超级微波消解-碰撞池-电感耦合等离子体质谱法测定氮化铝粉中钠钨铁锌钛锰

作为制备氮化铝材料的原料,氮化铝粉体中的杂质金属元素含量会对氮化铝制品的导热和介电性能产生重要影响。实验采用硫磷混酸以超级微波消解法处理样品,解决了氮化铝粉难以溶解完全的问题。选择²³Na、¹⁸²W、⁵⁴Fe、⁶⁶Zn、⁴⁶Ti和⁵⁵Mn为待测同位素,控制氦气流量为1.52 mL/min、以氦气碰撞池模式(CCT mode)消除质谱干扰,用50 μg/L ⁸⁹Y校正²³Na、⁵⁴Fe、⁶⁶Zn、⁴⁶Ti、⁵⁵Mn,用50 μg/L ¹⁸⁵Re校正¹⁸²W,建立了碰撞池-电感耦合等离子体质谱法(ICP-MS)测定钠、钨、铁、锌、钛、锰6种杂质金属元素的方法。在优化的实验条件下,6种元素的检出限为0.03~0.64 mg/kg,定量限为0.10~2.13 mg/kg。采用实验方法对氮化铝粉样品进行测定,6种元素测定结果的相对标准偏差(RSD,n=6)均小于4%,加标回收率为96%~103%。采用电感耦合等离子体原子发射光谱法(ICP-AES)和石墨炉原子吸收光谱法进行方法对照试验,测定结果与实验方法基本一致。

Determination of sodium,tungsten,iron,zinc,titanium and manganese in aluminum nitride powder by super microwave digestion-inductively coupled plasma mass spectrometry with collision cell

Aluminum nitride powder is the raw material for the preparation of aluminum nitride materials. The content of impurity metal elements in aluminum nitride powder will have an important impact on the thermal conductivity and dielectric properties of aluminum nitride products. In experiments, the samples were treated by super microwave digestion with mixture of sulfuric acid and phosphoric acid, which solved the problem that the aluminum nitride powder sample was difficult to be dissolved completely. ²³Na, ¹⁸²W, ⁵⁴Fe, ⁶⁶Zn, ⁴⁶Ti and ⁵⁵Mn were selected as the isotopes to be measured. The flow rate of helium was controlled at 1.52 mL/min to eliminate the mass spectrum interference using helium collision cell technology mode (CCT mode). 50 μg/L of ⁸⁹Y was used to correct ²³Na, ⁵⁴Fe, ⁶⁶Zn, ⁴⁶Ti and ⁵⁵Mn, while 50 μg/L ¹⁸⁵Re was used to correct ¹⁸²W. Consequently, a method for the determination of six impurity metal elements (including sodium, tungsten, iron, zinc, titanium and manganese) by inductively coupled plasma mass spectrometry (ICP-MS) with collision cell was established. Under the optimized experimental conditions, the limits of detection for six elements were in range of 0.03-0.64 mg/kg, and the limits of quantification were in range of 0.10-2.13 mg/kg. The aluminum nitride powder sample was determined according to the experimental method. The relative standard deviations (RSD, n=6) of determination results for six elements were all less than 4%. The recoveries were between 96% and 103%. The method comparison tests were conducted by inductively coupled plasma atomic emission spectrometry (ICP-AES) and graphite furnace atomic absorption spectrometry (GF-AAS), and the determination results were basically consistent with those obtained by the experimental method.