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实验在pH=5.5的酸度下,使用PMBP-苯溶剂定量萃取化探样品中15种稀土元素和钍,然后用甲酸-8-羟基喹啉溶液反萃取稀土元素并在萃取后的有机相中再用50%盐酸反萃取钍,分离后ICP-AES同时测定的新方法。成功解决了盐酸、硝酸、氢氟酸、高氯酸消解后ICP-AES直接测定稀土元素基体成分复杂,质谱干扰严重,方法检出限高等问题,试样用过氧化钠-氢氧化钾熔融后,水提取,过滤,滤渣酸溶,经过沉淀和溶剂萃取等分离富集,对稀土组份进行全分析。其检出限为0.003μg/ml~0.068μg/ml,相对标准偏差(RSD)0.6%~2.0%,准确度及精密度符合国家及行业规范要求。采用建立的方法测定稀土铌钽矿中的稀土元素及钍,结果满意且具有实际应用价值。
Experiments Quantitative extraction of 15 kinds of rare earth elements and thorium in geochemical exploration samples with PMBP-benzene solvent under the pH of 5.5, followed by stripping rare earth elements with the formic acid-8-quinolinol solution and extracting the rare earth elements in the extracted organic phase Thorium stripping with 50% hydrochloric acid, a new method for the simultaneous determination of ICP-AES after separation. Successfully solved the hydrochloric acid, nitric acid, hydrofluoric acid, perchloric acid digestion ICP-AES direct determination of rare earth elements matrix composition is complex, serious interference of mass spectrometry, the detection limit of the method is high, the sample with sodium hydroxide - potassium hydroxide after melting , Water extraction, filtration, acid-soluble residue, after precipitation and solvent extraction, such as separation and enrichment, the full analysis of rare earth components. The detection limits were 0.003μg / ml ~ 0.068μg / ml, RSD was 0.6% ~ 2.0%. The accuracy and precision met the national and industry specifications. The determination of rare earth elements and thorium in the rare earth niobium and tantalum ore by the established method is satisfactory and has practical value.