偏硼酸锂熔融-酒石酸络合-超声提取-电感耦合等离子体原子发射光谱法测定岩矿型锆矿石中10种元素的含量

Determination of 10 Elements in Zirconium Ores of Hard-Rock Type by Inductively Coupled Plasma Atomic Emission Spectrometry with Lithium Metborate Fusion,Tartaric Acid Complexation,and Ultrasonic Extraction

为实现岩矿型锆矿石样品中锆、铪、钾、钙、钠、镁、铝、铁、钛、锰等10种元素含量的准确测定,优化了熔融、提取等试验条件,提出了题示方法。取干燥后的样品0.1 g于铂坩埚中,加入0.5 g偏硼酸锂,搅匀后盖上坩埚盖,于1 000℃熔融30 min。冷却后将铂坩埚置于装有25 mL含20 g·L^(-1)酒石酸的20%(体积分数)盐酸溶液中,超声振荡至熔块完全溶解,用水定容至100 mL,用电感耦合等离子体原子发射光谱仪测定。结果显示:上述10种元素的质量浓度分别在一定范围内与对应的谱线强度呈线性关系,检出限(3s)为1.90~40.8μg·g-1;方法用于由锆含量较低的基性岩岩石标准物质和锆精矿标准物质复配成的以锆石、斜锆石为主的岩矿型锆矿石样品的分析,测定值的相对误差为-1.9%~4.0%,测定值的相对标准偏差(n=12)为0.46%~4.5%,准确度和精密度试验结果的绝对值均优于DZ/T 0130.3-2006规定的控制指标,且方法可拓展应用于砂矿型锆矿石的准确测定。

In order to accurately determine 10 elements such as zirconium,hafnium,potassium,calcium,sodium,magnesium,aluminum,iron,titanium,and manganese in zirconium ore samples of hard-rock type,test conditions of melting and extraction were optimized,and the method mentioned by the title was proposed.The 0.1 g of the dried sample was placed into a platinum crucible,and 0.5 g of lithium metaborate was added.The mixture was mixed well,covered by the crucible lid,and melted at 1000℃for 30 min.After cooling,the platinum crucible was placed into the 25 mL of 20%(volume fraction)hydrochloric acid solution containing 20 g·L^(-1)tartaric acid,and ultrasonic extraction was performed until the frit was completely dissolved.The solution obtained was made its volume up to 100 mL by water,and analyzed by the inductively coupled plasma atomic emission spectrometer.It was shown that linear relationships between values of the mass concentration and the spectral line intensity of the above 10 elements were kept in definite ranges,with detection limits(3s)in the range of 1.90-40.8μg·g^(-1).The proposed method was used for the analysis of zirconium ore samples of hard-rock type composed mainly of zircon or baddeleyite,which were consisted of basic rock reference materials with low zirconium content and zirconium concentrate reference materials.The relative errors of the determined values were in the range of-1.9%-4.0%,and RSDs(n=12)of the determined values were in the range of 0.46%-4.5%.The absolute values of accuracy and precision results were better than the control indicators specified in DZ/T 0130.3-2006,and the proposed method could also be applied to the accurate determination of zirconium ores of sand type.