GOST 25278.10-82. Alloys and ligatures of rare metals. Methods for the determination of zirconium
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Methods for determination of zirconium in alloys. Photometry
In GOST 25278.10−72 «Alloys and alloys of rare metals» discusses methods of determination of zirconium. The standard establishes establishes the following methods for determination of zirconium:
- spectral (from 0.3 to 3%) for alloys based on niobium and vanadium;
from 0.2 to 5% for alloys (alloys) on the basis of niobium (components of aluminium not more than 20%, vanadium not more than 0.5%, tungsten not exceeding 25%, molybdenum not more than 25%, carbon not more than 0.2%);
from 0.5 to 5% for alloys (ligatures) based on vanadium (components: niobium, not more than 40%, of yttrium is not more than 30%);
from 1 to 5% for alloys (ligatures) based on vanadium, which does not contain niobium;
80 to 90% for binary alloys zirconium-aluminium;
from 5 to 30% for alloys based on niobium containing no aluminum;
from 1 to 30% for alloys based on niobium containing aluminum, and for alloys based on vanadium-containing niobium.
The photometric method for the determination of zirconium in alloys based on niobium
based on the formation of colored complex compounds of zirconium and selenology orange in sulfuric acid 0.2 mol/dm3 solution. The hydrolysis of niobium (base alloy) to prevent the introduction of hydrogen peroxide. Absorption of complexes of niobium, of tungsten and molybdenum with selenology orange take into account, by measuring the total absorption of complexes of niobium, tungsten, molybdenum and zirconium in relation to the other equal aliquots of the sample in which it is added Trilon B, masking only zirconium.
The definition does not interfere up to 2 mg of aluminium, up to 7 mg of yttrium, up to 10 mg of molybdenum 3 mg of tungsten, and up to 50 µg of vanadium in fotometriya solution.
The analysis lead to the following sequence. A portion of the sample-based alloy of niobium with a mass of 0.1 g depending on the carbon content dissolved by heating into a heat-resistant glass and fused in a muffle furnace at a temperature of 800 — 900 °C. After the complete decomposition of a sample of the melt is cooled, taken 10 cm3 of solution in a volumetric flask and measure the optical density of the solution. The mass of zirconium find the calibration schedule.
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Methods for determination of zirconium in alloys. Complexometry and spectrometry
Method for the determination of zirconium in vanadium alloys is based on formation of colored complex compounds of zirconium and selenology orange in sulfuric acid 0.2 mol/dm3 solution. The definition does not interfere up to 10 mg of yttrium and 5 mg of vanadium when the content of zirconium in fotometriya the amount of not less than 25 micrograms.
A portion of the sample placed in a quartz crucible, add 2 to 4 grams of potassium persulphate and fused in a muffle at a temperature of 900 °C to obtain a homogeneous melt. The smelt is dissolved by heating in 36 cm3 of sulphuric acid (1:5), the solution was cooled and transferred to volumetric flask with a capacity of 200 cm3, was adjusted to the mark with water.
To determine zirconium in a volumetric flask with a capacity of 50 cm3 is taken aliquot part of a solution containing 25 — 35 µg of zirconium and diluted to 20 cm3 sulphuric acid 0.5 mol/dm3, pour 1 cm3 of the solution kylinalove orange, bring to the mark with water and mix. After 20 minutes, measure the optical density of the solution on photoelectrocolorimeter at = 536 nm in a cuvette with the thickness of the light absorbing layer 30 mm in relation to the zero solution. The mass of zirconium find the calibration schedule.
Spectral method for the determination of zirconium based on the dependence of the intensity of spectral lines of zirconium from its mass fraction in the analyzed sample in the excitation spectrum in the condensed spark discharge.
A portion of the sample weighing 0.5 g was placed in a quartz crucible and calcined in a muffle until constant mass at 850 °C. the Oxide is removed from the crucible or platinum cups, as specified in clause 5.2.2, and triturated. Weighed on a torsion scale 40 mg of the prepared sample and mix it with vaseline. The resulting mixture is applied with a spatula on a three-electrode with a spherical recess at the end. The electrode with the sample installed in the lower holder tripod. In the upper holder set carbon electrode, sharpened to a convex hemisphere. The index of the scale of the wavelength of the spectrograph is mounted so that a part of the spectrum around 320 nm appeared in the middle of the spectrogram. Intermediate diaphragm on the condenser are selected such as to ensure the normal blackening of analytical lines. Between the electrodes ignite the spark.
Circuit of the generator IG-3 is difficult.
The current in the primary circuit of the transformer — A. 3
The voltage in the primary circuit of the transformer 220 V.
Capacity is 0.1 µf.
The inductance of 0.15 mH.
The auxiliary gap is 2.5 mm.
The analytical gap is 3.5 mm.
Exposure — 15 seconds.
Each of the obtained spectrograms with photoretrieval find the blackening of analytical lines of zirconium.
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