锆、钼、钨改性石墨管-石墨炉原子吸收法测定电子级二乙二醇甲醚中铅含量

Zirconium,Molybdenum and Tungsten Modified Graphite Tube-Determination of Lead in Electronic Grade Diethylene Glycol MethylEther by Graphite Furnace Atomic Absorption Spectrometry

分别使用氧氯化锆、钼酸铵、钨酸钠对石墨管进行改性,采用X射线衍射(XRD)、扫描电镜(SEM)对改性前后石墨管进行了表征,通过测定电子级二乙二醇甲醚中铅含量对改性后石墨管的分析性能进行考察。研究结果表明改性后石墨管表面形成了高强度、高熔点的碳化钼、碳化钨和氧化锆,提高了测定的灵敏度与精度。采用氧氯化锆改性石墨管测定电子级二乙二醇甲醚中铅含量,相对标准偏差≤3.21%,线性相关系数为0.9814,加标回收率为98.7%~110.6%;采用钼酸铵改性石墨管测定的相对标准偏差≤2.20%,线性相关系数为0.9994,加标回收率为99.3%~106.4%;采用钨酸钠改性石墨管测定的相对标准偏差≤3.38%;线性相关系数为0.9947,加标回收率为98.5%~106.8%。以钼酸铵改性石墨管的分析性能最好。

In this paper,the graphite tube was modified by zirconium oxychloride,ammonium molybdate and sodium tungstate respectively,and then the graphite tubes before and after modification were characterized by X-ray diffraction(XRD)and scanning electron microscope(SEM).The analytical performance of modified graphite tube was studied through the determination of lead in electronic grade diethylene glycol ether.The research results showed that:The formation of molybdenum carbide,tungsten carbide and zirconium oxide of high strength and high melting point on the surface of graphite tube after modified by ammonium molybdate,zirconyl chloride sodium tungstate could improve the sensitivity and accuracy of determination.The relative standard deviation of the graphite tube modified by zirconium oxychloride was≤3.21%.The linear correlation coefficient was 0.9814,and the recovery rate was 98.7%—110.6%;the relative standard deviation of the graphite tube modified by ammonium molybdate was≤2.20%.The linear correlation coefficient was 0.9994,and the recovery rate was 99.3%—106.4%;the relative standard deviation of the graphite tube modified by sodium tungstate was≤3.38%.The linear correlation coefficient was 0.9947,and the recovery rate was 98.5%—106.8%.The analytical performance of the graphite tube modified by ammonium molybdate was the best.