Preparation and characterization of potassium chloride template nitrogen-sulfur doped microporous carbon material and its application in determination of trace gold in copper concentrates
ZHAN Bing1, LI Sijin2, LIU Shu*2, HONG Xi1, CUI Hezhen1, HOU Xiufeng*1
1. Department of Chemistry, Fudan University, Shanghai 200433, China; 2. Technical Center for Industrial Product and Raw Material Inspection and Testing of Shanghai Customs, Shanghai 200135, China
Abstract：Gold is the valuation element of copper concentrate. The accurate determination of gold content in copper concentrate is of great significance for the comprehensive utilization of imported copper concentrates. A novel nitrogen-sulfur doped microporous carbon material (NS-MC) was prepared by the processes including pyrolysis and activation. The waste boat-fruited sterculia seeds pulp was used as raw material. Potassium chloride was selected as the hard template, and thioacetamide was used as the additive. The prepared NS-MC was employed for the adsorption-ashing separation of gold in the digestion solution of copper concentrate. The determination of trace gold in copper concentrate by inductively coupled plasma mass spectrometry (ICP-MS) was realized. NS-MC was characterized by elemental analysis, infrared spectroscopy, scanning electron microscopy, and nitrogen adsorption-desorption. The results proved that nitrogen and sulfur had been successfully doped into the microporous carbon. The specific surface area of this material was 2 503.34 m2/g, and the average pore diameter was 1.98 nm. The effects of initial pH, initial concentration and adsorption time on the adsorption performance of gold ions were discussed. The results showed that the adsorption reached equilibrium within 90 min under the follow conditions: 25 ℃, initial gold mass concentration of 60 mg/L, and pH=3.0. The equilibrium adsorption capacity for gold ions was 368 mg/g. For the coexisting elements of Cu (II), Fe (III), Ca (II), Mg (II), Zn (II) and Pb (II), the adsorption capacity of NS-MC for gold ions was 5-fold higher, especially 7.4 times higher than that of Cu (II) which had highest content in copper concentrate. The prepared NS-MC exhibited good adsorption selectivity. Three certified reference materials of copper concentrate were determined by the experimental method, and the found results were consistent with the certified values. Three imported copper concentrate samples were determined by the proposed method and standard method (i.e., fire assay-atomic absorption spectrometry in GB/T 3884.2-2012). The measured results of two methods were basically consistent. The relative standard deviations (RSD, n=3) were between 0.90% and 7.1%.
詹兵, 李思瑾, 刘曙, 洪熙, 崔荷珍, 侯秀峰. 氯化钾模板氮、硫掺杂微孔碳材料的制备、表征及其在检测铜精矿中痕量金的应用[J]. 冶金分析, 2021, 41(11): 8-14.
ZHAN Bing, LI Sijin, LIU Shu, HONG Xi, CUI Hezhen, HOU Xiufeng. Preparation and characterization of potassium chloride template nitrogen-sulfur doped microporous carbon material and its application in determination of trace gold in copper concentrates. , 2021, 41(11): 8-14.
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