微波消解-电感耦合等离子体原子发射光谱法测定一氧化碳助燃剂中贵金属含量
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摘要
采用微波消解技术,使用盐酸、硝酸和氢氟酸对一氧化碳助燃剂进行处理,得到测定样品的水溶液,选择波长265.945 nm和340.458 nm作Pt和Pd的分析线,采用电感耦合等离子体原子发射光谱法测定一氧化碳助燃剂中贵金属的含量。结果表明:Pt、Pd元素校准曲线的线性相关系数均不小于0.999 0,Pt、Pd检出限分别为0.030 mg/L和0.014 mg/L;共存元素Si和Al的存在对Pt和Pd测定结果影响不大;按照本方法测定一氧化碳助燃剂样品中Pt、Pd含量的相对标准偏差(n=6)均小于3%,回收率为97.6%～103.2%。
The CO combustion promoter was treated using mixed acid of HCl,HNO_3 and HF by microwave digestion technique to prepare sample water solution.Pt 265.945 nm and Pd 340.458 nm were selected as the analytical lines,using the determination method of inductively coupled plasma atom emission spectrometry.According to the results,the linear correlation coefficient of the calibration curve of each element was not less than 0.999 0.The detection limits of Pt and Pd were 0.030 mg/L and 0.014 mg/L,respectively.The presence of coexisting elements,Si and Al,had little effect on the determination results of Pt and Pd.According to the method of this experiment,the relative standard deviations(RSD,n=6)of results were less than 3%.The recoveries were between 97.6% and 103.2%.
The CO combustion promoter was treated using mixed acid of HCl,HNO_3 and HF by microwave digestion technique to prepare sample water solution.Pt 265.945 nm and Pd 340.458 nm were selected as the analytical lines,using the determination method of inductively coupled plasma atom emission spectrometry.According to the results,the linear correlation coefficient of the calibration curve of each element was not less than 0.999 0.The detection limits of Pt and Pd were 0.030 mg/L and 0.014 mg/L,respectively.The presence of coexisting elements,Si and Al,had little effect on the determination results of Pt and Pd.According to the method of this experiment,the relative standard deviations(RSD,n=6)of results were less than 3%.The recoveries were between 97.6% and 103.2%.
引文
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[2] 程秉容. 一氧化碳助燃剂中铂分析溶样方法的探讨[J]. 理化检验-化学分册,1995,31(2):88
[3] 周天泽. 原子光谱样品处理技术[M]. 北京:化学工业出版社,2006:41-45
[4] 郭国龙,杨丹丹,王春叶,等. 微波消解-电感耦合等离子体原子发射光谱法测定废脱硝催化剂中钨和钛[J]. 冶金分析,2018,38(1):70-74
[5] Mustafa T,Hayati S,Mustafa S,et al.Microwave and wet digestion procedures for atomic absorption spectrometric determination of trace metals contents of sediment samples[J].Analytical Letters,2004,37(9):1925-1936
[6] Baghalha M,Khosravian H,Mortaheb H,et al.Kinetics of platinum extraction from spent reforming catalysts in aqua-regia solutions[J].Hydrometallurgy,2009,95:247-253
[7] Niemel? M,Pitk?aho S,Ojala S,et al.Microwave-assisted aqua regia digestion for determining platinum,palladium,rhodium and lead in catalyst materials[J].Microchemical Journal,2012,101:75-79
[8] 成春喜,钱胜涛. ICP-OES内标法测定氧化铝基催化剂中的钯含量[J]. 福建分析测试,2016,25(5):42-45
[9] 朱若华,邹洪,贺闰娟. 贵金属元素铂、铑、钯的分析进展[J]. 分析实验室,2004,23(2):82-89
[10] 魏小娟,刘秋香,谢智平,等. 电感耦合等离子体原子发射光谱法测定废钯炭催化剂中钯[J]. 冶金分析,2014,34(11):32-36
[11] 辛仁轩. 等离子发射光谱分析[M]. 北京:化学工业出版社,2005:152-153,212-213
[12] 王艳洁,那广水,王震,等. 检出限的涵义和计算方法[J]. 化学分析计量,2012,21(5):85-88