用微波消解—ICP-AES法测定TBP萃取剂中的铌、钛  

Determination of Nb and Ti in TBP Extractant by ICP-AES With Microwave Digestion

作　　者：郭国龙[1] 杜凯华 张御帆 韦溪 曹淑琴[1] 龚明明[1] 黄辉[2] GUO Guolong;DU Kaihua;ZHANG Yufan;WEI Xi;CAO Shuqin;GONG Mingming;HUANG Hui(Beijing Research Institute of Chemical Engineering and Metallurgy,CNNC,Beijing 101149,China;CNGC Institute53,Jinan 250031,China)

机构地区：[1]核工业北京化工冶金研究院,北京101149 [2]中国兵器工业集团第五三研究所,山东济南250031

出　　处：《湿法冶金》2022年第6期562-566,共5页Hydrometallurgy of China

基　　金：国防科工局技术基础项目(JSJL2019208A008)。

摘　　要：建立了微波消解—ICP-AES法测定TBP萃取剂中铌、钛的方法。研究了酸种类、酸用量、消解时间、最高消解温度、配合剂用量对微波消解的影响。结果表明:最佳消解条件为浓硝酸用量10 mL,氢氟酸用量1.0 mL,150 g/L酒石酸用量0.2 mL,最高消解温度190℃,消解时间30 min;有机相中铌、钛的相对标准偏差分别为1.63%和1.44%,加标回收率分别为96.2%~98.0%和92.0%~95.5%,检出限分别为0.282μg/L和0.0075μg/L。该法简单、准确,可满足有机相中铌和钛的检测要求。A method for determination of Nb and Ti in TBP extractants by microwave digestion—ICP-AES was established.The effects of acid type,acid dosage,digestion temperature,digestion time,and the dosage of complexing agent on microwave digestion were studied.The results show that the optimum digestion conditions are concentrated nitric acid dosage of 10 mL,hydrofluoric acid dosage of 1.0 mL,150 g/L tartaric acid dosage of 0.2 mL,digestion temperature of 190℃,digestion time of 30 min.The relative standard deviation(RSD)of Nb and Ti in organic phase are 1.63%and 1.44%,the recoveries are 96.2%~98.0%and 92.0%~95.5%,the detection limits are 0.282μg/L and 0.0075μg/L,respectively.The method is simple and accurate,and can meet the requirements for the determination of Nb and Ti in organic phase of zirconium production.

关 键 词：有机相 负载 锆 TBP 微波消解 ICP-AES 铌 钛 

分 类 号：O657.31[理学—分析化学]