干扰系数校正-电感耦合等离子体原子发射光谱法测定镍基高温合金中硅  

Determination of silicon content in nickel-based alloys by interelement correction-inductively coupled plasma atomic emission spectrometry

作　　者：颜京 王志远 张佩佩 高晋峰 YAN Jing;WANG Zhiyuan;ZHANG Peipei;GAO Jinfeng(AECC Beijing Institute of Aeronautical materials,Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation,Key Laboratory of Aeronautical Materials Testing and Evaluation,Aero Engine Corporation of China,Beijing 100095,China)

机构地区：[1]中国航发北京航空材料研究院,航空材料检测与评价北京市重点实验室,材料检测与评价航空科技重点实验室,中国航空发动机集团材料检测与评价重点实验室,北京100095

出　　处：《化学分析计量》2024年第7期96-100,共5页Chemical Analysis And Meterage

摘　　要：建立了电感耦合等离子体原子发射光谱法测定含钼、铼、镍基高温合金中的硅。采用盐酸、硝酸和氢氟酸将镍基高温合金试样溶解,以Si 251.611 nm作为分析线,分析功率为1.3 kW,辅助气流量为0.2 L/min,载气流量为0.65 L/min,冷却气流量为14 L/min,利用干扰系数校正谱线干扰。结果表明,镍基高温合金中的钼、铼共存元素会对硅元素的测定造成严重的谱线干扰,导致ICP-AES测定结果与实际值存在偏差,但采用干扰系数校正能有效消除钼、铼对硅的谱线干扰。硅的质量分数在0.005%~0.50%范围内与发射强度线性关系良好,相关系数不小于0.9999。按照实验方法对含钼、铼镍基高温合金标准样品中的硅含量进行测定,检测结果的相对标准偏差为0.41%~1.58%(n=8),测定值在认定值的置信区间内,该方法的可靠性和稳定性均较高,能够实现镍基高温合金中硅含量的测定。An inductively coupled plasma atomic emission spectrometry method was established to determine the silicon content in Ni-based superalloys containing Mo and Re element.Nickel-based superalloy samples were dissolved by hydrochloric acid,nitric acid and hydrofluoric acid.With Si 251.611 nm as the analysis line,the analysis power was set at 1.3 kW,the auxiliary gas flow rate was 0.2 L/min,the carrier gas flow rate was 0.65 L/min,and the cooling gas flow rate was 14 L/min.The interference coefficient was used to correct spectral line interference.The results showed that the coexistence of molybdenum and rhenium in nickel-based superalloy will cause serious spectral line interference to the determination of silicon,resulting in the deviation of the ICP-AES measurement results from the actual value,but the use of interference coefficient correction can effectively eliminate the spectral line interference.In the range of 0.005%-0.50%,the mass fraction of silicon is linear,and the correlation coefficient is not less than 0.9999.According to the experimental method,the silicon content in the standard samples of nickel based high-temperature alloys containing molybdenum and rhenium was determined.The relative standard deviation of the test results was 0.41%-1.58%(n=8),and the measured values were within the confidence interval of the determined values.This method has high reliability and stability,and can achieve the determination of silicon content in nickel based high-temperature alloys.

关 键 词：电感耦合等离子体原子发射光谱法 镍基高温合金 干扰系数校正 硅含量 

分 类 号：O657.6[理学—分析化学]