Determination of lead in rare earth compound thermal stabilizer used for polyvinyl chloride processing by inductively coupled plasma mass spectrometry
BAO Xiang-chun1,2,3, GAO Li-hong*1,2,3
1. State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization, Baotou 014030, China;2. Ruike National Engineering Research Center of Rare Earth Metallurgy and Function Materials, Baotou 014030, China; 3. Baotou Research Institute of Rare Earths, Baotou 014030, China
Abstract：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 30min. 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 208Pb as the determination isotope. 10.00ng/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 0.50-25.00ng/mL as x-axis and the signal strength ratio of lead to thallium as y-axis. The correlation coefficient was higher than 0.9995. The detection limit of method was 0.06ng/mL, and the low limit of determination was 0.19ng/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%.
包香春, 高立红. 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[J]. 冶金分析, 2018, 38(9): 48-52.
BAO Xiang-chun, GAO Li-hong. Determination of lead in rare earth compound thermal stabilizer used for polyvinyl chloride processing by inductively coupled plasma mass spectrometry. , 2018, 38(9): 48-52.
康洁,李侃社,陈创前.新型稀土热稳定剂的制备及其对PVC热降解反应动力学性能的研究[J].应用化工,2017,46(3):463-467.KANG Jie,LI Kan-she,CHEN Chuang-qian.Preparation of the new heat stabilizers and the kinetics study of thermal degradation on PVC[J].Applied Chemical Industry,2017,46(3):463-467.
[2]
张玉玺,陈明光.稀土复合热稳定剂的产业化研究[J].稀土信息,2016(9):32-34.ZHANG Yu-xi,CHEN Ming-guang.Industrialization research of rare earth compound thermal stabilizer[J].Rare Earth Information,2016(9):32-34.
[3]
杨宇,张巍.我国PVC用稀土类热稳定剂专利技术综述[J].塑料助剂,2015(5):15-19.YANG Yu,ZHANG Wei.Review of patent technology related to rare earth thermal stabilizer for PVC in China[J]. Plastic Additives,2015(5):15-19.
[4]
曹鸿璋.稀土在PVC稳定剂中的应用[M].中国稀土强国之梦,2017:215-220.
[5]
李梅,姜在勇,柳召刚,等.镧铈稀土PVC热稳定剂的制备及性能研究[J].塑料科技,2013,41(1):101-104.LI Mei,JIANG Zai-yong,LIU Zhao-gang,et al.Study on performance of La/Ce rare-earth PVC thermal stabilizer and its preparation[J].Plastic Technology,2013,41(1):101-104.
[6]
刘伟,蔡春平,梁鸣,等.电感耦合等离子体原子发射光谱法测定聚氯乙烯热稳定剂中的金属元素[J].理化检验:化学分册,2009,45(6):698-700.LIU Wei,CAI Chun-ping,LIANG Ming,et al.ICP-AES determination of metal elements in PVC thermal stabilizer[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2009,45(6):698-700.
[7]
贺惠,谢华林.聚氯乙烯复合热稳定剂中铅镉钡的同时测定[J].理化检验:化学分册,2006(3):217-218.HE Hui,XIE Hua-lin.Simultaneous determination of lead,cadmium and barium in polyvinyl chloride compound thermal stabilizer[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2006(3):217-218.
[8]
刘雷,熊金平,冯流星.不同微波消解条件对聚氯乙烯中Cd、Cr、Hg、Pb测定结果的影响[J].北京化工大学学报:自然科学版,2013,40(2):25-30.LIU Lei,XIONG Jin-ping,FENG Liu-xing.The influence of different microwave digestion conditions on the determination of Cd,Cr,Hg and Pb in polyvinyl chloride (PVC)[J].Journal of Beijing University of Chemical Technology:Natural Science,2013,40(2):25-30.
[9]
潘丹杰,徐明雅,张烝彦,等.钢衬F4高压密闭消解在测定粮食及其制品中有害元素铅、镉、汞、砷、铝的应用[J].粮食与饲料工业,2014(7):57-59.PAN Dan-jie,XU Ming-ya,ZHANG Zheng-yan,et al.Steel liner F4 high pressure digestion applications in determination of harmful elements in grain and agricultural products of Pb,Cd,Hg,As and Al[J].Cereal & Feed Industry,2014(7):57-59.
[10]
张瑞仙,崔智勇,王建绣,等.高压罐消解和湿法消解测定食品中铅的比较[J].中国卫生检验杂志,2016(17):2468-2470.ZHANG Rui-xian,CUI Zhi-yong,WANG Jian-xiu,et al.Comparison between high pressure tank digestion and wet digestion in the determination of lead in food[J].Chinese Journal of Health Laboratory Technology,2016(17):2468-2470.
[11]
靳兰兰,王秀季,李会来,等.电感耦合等离子体质谱技术进展及其在冶金分析中的应用[J].冶金分析,2016,36(7):1-14.JIN Lan-lan,WANG Xiu-ji,LI Hui-lai,et al.Progress in inductively coupled plasma mass spectrometry technology and its application in metallurgical analysis[J].Metallurgical Analysis,2016,36(7):1-14.
[12]
黄楚楚,李青,张国霞,等.上海市区大气颗粒物(PM2.5)中铅、镉的分析测定和污染特征研究[J].分析化学,2016,44(7):1047-1052.HUANG Chu-chu,LI Qing,ZHANG Guo-xia,et al.Analysis of pollution characteristics of cadmium and lead in atmospheric particulates (PM2.5) of shanghai downtown[J].Chinese Journal of Analytical Chemistry,2016,44(7):1047-1052.
[13]
葛晶晶,刘洁.电感耦合等离子体质谱法测定高纯锌中7种痕量元素[J].冶金分析,2016,36(9):37-41.GE Jing-jing,LIU Jie.Determination of seven trace elements in high purity zinc by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(9):37-41.
[14]
田衎,孙自杰,周欲敏,等.电感耦合等离子体质谱法分析高纯金属银中痕量杂质元素[J].冶金分析,2016,36(7):51-55.TIAN Kan,SUN Zi-jie,ZHOU Yu-min,et al.Determination of trace impurity elements in high purity metal silver by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(7):51-55.
