电感耦合等离子体原子发射光谱法测定辛酸铑催化剂中铂钯铅铁铜铝镍
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摘要
准确测定辛酸铑催化剂中杂质元素含量,是判定产品是否合格的重要指标之一。以往常采用直流电弧发射光谱法(摄谱法)进行检测,但测定周期长,且重复性较差。用电感耦合等离子体原子发射光谱法(ICP-AES)测定辛酸铑催化剂中微量杂质元素时,辛酸铑催化剂样品中含有的大量有机组分和铑基体会对测定有严重干扰。实验采用反复滴加硝酸消解样品中有机组分,再用王水溶解盐类,选用合适背景点扣除的方式消除铑基体的干扰,建立了使用ICPAES测定辛酸铑催化剂中0.001%～0.1%(质量分数)Pt、Pd、Pb、Fe、Cu、Al、Ni等7种微量杂质元素的方法。各元素在0.10～10.00μg/mL范围内与其发射强度呈线性关系,相关系数均大于0.9999;方法检出限(μg/mL)为0.075(Pt)、0.0033(Pd)、0.015(Pb)、0.0036(Fe)、0.010(Cu)、0.001(Al)、0.012(Ni)。实验方法用于测定辛酸铑催化剂样品中Pt、Pd、Pb、Fe、Cu、Al、Ni,结果的相对标准偏差为(RSD,n=7)为1.4%～9.6%。按照实验方法测定辛酸铑催化剂中Pt、Pd、Pb、Fe、Cu、Al、Ni,并与直流电弧发射光谱法的测定结果进行比对,结果相一致。
The accurate determination of impurity elements in rhodium octanoate dimer catalyst was one of important indicators to judge whether the product was qualified or not.The common method in the past was direct current arc emission spectrometry(spectrographic method).However,the detection period was long and the repeatability was poor.The determination of trace impurity elements in rhodium octanoate dimer catalyst by inductively coupled plasma atomic emission spectrometry(ICP-AES)was seriously interfered due to the presence of many organic components and rhodium matrix in catalyst sample.The organic components in sample were digested by dropwise adding nitric acid repeatedly.The salts were then dissolved with aqua regia.The interference of rhodium matrix was eliminated by selecting appropriate deduction of background points.Thus,a determination method of seven micro impurities in rhodium octanoate catalyst(including Pt,Pd,Pb,Fe,Cu,Al and Ni with mass fraction of 0.001%-0.1%)by ICP-AES was established.The mass concentration of elements in range of 0.10-10.00μg/mL was linear to the corresponding emission intensity with correlation coefficients higher than 0.999 9.The detection limit(μg/mL)of the method was 0.075(Pt),0.003 3(Pd),0.015(Pb),0.003 6(Fe),0.010(Cu),0.001(Al)and 0.012(Ni).The experimental method was applied for determination of Pt,Pd,Pb,Fe,Cu,Al and Ni in rhodium octanoate dimer catalyst samples.The relative standard deviations(RSD,n=7)of the determination results were between 1.4%and 9.6%.The content of Pt,Pd,Pb,Fe,Cu,Al and Ni in rhodium octanoate dimer catalyst was determined according to the experimental method and the found results were consistent with those obtained by direct current arc emission spectrometry.
The accurate determination of impurity elements in rhodium octanoate dimer catalyst was one of important indicators to judge whether the product was qualified or not.The common method in the past was direct current arc emission spectrometry(spectrographic method).However,the detection period was long and the repeatability was poor.The determination of trace impurity elements in rhodium octanoate dimer catalyst by inductively coupled plasma atomic emission spectrometry(ICP-AES)was seriously interfered due to the presence of many organic components and rhodium matrix in catalyst sample.The organic components in sample were digested by dropwise adding nitric acid repeatedly.The salts were then dissolved with aqua regia.The interference of rhodium matrix was eliminated by selecting appropriate deduction of background points.Thus,a determination method of seven micro impurities in rhodium octanoate catalyst(including Pt,Pd,Pb,Fe,Cu,Al and Ni with mass fraction of 0.001%-0.1%)by ICP-AES was established.The mass concentration of elements in range of 0.10-10.00μg/mL was linear to the corresponding emission intensity with correlation coefficients higher than 0.999 9.The detection limit(μg/mL)of the method was 0.075(Pt),0.003 3(Pd),0.015(Pb),0.003 6(Fe),0.010(Cu),0.001(Al)and 0.012(Ni).The experimental method was applied for determination of Pt,Pd,Pb,Fe,Cu,Al and Ni in rhodium octanoate dimer catalyst samples.The relative standard deviations(RSD,n=7)of the determination results were between 1.4%and 9.6%.The content of Pt,Pd,Pb,Fe,Cu,Al and Ni in rhodium octanoate dimer catalyst was determined according to the experimental method and the found results were consistent with those obtained by direct current arc emission spectrometry.
引文
[1]陈新坤.电感耦合等离子体光谱法原理和应用[M].天津:南开大学出版社,1987:193-235.
[2]辛仁轩.离子体发射光谱分析[M].北京:化学工业出版社,2005:155-171.
[3]龚琦.对电感耦合等离子体发射光谱法中一些问题的认识[J].冶金分析,2018,38(9):26-30.GONG Qi.Understanding of some issues about inductively coupled plasma optical emission spectrometry[J].Metallurgical Analysis,2018,38(9):26-30.
[4]Metody Karadjov,Nikolaya Velitchkova,Olga Veleva,et al.Spectral interferences in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry(ICP-OES)[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2016,119:76-82.
