GOST 16274.10-77
GOST 16274.10−77 Bismuth. Spectral method of determination of mercury content (with Amendments No. 1, 2, 3)
GOST 16274.10−77
Group B59
STATE STANDARD OF THE USSR
BISMUTH
Spectral method of determination of mercury content
Bismuth.
Spectral method for determination of mercury content
AXTU 1709
Date of introduction 1978−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
PS Poklonsky, F. M. Manji, G. V. Khabarova
2. APPROVED AND promulgated by the Decree of the State Committee of standards of Ministerial Council of the USSR from
3. The frequency of inspection 5 years
4. Introduced for the first time
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Paragraph number section |
| GOST 4658−73 |
Sec. 2 |
| GOST 10691.1−84 |
Sec. 3 |
| GOST 10928−90 |
Sec. 2 |
| GOST 16274.0−77 |
1.1 |
| GOST 16274.8−77 |
4.1 |
| GOST 18300−87 |
Sec. 2 |
6. Resolution of the state standard from
7. REPRINT (July 1997) with Amendments No. 1, 2, 3, approved in January 1983, June 1987, July 1992 (IUS 5−83, 11−87, 10−92)
This standard applies to bismuth brands Ви0000, Ви000 and sets the spectral method for the determination of mercury content with the mercury content of from 5·10to 1·10
%.
The method is based on prior fusion of the sample the sample in the crater of the carbon electrode at 350−400 °C and initiate it in the arc DC.
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 16274.0.
2. APPARATUS, REAGENTS AND SOLUTIONS
The quartz spectrograph medium dispersion type of ISP-30 (complete set).
A constant current source providing a voltage of 200 volts and a current of 20 A.
Vertical tubular furnace for melting the metal in a coal electrode at 300 W (figure).
1 — electrode with the sample; 2 — quartz tube; 3 — the heater 300 W; 4 — furnace body;
5 — pusher; 6 — retainer
The lathe with a set of shaped cutters for sharpening carbon electrodes.
Carbon electrodes, carbon from spectral coals brand C-2 or C-3 with a diameter of 6 mm, forms a «glass» of the following dimensions: head height 17 mm, neck length 4 mm, diameter 2 mm, depth 15 mm of the crater, the crater diameter of 4.5 mm.
Contradicted, one end of which is sharpened to a truncated cone.
Microphotometer any system designed to measure pucherani spectral lines (complete set).
Spectrographic plates of the type I.
The technical rectified ethyl alcohol according to GOST 18300.
Mercury brand P1 according to GOST 4658.
Libra torsione type W, the weighing limit up to 1000 mg.
Sample comparison with a mercury content of 0.1%; prepared by the method of fusing sample of mercury with a metallic bismuth in an iron crucible at a temperature of 350−400 °C under molten paraffin. A series of working samples comparison, which differ from each other in 2−2,5 times, preparing serial dilution of the first sample comparison, bismuth, mercury.
To work at concentrations of 5·10-1·10
% using the method of fractional sample. In the carbon electrodes are placed a calculated sample reference sample with a mercury content of 5·10
% bismuth and mercury.
Bismuth GOST 10928 with a mass fraction of mercury less than 1·10%.
Laboratory autotransformer type CTL-250−2.
Note. Allowed the use of devices with photovoltaic spectra and other spectral instruments, other reagents, materials and photographic plates, generating accuracy metrics defined in this standard.
(Changed edition, Rev. N 1, 2, 3).
3. ANALYSIS
Reheating furnace (see drawing) include the network through an autotransformer and is heated to a temperature of 350−500 °C. the Pusher 5 raised to the upper position and a pair of tweezers mounted in an opening of the furnace carbon electrode with a suspension of sample or reference sample. The pusher together with the electrode lowered to the lower position. The sample is melted in Wren at a temperature of 400 °C in 10−15 s.
Then, the electrode pusher lift up and transferred with tweezers to the metal pad (the stand). The spectra are photographed on the plate of type I when the width of the slit of a spectrograph 0,015 mm. Slit spectrograph covering the two-condenser.
Normalisierung condenser with a focal length of 75 mm set of light source at 100 mm from the slit 316 mm. Evaporation of the sample and the excitation spectrum to produce an arc DC current of 15 A. the exposure Time of 20 s.
(Changed edition, Rev. N 2, 3).
4. PROCESSING OF THE RESULTS
4.1. Three range of samples comparisons and six spectra each of the samples are photographed on a single photographic plate. For analysis using the analytical line of the mercury 253,6 nm. The blackening of the line of mercury and nearby background measured on microphotometer. From pucherani lines and background to the intensity of the line with accounting background are moving with the help of characteristic curve. The calculation of the analysis results produced by the method given in GOST 16274.8.
(Changed edition, Rev. N 1, 3).
4.2. Discrepancies in the results of two parallel measurements () and the results of two tests (
) at a confidence probability of 0.95 should not exceed the values given in the table.
| Mass fraction of mercury, % |
The discrepancy between the results of two parallel definitions % | The discrepancy between the results of two tests, % |
5·10 |
2·10 |
2·10 |
1·10 |
0,3·10 |
0,4·10 |
5·10 |
2·10 |
2·10 |
1·10 |
0,3·10 |
0,4·10 |
Permitted discrepancies for the intermediate mass fraction calculated using linear interpolation or according to the formulas:
where is the arithmetic mean of the results of parallel measurements;
— the arithmetic mean of the results of the two tests.
The analysis result should be the arithmetic mean of two parallel definitions for the three spectrograms, each received on the same photographic plate.
(Changed edition, Rev. N 3).
