样品(0.200 0 g)于聚四氟乙烯烧杯中用硝酸10 mL、氢氟酸5 mL及高氯酸8 mL低温溶解后蒸发至冒白烟,稍冷,再加高氯酸2 mL并蒸发至冒白烟以除去氢氟酸,冷却,加入硝酸(1+5)溶液2 mL溶解盐类,溶液移入100 mL容量瓶中,加入100 g·L-1 OP溶液2 mL作为消除大量共存铝(Ⅲ)干扰的抑制剂,加水定容后按火焰原子吸收光谱条件测定试液中含锰量。锰的质量浓度在0.50 mg·L-1以内与其吸光度呈线性关系,检出限(3s)为0.046 mg·L-1。方法应用于硅铝合金样品的分析,锰测定值的相对标准偏差(n=5)在1.3%~1.9%之间。用标准加入法进行回收试验,测得回收率在102%~103%之间。

The sample (0.200 0 g) was dissolved with HNO3 (10 mL), HF (5 mL) and HClO4 (8 mL) in a PTFE beaker heated at low temperature, and the solution was evaporated to fume of HClO4, after cooling, HClO4 (2 mL) was added and fumed again to expel HF. Cool again and the salts were taken up with 2 mL of HNO3 (1+5) and the solution was transfered into a 100 mL volumetric flask. A portion of 100 g·L-1 OP solution (2 mL) was added to the solution to restrain the interference of macroamounts of coexisting Al(Ⅲ), and the solution was diluted to 100 mL with water. Manganese in the solution was determined by FAAS under the prescribed conditions. Linear relationship between values of absorbance and mass concentration of manganese was obtained in the range within 0.50 mg·L-1, with detection limit (3s) of 0.046 mg·L-1. The proposed method was applied to the analysis of silicon aluminum alloy (FeAl40Si15), giving values of RSD′s (n=5) for manganese in the range of 1.3%-1.9%. Test for recovery was performed by standard addition method, giving values of recovery in the range of 102%-103%.