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自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲
引用本文:程秀花,黎卫亮,郑民奇,王海蓉.自制氢化物发生装置与电感耦合等离子体质谱仪联用测定地质样品中的稀散元素锗和碲[J].岩矿测试,2016,35(3):265-270.
作者姓名:程秀花  黎卫亮  郑民奇  王海蓉
作者单位:国家地质实验测试中心, 北京 100037,国家地质实验测试中心, 北京 100037,国家地质实验测试中心, 北京 100037,国家地质实验测试中心, 北京 100037,国家地质实验测试中心, 北京 100037
基金项目:国家重大科学仪器设备开发专项项目资助(2011YQ140147);中国地质大调查项目资助(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5.58 μg/g,钽5.87 μg/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42 μg/g~19%和Ta2O5含量在86 μg/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。

关 键 词:铌钽矿      微波溶样  电感耦合等离子体光谱法  耐氢氟酸系统
收稿时间:2015/7/31 0:00:00
修稿时间:5/5/2016 12:00:00 AM

Determination of Germanium and Tellurium in Geological Samples by A Self-developed Hydride Generation Device Paired with Inductively Coupled Plasma-Mass Spectrometer
CHENG Xiu-hu,LI Wei-liang,ZHENG Min-qi and WANG Hai-rong.Determination of Germanium and Tellurium in Geological Samples by A Self-developed Hydride Generation Device Paired with Inductively Coupled Plasma-Mass Spectrometer[J].Rock and Mineral Analysis,2016,35(3):265-270.
Authors:CHENG Xiu-hu  LI Wei-liang  ZHENG Min-qi and WANG Hai-rong
Institution:National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China,National Research Center for Geoanalysis, Beijing 100037, China and National Research Center for Geoanalysis, Beijing 100037, China
Abstract:Niobium and tantalum in hydrofluoric acid to form a stable solution, niobium and tantalum content of niobium tantalum ore can be determined accurately using inductively coupled plasma-optimal emission spectrometry (ICP-OES) with hydrofluoric acid resistant system. This paper established the determination method of Nb and Ta in niobium-tantalum ore, by using modular small tank, multi digestion tank assembly (70/group) of microwave digestion mode, and hydrofluoric acid resistant system of ICP-OES. This method reduced sample dissolution time of Nb and Ta, from 48 hours to 1 hour, and hydrofluoric acid medium could avoid the hydrolysis of high content Nb and Ta in low acid concentration media. The method detection limit of Nb is 5.58 g/g, and the detection limit of Ta is 5.87 g/g. The method is used to determine Nb-Ta concentrate, and the result is consistent with alkali-melting process. This method could be used to determine whether high-grade or low-grade niobium tantalum ore. The main advantage of this method is accurate for high-grade niobium-tantalum ore.
Keywords:niobium-tantalum ore  niobium  tantalum  microwave melting  Inductively Coupled Plasma-Optimal Emission Spectrometry  hydrofluoric acid-resistant system
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