FIELD: chemistry.
SUBSTANCE: invention can be used in technological control of electrolyte composition by quantitative X-ray fluorescence analysis of a potassium-containing electrolyte with either calcium, or calcium and magnesium added. A method for preparing samples for quantitative X-ray fluorescence analysis consists in the fact that crystalline samples taken from baths are exposed to a doping procedure followed by heat treating. To this effect, a weighed portion of the ground sample is mixed with a weighed portion of sodium fluoride to transform the sample composition into the high-proportion area, e.g. taken in ratio 1:2 to the sample weight. The mixture is placed into a furnace heated to desired temperature 650-750°C, and kept for 20-40 minutes to solve sodium fluoride in the sample and re-crystallise the sample with the desired phase composition followed by air-cooling. The doped sample is placed in the furnace heated to temperature 420-450°C, and kept there within 15-30 minutes. The doped sample is removed from the furnace, air-cooled with analysing the composition by any of quantitative X-ray fluorescence analysis, and taking into account introduced NaF, the initial sample composition is calculated.
EFFECT: using the doping of the taken samples with additional heat treatment enables producing the samples having the crystalline phases and good phase crystallinity in the sample that is required when using the quantitative X-ray fluorescence analysis.
3 cl, 3 dwg, 2 tbl
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Authors
Dates
2015-02-27—Published
2013-12-19—Filed