GOST 12550.2-82
GOST 12550.2−82 Alloys palladium-iridium. Methods of spectral analysis (with Change No. 1)
GOST 12550.2−82
Group B59
INTERSTATE STANDARD
ALLOYS OF PALLADIUM AND IRIDIUM
Methods of spectral analysis
Palladium-iridium alloys. Methods of analysis spectrografic
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, PhD. tech. science; N.And.Timofeyev, Cand. tech. Sciences; G. S. Haak; N. With. Stepanova, N. D. Sergienko, PhD. chem. Sciences; A. A. Osintseva; T. I. Belyaev; E. E. Safonova
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 22.09.82 1982 N 3703
3. INSTEAD 12550−67* in section 3
________________
* Probably a mistake of the original. Should read: GOST 12550−67. — Note the manufacturer’s database.
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
Section number, paragraph |
GOST 3118−77 |
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. The re-release (December 1998) with amendment No. 1, approved in April 1988 (I & C 7−88)
This standard establishes a spectral method for the determination of platinum, rhodium, gold and iron in palladium-iridium alloys (in mass fraction of platinum and rhodium from 0.02 to 0.40% each, gold from 0.01 to 0.20% of iron and from 0.02 to 0.20%) .
The method is based on measuring the intensity of impurity lines in an arc spectrum. Quantification of the mass fraction of impurities 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.
(Added, Rev. N 1).
2. APPARATUS, REAGENTS AND SOLUTIONS
The quartz spectrograph medium dispersion.
Arc generator of alternating current.
The three-stage attenuator.
Microphotometer.
Clips (electrode holders).
Standard samples of the enterprise.
The electrodes are made of spectral pure coal of 6 mm in diameter, sharpened to a hemisphere or a truncated cone with ground diameter of 1.5−2 mm.
Grinding machine carbon electrodes.
Photographic plates of the spectral type II, sensitivity of 10−15 conventional units.
The N developer 1 and fixer.
Hydrochloric acid according to GOST 3118, diluted 1:1.
(Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
Samples for analysis must be in the form of pieces of metal weighing 40−70 g, with a platform size of 300−400 mm, cleaned with a file.
The surface of the samples to remove surface contamination is boiled in hydrochloric acid (1:1) for 3 min, washed with water and dried.
4. ANALYSIS
Spectra photographed at slit width of the spectrograph 0.015 mm, the distance between the electrodes is 1.5 mm, a current of 5 A, exposure of 30 s, through a three-stage attenuator.
Analyzed and standard samples serve as the lower electrodes. As the top electrodes used carbon rods, sharpened to a hemisphere or truncated cone.
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 simultaneous spectrogram.
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, dried and photometric.
(Changed edition, Rev. N 1).
5. PROCESSING OF THE RESULTS
5.1. Wavelength of analytical spectral lines is given in the table.
Define item |
Wavelength of lines of the designated element, nm |
Element comparison | The wavelength of the line item comparisons, nm |
Rhodium |
339,68 | Iridium | 333,42 |
Platinum |
270,24 | 270,46 | |
Iron |
259,84 | 260,82 | |
Gold |
267,59 | 267,36 |
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 element. Y-axis delay value difference pucherani line defined and the base element, and the abscissa shows the values of the logarithms of the concentration of standard samples.
5.2 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).