Abstract：Spark discharge atomic emission spectrometry (SD-AES) is a relative analysis method, and therefore its precision is very important. The stability of the spectrometer, homogeneity of the samples and operating conditions will directly influence on the precision of determination by SD-AES. The spectrometer operation and the changes of relative intensity of analytical line were discussed in experiments. The effects of argon operating pressures and surface roughness (Ra) of the samples on the precision of SD-AES were investigated. The results showed that the smaller Ra of the sample was, the higher the precision of SD-AES was. In order to obtain good precision and trueness, the Ra of the samples was in the range of 0.2-2.5 μm, and the operating pressures of argon was at the rated or smallish pressures for routine analysis. The grinding could obtain analytical surface with smaller roughness. Careful maintenance of the spectrometer was the key to maintain its original properties. The necessity of assessing surface quality of the samples with surface roughness was further pointed out.
[1] 贾云海,孙晓飞.火花放电原子发射光谱分析全流程正确度控制方法研究[J].冶金分析,2020,40(7):1-7. JIA Yunhai,SUN Xiaofei.Research on trueness control method of full process in spark discharge atomic emission spectrometric analysis[J].Metallurgical Analysis,2020,40(7):1-7. [2] 李传启,唐道敏,杨崇秀.ZG25Mn18Cr4光谱分析控制样品的研制[J].广州化学,2021,46(6):76-79. LI Chuanqi,TANG Daomin,YANG Chongxiu.Development of ZG25Mn18Cr4 control sample for spark discharge atomic emission spectrometry[J].Guangzhou Chemistry,2021,46(6):76-79. [3] 李传启,杨辉,唐道敏.火花放电原子发射光谱法样品的制备与表征[J].广州化学,2021,46(5):77-81. LI Chuanqi,YANG Hui,TANG Daomin.Preparation and characterization of the metallic samples for spark discharge atomic emission spectrometry[J].Guangzhou Chemistry,2021,46(5):77-81. [4] 武汉大学.分析化学:下册[M].5版.北京:高等教育出版社,2007:87-88. [5] 郑国经.分析化学手册:原子光谱分析[M].3版.北京:化学工业出版社,2016:287-290. [6] 国家质量监督检验检疫总局.GB/T14203—2016火花放电原子发射光谱分析法通则[S].北京:中国标准出版社,2016. [7] 张彦荣.样品铣削技术对火花源原子发射光谱法测定精度的影响研究[J].冶金分析,2013,33(11):54-58. ZHANG Yanrong.Study on the influence of sample milling technique on the determination precision of spark source atomic emission spectrometry[J].Metallurgical Analysis,2013,33(11):54-58. [8] 崔隽,梁建伟,郭芳,等.火花光谱自动分析技术在炼钢现场的应用[J].冶金分析,2008,28(9):20-24. CUI Jun,LIANG Jianwei,GUO Fang,et al.Application of automation analysis technology for spark source optical emission spectrum on the spot of steelmaking[J].Metallurgical Analysis,2008,28(9):20-24. [9] 李传启,杨崇秀.手持式X-射线荧光光谱仪在金属材料检测中的应用[J].广州化学,2016,41(6):29-33. LI Chuanqi,YANG Chongxiu.Application of handheld X-ray fluorescence spectrometer in detection of metallic materials[J].Guangzhou Chemistry,2016,41(6):29-33. [10] 沈克,张兆雄,张昌强,等.火花放电原子发射光谱分析中优先放电成因探讨[J].冶金分析,2016,36(10):1-9. SHEN Ke,ZHANG Zhaoxiong,ZHANG Changqiang,et al.Discussion on the phenomenon of preferential discharges in spark source atomic emission spectrometry[J].Metallurgical Analysis,2016,36(10):1-9. [11] 张永丰.火花源原子发射光谱单次火花放电行为探讨[J].冶金分析,2016,36(1):4-10. ZHANG Yongfeng.Investigation on the behavior of single spark discharge in spark source atomic emission spectrometry[J].Metallurgical Analysis,2016,36(1):4-10. [12] 贾云海,程海明,杨敬巍,等.火花放电原子发射光谱分析标准GB/T 14203—2016和GB/T 4336—2016修订要点及应用[J].冶金分析,2017,37(9):1-10. JIA Yunhai,CHENG Haiming,YANG Jingwei,et al.Key points and application of revised spark discharge atomic emission spectrometry standards including GB/T14203-2016 and GB/T4336-2016[J].Metallurgical Analysis,2017,37(9):1-10. [13] 孙晓飞,沈克,文孟喜,等.制定碳素钢火花放电原子发射光谱标准的精密度研究[J].冶金分析,2017,37(10):1-9. SUN Xiaofei,SHEN Ke,WEN Mengxi,et al.Study on the precision of spark discharge atomic emission spectrometry standard for carbon steel[J].Metallurgical Analysis,2017,37(10):1-9. [14] 王先逵.机械加工工艺手册:第2卷 加工技术卷[M].2版.北京:机械工业出版社,2007:1-26. [15] 国家质量监督检验检疫总局.GB/T 6060.2—2006 表面粗糙度比较样块 磨、车、镗、铣、插及刨加工表面[S].北京:中国标准出版社,2006.
