电感耦合等离子体质谱法测定烟道灰中铟  

Determination of indium in flue dust by inductively coupled plasma mass spectrometry

作　　者：倪文山[1,2,3] 张宏丽 高小飞[1,2,3] 姚明星 肖芳[1,2,3] 毛香菊 NI Wen-shan;ZHANG Hong-li;GAO Xiao-fei;YAO Ming-xing;XIAO Fang;MAO Xiang-ju(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006,China;China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China;Key Laboratory of Evaluation and Multipurpose Utilization of Polymetallic Ores Ministry of Land and Resources,Zhengzhou 450006,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,河南郑州450006 [2]国家非金属矿资源综合利用工程技术研究中心,河南郑州450006 [3]国土资源部多金属矿评价与综合利用重点实验室,河南郑州450006

出　　处：《冶金分析》2018年第3期8-13,共6页Metallurgical Analysis

基　　金：重要矿产和土地资源节约集约综合利用标准研究(2016YFF0201604)

摘　　要：电感耦合等离子体质谱法(ICP-MS)测定了烟道灰中In时,多原子分子离子和同量异位素^(115)Sn的干扰不可忽略。采用HCl、HNO_3、HF和HClO_4溶解烟道灰样品,选择^(115)In为被测同位素,100ng/mL185 Re作为内标,以动能歧视碰撞池(KED)消除多原子分子离子干扰,以数学校正方程消除同量异位素^(115)Sn的干扰,实现了电感耦合等离子体质谱法对烟道灰中In的测定。详细考察了^(115)Sn对^(115)In测定的干扰,结果表明,^(115)Sn对^(115)In的干扰量与Sn的含量呈线性相关,因此得到了对^(115)Sn干扰进行校正的数学校正方程。在测定中,考虑到样品溶液中Sn的含量较高,一般超出了ICP-MS的测定范围,故选择以ICP-AES对Sn进行测定,再采用数学校正方程对其干扰进行校正。分别在标准模式和KED模式下对烟道灰样品中In进行了测定,结果表明,KED模式下In的测定结果与对照值(乙酸丁酯萃取-原子吸收光谱法测定值)基本一致,而标准模式下的测定结果相对偏高;同时试验表明,KED模式下In的背景等效浓度和方法检出限约比标准模式低一个数量级。因此实验选用KED模式进行测定并对其条件进行了优化,最终确定碰撞气流量为4.90mL/min。在选定的实验条件下,In质谱强度与其质量浓度在5~100ng/mL范围内呈良好的线性关系,校准曲线相关系数为0.999 4,方法检出限为0.004 6ng/mL。将实验方法应用于实际烟道灰样品中In的测定,所得结果的相对标准偏差(RSD,n=6)为0.20%~1.3%,加标回收率为98%~102%。During the determination of indium in flue dust by inductively coupled plasma mass spectrometry(ICP-MS),the interference of polyatomic molecular ion and isobar of 115 Sn could not be ignored.The flue dust sample was dissolved with HCl,HNO 3,HF and HClO 4.115 In was selected as testing isotope and 100 ng/mL 185 Re was used as internal standard.The interference of polyatomic molecular ion was eliminated by kinetic energy discrimination collision cell(KED).The interference of isobar of 115 Sn was eliminated by mathematical correction equation.The determination of indium in flue dust by ICP-MS was realized.The interference of 115 Sn with the determination of 115 In was systemically investigated.The results showed that the interference amount of 115 Sn with 115 In was linearly related to the content of Sn.Therefore,the mathematical correction equation for the correction of 115 Sn interference was obtained.The content of Sn in sample solution was relatively high,which usually exceeded the determination range of ICP-MS.Thus ICP-AES was selected for determination of Sn followed by correction of Sn with mathematical correction equation.The content of indium in flue dust sample was determined in standard mode and KED mode,respectively.The results indicated that the determination results of indium in KED mode were basically consistent with the comparison values(the determination results obtained by butyl acetate extraction-atomic absorption spectrometry),while the determination results in standard mode were relatively high.Meanwhile,it was found that the background equivalent concentration of indium and detection limit of method in KED mode were about one order of magnitude lower than those in standard mode.Therefore,the KED mode was employed and its experimental conditions were optimized.The flow rate of collision gas at 4.90 mL/min was selected.Under the selected experimental conditions,the mass spectral intensity showed good linear relationship with the corresponding mass concentration in range of 5-100 ng/mL.The correla

关 键 词：烟道灰 铟 数学校正 动能歧视碰撞池(KED) 电感耦合等离子体质谱法(ICP-MS) 

分 类 号：O657.63[理学—分析化学]