ICS 2−93)

7. REVISED (June 1997) with Amendments No. 1, 2, 3, approved in January 1982, June 1987-February 1993 (IUS 4−82, 9−87, 9−93)

Editor V. N. Kopysov Technical editor V. N. Prusakova Concealer M. S. Kabasawa DTP A. I. Zolotareva

Ed. No. 021007 from 10.08.95. Put in a set 15.07.97. Signed in print 19.08.97. UK.PECs.l. 0,47. Uch,-ed.l. 0,38. Edition of 110 copies With 811. Zach. 594_

And PC Publishing house of standards, 107076, Moscow, kolodezny per., 14, Typed in Publisher on a PC

The branch office of IPK Publishing house of standards type. «Moscow printer»

Moscow, Lyalin per., 6 PCR No. 080102