[5]Gazulla M F,Rodrigo M,Ordu1a M,et al.High precision measurement of silicon in aphthas by ICP-OES using isooctane as diluent[J].Talanta,2017,164:563-569.
[6]方卫,侯文明,罗一江,等.ICP-AES法测定RhCl3中微量杂质元素[J].贵金属,2008,29(2):34-37.FANG Wei,HOU Wen-ming,LUO Yi-jiang,et al.Determination of impurities in RhCl3by ICP-AES[J].Precious Metals,2008,29(2):34-37.
[7]李光俐,甘建壮,马媛,等.多元光谱拟合校正电感耦合等离子体原子发射光谱法测定铑粉中19种杂质元素[J].冶金分析,2014,34(5):35-40.LI Guang-li,GAN Jian-zhuang,MA Yuan,et al.Determination of nineteen impurity elements in rhodium powder by inductively coupled plasma atomic emission spectrometry with multi-component spectral fitting correction[J].Metallurgical Analysis,2014,34(5):35-40.
[8]方卫,冯璐,李青,等.ICP-AES法测定三苯基膦氯化铑中的微量杂质[J].贵金属,2016,37(3):56-59.FANG Wei,FENG Lu,LI Qing,et al.Determination of impurities in tris(triphenylphosphine)rhodium(I)chloride by ICP-AES[J].Precious Metals,2017,38(3):66-71.
[9]任传婷,方卫,冯璐,等.ICP-MS法测定纯铑中16个杂质元素[J].贵金属,2017,38(3):66-71.REN Chuan-ting,FANG Wei,FENG Lu,et al.Determination of 16impurities in pure rhodium by ICP-MS[J].Precious Metals,2017,38(3):66-71.
[10]朱利亚,赵忆宁,赵辉,等.微波消解技术应用于难分解贵金属化合物的分析[J].冶金分析,2007,27(12):11-16.ZHU Li-ya,ZHAO Yi-ning,ZHAO Hui,et al.Application of microwave digestion technique to analysis of indissoluble precious metal compounds[J].Metallurgical Analysis,2007,27(12):11-16.
[11]朱利亚,刘云,胡秋芬,等.微波消解技术在难处理贵金属合金PtPdRhIr分析中的研究与应用[J].分析试验室,2005,24(9):63-66.ZHU Li-ya,LIU Yun,HU Qiu-fen,et al.Study and application for microwave-assisted digestion technique for annalysis of Pt Pd Rh Ir in precious metal alloys[J].Chinese Journal of Analysis Laboratory,2005,24(9):63-66.
[2]辛仁轩.离子体发射光谱分析[M].北京:化学工业出版社,2005:155-171.
[3]龚琦.对电感耦合等离子体发射光谱法中一些问题的认识[J].冶金分析,2018,38(9):26-30.GONG Qi.Understanding of some issues about inductively coupled plasma optical emission spectrometry[J].Metallurgical Analysis,2018,38(9):26-30.
[4]Metody Karadjov,Nikolaya Velitchkova,Olga Veleva,et al.Spectral interferences in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry(ICP-OES)[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2016,119:76-82.
[5]Gazulla M F,Rodrigo M,Ordu1a M,et al.High precision measurement of silicon in aphthas by ICP-OES using isooctane as diluent[J].Talanta,2017,164:563-569.
[6]方卫,侯文明,罗一江,等.ICP-AES法测定RhCl3中微量杂质元素[J].贵金属,2008,29(2):34-37.FANG Wei,HOU Wen-ming,LUO Yi-jiang,et al.Determination of impurities in RhCl3by ICP-AES[J].Precious Metals,2008,29(2):34-37.
[7]李光俐,甘建壮,马媛,等.多元光谱拟合校正电感耦合等离子体原子发射光谱法测定铑粉中19种杂质元素[J].冶金分析,2014,34(5):35-40.LI Guang-li,GAN Jian-zhuang,MA Yuan,et al.Determination of nineteen impurity elements in rhodium powder by inductively coupled plasma atomic emission spectrometry with multi-component spectral fitting correction[J].Metallurgical Analysis,2014,34(5):35-40.
[8]方卫,冯璐,李青,等.ICP-AES法测定三苯基膦氯化铑中的微量杂质[J].贵金属,2016,37(3):56-59.FANG Wei,FENG Lu,LI Qing,et al.Determination of impurities in tris(triphenylphosphine)rhodium(I)chloride by ICP-AES[J].Precious Metals,2017,38(3):66-71.
[9]任传婷,方卫,冯璐,等.ICP-MS法测定纯铑中16个杂质元素[J].贵金属,2017,38(3):66-71.REN Chuan-ting,FANG Wei,FENG Lu,et al.Determination of 16impurities in pure rhodium by ICP-MS[J].Precious Metals,2017,38(3):66-71.
[10]朱利亚,赵忆宁,赵辉,等.微波消解技术应用于难分解贵金属化合物的分析[J].冶金分析,2007,27(12):11-16.ZHU Li-ya,ZHAO Yi-ning,ZHAO Hui,et al.Application of microwave digestion technique to analysis of indissoluble precious metal compounds[J].Metallurgical Analysis,2007,27(12):11-16.
[11]朱利亚,刘云,胡秋芬,等.微波消解技术在难处理贵金属合金PtPdRhIr分析中的研究与应用[J].分析试验室,2005,24(9):63-66.ZHU Li-ya,LIU Yun,HU Qiu-fen,et al.Study and application for microwave-assisted digestion technique for annalysis of Pt Pd Rh Ir in precious metal alloys[J].Chinese Journal of Analysis Laboratory,2005,24(9):63-66.