GOST 12563.2-83
GOST 12563.2−83 Alloys gold-palladium. Method of spectral analysis (with Change No. 1)
GOST 12563.2−83
Group B59
STATE STANDARD OF THE USSR
ALLOYS OF GOLD-PALLADIUM
Method of spectral analysis
Gold-palladium alloys. Method of spectral analysis
GST 17 5350
AXTU 1709*
______________
* Introduced later. Izm. N 1.
Valid from 01.07.84
to 01.07.89*
_________________________________
* Expiration removed by Protocol No. 3−93
The interstate Council for standardization,
Metrology and certification (ICS No. 5/6, 1993). -
Note the manufacturer’s database.
DEVELOPED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
A. A. Kuranov, G. S. HAK, N. With. Stepanova, N. D. Sergienko, T. I. Belyaeva
INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
Member Of The Board Of A. P. Snurnikov
APPROVED AND promulgated by the Decree of the State Committee USSR on standards on March 25, 1983 N 1373
REPLACE GOST 12563−67 in part of sec. 3
The Change N 1, approved and put into effect by the Decree of the USSR State Committee for standards from
Change No. 1 made by the manufacturer of the database in the text IUS N 2, 1989
This standard specifies the spectral method of determination of impurities of platinum, iridium, rhodium, iron and lead into gold-palladium alloys (with a mass fraction of platinum, iridium, rhodium, from 0.01 to 0.20% each of iron from 0.01 to 0.10%, and lead from 0.001 to 0.016%).
The method is based on the translation of alloy into the globule (liquid drop of melt) and measuring the intensity of the impurity lines in the arc spectrum. Quantification of the mass fraction of impurities is set by calibration with standard samples.
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 22864−83.
(Changed edition, Rev. N 1).
1.2. The numerical value of the result of the analysis must end with the digit the same category, and permissible differences.
(Added, Rev. N 1).
2. EQUIPMENT, REAGENTS, SOLUTIONS
The large quartz spectrograph dispersion.
The three-stage attenuator.
Arc generator of alternating current.
Microphotometer.
Electrodes, carbon, made from coal spectralinehandy brand high purity-7.
Standard samples of the enterprise.
Machine bench lathe for sharpening electrodes.
Photographic plates of the spectral type II sensitivity of 10−15 conventional units.
The developer and fixer.
Hydrochloric acid by the GOST 3118−77, diluted 1:1.
(Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
Samples for analysis must be in the form of tape, wire or shavings. To remove surface contamination samples before taking the test portions are boiled in hydrochloric acid (1:1) for 2 min, washed with water and dried.
The electrodes were applied to the spectral coals with a diameter of 6 mm. the Lower electrode is notched with millimeter recess in the end face, in which is placed the sample to be analyzed or of standard sample mass of 0.10−0.15 as an upper electrode apply a charcoal sharpened to a hemisphere or a truncated cone with ground diameter of 1.5−2 mm.
(Changed edition, Rev. N 1).
4. ANALYSIS
The spectra photographed using a three-step attenuator and a width of slit of the spectrograph 0,020−0,025 mm, exposure 40−60 s, a current of 4 A (for alloys with a mass fraction of gold from 70% to 90%) and 6 A (for alloys with a mass fraction of gold from 50 to 70%). The distance between electrodes 2.5 mm is adjusted during the exposure on the intermediate diaphragm. Drum wavelength set at 295 nm.
Together with the analyzed samples on the same plate photographed spectra of standard samples. For each of the analyzed and the standard sample receive three concurrent spectrogram.
A photographic plate at the temperature shown developer of 18−20 °C for 3 min. Shown photographic plate is rinsed in water, fixed, washed in running water, dried and photometric.
(Changed edition, Rev. N 1).
5. PROCESSING OF THE RESULTS
5.1. The wavelengths of the analytical lines given in the table.
The designated element |
Wavelength of lines of the designated element, nm |
Element comparison |
The wavelength of the line item comparisons, nm |
Platinum |
299,80 |
Gold |
319,47 |
« |
265,94 |
The same |
268,87 |
Iridium |
313,33 |
« |
319,47 |
Rhodium |
339,68 |
« |
319,47 |
Iron |
259,84 |
« |
259,00 |
« |
259,94 |
« |
268,87 |
Lead |
280,20 |
« |
268,87 |
5.2. Determination of the mass fraction of the elements are by the method of «three standards» with the objective photoretrieval. The calibration graphs are built for each analyzed element. Y-axis delay value difference pucherani lines and determined the main element, and the abscissa shows the values of the logarithms of the concentration 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.
5.3. The convergence of the method is characterized by the relative standard deviation of 0.15.
The final result of the 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).