电感耦合等离子体原子发射光谱法测定二月桂酸二丁基锡中锡
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摘要
准确测定二月桂酸二丁基锡中锡含量,对判定其催干性能具有重要意义。二月桂酸二丁基锡经氧化、分解、硝化有机物质,使有机锡转化为无机锡,再采用电感耦合等离子体原子发射光谱法(ICP-AES)测定二月桂酸二丁基锡中锡。通过筛选分析谱线、合理设置背景扣除位置,避免了光谱干扰;采用基体匹配法配制标准溶液系列并绘制校准曲线可消除基体效应的影响。实验表明。锡质量浓度在0.10～25μg/mL范围内与其发射强度呈线性,相关系数为0.999 9,检出限为0.03%(质量分数)。按照实验方法测定3个二月桂酸二丁基锡样品中锡含量,结果的相对标准偏差(RSD,n=6)小于0.03%,并与氧化还原滴定法的测定结果相吻合。
The accurate determination of tin content in dibutyltin dilaurate was of great significance for evaluating its drying performance.The dibutyltin dilaurate was treated by oxidation,decomposition and nitration of organic substances.The organic tin was converted to the inorganic tin,which was then determined by inductively coupled plasma atomic emission spectrometry.The spectral interference was avoided by selecting analytical lines and properly setting the background deduction position.The influence of matrix effect could be eliminated by plotting the calibration curve and preparing the standard solution series with matrix matching method.The results showed that the mass concentration of tin in range of 0.10-25μg/mL was linear to the emission intensity with correlation coefficient of 0.999 9.Detection limit was 0.03%(mass fraction).The content of tin in three dibutyltin dilaurate samples was determined according to the experimental method.The relative standard deviations(RSD,n=6)of determination results were less than 0.03%.The results were consistent with those obtained by oxidation-reduction titration method.
The accurate determination of tin content in dibutyltin dilaurate was of great significance for evaluating its drying performance.The dibutyltin dilaurate was treated by oxidation,decomposition and nitration of organic substances.The organic tin was converted to the inorganic tin,which was then determined by inductively coupled plasma atomic emission spectrometry.The spectral interference was avoided by selecting analytical lines and properly setting the background deduction position.The influence of matrix effect could be eliminated by plotting the calibration curve and preparing the standard solution series with matrix matching method.The results showed that the mass concentration of tin in range of 0.10-25μg/mL was linear to the emission intensity with correlation coefficient of 0.999 9.Detection limit was 0.03%(mass fraction).The content of tin in three dibutyltin dilaurate samples was determined according to the experimental method.The relative standard deviations(RSD,n=6)of determination results were less than 0.03%.The results were consistent with those obtained by oxidation-reduction titration method.
引文
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[11]王巧,王志萍,孙洪涛.碱熔融-电感耦合等离子体原子发射光谱法测定氧化铟锡烧结混合粉中5种杂质元素[J].分析测试技术与仪器,2018,24(1):47-51.WANG Qiao,WANG Zhi-ping,SUN Hong-tao.Determination of 5 elements in In2O3-SnO2 sintered mix powder by inductively coupled plasma atomic emission spectrometry with alkali-melt[J].Analysis and Testing Technology and Instruments,2018,24(1):47-51.
[12]万晓东,冀克俭,赵华,等.电感耦合等离子体发射光谱法测定稀土发火合金中铁、镁、铜和锌[J].化学分析计量,2017,26(6):75-77,81.WAN Xiao-dong,JI Ke-jian,ZHAO Hua,et al.Determination of iron,magnesium,copper and zinc in rare earth pyrophoric alloy by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage,2017,26(6):75-77,81.
[2]张连春.有机锡热稳定剂在PVC加工中的应用[J].聚氯乙烯,2003,5(4):41-43.ZHANG Lian-chun.Application of organotin heat stabilizer in PVC processing[J].Polyvinyl Chloride,2003,5(4):41-43.
[3]郭睿,吴从华,赵亮.热稳定剂二月桂酸二丁基锡合成工艺改进[J].应用化工,2005,34(6):379-382.GUO Rui,WU Cong-hua,ZHAO Liang.The improvement on synthetic process of heat stabilizer dibutyltin dilaurate[J].Applied Chemical Industry,2005,34(6):379-382.
[4]任友直,张秀梅,张雅娟,等.涂料工业用原材料技术标准手册[M].北京:化学工业出版社,1992:815-817.
[5]徐仲诚,李坚,易达成.二丁基二月桂酸锡中锡含量测定方法的探讨[J].涂料工业,2010,40(4):23-27.XU Zhong-cheng,LI Jian,YI Da-cheng.Discussion on determination of stannum content in dibutyltin dilaurate[J].Paint &Coatings Industry,2010,40(4):23-27.
[6]李延超,李来平,张新,等.电感耦合等离子体原子发射光谱法测定碳化钼催化剂中钼[J].冶金分析,2014,34(11):61-64.LI Yan-chao,LI Lai-ping,ZHANG Xin,et al.Determination of molybdenum in molybdenum by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):61-64.
[7]李延超,林小辉,李来平,等.电感耦合等离子体原子发射光谱法测定TaNb6合金中铌和10种杂质元素[J].冶金分析,2016,36(5):64-68.LI Yan-chao,LIN Xiao-hui,LI Lai-ping,et al.Determination of niobium and ten impurity elements in TaNb6alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(5):64-68.
[8]何志明,吴益青,贺萍.电解脱锡-电感耦合等离子体原子发射光谱法测定镀锡板镀层中铅[J].冶金分析,2016,36(5):39-43.HE Zhi-ming,WU Yi-qing,HE Ping.Determination of lead in tin plating layer by inductively coupled plasma atomic emission spectromertry after electrolytic detinning[J].Metallurgical Analysis,2016,36(5):39-43.
[9]吕琦,沈克,郭芳.电感耦合等离子体原子发射光谱法测定蛭石中4种氧化物[J].冶金分析,2016,36(5):44-48.LQi,SHEN Ke,GUO Fang.Determination of four oxides in verminculite by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(5):44-48.
[10]李延超,李来平,周恺,等.加压氧化钼精矿浸出液中铼的测定[J].分析试验室,2014,33(9):1030-1033.LI Yan-chao,LI lai-ping,ZHOU Kai.Determination of rhenium in leaching solution of molybdenum oxide under pressure[J].Chinese Journal of Analysis Laboratory,2014,33(9):1030-1033.
[11]王巧,王志萍,孙洪涛.碱熔融-电感耦合等离子体原子发射光谱法测定氧化铟锡烧结混合粉中5种杂质元素[J].分析测试技术与仪器,2018,24(1):47-51.WANG Qiao,WANG Zhi-ping,SUN Hong-tao.Determination of 5 elements in In2O3-SnO2 sintered mix powder by inductively coupled plasma atomic emission spectrometry with alkali-melt[J].Analysis and Testing Technology and Instruments,2018,24(1):47-51.
[12]万晓东,冀克俭,赵华,等.电感耦合等离子体发射光谱法测定稀土发火合金中铁、镁、铜和锌[J].化学分析计量,2017,26(6):75-77,81.WAN Xiao-dong,JI Ke-jian,ZHAO Hua,et al.Determination of iron,magnesium,copper and zinc in rare earth pyrophoric alloy by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage,2017,26(6):75-77,81.
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