Determination of trace and ultratrace arsenic in zirconium oxychloride by inductively coupled plasma atomic emission spectrometry after distillation separation
CUI Qing-xiong,XIE Hong-bing,MAO Yu-ping
1.Yunnan Xinli Nonferrous Metals Co., Ltd., Kunming 650100, China; 2.Kunming Metallurgical Research Institute, Kunming 650031, China
Abstract:A simple and accurate determination method of trace and ultratrace arsenic in zirconium oxychloride (ZrOCl2.8H2O) was proposed. According to the content of arsenic in sample, less than 10 g of sample was put into a simple distillator. After adding certain amount of hydrochloric acid (containing little potassium bromide and ferrous sulfate), the sample was heated and decomposed. The distilled arsenic trichloride was absorbed with cold water. After dilution to constant volume, the content of arsenic in solution was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) under selected instrumental conditions. The response intensity of arsenic was in direct ratio to its concentration in range of 0.0-10.0μg/mL. The correlation coefficient of calibration curve (r) was higher than 0.999 9. The recoveries of standard addition were between 99% and 112%. The relative standard deviation (RSD, n=5) was in range of 0.5%-2.0%. The proposed method was applied to the determination of trace and ultratrace arsenic in zirconium oxychloride. The found results were consistent with those obtained by catalytic polarography or atomic fluorescence spectrometry.
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