高压密闭消解-电感耦合等离子体质谱法测定锰矿石中钛钒锶

采用高压密闭消解系统,以6 mL HNO₃-1 mL HF-3 mLHCl酸体系消解锰矿石,建立了电感耦合等离子体质谱法(ICP-MS)测定锰矿石中钛、钒、锶3种金属元素的方法。选择⁴⁸Ti、⁵¹V和⁸⁸Sr为待测同位素,以钪(⁴⁵Sc)和铟(¹¹⁵In)为内标校正了基体效应与信号漂移。钛、钒和锶校准曲线的线性相关系数均为0.999 9,检出限分别为0.12、0.003 0和0.014 ng/mL。将方法用于锰矿石实际样品分析,结果与电感耦合等离子体原子发射光谱法(ICP-AES)基本一致,相对标准偏差(RSD, n=11)不大于2.0%,加标回收率在99%~102%之间。

Determination of titanium,vanadium and strontium inmanganese ore by inductively coupled plasma mass spectrometry with high-pressure closed digestion

After the sample was decomposed with 6 mL of HNO₃, 1 mL of HF and 3 mL of HCl in high-pressure closed vessel digestion system, titanium, vanadium and strontium in manganese ore was determined by inductively coupled plasma mass spectrometry (ICP-MS). ⁴⁸Ti, ⁵¹V and ⁸⁸Sr were selected as test isotopes. The matrix effect and signal drift were corrected with ⁴⁵Sc and ¹¹⁵In as internal standard. The linear correlation coefficients of calibration curve were all 0.999 9 for titanium, vanadium and strontium, and the detection limit was 0.12, 0.003 0 and 0.014 ng/mL, respectively. The proposed method was applied to the determination of manganese ore actual samples. The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The relative standard deviation (RSD, n=11) was equal to or less than 2.0%. The recoveries of standard addition were between 99% and 102%.