光谱学与光谱分析, 2011, 31 (12): 3289, 网络出版: 2012-01-05
自由定标激光诱导击穿光谱技术在炉渣成分定量分析中的应用
Quantitative Analysis of Slag by Calibration-Free Laser-Induced Breakdown Spectroscopy
自由定标 激光诱导击穿光谱 炉渣 定量分析 多元素分析 Calibration free Laser-induced breakdown spectroscopy (LIBS) Slag Quantitative analysis Multi-elements analysis
摘要
采用自由定标激光诱导光谱技术(CF-LIBS)对炉渣中几种主要成分(CaO, SiO2, Al2O3, MgO)进行了定量分析。 利用Nd∶YAG激光脉冲在空气中烧蚀炉渣样品产生等离子体, 等离子体光谱由中阶梯光栅光谱仪记录。 通过几种主要元素的原子谱线和离子谱线的玻尔兹曼图, 计算了等离子体的温度。 利用Ca的一条谱线Stark展宽估算了等离子体电子密度, 从而验证了实验中等离子体处于局部热平衡的假设是成立的。 在此基础上使用自由定标算法, 得出了几种元素的质量百分比, 进而反演出几种氧化物的含量。 对炉渣中主量成分的测量结果相对误差在15%以内。 实验结果表明CF-LIBS方法可以用于无标准物质的样品的多元素同时快速测定。
Abstract
Calibration-free laser induced breakdown spectroscopy (CF-LIBS) was employed for the quantitative analysis of slag. Nd∶YAG laser ablation was performed in air. The laser-induced plasma emission was measured by an Echelle spectrometer equipped with an ICCD. The plasma temperature and electron number density were determined from Boltzmann plots and a CaⅠ line width, respectively. The assumption of local thermal equilibrium was validated by the Ne criterion. The concentration of oxides was obtained from the concentration of elements by using stoichiometric relation. The calculated oxide concentrations were compared with those obtained by XRF. The relative errors of major elements were less than 15%. The results indicate that this method can be employed for the analysis of major elements in multi-component complex materials without certified reference.
陈兴龙, 董凤忠, 王琦, 余嵘华, 梁云仙, 王静鸽, 杨阳, 倪志波, 徐明明, 吴边. 自由定标激光诱导击穿光谱技术在炉渣成分定量分析中的应用[J]. 光谱学与光谱分析, 2011, 31(12): 3289. CHEN Xing-long, DONG Feng-zhong, WANG Qi, YU Rong-hua, LIANG Yun-xian, WANG Jing-ge, YANG Yang, NI Zhi-bo, XU Ming-ming, WU Bian. Quantitative Analysis of Slag by Calibration-Free Laser-Induced Breakdown Spectroscopy[J]. Spectroscopy and Spectral Analysis, 2011, 31(12): 3289.