| 直流电弧原子发射光谱法测定钛和钛合金中微量杂质元素 |
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| 引用本文： | 王辉,马晓敏,郑伟,王宽.直流电弧原子发射光谱法测定钛和钛合金中微量杂质元素[J].岩矿测试,2014,33(4):506-511. |
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| 作者姓名： | 王辉 马晓敏 郑伟 王宽 |
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| 作者单位： | 西北有色金属研究院, 陕西 西安 710016;西北有色金属研究院, 陕西 西安 710016;西北有色金属研究院, 陕西 西安 710016;西北有色金属研究院, 陕西 西安 710016 |
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| 摘 要： | 高纯度的钛及钛合金具有良好的可塑性,当有杂质存在时变得脆而硬而影响其性能,准确分析杂质元素的含量有利于对钛生产工艺进行质量控制。对于杂质元素的分析,现行国家标准方法是采用样品蒸发温度较高的直流电弧作为光源,摄谱仪测定,需要经过显影、定影、测量黑度等步骤,操作繁琐,流程长,测量误差较大。本文应用中阶梯光栅和电荷耦合器件(CCD)组成的直流电弧(DC Arc)原子发射光谱仪(波长范围200~800nm),谱线干扰分析和谱线强度测量可以同时进行,能更大限度地获取光谱信息,建立了快速测定钛及钛合金中10种微量杂质元素(锰锡铬镍铝钼钒铜锆钇)的分析方法。实验讨论了测定过程中的四类谱线干扰,包括钛作为基体元素的谱线干扰、钛合金中添加的化学成分元素干扰、铁谱线的干扰、杂质元素之间的干扰,确定了适当的分析线;并应用一种浅孔薄壁细颈杯形电极装入试样,提高了样品的蒸发效果;用氯化银和碳粉的混合物作缓冲剂,提高了待测元素的谱线强度。本方法的检测范围为0.001%~0.06%,精密度小于15%,回收率为90.0%~110.0%,适合于大批量钛及钛合金样品中杂质元素的同时检测。
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| 关 键 词： | 钛及钛合金 杂质元素 原子发射光谱法 直流电弧 电荷耦合器件 |
| 收稿时间： | 2013/5/10 0:00:00 |
| 修稿时间： | 2014/1/20 0:00:00 |
Determination of 10 Trace Impurity Elements in Titanium and Titanium Alloys with DC Arc Atomic Emission Spectrometry |
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| WANG Hui,MA Xiao-min,ZHENG Wei and WANG Kuan.Determination of 10 Trace Impurity Elements in Titanium and Titanium Alloys with DC Arc Atomic Emission Spectrometry[J].Rock and Mineral Analysis,2014,33(4):506-511. |
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| Authors: | WANG Hui MA Xiao-min ZHENG Wei and WANG Kuan |
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| Institution: | Northwest Institute for Non-ferrous Metal Research, Xi'an 710016, China;Northwest Institute for Non-ferrous Metal Research, Xi'an 710016, China;Northwest Institute for Non-ferrous Metal Research, Xi'an 710016, China;Northwest Institute for Non-ferrous Metal Research, Xi'an 710016, China |
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| Abstract: | High purity titanium and titanium alloy have good plasticity, but with the presence of impurity, their performance will become brittle and hard. The accurate quantitative analysis of impurity elements is useful for carrying on the quality control of titanium products. For analysis of impurity elements, in the current national standard method, DC Arc was used as an excitation source with a higher evaporation temperature, the spectrograph process includes developing, fixing, blackness measurement and other steps, the procedure is too complicated and tedious with large measurement error. In this paper, DC Arc Atomic Emission Spectrometer (wavelength range of 200-800 nm) equipped with echelle grating and charge-coupled detector (CCD) is applied, the spectral lines interference analysis and spectral intensity measurement can be conducted at the same time, and the instrument provides more spectral information. Based on this, a rapid analysis method for 10 trace elements (Mn, Sn, Cr, Ni, Al, Mo, V, Cu, Zr, Y) in titanium and titanium alloy was been established. In the process of experiments, four types of spectral interference from titanium matrix, added chemical component elements, iron and impurity elements were studied, and the appropriate analytical were determined. Meanwhile, through application of a kind of shallow, thin and narrow cup-shaped electrode as working electrode, evaporation of sample was improved. With a mixture of AgCl and carbon powder used as buffer, the spectral line intensity of the measured elements was increased. The detection range of the method is 0.001%-0.06%, the precision is less than 15%, the recoveries are 90.0%-110.0%. The method is suitable for simultaneous determination of impurity elements in large quantities of titanium and titanium alloy samples. |
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| Keywords: | titanium and titanium alloys impurity elements Atomic Emission Spectroscopy DC Arc charge-coupled device |
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