电感耦合等离子体原子发射光谱法测定镧玻璃废粉中五氧化二铌、二氧化锆和二氧化钛

摘要

采用氢氧化钠和过氧化钠高温熔融样品,用热水提取熔融物,在碱性条件下,分离硅、硼及钠盐。以盐酸和氢氟酸溶解沉淀,选择Nb 309．418 nm、Zr 257．139 nm、Ti 334．941 nm作为分析线,使用电感耦合等离子体原子发射光谱法( ICP-AES)同时测定了Nb2 O5、ZrO2和TiO2含量,从而建立了镧玻璃废粉中Nb2 O5、ZrO2和TiO2的测定方法。试验确定了最佳熔样条件,结果如下：在0．5 g样品中加入3．0 g氢氧化钠、1．5 g过氧化钠,在750℃下熔融10 min。通过谱线及背景轮廓、信背比、信号强度等条件选择了最佳分析线。试验表明基体的质量浓度在0．1 mg/mL以下对待测组分无影响,共存元素 La、Ni、Ce、Ba、Sr、Si、B 的干扰可以忽略。Nb2 O5、ZrO2和TiO2的线性范围分别是1．00~15．0μg/mL、1．00~10．0μg/mL和1．00~15．0μg/mL。各组分的校准曲线线性相关系数均为0．9999；检出限为0．013%~0．016%。按照实验方法对镧玻璃废粉实际样品中Nb2 O5、ZrO2和TiO2进行测定,结果的相对标准偏差( RSD,n=11)在0．59%~1．2%之间；并与 X 射线荧光光谱法( Nb2 O5)、重量法( ZrO2)和滴定法( TiO2)的结果进行比对,测定结果相吻合。%The sample was melted with sodium hydroxide and sodium peroxide at high temperature, and the melt was extracted with hot water. Thus, silicon, boron and sodium salts was separated from precipitate under alkaline condition. After the precipitate was dissolved with hydrochloric acid and hydrofluoric acid, the content of Nb2 O5 , ZrO2 and TiO2 was simultaneously determined by inductively coupled plasma atomic emission spectrometry ( ICP-AES) with Nb 309. 418 nm, Zr 257. 139 nm and Ti 334. 941 nm as analytical lines. Consequently, a determina-tion method of Nb2 O5 , ZrO2 and TiO2 in waste powder of lanthanum glass was established. The optical sample fu-sion conditions were explored as follows:3. 0 g of sodium hydroxide and 1 . 5 g of sodium peroxide were added into 0. 5 g of sample followed by fusion at 750 ℃ for 10 min. The optimal analysis lines were selected by spectral line, background profile, signal-to-background ratio and signal intensity. The results showed that the mass concentration of matrix below 0. 1 mg/mL had no influence on the determination. The interference of coexisting elements inclu-ding La, Ni, Ce, Ba, Sr, Si and B could be ignored. The linear range of Nb2 O5 , ZrO2 and TiO2 was 1. 00-15. 0μg/mL,1. 00-10. 0 μg/mL and 1. 00-15. 0 μg/mL, respectively. The linear correlation coefficients of calibration curves were all 0. 999 9. The detection limits were between 0. 013% and 0. 016%. The content of Nb2 O5 , ZrO2 and TiO2 in actual sample of waste powder of lanthanum glass was determined according to the experimental meth-od. The relative standard deviations (RSD, n=11) were between 0. 59% and 1. 2%. The results were consistent with those obtained by X-ray fluorescence spectrometry ( Nb2 O5 ) , gravimetry( ZrO2 ) and titration method( TiO2 ) .