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GOST 12224.1-78

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

GOST 12224.1−78 Osmium. Chemical-spectral method of analysis (with Amendments No. 1, 2, 3)


GOST 12224.1−78

Group B59


INTERSTATE STANDARD

OSMIUM

Chemical-spectral method of analysis

Osmimum. Chemical-spectral method of 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., Dementieva, I., Karshakevich

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on standards 04.07.78 N 1794

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 2249

The adoption voted:

   
The name of the state
The name of the national authority for standardization
The Republic Of Azerbaijan
Azgosstandart
The Republic Of Belarus
Gosstandart Of Belarus
The Republic Of Kazakhstan
Gosstandart Of The Republic Of Kazakhstan
The Republic Of Moldova
Moldovastandart
Russian Federation
Gosstandart Of Russia

3. REPLACE GOST 12224−66 in part of sec. 2

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced Section number, paragraph
GOST 4328−77 2
GOST 6563−75 2
GOST 9147−80 2
GOST 10691.0−84 2
GOST 10691.1−84 2
GOST 18300−87 2
GOST 22864−83 1.1
THAT 6−17−647−80 2

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 specifies the chemical-spectral method of determination of platinum, iridium, iron, Nickel, ruthenium (when the mass fraction of from 0.001 to 0.02% of each), palladium, rhodium, gold, silver, copper, silicon, barium, sodium, aluminum (with a mass fraction of from 0.0005 to 0.02% of each), magnesium (with a mass fraction of from 0.0001 to 0.004%) in osmium.

The method is based on the Stripping of osmium in the tetroxide and the evaporation residue, mixed with graphite powder from the crater of the graphite electrode arc AC.

(Changed edition, Rev. N 3).

1. GENERAL REQUIREMENTS

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

(Changed edition, Rev. N 1).

2. APPARATUS, REAGENTS AND SOLUTIONS


Tubular electric furnace at 1000 °C.

The vacuum pump.

The quartz spectrograph medium dispersion (like ISP-30).

Trehlistnyj glass spectrograph (ISP-51 with a camera 270 mm).

Spectrograph with crossed dispersion, STE-1 (can be used instead of the first two for simultaneous detection of ultraviolet and visible region of the spectrum).

The generator is activated the arc AC.

Microphotometer geregistreerde.

Flask Bunsen.

Pumps platinum according to GOST 6563.

Pumps porcelain N 3 according to GOST 9147.

Analytical scale.

Agate mortar with pestle.

Spatula made of organic glass and a paint brush to extract residue from the boat after the distillation of osmium.

Buxy, desiccators for storage of samples and calibration samples; cell and tweezers for the treatment of photographic films or photographic plates.

Powder high purity graphite brand.

The spectral graphite electrodes-pure grades p-3, p-2, with a diameter of 6 mm.

Samples of the calibration.

Rectified ethyl alcohol technical GOST 18300 to wipe the sealed jars, weights and equipment.

Phototechnical film «Mikrat-200» and film positive MZ-35 on the other 6−17−647 or photographic plates of the spectral type of ES the relative sensitivity of 5−10 units, and «pangram».

Sodium hydroxide according to GOST 4328, a solution of 2.5 mol/DMГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3).

The flask Drexel with a capacity of 500 cmГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3).

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

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

Section 2. (Changed edition, Rev. N 1, 2).

3. PREPARATION FOR ASSAY

3.1. Metal weight 3.0 g was placed in a platinum boat, inserted in a porcelain boat and placed in a tubular electric furnace. One end quartz tube electric furnace remains open, and the other is hermetically connected with a Bunsen flask, the flask Drexel and vacuum line.

In a flask Bunsen poured 500 ml, and the flask Drexel 250 cmГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3)of sodium hydroxide solution, turn on the furnace and the system connected to vacuum lines. The furnace is gradually heated to 600 °C and held at this temperature for 1.5−2 h. Then a solution of sodium osmate from the flask Bunsen decanted into another flask, and the flask Bunsen poured fresh solution of sodium hydroxide and heating was continued. If within 30 minutes of the alkaline solution is not colored, oxidation and Stripping of osmium considered complete. The boat is removed from the furnace and cooled.

(Changed edition, Rev. N 1, 2).

3.2. The platinum boat with the rest placed 50 mg of graphite powder. The balance together with graphite powder carefully extracted from a platinum boat in an agate mortar, add graphite powder to 300 mg, triturated for 30 min and 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.

3.3. Calibration samples for the spectral analysis are prepared by mixing powders of impurities (qualifications hç particle size of 0.15 mm), with graphite powder. First, prepare the basic pattern from which you select a few samples to check the homogeneity of the distribution of impurities. The sample diluted with graphite powder to obtain a series of six samples in the range of a mass fraction of from 0.0001 to 0.2%.

Allowed the preparation of calibration samples in a different way.

3.2, 3.3. (Changed edition, Rev. N 2).

4. ANALYSIS

4.1. Spectra of the calibration samples, the standard sample and samples photographed on the coupled spectrographs under the following conditions: the width of the slit of the quartz spectrograph of 0.015 mm, the width of the slit of a glass spectrograph 0.005 mm; illumination slit being a condenser, an arc gap of 2.5 mm, the current strength of 6.5−7 A, exposition 60 s.

The ultraviolet portion of the spectrum photographed on the quartz spectrograph to a positive film type MZ-35 or a photographic plate of the type ES.

The visible portion of the spectrum photographed on the glass spectrograph on phototechnical film «Mikrat-200» or a photographic plate of the type «pangram». Photographic film (photographic plates) are within 5 min at a 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 1, 2, 3).

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

The wavelengths of the analytical lines given in table.1.

Table 1

   
The designated element
Wavelength of analytical lines, nm
Sodium 588,99
Barium 493,40
Palladium 342,12
Nickel 341,47
Rhodium 339,68
Silver 328,06
Copper 327,39;
324,75
Aluminium 309,27
Silicon 288,15
Magnesium 285,21
Gold 267,59
Iridium 266,47
Platinum 265,94
Iron 259,95
Ruthenium 287,49;
343,67



The calibration graphs are built in coordinates ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3), the abscissa shows the delay ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3)(the logarithm of the mass fraction of the calibration samples), y-axis ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3)(the logarithm of the ratio of the intensity of impurity lines to the background). For the calibration chart to find the mass fraction of impurities in the analyzed samples.

(Changed edition, Rev. N 2, 3).

5.2. Mass fraction of impurities (ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3)) in percent is calculated by the formula

ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3),


where ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3) — mass fraction of the element in graphite powder, %;

ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3) — mass analyze of graphite powder mg;

ГОСТ 12224.1-78 Осмий. Химико-спектральный метод анализа (с Изменениями N 1, 2, 3) — weight of sample, mg.

5.3. 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
From 0.0005 to 0.001 incl. 0,001
0,001
SV. 0,001 «0,003 « 0,004
0,005
«Of 0.003» to 0.01 « 0,006
0,008
«Is 0.01» to 0.03 « 0,01
0,02
«0,03» 0,1 « 0,02
0,03

5.2, 5.3. (Changed edition, Rev. N 2).