微波消解-电感耦合等离子体原子发射光谱法测定磷矿石中9种主次元素  

Determination of 9major and minor elements in phosphate rock by inductively coupled plasma atomic emission spectrometry with microwave digestion

作　　者：樊蕾 郭晓瑞 王甜甜 倪文山[1,2,3] 毛香菊 FAN Lei;GUO Xiaorui;WANG Tiantian;NI Wenshan;MAO Xiangju(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006,China;Key Laboratory for Polymetallic Ores′Evaluation and Utilization,MNR,Zhengzhou 450006,China;China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,河南郑州450006 [2]自然资源部多金属矿综合利用评价重点实验室,河南郑州450006 [3]国家非金属矿资源综合利用工程技术研究中心,河南郑州450006

出　　处：《冶金分析》2023年第9期56-61,共6页Metallurgical Analysis

基　　金：国家自然科学基金(22106148)。

摘　　要：磷矿石中多种元素的准确测定对磷矿石的开发利用具有重要指导作用。采用微波消解法以盐酸、硝酸和氢氟酸处理磷矿石,消解完成后加入20mL饱和硼酸溶液中和残余的氢氟酸从而避免刻蚀玻璃引入杂质;再使用电感耦合等离子体原子发射光谱法(ICP-AES)测定磷、钾、钠、钙、镁、硅、铝、铁、钛,建立了微波消解-ICP-AES测定磷矿石中9种主次元素的分析方法。试验探究了微波消解用酸,结果表明仅使用盐酸和硝酸不能完全消解磷矿石,使用盐酸、硝酸和氢氟酸才能使磷矿石溶解完全;对氢氟酸用量进行了优化,选择加入2mL氢氟酸。在优化的实验条件下,各元素质量浓度在线性范围内与其对应的发射光谱强度呈良好的线性关系,相关系数均不小于0.9997;方法中各元素的检出限为0.003%~0.078%(质量分数)。按照实验方法测定磷矿石标准物质,测定值与认定值一致,测定结果的相对标准偏差(RSD,n=5)均小于3%。按照实验方法测定磷矿石样品,测定结果的相对标准偏差(n=5)在0.26%~1.9%之间,加标回收率在90%~105%之间。The accurate determination of various elements in phosphate rock plays an important guiding role in the development and utilization of phosphate rock.The phosphorus rock sample was treated in hydrochloric acid,nitric acid and hydrofluoric acid with microwave digestion.After digestion,20mL of saturated boric acid solution was added to neutralize the residual hydrofluoric acid to avoid impurities introduced by etching glass.The contents of phosphorus,potassium,sodium,calcium,magnesium,silicon,aluminum,iron and titanium were determined by inductively coupled plasma atomic emission spectrometry(ICPAES).Thus,a method for determination of 9major and minor elements in phosphate rock was established by ICP-AES with microwave digestion.The acid for microwave digestion was investigated.The results showed that the phosphate rock sample could not be completely digested with hydrochloric acid and nitric acid,but the sample could be fully digested with hydrochloric acid,nitric acid and hydrofluoric acid.The dosage of hydrofluoric acid was optimized,and 2mL of hydrofluoric acid was selected.Under the optimized experimental conditions,the mass concentrations of elements had good linear relationships with their corresponding emission spectral intensities.The linear correlation coefficients were all not less than 0.9997.The limits of detection for elements were between 0.003%and 0.078%(mass fraction).The certified reference materials of phosphate rock were determined according to the proposed method.The results were consistent with the certified values.The relative standard deviations(RSD,n=5)were all less than 3%.The proposed method was applied for determination of phosphate ore samples.The relative standard deviations(n=5)of determination results were between 0.26%and 1.9%.The recoveries were between 90%and 105%.

关 键 词：磷矿石 微波消解 电感耦合等离子体原子发射光谱法(ICP-AES) 主次元素 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]