Determination of trace amounts of iron, nickel, and tin in zircaloys by X-ray fluorescence spectrometry after coprecipitation with hexamethyleneammonium hexamethylenedithiocarbamate.

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A rapid and precise X-ray fluorescence spectrometry is proposed for the determination of the trace amounts of iron, nickel, and tin in zircaloys. A zircaloy sample was dissolved in a mixture of tetrafluoroboric acid and hydrochloric acid, diluted to a definite volume with water. After the addition of 3 cm3 of 1% (R,R)-tartaric acid solution as an auxiliary chelating agent and 50 μg of cobalt as an internal standard to an aliquot (less than 200 μg of tin) of the solution, the pH was adjusted to 2 with ammonia solution and 3 cm3 of 1% hexamethyleneammonium hexamethylenedithiocarbamate (HMA–HMDC) was added. The resulting HMA–HMDC complexes were collected on a membrane filter and dried. The contents of iron, nickel, and tin in zircaloys were calculated by the calibration curves with the ratios of Kα intensities for each element to that for cobalt. The coefficients of variation (5 results for each metal) were 2.16, 0.63, and 1.52% for 10, 10, and 200 μg of iron, nickel, and tin, respectively. The analytical results of iron, nickel, and tin in zircaloy samples by the proposed method agreed with the certified values.
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