Determination of lead, zinc, copper, arsenic, antimony, bismuth and cadmium in silver concentrate by inductively coupled plasma atomic emission spectrometry after microwave digestion
WEI Ya-juan1,2, WU Xue-ying1,2, JIANG Jing1,2, YE Ling-ling1,2
1. China Certification & Inspection Group Guangxi Co., Ltd., Fangchenggang 538001, China; 2. China Certification &Inspection Group Guangxi Co., Ltd., Fangchenggang Branch Office, Fangchenggang 538001, China
Abstract：The sample was treated by microwave digestion in hydrochloric acid-nitric acid-hydrofluoric acid system. After perchloric acid fuming to dryness, the salts were dissolved with hydrochloric acid. Pb 220.353nm, Zn 206.200nm, Cu 327.393/Cu 324.752nm, As 193.696nm, Sb 206.836nm, Bi 190.171nm and Cd 214.440nm/Cd 226.502nm were selected as the analytical lines. The simultaneous determination method of lead, zinc, copper, arsenic, antimony, bismuth and cadmium in silver concentrate by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The linearity of calibration curves was good for lead, zinc and antimony (0.50%-5.00%), copper and bismuth (0.10%-5.00%), arsenic (0.10%-3.00%) and cadmium (0.050%-0.50%). The linear correlation coefficients (r) were all higher than 0.9999. The detection limits of elements were in range of 0.001%-0.014%. The experimental method was applied for the determination of lead, zinc, copper, arsenic, antimony, bismuth and cadmium in two silver concentrate samples. The relative standard deviations (RSD, n=11) of measured results were between 0.74% and 2.9%. The found results were consistent with those obtained by national standard methods: flame atomic absorption spectrometry (YS/T 445.9-2001) for lead and zinc, flame atomic absorption spectrometry (YS/T 445.2-2001) for copper, hydride generation-atomic fluorescence spectrometry (YS/T 445.3-2001) for arsenic and bismuth, reference of hydride generation-atomic fluorescence spectrometry (YS/T 445.3-2001) for antimony, and atomic absorption spectrometry (YS/T 445.8-2001) for cadmium. The contents of lead, zinc, copper, arsenic, antimony, bismuth and cadmium in two silver concentrate samples were determined according to the experimental method. Meanwhile, the recovery tests were also conducted. The recoveries were between 96% and 105%.
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