摘要
硫醇甲基锡因其卓越的稳定性、良好的透明性、优异的兼容性和耐候性,目前是聚氯乙烯（PVC）加工过程中效果最好、使用最广泛的一类热稳定剂,其中硫和锡的含量是影响其质量和性能非常重要的指标,因此发展同时测定硫和锡的分析方法具有十分重要的意义。电感耦合等离子体原子发射光谱法（ICP-OES）因其检出限低,线性范围宽,干扰小,可多元素同时分析,样品通量高,已被广泛用于复杂样品的分析。微波消解做样品前处理可大幅缩短消化时间,且样品和试剂的使用量少,相对于传统的敞开消解法,还可减少挥发性元素的损失。我们建立了一种微波辅助酸消解-ICP-OES同时测定硫醇甲基锡中的硫和锡的新方法,该方法简单、快速、准确、绿色、样品用量少。采用DX-181样品,通过与化学分析方法的测试结果相比较,优化了微波辅助酸消解体系和消解时间。在消解体系为HNO3-HCl-HClO4（v/v/v=9∶3∶1）,消解时间为10min的优化条件下,分别用标准加入法和标准曲线法测定了DX-181样品中硫和锡的含量,测定结果无显著性差异,与化学方法测定参考值的相对偏差均小于2%。最后选择标准曲线法测定了元素含量分别为高、中、低的三个样品（DX-181,DX-990,DX-960）,相对偏差小于3%,加标回收率在99%~102%之间,结果令人满意。
Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride （PVC）thermal process-ing due to its excellent stability,good transparency,high compatibility and weather resistance.The content of sulfur and tin sig-nificantly affects its quality and performance,so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin.Inductively coupled plasma atomic emission spectrometry （ICP-OES）has been a powerful analyt-ical tool for a myriad of complex samples owing to its advantages of the low detection limits,rapid and precise determinations o-ver wide dynamic ranges,freedom from chemical inter-element interferences,the high sample throughput and above all,simulta-neous multi-elements analysis.Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion.Hereby,a microwave-assisted acid digestion （MW-AAD）procedure followed by inductively coupled plasma optical emission spectroscopy （ICP-OES）analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide.This method has the advantages of sim-plicity,rapidness,good accuracy,green and less use of samples.Parameters affecting the MW-AAD such as the digestion solu-tion and digestion time were optimized by using a chemical analyzed reference sample （DX-181）to attain tin and sulfur quantita-tive recoveries.HNO3-HCl-HClO4 （v/v/v=9∶3 ∶1）and 10 min were the optimum digestion solution and digestion time,re-spectively.Under optimum conditions,the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181.There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%.Additionally,the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples （DX-181
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
2015年第9期2393-2396,共4页
Spectroscopy and Spectral Analysis
基金
国家自然科学基金项目(21175093)资助
