光谱学与光谱分析, 2020, 40 (9): 2974, 网络出版: 2020-12-01  

便携式能量色散X射线荧光光谱法对钢铁材料中的镧和铈的快速检测

The Rapid Detection of La and Ce in Steel Materials by Portable EDXRF
作者单位
1 钢铁研究总院, 北京 100081
2 钢研纳克检测技术股份有限公司, 北京 100094
3 北方工业大学电气与控制工程学院, 北京 100144
摘要
稀土元素具有独特的电子结构, 化学性质活泼, 是冶金工业中重要的添加剂, 在许多领域发挥了重要的作用。 稀土添加剂不仅可以作为脱氧剂和脱硫剂对钢液进行净化, 还会对钢材产生变质作用和合金化作用, 改善钢组织, 提升钢种的性能。 但是钢铁材料中稀土元素的含量添加只有在一定范围内, 才会表现出较好的性能。 而通常使用电感耦合等离子体质谱法和电感耦合等离子体发射光谱法对钢铁材料中稀土元素进行检测, 这两种方法均需要对样品进行消解处理, 操作繁琐, 测试周期长。 使用便携式能量色散X射线荧光光谱法可以实现钢铁材料中稀土元素镧和铈的快速检测, 且整个仪器重量小于10 kg, 便于现场应用。 在传统便携式仪器的基础上, 使用大功率的光管对稀土元素的K系谱线进行激发, 与选择L系谱线进行分析对比, 不仅提高了谱线强度, 同时还避免了钢铁材料中其他常见组分对待测元素谱峰的重叠干扰。 测试时间设置为120 s, 通过研究不同的管电流和管电压研究峰强度和峰背比的变化情况, 最终选择800 μA和65 kV对样品进行激发。 使用参考物质绘制工作曲线, 同时使用背景强度对基体效应进行校正后, 镧和铈的线性相关系数分别可达到0.999 2和0.998 8; 对含量较低的参考样品GBW01135进行测试, 计算方法的检出限和定量限, 镧和铈的检出限分别为0.001 1%和0.000 5%, 定量限分别为0.003 8%和0.001 6%, 满足实际样品的测试需求。 使用样品GBW01132a进行11次连续测定, 对测试结果的稳定性进行研究, 镧和铈的相对标准偏差分别为2.42%和2.00%; 同时对测试结果的准确性进行研究, 对多个样品进行测试并与参考值进行对比, 结果表明除了一个低于检出限的样品之外, 其余样品的相对误差均小于20%,其中70%的样品的相对误差小于10%。 能量色散X射线荧光光谱法可实现钢铁材料中稀土元素的快速检测, 样品只需要简单的打磨处理就可以直接进行测试, 对进一步研究钢铁材料的性能具有一定的意义。
Abstract
Rare earth elements, with their unique electronic structure and active chemical properties, are important additives in the metallurgical industry and play an important role in many fields. Not only can rare earth additives be used as deoxidizer and desulfurized to purify the molten steel, but also have metamorphism and alloying effects on the steel, which can improve the structure and performance of the steel materials. However, only with a certain range can the addition of rare earth elements in steel materials shows good properties. Although inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry are usually used to detect rare earth elements in steel materials, which require sample digestion and tedious operations for a long test period. In this study, portable energy dispersive X-ray fluorescence spectrometry was used to realize the rapid detection of lanthanum and cerium in steel materials, and the whole weight of the instrument is less than 10 kg, which is convenient to test on-site. Compared with selecting L series lines for analysis and testing in the traditional portable instrument, a high-power X-ray tube is used to excite the K series spectral lines for rare earth elements, which can increase the intensity of analyzed peaks and avoid overlap interference of other common components in steel materials. The intensity and peak-to-background ratio were studied at different X-ray tube current and voltage when the measured time was set at 120s, and finally, the optimized parameters were chosen as 800 μA and 65 kV for irradiating samples. The calibration curves were drawn with reference materials, and the linear correlation coefficients of lanthanum and cerium were 0.999 2 and 0.998 8 respectively, after the correction of matrix effect by the intensity of the background. Reference samples of GBW01135 were chosen to calculate the detection limit and quantitation limit because both the content of La and Ce were of low content. Moreover,the detection limit of La and Ce was 0.001 1% and 0.000 5% respectively, and the quantitation limit was 0.003 8% and 0.001 6%, which satisfied the requirement of the actual test. The stability of the test was studied by 11 consecutive measurements for the sample of GBW01132a, and the relative standard deviation was 2.42% and 2.00% for La and Ce. Furthermore,the accuracy of the test results was also studied by testing multiple samples and comparing with reference values. The results showed that the relative error of the results were less than 20% except for one sample which was below the detection limit, and the relative error of more than 70% samples were less than 10%. The energy dispersive X-ray fluorescence spectrometry can realize the rapid detection of rare earth elements in steel materials, and the samples can be directly tested with simply polishing pretreatment, which is of certain significance for further research on the properties of steel materials.

倪子月, 程大伟, 刘明博, 韩冰, 李小佳, 陈吉文. 便携式能量色散X射线荧光光谱法对钢铁材料中的镧和铈的快速检测[J]. 光谱学与光谱分析, 2020, 40(9): 2974. NI Zi-yue, CHENG Da-wei, LIU Ming-bo, HAN Bing, LI Xiao-jia, CHEN Ji-wen. The Rapid Detection of La and Ce in Steel Materials by Portable EDXRF[J]. Spectroscopy and Spectral Analysis, 2020, 40(9): 2974.

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