摘要
高纯五氧化二钒样品在硝酸-氢氟酸(4+1)混合液中经微波消解处理,采用电感耦合等离子体质谱法测定样品溶液中15种杂质元素(钛、硅、铝、铬、镍、铜、铅、砷、磷、铁、锰、钙、镁、钾、钠)的含量。采用内标法消除基体的影响。方法的检出限(3s/k)在0.03~0.89μg·L-1之间。方法的加标回收率在90.0%~113%之间,相对标准偏差(n=8)小于5.0%。五氧化二钒5号样品中8种杂质元素的测定值与石墨炉原子吸收光谱法进行核对,测得结果互相符合。
The sample of vanadium pentoxide was treated with a mixture of HNO3and HF(4+1)by microwave assisted digestion,and contents of 15impurity elements(i.e.Ti,Si,Al,Cr,Ni,Cu,Pb,As,P,Fe,Mn,Ca,Mg,K and Na)in the sample solution were determined by ICP-MS.The matrix interference was eliminated by internal standard method.Detection limits(3s/k)of the method found were in the range of 0.03-0.89μg·L-1.Tests for recovery were made by standard addition method,giving values of recovery in the range of90.0%-113%and RSD′s(n=8)found were less than 5.0%.Contents of 8impurity elements in sample 5#were checked by GF-AAS method,consistent values were obtained.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2014年第6期745-748,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)