二溴对氯偶氮氯膦固相萃取-分光光度法测定痕量钇  

Spectrophotometric determination of trace yttrium with dibromo-p-chlorochlorophosphonazo solid phase extraction

作　　者：李慧芝[1] 张瑾[1] 解文秀[1] 曹法全[1] 

机构地区：[1]济南大学化学化工学院,山东济南250022

出　　处：《冶金分析》2010年第10期66-69,共4页Metallurgical Analysis

基　　金：国家自然科学基金资助项目(50872042);山东省自然科学基金资助项目(No.Y2003F03)

摘　　要：在pH3.0的盐酸-醋酸钠缓冲介质中,在甜菜碱存在下,二溴对氯偶氮氯膦（DBCC-PA）与钇Ⅲ反应生成摩尔比为2∶1的稳定络合物,该络合物可用阳离子交换树脂固相萃取柱富集,吸附柱上富集的络合物用乙醇＋盐酸洗脱后用分光光度法测定。分离后的测定液中,络合物最大吸收波长为620 nm,表现摩尔吸光系数ε=1.065×10^5L·mol^-1·cm^-1,钇Ⅲ含量在0～1.0μg/mL内符合比尔定律,相关系数r=0.989 6。对30余种共存离子进行试验,结果表明大多数常见离子不干扰测定。方法用于合金、矿石、粉煤灰等样品中钇的分析,相对标准偏差小于3%,加标回收率在96%～104%之间,测定值与ICP-AES法的结果一致。In the presence of betaine and HCl-NaAc buffer solution（pH = 3.0）,dibromo-p-chloro-chlorophosphonazo reacts with yttrium Ⅲ,forming a stable（2∶1） complex.The complex can be extracted by cation exchange resin cartridge and eluted from cartridge with ethanol＋HCl before it is determined by spectrophotometry.Its apparent molar absorptive coefficient ε is 1.065×10^5 L·mol-^1·cm^-1 at 620 nm.Beer＇s law is obeyed in range of 0-1.0 μg/mL for YⅢ and the correlation coefficient was 0.989 6.More than 30 categories of co-existing ions are tested,and it proves that most common ions have no interference with the determination of yttrium.This method has been applied to the determination of yttrium in samples with the RSD smaller than 3% and the recovery of 95%-105%.The found values are consistent with those by ICP-AES.

关 键 词：固相萃取 二溴对氯偶氮氯膦 钇Ⅲ 分光光度法 

分 类 号：TG115.3[金属学及工艺—物理冶金]