电感耦合等离子体质谱法测定富铀矿样中的微量钍
宋茂生,张鑫,柳金良,鄢飞燕,张皓
核工业230研究所,长沙 410007
Determination of trace thorium in uranium-enriched samples by ICP-MS
宋茂生,张鑫,柳金良,鄢飞燕,张皓
Research Institute No.230, CNNC, Changsha 410007, China
摘要:建立电感耦合等离子体质谱(ICP-MS)法测定富铀矿样中微量钍的方法。富铀矿样经Na2O2分解,用乙二胺四乙酸二钠(EDTA-2Na)-三乙醇胺(TEA)-H2O2溶液提取,以Mg(OH)2作载体共沉淀提取液中的过氧化钍,使钍与大部分金属离子和UO22+分离。沉淀用2 mol/L热HNO3溶液溶解,定容后用ICP-MS法测定。该方法消除了样品中高含量铀组分对仪器进样系统的污染。钍的质量浓度在0~100 μg/L范围内具有良好的线性关系,线性相关系数为0.9997,钍的检出限为0.185 μg/L。测定结果的相对标准偏差为2.23%~5.91%(n=6),用该法测定3种国家标准物质,测定值与标准值的相对误差小于4.96%。该法样品分解彻底,铀分离较充分,检测速度快,检出限低,测定结果稳定可靠,适用于富铀矿样中微量钍的测定。
Abstract:A method for the determination of trace thorium in uranium-rich samples by inductively coupled plasma mass spectrometry(ICP-MS) was established. The mineral sample was decomposed by Na2O2 and extracted with EDTA-2Na-TEA-H2O2 solution, and using Mg(OH)2 as the carrier to precipitate thorium dioxide, and thorium was separated from most metal ions including UO22+. The precipitate was dissolved by 2 mol/L hot HNO3 solution, and the thorium was determined by ICP-MS. The method eliminates the contamination of the sample injection system with high levels of uranium in the sample. The mass concentration of thorium had a good linear relation in the range of 0-100 μg/L, and the linear correlation coefficient was 0.9997, the detection limit of thorium was 0.185 μg/L. The relative standard deviation of determination result was 2.23%-5.91%(n=6). Three national standard substances were determined by this method, the relative errors between the determined value and the standard value were less than 4.96%. The samples of this method are thoroughly decomposed, the uranium separation is sufficient, the result is stable and reliable. The method is applicable to the determination of trace thorium in the uranium sample with fast speed, low detection limit.
关键词:钍;铀矿样;过氧化钠;ICP-MS;EDTA-2Na-TEA-H2O2
Keywords:thorium; uranium samples; Na2O2; ICP-MS; EDTA-2Na-TEA-H2O2
本文引用格式:
宋茂生,张鑫,柳金良,等. 电感耦合等离子体质谱法测定富铀矿样中的微量钍[J]. 化学分析计量,2018,27(1):27-30.
SONG M S,ZHANG X,LIU J L,et al. Determination of trace thorium in uranium-enriched samples by ICP-MS[J]. Chemical analysis and meterage,2018,27(1):27-30.
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