微波消解-电感耦合等离子体发射光谱法测定铝质粘土岩型锂矿中锂、钙、镁、铁、钛  

Determination of lithium,calcium,magnesium,iron and titanium in aluminous claystone lithium ore by inductively coupled plasma emission spectrometry with microwave digestion

作　　者：苏凌云 戴涛 王帅 李玲娜 李铨 SU Lingyun;DAI Tao;WANG Shuai;LI Lingna;LI Quan(Yunnan Nuclear Industry 209 Geological Brigade,Kunming 650000,China)

机构地区：[1]云南省核工业二〇九地质大队,昆明650000

出　　处：《化学分析计量》2024年第11期79-84,128,共7页Chemical Analysis And Meterage

摘　　要：建立微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法测定铝质粘土锂矿中锂、钙、镁、铁、钛。采用硝酸-盐酸-氢氟酸-高氯酸酸溶体系,在180℃时采用微波法消解铝质粘土锂矿样品。以Li 670.784 nm、Ca 317.930 nm、Mg 279.533 nm、Fe 238.204 nm、Ti 336.121 nm作为分析线,采用ICP-AES法进行测定。通过标准加入法消除铝基体效应,目标元素锂、钙、镁、铁、钛相互之间无干扰。锂、钙、镁、铁、钛5种元素的质量浓度在一定范围内与发光强度线性关系良好,相关系数均不小于0.9995,方法检出限依次为0.002%、0.002%、0.009%、0.006%、0.003%。将方法用于测定粘土矿、铝土矿、锂矿石国家标准物质和实际铝质粘土锂矿样品,标准物质的测定值和认定值基本一致,测定结果的相对标准偏差为0.89%~4.76%(n=12),相对误差为-4.78%~4.49%(n=12);实际铝质粘土锂矿样品的测定结果的相对标准偏差为0.58%~4.71%(n=12)。该方法操作简便、成本低、污染小,具有实际应用前景。An inductively coupled plasma atomic emission spectrometry(ICP-AES)method with microwave digestion and was established for the determination of lithium,calcium,magnesium,iron and titanium in aluminium-clayite.Using the acid solution system of nitric acid,hydrofluoric acid,and perchloric acid,the samples of aluminum clay lithium ore can be completely digested at 180℃.Li 670.784 nm,Ca 317.930 nm,Mg 279.533 nm,Fe 238.204 nm and Ti 336.121 nm were used as analysis lines for determination by ICP-AES method.The aluminum matrix effect was eliminated by standard addition method,and there is no interference between lithium,calcium,magnesium,iron and titanium.The mass concentration of lithium,calcium,magnesium,iron and titanium had a good linear relationship with the luminescence intensity within a certain range,and the correlation coefficients were all greater than 0.9995.The detection limits were 0.002%,0.002%,0.009%,0.006%and 0.003%.The method was applied to the samples of clay ore,bauxite,lithium ore and actual lithium bauxite.The measured values of the standard substances were basically consistent with the certified values.The relative standard deviations of the measured results were 0.89%-4.76%(n=12),and the relative errors were-4.78%-4.49%(n=12).The relative standard deviation of the measured results of the actual aluminum clay lithium ore samples was 0.58%-4.71%(n=12).The method has the advantages of simple operation,low cost and low pollution,which has practical application prospect.

关 键 词：铝质粘土锂矿 微波消解 电感耦合等离子体发射光谱法 

分 类 号：O657.3[理学—分析化学]