阳极泥中锑测定方法研究  

Research on the determination method of antimony in anode mud

作　　者：关国军 陈永红 芦新根 洪博 葛仲义 Guan Guojun;Chen Yonghong;Lu Xingen;Hong Bo;Ge Zhongyi(Changchun Gold Research Institute Co.,Ltd.;National Quality Inspection and Testing Center for Gold and Silver Product(Changchun))

机构地区：[1]长春黄金研究院有限公司 [2]国家金银及制品质量检验检测中心(长春)

出　　处：《黄金》2023年第8期108-112,共5页Gold

摘　　要：阳极泥样品成分复杂,对锑的准确测定存在干扰。采用硫酸铈滴定法测定阳极泥中锑,利用过氧化氢破坏砷、锑、铋之间复杂的化学反应,锑完全被氧化;硝酸-酒石酸混酸抑制锑的水解,同时辅助溶解样品。如果样品含碳过高,在冒硫酸白烟时逐滴加入硝酸除碳,之后用尿素除硝酸。在滴定过程中使用甲基橙-亚甲基蓝双指示剂,终点颜色变化更明显,判断更准确。本方法测定结果的相对标准偏差为0.16%~0.37%,加标回收率为98.40%~101.20%,准确度和精密度良好,满足分析要求。The composition of anode mud samples is complex,which poses challenges in accurately determining antimony.The cerium sulfate titration method was used to determine antimony in anode mud.Hydrogen peroxide was used to disrupt the complex chemical reactions between arsenic,antimony,and bismuth,ensuring complete oxidation of antimony.Nitric acid-tartaric acid mixed acid was used to suppress the hydrolysis of antimony and assist in sample dissolution.If the sample contains excessive carbon,nitric acid was added dropwise to remove carbon during the emission of white smoke from sulfuric acid,followed by nitrate removal using urea.Methyl orange-methyl blue dual indicator was used during titration for a more distinct color change at the endpoint,ensuring more accurate judgment.The relative standard deviation of the results obtained from this method ranged from 0.16% to 0.37%,with a recovery rate of standard substances ranging from 98.40% to 101.20%.The method demonstrates good accuracy and precision,meeting analytical requirements.

关 键 词：阳极泥 锑 硫酸铈滴定法 过氧化氢 干扰去除 

分 类 号：TD926.3[矿业工程—选矿] O655.2[理学—分析化学]