高氯酸蔗糖介质火焰原子吸收光谱法测定地质样品中钼  

Determination of molybdenum in geological sample by flame atomic absorption spectrometry with perchloric acid-sucrose medium

作　　者：任金鑫 杨牧青 班俊生 REN Jinxin;YANG Muqing;BAN Junsheng(Henan Second Geological Brigade Co.,LTD.,Zhengzhou 450000,China;Henan Non-ferrous Geology and Mineral Resources Group Co.,LTD.,Zhengzhou 450000,China)

机构地区：[1]河南省第二地质大队有限公司,河南郑州450000 [2]河南有色地质矿产集团有限公司,河南郑州450000

出　　处：《冶金分析》2024年第7期68-73,共6页Metallurgical Analysis

基　　金：河南省豫地科技集团有限公司2023年度科技项目(JTZCKY2023019)。

摘　　要：准确快速测定地质样品中钼的含量对于钼矿的开发利用、地质科学研究等许多领域都具有十分重要的意义。由于钼为难电离元素,采用火焰原子吸收光谱法(FAAS)测定时灵敏度较低、检出限较高。本文利用氧化还原体系进样会提高空气-乙炔火焰温度进而对钼的吸光度产生增敏效应的原理,以高氯酸为氧化剂,蔗糖为还原剂,建立了火焰原子吸收光谱法测定地质样品中0.002%钼的方法。在优化的实验条件下,钼的质量浓度在2~20μg/mL范围内与其对应的吸光度呈良好的线性关系,相关系数为0.9998,灵敏度为0.0106 mL/μg,方法检出限为0.0007%,定量限为0.002%。应用实验方法测定钼矿石成分分析标准物质中钼,测定值与认定值的最大相对误差均小于DZ/T 0130—2006《地质矿产实验室测试质量管理规范》中的相对误差允许限(YB);测定结果的相对标准偏差(RSD,n=9)为1.5%~8.2%。The accurate and rapid determination of molybdenum content in geological samples is of great significance for the development and utilization of molybdenum ore,geological scientific research,and many other fields.Since molybdenum is an element which is hardly ionized,the determination method by flame atomic absorption spectrometry(FAAS)usually has low sensitivity and high limit of detection.The sampling of redox system can increase the air-acetylene flame temperature,thus enhancing the absorbance sensitivity of molybdenum.On the basis of this principle,a method for the determination of molybdenum(0.002%)in geological samples by FAAS was established using perchloric acid as the oxidant and sucrose as the reducing agent.Under the optimized experimental conditions,the mass concentration of molybdenum in range of 2-20μg/mL had a good linear relationship with the corresponding absorbance,with a correlation coefficient of 0.9998.The sensitivity was 0.0106 mL/μg,the limit of detection was 0.0007%,and the limit of quantification was 0.002%.The content of molybdenum in certified reference materials of molybdenum ore for composition analysis was determined according to the experimental method.The maximum relative error between the found results and the certified values were all less than the relative error tolerance(Y_B)specified in DZ/T 0130-2006 The Specification of Testing Quality Management for Geological Laboratories.The relative standard deviations(RSD,n=9)of the determination results were between 1.5%and 8.2%.

关 键 词：高氯酸蔗糖介质 火焰原子吸收光谱法(FAAS) 地质样品 钼 

分 类 号：O657.31[理学—分析化学] TF841.2[理学—化学]