GOST 12562.2-82
GOST 12562.2−82 Alloys gold-platinum. Methods of spectral analysis (with Change No. 1)
GOST 12562.2−82
Group B59
INTERSTATE STANDARD
ALLOYS GOLD-PLATINUM
Methods of spectral analysis
Alloys gold-platinum. Methods of spectral analysis
AXTU 1709
Date of introduction 1984−01−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
DEVELOPERS
A. A. Kuranov, G. S. HAK, N. D. Sergienko, N. With. Stepanov, L. D. Bedrin, T. I. Belyaev, E. E. Safonova
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. REPLACE GOST 12562−67 in part of sec. 3
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
Item number |
GOST 3118−77 |
Sec. 2 |
GOST 22864−83 |
1.1 |
5. Limitation of actions taken by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification (ICS 5−6-93)
6. REPRINT (March 1999) with amendment No. 1, approved in June 1988 (IUS 10−88)
This standard specifies the method of spectral determination of palladium, iridium, rhodium, iron and lead to gold-platinum alloys (in mass proportion of palladium, iridium, rhodium, iron from 0.001 to 0.2% each, and lead from 0.001 to 0.02%).
The method is based on placing the sample of the alloy in the globule (liquid drop of melt), photographing its spectrum in the arc discharge and the measurement of line intensities of impurities. The relationship of the intensity of a spectral line with a mass fraction of the impurity is set by calibration with standard samples.
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 22864.
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.
2. EQUIPMENT, REAGENTS, SOLUTIONS
The spectrograph diffraction large dispersion.
The three-stage attenuator.
Arc generator of alternating current.
Microphotometer.
Standard samples of the enterprise.
Electrodes, carbon, made of spectral pure coals brand-2 or high purity-7−3.
Photographic plates of the spectral type P, a sensitivity of 10−15 conventional units.
Grinding machine carbon electrodes.
Hydrochloric acid according to GOST 3118, diluted 1:1.
The developer and fixer.
(Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
3.1. Samples for analysis must be in the form of tape, wire or shavings with a mass of 2.0 g For the removal of surface contamination, the samples are boiled in hydrochloric acid (1:1) for 3 min, washed with water and dried.
4. ANALYSIS
4.1. The spectra are photographed on the big dispersion spectrograph with slit width 0.02 mm and being the lighting system, the distance between the electrodes is 2.5 mm, current 4 A, the exposure time 40−60 s using a three-step attenuator.
The electrodes were applied to the spectral coals with a diameter of 6 mm. Bottom electrode figure with millimeter recess. In the recess is placed a sample to be analyzed or of standard sample mass of 0.1 g For the upper electrodes used charcoal, sharpened to a hemisphere or a truncated cone with ground diameter of 1.5 mm.
Together with the analyzed samples on the same plate photographed spectra of standard samples analyzed grade alloy.
A photographic plate showing within 3 to 6 min at developer temperature of 20 °C. the Shown plate is rinsed in water, fixed, washed in running water and dried.
5. PROCESSING OF THE RESULTS
5.1. Wavelength of analytical spectral lines are given in table.1.
Table 1
The designated element |
Wavelength of lines of the designated element, nm |
Element comparison |
The wavelength of the line item comparisons, nm |
Palladium |
342,12 |
Gold |
319,47 |
Iridium |
313,33 |
319,47 | |
Rhodium |
339,68 |
319,47 | |
Iron |
259,84 |
259,00 | |
Iron |
259,94 |
268,87 | |
Lead |
280,20 |
268,87 |
Determination of the mass fraction of the elements are by the method of «three standards» with the objective photoretrieval.
Build calibration graphs for each of the designated element on the y-axis delay value difference pucherani line of the element and element comparison, and the abscissa shows the values of the logarithms of the concentrations of standard samples.
With the help of calibration curve by the known values of the difference of pochernenija find the contents of the analyzed element in the sample.
5.2. The convergence of the method is characterized by the relative standard deviation given in table.2.
Table 2
Mass fraction of impurities, % |
The value of standard deviation , % |
From 0.001 to 0.01 |
0,30 |
SV. The 0.01 «to 0.05 |
0,15 |
«To 0.05» to 0.20 |
0,10 |
For the results analysis be the arithmetic mean of three parallel measurements under the condition of
,
where is the greatest result of the parallel measurements;
least the result of the parallel measurements;
— relative standard deviation describing repeatability of measurements;
— the arithmetic mean calculated from parallel measurements (3).