火花放电原子发射光谱法分析铜锌钎料中铜锌锰结果稳定性的探讨
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摘要
铜锌钎料中Cu、Zn、Mn的化学成分测定长期采用化学湿法,但因为分析周期相对较长,很难满足现代生产企业对分析效率的要求。实验主要探讨了采用火花放电原子发射光谱法分析焊材铜锌钎料中Cu、Zn、Mn时,试样的制备、氩气输出压力、各项激发参数的设定等对Cu、Zn、Mn分析结果稳定性的影响。通过试验,确定镍基块状样品进行压样分析、采取酒精湿磨的样品表面处理方式;调节氩气输出压力为3.0MPa;选择光源分析参数中冲洗时间为4s、预燃时间为25s、积分时间为5s的改进措施。在优化的实验条件下,对1.5mm厚度铜锌钎料样品进行精密度考察,Cu、Zn、Mn测定结果的相对标准偏差(RSD,n=10)分别为0.14%、0.15%和0.98%;测定值与其他单位实验室提供的参考值一致。
The chemical composition of copper,zinc and manganese in copper-zinc brazing filler metal was usually determined by chemical wet method.But the analytical periods were relatively long,which could not meet the requirements of analysis efficiency in modern production enterprises.The influence factors on determination stability of copper,zinc and manganese in copper-zinc brazing filler metal by spark discharge atomic emission spectrometry were investigated,including the preparation of samples,the setting of argon output pressure and various excitation parameters.The following conditions were selected by experiments:the nickel-based block sample was prepared for analysis by tabletting method;the alcohol wet milling was selected for the sample surface treatment;the output pressure of argon was adjusted at 3.0 MPa;for light source analysis parameters,the flush time was 4 s,the pre-combustion time was 25 sand the integral time was 5 s.Under the optimized experimental conditions,the copper-zinc brazing filler metal with thickness of 1.5 mm was used for precision test.The relative standard deviation(RSD,n=10)of determination results was 0.14%,0.15%and 0.98%for copper,zinc and manganese,respectively.The found results were consistent with the reference values provided by other laboratories.
The chemical composition of copper,zinc and manganese in copper-zinc brazing filler metal was usually determined by chemical wet method.But the analytical periods were relatively long,which could not meet the requirements of analysis efficiency in modern production enterprises.The influence factors on determination stability of copper,zinc and manganese in copper-zinc brazing filler metal by spark discharge atomic emission spectrometry were investigated,including the preparation of samples,the setting of argon output pressure and various excitation parameters.The following conditions were selected by experiments:the nickel-based block sample was prepared for analysis by tabletting method;the alcohol wet milling was selected for the sample surface treatment;the output pressure of argon was adjusted at 3.0 MPa;for light source analysis parameters,the flush time was 4 s,the pre-combustion time was 25 sand the integral time was 5 s.Under the optimized experimental conditions,the copper-zinc brazing filler metal with thickness of 1.5 mm was used for precision test.The relative standard deviation(RSD,n=10)of determination results was 0.14%,0.15%and 0.98%for copper,zinc and manganese,respectively.The found results were consistent with the reference values provided by other laboratories.
引文
[1]文孟喜,孙晓飞,贾云海,等.火花放电原子发射光谱测定镍基合金中铁元素的校准曲线探讨[J].冶金分析,2018,38(2):9-17.WEN Meng-xi,SUN Xiao-fei.JIA Yun-hai,et al.Discussion on calibration curve for determination of iron in nickel based alloy by spark discharge atomic emission spectrometry[J].Metallurgical Analysis,2018,38(2):9-17.
[2]中华人民共和国质量监督检验检疫总局,国家标准化管理委员会.GB/T 6418-2008铜基钎料[S].北京:中国标准出版社,2009.
[3]中华人民共和国有色金属行业标准,国家发展和改革委员会.YS/T 482-2005铜及铜合金分析方法光电发射光谱[S].北京:中国标准出版社,2005.
[4]吴金龙,晁小芳,赵挺,等.样品形状对直读光谱分析结果的影响[J].检验检疫学刊,2013,23(3):15-18.WU Jin-long,CHAO Xiao-fang,ZHAO Ting,et al.The effect of shape of specimens on the results with directreading spark spectrometry[J].Journal of Inspection and Quarantine,2013,23(3):15-18.
[5]刘满雨,李振华,冯伟,等.火花放电原子发射光谱法分析带极堆焊熔敷金属中7种元素[J].冶金分析,2018,38(11):1-6.LIU Man-yu,LI Zhen-hua,FENG Wei,et al.Determination of seven elements in strip surfacing deposited metal by spark discharge atomic emission spectrometry[J].Metallurgical Analysis,2018,38(11):1-6.
[6]金献忠,蔡继杰,丘寅.纯铜带的电火花-直读光谱分析[J].检验检疫科学(Journal of Inspection and Quarantine Science),2010,10(3):18-48.
[7]孙晓飞,杨丹丹,文孟喜,等.经验系数-X射线荧光光谱法测定镁质耐火材料中10种组分[J].冶金分析,2017,37(5):12-18.SUN Xiao-fei,YANG Dan-dan,WEN Meng-xi,et al.Determination of ten components in magnesia refractory material by X-ray fluorescence spectrometry with empirical coefficient method.[J].Metallurgical Analysis,2017,37(5):12-18.
[2]中华人民共和国质量监督检验检疫总局,国家标准化管理委员会.GB/T 6418-2008铜基钎料[S].北京:中国标准出版社,2009.
[3]中华人民共和国有色金属行业标准,国家发展和改革委员会.YS/T 482-2005铜及铜合金分析方法光电发射光谱[S].北京:中国标准出版社,2005.
[4]吴金龙,晁小芳,赵挺,等.样品形状对直读光谱分析结果的影响[J].检验检疫学刊,2013,23(3):15-18.WU Jin-long,CHAO Xiao-fang,ZHAO Ting,et al.The effect of shape of specimens on the results with directreading spark spectrometry[J].Journal of Inspection and Quarantine,2013,23(3):15-18.
[5]刘满雨,李振华,冯伟,等.火花放电原子发射光谱法分析带极堆焊熔敷金属中7种元素[J].冶金分析,2018,38(11):1-6.LIU Man-yu,LI Zhen-hua,FENG Wei,et al.Determination of seven elements in strip surfacing deposited metal by spark discharge atomic emission spectrometry[J].Metallurgical Analysis,2018,38(11):1-6.
[6]金献忠,蔡继杰,丘寅.纯铜带的电火花-直读光谱分析[J].检验检疫科学(Journal of Inspection and Quarantine Science),2010,10(3):18-48.
[7]孙晓飞,杨丹丹,文孟喜,等.经验系数-X射线荧光光谱法测定镁质耐火材料中10种组分[J].冶金分析,2017,37(5):12-18.SUN Xiao-fei,YANG Dan-dan,WEN Meng-xi,et al.Determination of ten components in magnesia refractory material by X-ray fluorescence spectrometry with empirical coefficient method.[J].Metallurgical Analysis,2017,37(5):12-18.