AFS Determination of Pb, As and Hg in Crude Oil with Microwave Assisted Sample Digestion
摘 要
采用微波消解法,用硝酸-过氧化氢(10+2)溶液作消解剂,以硫脲溶液作为预还原剂,以溶于氢氧化钾溶液中的硼氢化钾溶液作为还原剂,利用原子荧光光谱法测定原油中铅、砷和汞的含量。分析中采用载气及屏蔽气的流量依次为300 mL·min-1及800 mL·min-1。铅、砷和汞的荧光强度与它们的质量浓度依次在2.0~80.0,2.0~100.0,1.0~20.0 μg·L-1之间呈线性关系,方法的检出限(3S/N)依次为0.05,0.05,0.01 mg·kg-1。应用此法对原油样品进行分析,铅、砷和汞的回收率分别在103%~115%,87.5%~92.1%,87.5%~102%之间。
Abstract
AFS was applied to the determination of Pb, As and Hg in crude oil. The sample was digested with mixed solution of HNO3-H2O2(10+2), and thiourea solution was added to the sample solution as pre-reductant and KBH4 solution (dissolved in KOH solution) as reductant. Flow-rates of 300 mL·min-1 for carrier gas and 800 mL·min-1 for shielding gas were taken in the analysis. Linear relationships between values of fluorescence intensity and mass concentration of Pb, As and Hg found were in the ranges of 2.0-80.0, 2.0-100.0 and 1.0-20.0 μg·L-1, with detection limit (3S/N) of 0.05, 0.05 and 0.01 mg·kg-1 respectively. The proposed method was applied to the analysis of samples of crude oil, giving values of recovery in the ranges of 103%-115% for Pb, 87.5%-92.1% for As and 87.5%-102% for Hg.
中图分类号 O657.31
所属栏目 工作简报
基金项目 国家质检总局科技计划项目(2006IK057)
收稿日期 2011/7/18
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备注王豪(1980-),男,浙江宁波人,工程师,从事化工品检验及仪器分析工作。
引用该论文: WANG Hao,WU Bei-lei,CHEN Ping,LIN Zhen-xing,SUN Ni-ni,PAN Yi-long. AFS Determination of Pb, As and Hg in Crude Oil with Microwave Assisted Sample Digestion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(9): 1027~1029
王豪,邬蓓蕾,陈平,林振兴,孙妮妮,潘意隆. 微波消解样品-原子荧光光谱法测定原油中铅、砷和汞含量[J]. 理化检验-化学分册, 2012, 48(9): 1027~1029
被引情况:
【1】刘崇华,周小丽,沈晓銮,黄刚, "微波消解样品-氢化物发生-原子荧光光谱法测定橡胶及其制品中微量汞",理化检验-化学分册 50, 1567-1570(2014)
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参考文献
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【3】梁丽娜,江桂斌.高效液相色谱及其联用技术在汞形态分析中应用[J].分析科学学报, 2002,21(1):89-94.
【4】杨莉丽,高丽珠,张德强.树脂分离-氢化物发生-原子荧光光谱法测定中草药中不同形态的砷[J].光谱学与光谱分析, 2004,24(4):491-494.
【5】王壁.砷的形态和微量分析研究新进展[J].理化检验-化学分册, 2003,38(12):643-643.
【6】翟毓秀,郝林桦.氢化物发生原子荧光光谱法测定食品和饲料中的铅[J].分析化学, 2000,28(4):176-179.
【7】蔡宇春,梁剑锋.用原子荧光法测定食品中总砷的经验介绍[J].分析测试技术与仪器, 2009,15(3):188-190.
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