微波消解-电感耦合等离子体质谱法测定钽酸锂中痕量杂质元素

钽酸锂中杂质元素含量是划分产品等级的重要参数.样品中加入硝酸和氢氟酸后用微波消解法溶解样品,在线加入1.00 μg/mL的Cs内标溶液后,在H2动态反应池模式下测定Ca、Fe、As、Se,在标准模式下测定其余元素,建立了微波消解-电感耦合等离子体质谱法(ICP-MS)测定钽酸锂中Be、B、Na、Mg、Al、K、Ca、T...

Determination of trace impurities in lithium tantalate by inductively coupled plasma mass spectrometry with microwave digestion

The content of impurity elements in lithium tantalate was an important parameter for grading products. The sample was dissolved by microwave digestion with nitric acid and hydrofluoric acid. 1.00 μg/mL Cs internal standard solution was added online. Ca, Fe, As and Se were determined at H₂ dynamic reaction cell mode, while other elements were determined at standard mode. Thus, a determination method of twenty-eight impurity elements (Be, B, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Zr, Nb, Mo, Cd, Sb, Ba, Hf, W, Pb and Bi) in lithium tantalate was established by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion. The sample dissolution method was optimized. The following microwave digestion conditions were used: the sample was digested in microwave with 2 mL of nitric acid and 2 mL of hydrofluoric acid at 190 ℃ for 120 min. Under the selection experimental conditions, the limits of detection for 28 elements were between 0.003 μg/g and 0.37 μg/g, and the limits of quantification were in range of 0.01-0.74 μg/g. The proposed method was applied for the determination of twenty-eight impurity elements such as Mg, Al, Ca and Ti in commercial lithium tantalate samples. The relative standard deviations (RSD, n=7) of determination results were less than 5%, and the recoveries were between 87% and 112%. The content of Fe in sample was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), and the result was basically consistent with the experimental method.