电感耦合等离子体质谱法测定聚氯乙烯加工用稀土复合热稳定剂中铅  

Determination of lead in rare earth compound thermal stabilizer used for polyvinyl chloride processing by inductively coupled plasma mass spectrometry

作　　者：包香春 高立红[1,2,3] BAO Xiang-chun;GAO Li-hong(State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou 014030,China;Ruike National Engineering Research Center of Rare Earth Metallurgy and Function Materials, Baotou 014030,China;Baotou Research Institute of Rare Earths,Baotou 014030,China)

机构地区：[1]白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]瑞科稀土冶金及功能材料国家工程研究中心,内蒙古包头014030 [3]包头稀土研究院,内蒙古包头014030

出　　处：《冶金分析》2018年第9期48-52,共5页Metallurgical Analysis

摘　　要：稀土复合热稳定剂中含有有机化合物,为确保试样溶解完全,实验采用先灼烧再用混合酸消解的方法对试样进行前处理。实验表明,采用马弗炉于600℃灼烧30min,试样可变为灰白色,再用硝酸-氢氟酸-高氯酸进行消解,以2%(V/V)硝酸为测定介质,以208 Pb作为测定同位素,可实现电感耦合等离子体质谱法(ICP-MS)对聚氯乙烯加工用稀土复合热稳定剂中铅的测定。采用10.00ng/mL铊为内标校正基体效应和信号漂移;在0.50~25.00ng/mL的质量浓度范围内,以铅质量浓度为横坐标,铅与铊内标信号强度的比值为纵坐标绘制校准曲线,其相关系数大于0.999 5。方法检出限为0.06ng/mL,方法测定下限为0.19ng/mL。采用实验方法测定两个聚氯乙烯加工用稀土复合热稳定剂试样中铅的含量,其质量分数分别为1.70和1.20μg/g,其相对标准偏差(n=11)小于10%,加标回收率为96%~105%。Because the rare earth compound thermal stabilizer contained organic compounds,the sample was pretreated by burning and then digested with mixed acids to ensure its complete dissolution.The experiments showed that the sample could change to gray white after burning in muffle furnace at 600℃for 30 min.Then it was digested in nitric acid-hydrofluoric acid-perchloric acid system.Consequently,the determination of lead in rare earth compound thermal stabilizer used for polyvinyl cloride processing was realized by inductively coupled plasma mass spectrometry(ICP-MS)with 2%(V/V)nitric acid as determination medium and 208 Pb as the determination isotope.10.00 ng/mL of thallium was selected as internal standard to correct the matrix effect and signal drift.The calibration curve was plotted with the mass concentration of lead in range of 0.50-25.00 ng/mL as x-axis and the signal strength ratio of lead to thallium as y-axis.The correlation coefficient was higher than 0.999 5.The detection limit of method was 0.06 ng/mL,and the low limit of determination was 0.19 ng/mL.The content of lead in two rare earth compound thermal stabilizer samples used for polyvinyl chloride processing was determined according to the proposed method,and the mass fraction was 1.70 and 1.20μg/g,respectively.The relative standard deviations(RSD,n=11)were less than 10%,and the recoveries were between 96%and 105%.

关 键 词：电感耦合等离子体质谱法(ICP-MS) 稀土复合热稳定剂 铅 聚氯乙烯加工 

分 类 号：O657.63[理学—分析化学] TF031[理学—化学]