光谱学与光谱分析, 2015, 35 (1): 245, 网络出版: 2015-01-28  

工作曲线法和偏最小二乘回归分析在XRF定量分析软玉样品中的应用

Application of Calibration Curve Method and Partial Least Squares Regression Analysis to Quantitative Analysis of Nephrite Samples Using XRF
作者单位
1 中国科学院上海光学精密机械研究所科技考古中心, 上海 201800
2 敦煌研究院, 甘肃 敦煌 736200
摘要
由于块状固体标准玉石样品的缺乏, 造成了便携式X射线荧光分析技术(pXRF)利用工作曲线法对玉石文物样品进行无损定量分析的困难。试图寻找一种pXRF可采用, 但不需要块状固体玉石标准样品的定量分析方法。选取24件软玉样品, 其中17件为校准样品, 7件为测试样品。所有软玉样品利用质子激发X射线荧光分析技术(PIXE)获得定量分析结果。根据校准软玉样品的PIXE定量分析结果建立兴趣元素的工作曲线, 利用工作曲线对测试软玉样品进行定量分析;然后, 利用pXRF对所有软玉样品进行定性分析, 获得其定性分析图谱, 利用校准软玉样品的定性分析图谱和PIXE定量分析结果, 采用最小偏二乘法对测试软玉样品兴趣元素含量进行分析。最后, 将工作曲线法、PLS方法和PIXE的定量分析结果进行了相互对比。通过误差分析, 评估了工作曲线法和PLS方法定量分析软玉样品的精确度。结果表明, PLS方法可以代替工作曲线法对玉石类样品进行定量分析。
Abstract
The authors tried to find a method for quantitative analysis using pXRF without solid bulk stone/jade reference samples. 24 nephrite samples were selected, 17 samples were calibration samples and the other 7 are test samples. All the nephrite samples were analyzed by Proton induced X-ray emission spectroscopy (PIXE) quantitatively. Based on the PIXE results of calibration samples, calibration curves were created for the interested components/elements and used to analyze the test samples quantitatively;then, the qualitative spectrum of all nephrite samples were obtained by pXRF. According to the PIXE results and qualitative spectrum of calibration samples, partial least square method (PLS) was used for quantitative analysis of test samples. Finally, the results of test samples obtained by calibration method, PLS method and PIXE were compared to each other. The accuracy of calibration curve method and PLS method was estimated. The result indicates that the PLS method is the alternate method for quantitative analysis of stone/jade samples.

刘松, 苏伯民, 李青会, 干福熹. 工作曲线法和偏最小二乘回归分析在XRF定量分析软玉样品中的应用[J]. 光谱学与光谱分析, 2015, 35(1): 245. LIU Song, SU Bo-min, LI Qing-hui, GAN Fu-xi. Application of Calibration Curve Method and Partial Least Squares Regression Analysis to Quantitative Analysis of Nephrite Samples Using XRF[J]. Spectroscopy and Spectral Analysis, 2015, 35(1): 245.

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