摘要
采用微波消解样品-石墨炉原子吸收光谱法测定镍基高温合金中的痕量银。采用硝酸-氢氟酸-水(5+1+5)溶液对样品进行微波消解,以硝酸钯-硝酸镁的混合溶液为基体改进剂,石墨炉灰化温度为1 000℃,原子化温度为1 850℃,采用塞曼校正技术扣除背景。方法的检出限(3s/k)为2.3pg,加标回收率在98.3%~104%之间。方法应用于镍基高温合金中痕量银的测定,ICPMS的测定结果与之相吻合。
Graphite furnace atomic absorption spectrometry combined with microwave digestion was applied for the determination of trace silver in nickel-base super alloys.The sample was digested by microwave in a mixture of nitric acid-hydrofluoric acid-water(5+1+5).A mixed solution of palladium nitrate and magnesium nitrate was used as matrix modifier.The ashing temperature was 1 000 ℃ and the atomization temperature was 1 850 ℃.Background interference was deducted by Zeeman correction technique.The detection limit(3s/k)was 2.3pg.The recovery rates measured by standard addition method were in the range of 98.3%-104%.The proposed method was used to determining trace silver in nickel-base super alloys,giving results consistent with that obtained by ICPMS.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2015年第3期317-320,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)