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    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

    • 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2.3 pg,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,ICP-MS的测定结果与之相吻合.

       

      Abstract: 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 2.3 pg. 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 ICP-MS.

       

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