微波消解-耐氢氟酸系统电感耦合等离子体发射光谱法测定铌钽矿中的铌和钽  

Determination of Nb and Ta in Nb-Ta Ore by Inductively Coupled Plasma-Optical Emission Spectrometry with a Combined Microwave Digestion Hydrofluoric Acid-resistant System

作　　者：马生凤[1] 温宏利[1] 李冰[1] 王蕾[1] 朱云[1] 

机构地区：[1]国家地质实验测试中心,北京100037

出　　处：《岩矿测试》2016年第3期271-275,共5页Rock and Mineral Analysis

基　　金：国家重大科学仪器设备开发专项项目(2011YQ140147);中国地质大调查项目(12120113014300)

摘　　要：铌、钽在氢氟酸介质中能够形成稳定的溶液,使用耐氢氟酸进样系统的电感耦合等离子体发射光谱(ICP-OES)有利于提高分析的准确性。本文采用模块化的小罐型、多罐体组合(70罐/组)酸溶罐体的微波消解溶样模式,结合ICP-OES仪器的耐氢氟酸进样系统,建立了测定铌钽矿中铌、钽的分析方法。本方法加快了酸溶的溶样速度,溶样时间从原来的48 h减少至1 h,且在氢氟酸介质中测定避免了高含量铌、钽在低酸度介质中容易水解的影响。方法检出限为铌5.58μg/g,钽5.87μg/g。本方法应用于测定铌钽精矿(19%Nb2O5,27%Ta2O5)的分析结果与碱熔方法一致,能够测定Nb2O5含量在42μg/g^19%和Ta2O5含量在86μg/g^27%高低品位的铌钽矿,尤其对于铌、钽在百分含量以上的铌钽矿具有优势。Niobium and tantalum in hydrofluoric acid can form a stable solution,and thus the Nb and Ta content of Nb-Ta ore can be determined accurately by Inductively Coupled Plasma-Optical Emission Spectrometry( ICP-OES)with a hydrofluoric acid resistant system. The determination method described in this paper for Nb and Ta in Nb-Ta ore,uses the microwave digestion mode of modular small tank and multiple digestion tank assembly( 70 tank /group),and hydrofluoric acid resistant system of ICP-OES. This method shortens the dissolution time from 48 h to1 h. By using a hydrofluoric acid medium the hydrolysis of high-level Nb and Ta in low acid concentration media is avoided. The detection limits of this method are 5. 58 μg / g for Nb and 5. 87 μg / g for Ta. The result of Nb-Ta concentrate with 19% Nb2O5 and 27% Ta2O5 is consistent with that acquired by the alkali fusion method and can be used to determine both high-grade and low-grade Nb-Ta ore with 42 μg / g- 19% of Nb2O5 and 86 μg / g- 27%of Ta2O5. The main advantage of this method is to accurately determine Nb and Ta in high-grade Nb-Ta ore.

关 键 词：铌钽矿 铌 钽 微波溶样 电感耦合等离子体光谱法 耐氢氟酸系统 

分 类 号：O614.511[理学—无机化学] O614.512[理学—化学]