微波消解样品-石墨炉原子吸收光谱法测定高温镍基合金中的痕量银  

Determination of Trace Silver in Nickel-base Super Alloys by GF-AAS Combined with Microwave Digestion

作　　者：郭颖[1,2] 陶美娟[1,2] 戴亚明[1,2] 

机构地区：[1]上海材料研究所检测中心,上海200437 [2]上海材料研究所上海市工程材料应用评价重点实验室,上海200437

出　　处：《理化检验（化学分册）》2015年第3期317-320,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

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.

关 键 词：石墨炉原子吸收光谱法 微波消解 镍基高温合金 银 

分 类 号：O657.31[理学—分析化学] TG115.33[理学—化学]