湿法球磨制备超细地质样品及取样量探究  

Study and Application of a Wet Ball Milling Ultra-fine Method for Geological Samples

作　　者：董学林 向兆 贾正勋 张楠[3] 童铄云 熊玉祥 DONG Xuelin;XIANG Zhao;JIA Zhengxun;ZHANG Nan;TONG Shuoyun;XIONG Yuxiang(Key Laboratory of rare earth and rare scattered minerals,Ministry of natural resources,Geological Experimental Testing Center of Hubei Province,Wuhan 430034,China;Hubei Key Laboratory of Resources and Eco-Environment Geology(Hubei Geological Bureau),Wuhan 430034,China;Tianjin Center of Geological Survey,China Geological Survey,Tianjin 300170,China)

机构地区：[1]自然资源部稀土稀有稀散矿产重点实验室,湖北省地质实验测试中心,湖北武汉430034 [2]资源与生态环境地质湖北省重点实验室,湖北省地质局,湖北武汉430034 [3]中国地质调查局天津地质调查中心,天津300170

出　　处：《岩矿测试》2023年第5期1052-1061,共10页Rock and Mineral Analysis

基　　金：国家重点研发计划项目(2021YFC2903000)课题“战略性矿产现场快速分析装备、技术和应用示范”;湖北省地质局科技计划项目(KJ2021-17)。

摘　　要：当前实验室制备的地质样品存在大颗粒微粒,影响了样品代表性和分析结果的准确度,制备超细样品是有效的解决办法。本文建立了水为助磨剂,湿法球磨制备超细地质样品的方法。结果表明,氧化锆或碳化钨材质的球磨罐会污染样品中锆、钨及钴等微量元素,而玛瑙材质的球磨罐污染样品的风险较小;采用玛瑙材质的球磨罐,20g样品,液固比为1∶1,磨球配置为大8颗、中16颗、小48颗,球磨时间30min,运用该方法对四种代表性样品(岩石、土壤、沉积物及稀土矿石)进行球磨,粒度检测结果表明,球磨后的样品粒度均达到1000目;对60件未知基质类型的样品进行湿法球磨后,D50均小于5μm,D90均小于19μm,表明该方法具有一定的适用性;微观形貌研究表明,球磨制备的样品,大颗粒微粒显著减少,颗粒分布更加均匀;对球磨后的岩石标准物质(GBW07104)进行了取样量试验,所检测的46种元素结果进行统计,除Mo、Cd、Cr等元素外,取样量可减少至2mg;制备的超细样品与电感耦合等离子体质谱(ICP-MS)技术联用,可发挥ICP-MS高灵敏度的效能,同时提高检测效率、减少环境污染。BACKGROUND:At present,there are large particles in geological samples prepared in the laboratory,which affect the representativeness of the samples and the accuracy of the analysis results[1-3].With the rapid development of modern analytical instruments,analytical methods based on inductively coupled plasma-mass spectrometry(ICPMS)have been widely used in laboratories across the country for the simultaneous determination of multiple elements in geological samples due to their low detection limit,high analytical flux,and wide linear range[10-14].Its characteristics of high sensitivity and analytical accuracy,small sample injection volume,and high requirements for sample representativeness are incompatible with the sample preparation technology that serves as the foundation of laboratory analysis work.Therefore,there is an urgent need to research and develop sample preparation methods that reduce sample size and improve representativeness,in order to meet the needs of ultra trace element detection.The main methods for preparing ultrafine geological samples include air flow pulverization and ball milling.Air flow pulverization is widely used in the preparation of geological standard material samples,but the sample size prepared in one step is large,which is prone to sample grading and requires secondary mixing[16-17].Dry ball milling is a common geological sample preparation method in laboratories.Prolonging the ball milling time is beneficial for sample refinement,but it can easily cause contamination by the characteristic elements of the ball milling tank material.Wet ball milling can form a slurry between the sample and the grinding aid,which is conducive to the flow of the sample and the grinding ball during the ball milling process,increasing the friction between them,and achieving the goal of further refining the sample[21].OBJECTIVES:To establish a method of preparing ultra-fine geological samples by wet ball grinding with water as the grinding aid.METHODS:Weigh 20g samples into the ball mill tank made of aga

关 键 词：地质样品 湿法球磨 超细化 微观形貌 电感耦合等离子体质谱法 

分 类 号：O657.63[理学—分析化学]