Abstract：The DD6 single crystal nickel base super alloy contained alloying elements such as Ta, Re and W, so it was difficult to dissolve the sample and the sample solution was also unstable. In this study, the sample was dissolved with hydrochloric acid-nitric acid system. The calibration curve was prepared using matrix matching method to eliminate the interference of nickel matrix. The determination method of arsenic in DD6 single crystal nickel base super alloy by hydride generation-atomic fluorescence spectrometry was established. The sample dissolution method was discussed. The results showed that when the sample was dissolved with 20mL of hydrochloric acid and 5mL of nitric acid followed by heating (about 100℃), although few undissolved substances still existed, the testing element (i.e., arsenic) had been completely extracted. In other words, the undissolved substances contained no arsenic. Therefore, this sample dissolution method was selected in experiments. The negative high voltage and lamp current of instrument were optimized: the negative high voltage was 280V and the lamp current was 60mA. According to the content of nickel in sample, the calibration curves were established without or with matrix matching. The results showed that for the standard solutions with same mass concentration of arsenic, the determination results in presence of nickel matrix were obviously lower than those in absence of nickel matrix. In other words, the interference of nickel matrix could not be ignored. Therefore, the calibration curve was prepared by nickel matrix matching method. The linear range of method was 0.00005%-0.001%, and the detection limit was 2×10-5 μg/mL. The experimental method was applied for the determination of six DD6 single crystal nickel base super alloy samples, and the found results were basically consistent with those obtained by high velocity glow discharge mass spectrometry. The relative standard deviations (RSD, n=8) of determination results were between 2.3% and 8.7%.
谢锡善.我国高温材料的应用与发展[J].机械工程材料,2004,28(1):2-11.XIE Xi-shan.The development and application of high temperature materials in China[J].Material Impurity in Mechanical Engineering,2004,28(1):2-11.
[2]
邢占平,黄朝晖,谭永宁,等.第二代定向凝固镍基高温合金的微观结构研究[J].中国有色金属学报,2004,10(14):10-12.XING Zhan-ping,HUANG Zhao-hui,TAN Yong-ning, et al.Microstructure of second generation DS superalloy[J].The Chinese Journal of Nonferrous Metals,2004,10(14):10-12.
[3]
孙晓峰,金涛,周亦胄,等.镍基单晶高温合金研究发展[J].中国材料进展,2012,31(12):1-11.SUN Xiao-feng,JIN Tao,ZHOU Yi-zhou,et al.Research progress of nickel-base single crystal superalloys[J].Materials China,2012,31(12):1-11.
[4]
豆德秋.原子荧光法与原子吸收法测定水质汞的对比分析[J].中国化工贸易(Chinese Journal of Chemical Industry and Trade),2016,(8):56.
[5]
江梅,柯真山.原子荧光法同时测定水中砷和硒的最佳条件[J].净水技术,2014,33(6):53-56.JIANG Mei,KE Zhen-shan.Optimum conditions of simultaneous determination of arsenic and selenium in water by atomic fluorescence spectrometry[J].Water Purification Technology.2014,33(6):53-56.
[6]
江梅,陈刚新,张凯,等.原子荧光法测定水中硒时防止铜干扰的方法[J].净水技术,2015,34(5):87-90.JIANG Mei,CHEN Gang-xin,ZHANG Kai,et al.Method of selenium determination in water while interference-free from copper with atomic fluorescence spectrometry[J].Water Purification Technology,2015,34(5):87-90.
[7]
李永福.原子荧光法测定土壤中痕量砷和汞[J].化学工程师,2016(11):26-28.LI Yong-fu.Atomic fluorescence method for determination of trace arsenic and mercury in soil[J].Chemical Engineer,2016(11):26-28.
[8]
郎春燕,周英,赖晨焕.氢化物发生原子荧光法测定稻田土中的锑形态[J].分析试验室,2012,31(12):95-99.LANG Chun-yan,ZHOU Ying,LAI Chen-huan.Determination of antimony species in rice paddy soils by hydride generation atomic fluorescence spetrometry[J].Chinese Journal of Analysis Laboratory,2012,31(12):95-99.
[9]
倪通文,范宁云,王宁,等.火焰-原子荧光法与石墨炉原子吸收法测定化探样品和矿石中金的对比研究[J].环保与分析,2012,5(33):56-59.NI Tong-wen,FAN Ning-yun,WANG Ning,et al.Comparative study on determination of trace gold in chemical prospecting samples and ores by graphite furnace atomic absorption spectrometry and flame-generation atomic fluorescence spectrometry[J].Journal of Environmental Protection and Analysis,2012,5(33):56-59.
贾进铎.氢化物发生原子荧光光谱法测定镍基高温合金中痕量硒和碲[J].理化检验:化学分册,2001,37(3):104-106.JIA Jin-duo.HG-AFS determination of trace amounts of se and te in nickel base superalloys[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2001,37(3):104-106.
[13]
Kenghsien Su,Xinwei Wang,Karol Puyera.高流速辉光放电质谱法检测镍基高温合金中痕量元素及其深度分布[J].冶金分析,2011,31(11):18-23.Kenghsien Su,Wang Xinwei,Karol Puyera.Depth resolved trace element analysis of Ni-base superalloys using fast-flow discharge mass spectrometry(FF-GDMS)[J].Metallurgical Analysis,2011,31(11):18-23.
