摘要
锡矿石是难分解的矿物,共生与伴生元素多,其中的锡钨钼在单一盐酸溶液中易沉淀,准确测定锡矿石中的主次量元素一直是分析技术难点。本文以过氧化钠为熔剂,高温熔融样品,在酒石酸-盐酸-双氧水体系中进行酸化,选用该矿种中仅含有少量的钴作为内标,建立了电感耦合等离子体发射光谱同时测定锡矿石中锡钨钼铜铅锌的分析方法。方法线性范围为0.00～40.0 mg/L;方法检出限为锡10 mg/kg,钨30mg/kg,钼3.3 mg/kg,铜12 mg/kg,铅15 mg/kg,锌40 mg/kg;方法精密度(n=9)小于5.0%,实际样品的测定值与传统化学方法及国家标准方法的测定值吻合较好。本方法采用过氧化钠碱熔锡矿石,溶样彻底,并省去了氢氟酸挥发硅的蒸酸过程,节约了样品处理时间;采用酒石酸-双氧水-盐酸体系溶解熔融物,有利于溶液中的锡钨钼形成稳定的络合物,避免了单纯盐酸体系下产生钨酸、钼酸和锡酸沉淀导致测定结果偏低的问题。
The work involved to accurately determine the major and minor elements in tin ore,which contains large quantities of paragenetic and associated elements is extremely challenging.It is difficult to decomposed tin ore and the Sn,W and Mo are easily precipitated in HC1 solution.A highly efficient analytic method which is capable of simultaneously determining Sn,W and Mo in tin ores by Inductively Coupled Plasma-Atomic Emission Spectrometry （ICP-AES） is reported in this paper.The ore samples are melted with Na2O2 and acidized by mixed tartaric acid,hydrochloric acid and hydrogen peroxide.Co is used as the internal standard element.The linear range of this present method is 0.00-40.0 mg/L,and the detection limits are 10 mg/kg for Sn,30 mg/kg for W,3.3 mg/kg for Mo,12 mg/kg for Cu,15 mg/kg for Pb and 40 mg/kg for Zn,respectively.The relative standard deviation （RSD,n =9） is less than 5.0％.All results of the National Standard Reference Materials determined by this method are consistent with the certified values.The samples can reach complete melting by using Na2 O2 and the step to evaporate the HF acid to remove Si can be avoided,which results in reducing the processing time of samples.The application of mixed tartaric acid-hydrochloric acid-hydrogen peroxide system assists Sn,W and Mo to form stable complexations,which solves the problem of lower determining results due to forming precipitations of tungstenic acid,molybdic acid and stannic acid in HCl solution.
出处
《岩矿测试》
CAS
CSCD
北大核心
2013年第6期887-892,共6页
Rock and Mineral Analysis
基金
河南省国土资源厅科技攻关项目(2011-622-25
2010-61-5)
河南省有色金属地质矿产局科研项目(YSDK2011-10
YSDK2012-03)
关键词
锡矿石
主次量元素
过氧化钠碱熔
电感耦合等离子体发射光谱法
tin ore
major and minor elements
alkali fusion with sodium peroxide
Inductively Coupled Plasma-Atomic Emission Spectrometry
