GOST 12551.2-82
GOST 12551.2−82 Alloys platinum-copper. Methods of spectral analysis (with Change No. 1)
GOST 12551.2−82
Group B59
STATE STANDARD OF THE USSR
ALLOYS PLATINUM-COPPER
Methods of spectral analysis
Alloys platinum-copper. Methods of spectral analysis
AXTU 1709*
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* Introduced advanced Edit. N 1.
Valid from 01.01.84
to 01.01.89*
_________________________________
* 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, I. G., Sazhin, T. I. Belyaeva, E. B. Safonov
INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
Zam. Minister Vladimir Boroday
APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards, dated 30 September 1982, N 3866
REPLACE GOST 12551−67 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 ICS N 7, 1988
This standard specifies the method of spectral determination of rhodium, iridium, gold, palladium and iron in the platinum-copper alloy (with a mass fraction of rhodium and iridium from 0.02 to 0.20% each, gold and palladium from 0.005 to 0.100% of each of iron and from 0.01 to 0.10%).
The method is based on measuring the intensity of impurity lines in an arc spectrum. Quantitative assessment of concentrations of pollutants are set by calibration with standard samples.
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 22864−83.
(Changed edition, Rev. N 1).
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), provided with water cooling.
Standard samples of the enterprise.
Furnace for melting beads.
Graphite crucibles for melting beads.
Silver GOST 6836−80* brand 999,9.
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* On the territory of the Russian Federation GOST 6836−2002. — Note the manufacturer’s database.
Photographic plates of the spectral type II sensitivity of 10−15 conventional units.
Developer N 1 fixer.
Hydrochloric acid by the GOST 3118−77 and diluted 1:1.
Mixture of nitric and hydrochloric acids with water in the ratio 1:4:10.
(Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
3.1. Samples for analysis must be in the form of strips or chips.
To remove surface contamination, the samples were placed in a glass, pour hydrochloric acid (1:1), boil 2 min, washed with water and dried.
3.2. To obtain Korolkov standard and analyzed samples sample mass 1.6 g (with mass fraction of copper from 2.0 to 3.0%) and 1.5 g (at a mass fraction of copper from 8.0 to 9.0%) two for each is placed in a graphite crucible, is added, respectively, 0.4 or 0.5 g of silver and melt.
Chilled Wren press press or prokovyvayut to 10 mm in diameter, placed in glasses, pour a mixture of acids is heated to weak staining solution, washed with water and dried.
Flattened kinglet serve as electrodes for analysis.
4. ANALYSIS
4.1. Photographing spectra is carried out at a slit width of the spectrograph 0.02 mm, a distance between electrodes of 1.5 mm, a current of 5 A, exposure 30 s. the Wrens are installed in the clips, provided with water cooling.
The spectra photographed using a three-step attenuator on the photographic plate of the type II.
For each standard and test sample receive three spectrograms.
A photographic plate showing within 3 to 6 min at developer temperature of 20 °C, rinsed in water, fixed, washed in running water, dried and photometric.
5. PROCESSING OF THE RESULTS
5.1. Wavelength of analytical spectral lines is 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 |
Rhodium | 365,80 | Platinum |
366,31 |
Palladium | 355,31 | 348,34 | |
Iridium | 269,42 |
267,46 | |
Gold | 267,59 |
267,46 | |
Iron | 259,96 |
267,46 |
5.2. Determination of the mass fraction of the elements are by the method of «three standards» with the objective photoretrieval; the calibration graphs built for each analyzed element. Y-axis delay value difference pucherani lines of impurities and the main substances, and the horizontal axis — 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.
5.3. The convergence of the method is characterized by the relative standard deviation of 0.15.
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).