破乳诱导萃取-电感耦合等离子体质谱法测定柴油中的锰、铁和铅
Determination of Mn,Fe and Pb in Diesel Oil by EIEB-ICP-MS
摘 要
采用破乳诱导萃取的前处理方法,结合电感耦合等离子体质谱技术(ICP-MS),测定了柴油中的锰、铁和铅元素.首先将样品和表面活性剂溶液(Triton X-114)混合形成稳定的油包水乳液,以硝酸作萃取剂充分萃取柴油中的锰、铁和铅,然后将乳液离心破乳分层,采用ICP-MS内标法测定酸性水相中的锰、铁和铅.3种元素的检出限(3S/N)在0.008~0.083 μg·L-1之间,测定下限(10S/N)在0.027~0.28 μg·L-1之间.应用该方法对柴油中金属元素进行测定,加标回收率在94.9%~106%之间,相对标准偏差(n=6)在0.66%~2.2%之间.
破乳诱导萃取
柴油
金属元素
ICP-MS
Extraction induced by emulsion breaking
Diesel oil
Metallic elements
Abstract
A method of ICP-MS coupled with extraction induced by emulsion breaking (EIES) was applied for determination of manganese,iron and lead in diesel oil. The diesel oil was emulsified with an acid surfactant (Triton X-114) solution in order to form a stable water-in-oil emulsion and then the metallic elements in diesel oil were fully extracted with nitric acid. Further,the emulsion was broken by centrifugation,yielding two separated phases. The metallic elements in the lower acidic aqueous phase were determined by ICP-MS using the internal standard method. The limits of detection (3S/N) and quantification (10S/N) were in the range of 0.008-0.083 μg·L-1 and 0.027-0.28 μg·L-1,respectively. The method was used to detect manganese,iron and lead in diesel oil,giving values of recovery in the range of 94.9%-106% and RSD (n=7) in the range of 0.66%-2.2%.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 浙江省质量技术监督系统重大科研项目(20120102)
收稿日期 2014/7/9
修改稿日期
网络出版日期
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备注贺杨明(1988-),男,江西吉安人,博士研究生,主要研究方向为元素分析.
引用该论文: HE Yang-ming,LIAO Shang-fu,HE Qiao-sang,ZHOU Ying. Determination of Mn,Fe and Pb in Diesel Oil by EIEB-ICP-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(3): 286～288
贺杨明,廖上富,何乔桑,周瑛. 破乳诱导萃取-电感耦合等离子体质谱法测定柴油中的锰、铁和铅[J]. 理化检验－化学分册, 2015, 51(3): 286～288
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参考文献
【1】DOYLE A,TRISTAO M L B,FELCMAN J. Study of fuel insolubles:formationconditions and characterization of copper compounds[J].Fuel,2006,85:2195-2201.
【2】SANT′ANA F W,SANTELLI R E,CASSELLA A R,et al. Optimization of an open-focused microwave oven digestion procedure for determination of metals in diesel oil by inductively coupled plasma optical emission spectrometry[J].J Hazard Mater,2007,149:67-74.
【3】HEILMANN J,BOULYGA S F,HEUMANN K G. Accurate determination of sulfur in gasoline and related fuel samples using isotope dilution ICP-MS with direct sample injection and microwave-assisted digestion[J].Anal Bioanal Chem,2004,380:190-197.
【4】REYES M N M,CAMPOS P C. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers[J].Spectrochim Acta Part B,2005,60:615-624.
【5】MARYUTINA T A,SOIN A V. Novel approach to the elemental analysis of crude and diesel oil[J].Anal Chem,2009,81:5896-5901.
【6】BOBAINA N F,BRUM D M,CASSELLA R J,et al. Application of the extraction induced by emulsion breaking for the determination of chromium and manganese in edible oils by electrothermal atomic absorption spectrometry[J].Talanta,2012,99:104-112.
【7】PEREIRA F M,ZIMPECK R C,BRUM D M,et al. Novel extraction induced by emulsion breaking as a tool for the determination of trace concentrations of Cu,Mn and Ni in biodiesel by electrothermal atomic absorption spectrometry[J].Talanta,2013,117:32-38.
【8】CALDAS R F S,BRUM D M,PAULA C E R,et al. Application of the extraction induced by emulsion breaking for the determination of Cu,Fe and Mn in used lubricating oils by flame atomic absorption spectrometry[J].Talanta,2013,110:21-27.
【9】李石秋,张萍.微波消解-ICP-MS法测定电解二氧化锰中的微量元素[J].化工时刊,2012,26(8):31-33.
【10】张莹,曾丹,柴微波,等.微波消解-电感耦合等离子体质谱法测定粮食中12种重金属元素[J].理化检验-化学分册,2014,50(7):875-878.
【11】曹璨.微波消解-ICP-MS法测定中链甘油三酸酯中铜、铅、铬、镍、锡[J].质谱学报,2014,35(4):341-346.
【12】张江义,王小菊,李国敏,等.微波消解-电感耦合等离子体质谱法同时测定食品中的主、微量元素[J].分析化学,2014,42(11):1706-1709.
【2】SANT′ANA F W,SANTELLI R E,CASSELLA A R,et al. Optimization of an open-focused microwave oven digestion procedure for determination of metals in diesel oil by inductively coupled plasma optical emission spectrometry[J].J Hazard Mater,2007,149:67-74.
【3】HEILMANN J,BOULYGA S F,HEUMANN K G. Accurate determination of sulfur in gasoline and related fuel samples using isotope dilution ICP-MS with direct sample injection and microwave-assisted digestion[J].Anal Bioanal Chem,2004,380:190-197.
【4】REYES M N M,CAMPOS P C. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers[J].Spectrochim Acta Part B,2005,60:615-624.
【5】MARYUTINA T A,SOIN A V. Novel approach to the elemental analysis of crude and diesel oil[J].Anal Chem,2009,81:5896-5901.
【6】BOBAINA N F,BRUM D M,CASSELLA R J,et al. Application of the extraction induced by emulsion breaking for the determination of chromium and manganese in edible oils by electrothermal atomic absorption spectrometry[J].Talanta,2012,99:104-112.
【7】PEREIRA F M,ZIMPECK R C,BRUM D M,et al. Novel extraction induced by emulsion breaking as a tool for the determination of trace concentrations of Cu,Mn and Ni in biodiesel by electrothermal atomic absorption spectrometry[J].Talanta,2013,117:32-38.
【8】CALDAS R F S,BRUM D M,PAULA C E R,et al. Application of the extraction induced by emulsion breaking for the determination of Cu,Fe and Mn in used lubricating oils by flame atomic absorption spectrometry[J].Talanta,2013,110:21-27.
【9】李石秋,张萍.微波消解-ICP-MS法测定电解二氧化锰中的微量元素[J].化工时刊,2012,26(8):31-33.
【10】张莹,曾丹,柴微波,等.微波消解-电感耦合等离子体质谱法测定粮食中12种重金属元素[J].理化检验-化学分册,2014,50(7):875-878.
【11】曹璨.微波消解-ICP-MS法测定中链甘油三酸酯中铜、铅、铬、镍、锡[J].质谱学报,2014,35(4):341-346.
【12】张江义,王小菊,李国敏,等.微波消解-电感耦合等离子体质谱法同时测定食品中的主、微量元素[J].分析化学,2014,42(11):1706-1709.
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