Determination of trace silver in uranium-niobium-leadpolymetallic ore by high resolution continuumsource flame atomic absorption spectrometry
GUO Xiao-rui1,2,3, SUN Qi-liang1,2,3, ZHANG Hong-li1,2,3, MAO Xiang-jü1,2,3, NI Wen-shan*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. Key Laboratory for Polymetallic Ores′ Evaluation and Utilization, MLR, Zhengzhou 450006, China; 3. Key Laboratory of Comprehensive Utilization of Gold Resource in Henan Province, Zhengzhou 450006, China
Abstract：The composition of uranium-niobium-lead polymetallic ore was complex. It was beneficial to recycle of silver for accurate and effective determination of trace silver in uranium-niobium-lead polymetallic ore. After the samples were dissolved by HCl-HNO3-HF-HClO4, a determination method of silver was established by high resolution continuum source flame atomic absorption spectrometry (HR-CS-AAS) with HCl(1+4) and 2g/L tartaric acid as test medium and λAg=328.068nm as the analytical line. The instrumental parameters were optimized. The background was corrected by iterative baseline correction (IBC) method. 5 pixels were used as the effective pixel points for the CCD detector. According to the average absorption spectrum of silver and the three-dimensional absorption spectrum of absorbance-wavelength-time, the resolution of CCD detector for silver was 0.0020nm/pixel. The analytical line of λAg=328.068nm was not interfered by the spectral lines of other coexisting elements in the solution in the range of 327.86-328.27nm. Under the optimized experimental conditions, the calibration curve was fitted with the absorbance of silver and its corresponding concentration in the range of 0.40-1.60μg/mL by least square method of quadratic equation, the correlation coefficient was 0.9999. The characteristic concentration was 0.0148μg/mL, and the detection limit of method was 0.0013μg/mL. Compared with the hollow cathode lamp atomic absorption spectrometry (HCL-AAS), the parameters for determination of silver in the sample by HR-CS-AAS have lower detection limit, lower characteristic concentration, and higher absorbance for the standard solution series. The uranium-niobium-lead polymetallic ore samples were determined according to the experimental method. The results were basically consistent with those by inductively coupled plasma mass spectrometry, and the relative standard deviations (RSDs, n=9) were between 0.63% and 3.3%. The spiked recovery test was conducted by addition of silver standard solution to the uranium-niobium-lead polymetallic ore samples according to the experimental method. The recoveries were between 97% and 104%, which met the requirements of the national geological and mineral industry standard DZ/T 0130-2006.
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