直接烧结-电感耦合等离子体发射光谱法测定钨钼矿石中钨钼及5种伴生元素  

Determination of Tungsten,Molybdenum and 5 Associated Elements in Tungsten-Molybdenum Ore by Inductively Coupled Plasma-Optical Emission Spectrometry with Direct Sintering

作　　者：宋洲 吉义平 王伟华 方绍敏 杨杰 罗火焰 周宇齐 SONG Zhou;JI Yiping;WANG Weihua;FANG Shaomin;YANG Jie;LUO Huoyan;ZHOU Yuqi(Hubei Province Geological Experimental Testing Center,Wuhan 430034,China;Key Laboratory of Rare Earth and Rare Scattered Mineral,Ministry of Natural Resources,Wuhan 430034,China;Hubei Key Laboratory of Resources and Eco-environment Geology(Hubei Geological Bureau),Wuhan 430034,China;Hubei Huaxiang Geological Environmental Testing Technology Co.,Ltd.,Wuhan 430000,China)

机构地区：[1]湖北省地质实验测试中心,湖北武汉430034 [2]自然资源部稀土稀有稀散矿产重点实验室,湖北武汉430034 [3]资源与生态环境地质湖北省重点实验室,湖北武汉430034 [4]湖北华祥地质环境检测科技有限公司,湖北武汉430000

出　　处：《岩矿测试》2023年第5期1041-1051,共11页Rock and Mineral Analysis

基　　金：国家重点研发计划项目(2021YFC2903000)课题“战略性矿产多元素同时分析技术和标准化”。

摘　　要：钨钼矿石一般由多种矿物组成,组分较为复杂,不溶于盐酸、硝酸和王水,常采用碱熔和混合酸酸溶法进行样品消解。然而,碱熔法带来的基体效应严重影响仪器测试的准确性和检出限,而酸溶法对钨钼等难溶元素溶出效率较低,并且需要使用氢氟酸和王水等多种无机强酸进行长时间且操作过程复杂的前处理流程,同时还会造成分析测试仪器损害的问题。因此,开发一种操作简单且高效定量分析钨钼矿石中钨钼及其伴生元素的方法十分必要。本文在碱熔和酸溶的基础上,探索并建立了一种由直接烧结、盐酸-磷酸-柠檬酸络合提取与电感耦合等离子体发射光谱仪(ICP-OES)联用的方法,同时准确定量分析钨钼矿石中钨钼铜铅锌钙铁7种元素。与传统碱熔法相比,通过高温直接烧结让样品中含目标元素的矿物转化为酸可溶态,随后在盐酸-磷酸-柠檬酸混合酸体系的络合作用下,将目标元素转移至溶液中,从而实现快速准确定量测定。最佳实验条件为:600℃烧结1h、5mL磷酸-盐酸(体积比1∶20)提取、5mL 10g/L柠檬酸络合,过滤后上机测定。采用钨矿标准物质(GBW07240和GBW07241)和钼矿标准物质(GBW07238和GBW07239)以及两种实际钨钼矿石样品对本方法进行验证,结果表明7种目标元素测定含量均在标准值范围内,相对误差和相对标准偏差(RSD)均在10%以内。本研究发现,高温直接烧结与盐酸-磷酸-柠檬酸混合酸体系络合提取联用的样品前处理方法,可有效地避免传统碱熔和混合酸酸溶法的缺点,具有更为环保和低能耗的优点,同时可有效地降低化学分析实验室样品分析测试过程中酸气污染物的排放,可为战略性钨钼矿床资源开发和综合利用提供基础支撑。BACKGROUND:Tungsten-molybdenum ore is generally composed of a variety of minerals with complex composition.It is insoluble in hydrochloric acid,nitric acid and aqua regia,and the alkali melting and mixed acid dissolution method was often selected for sample digestion.However,the matrix effect cause by the alkali melting method seriously affects the accuracy and detection limit of instrument testing;the acid dissolution method has low dissolution efficiency for tungsten,molybdenum and other insoluble elements,and requires a long time and a complex pretreatment process by using a variety of inorganic strong acids such as hydrofluoric acid and aqua regia,which can also cause damage to the analytical and testing instruments.OBJECTIVES:To develop a simple and efficient method for quantitative analysis of tungsten and molybdenum and its associated elements in tungsten-molybdenum ore.METHODS:Based on alkaline melting and acid dissolution,a method was established by inductively coupled plasma-optical emission spectrometry(ICP-OES)with direct sintering and complex extraction of hydrochloric acidphosphoric acid-citric acid.Seven elements(tungsten,molybdenum,copper,lead,zinc,calcium,and iron)were analyzed in tungsten-molybdenum ore.The tungsten ore standard substances(GBW07240 and GBW07241),molybdenum ore standard substances(GBW07238 and GBW07239)and two actual tungsten-molybdenum ore samples were used to verify the method.RESULTS:Compared with the traditional alkali melting method,the minerals containing the target elements in the samples were converted to acid soluble state by direct high-temperature sintering,and the target elements were transferred to the solution under the complexation of the mixed acid system of hydrochloric acid,phosphoric acid and citric acid,so as to achieve rapid and accurate quantitative determination.The optimal experimental conditions were:sintering at 600°C for 1h,extraction with 5mL mixed acid composed of phosphoric acid and hydrochloric acid(V/V=1:20),complexation with 5mL of citric acid wi

关 键 词：直接烧结 电感耦合等离子体发射光谱法 钨钼矿石 钨 钼 

分 类 号：O657.31[理学—分析化学]