电感耦合等离子体原子发射光谱法测定五氧化二钒中19种杂质元素

采用盐酸消解五氧化二钒样品及其中所含可溶性杂质,再以无水碳酸钾与硼酸高温熔融不可溶性杂质,然后以盐酸溶解熔块,合并溶液后以用电感耦合等离子体原子发射光谱法测定杂质元素铌、锆、钛、钨、硅、铝、钼、钴、铬、镍、铜、铅、镉、砷、磷、铁、锰、钙和镁的含量。试验了基体元素和共存元素对测定的干扰,优化各元素的分析谱线,运用同步背景校正消除基体影响。19种元素的检出限在10～225μg.L-1之间,背景等效浓度在5～150μg.L-1之间。方法用于分析五氧化二钒样品,测定结果与其它化学分析方法测定值一致;分析五氧化二钒标准样品(GSBH 42015-96)的测定值与标准值相一致。

ICP-AES Determination of 19 Impurity Elements in Vanadium Pentoxide

The soluble impurities in V2O5 sample were dissolved by digestion of the sample with HCl and HNO3,and the insoluble impurities were dissolved by fusion the residue with anhydrous K2CO3 and boric acid at 950 ℃,and dissolving the melt in HCl.The solutions were combined and made up to 100 mL,in which the impurity elements(including Nb,Zr,Ti,W,Si,Al,Mo,Co,Cr,Ni,Cu,Pb,Cd,As,P,Fe,Mn,Ca and Mg) were determined by ICP-AES.Interferences of the matrix elements and coexisting elements were tested and eliminated by synchronous background calibration.Analytical spectral lines of the 19 elements for the determination were optimized and selected.Values of detection limits of the 19 elements found were in the range of 10-225 μg·L-1,and values of background equivalent concentration were in the range of 5-150 μg·L-1.The proposed method was used in the analysis of V2O5 sample and standard sample of V2O5(GSBH 42015-96).The results obtained for V2O5 sample were in consistency with values obtained by chemical methods,and results obtained for the standard sample were in consistency,with the standard values.