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建立了利用激光诱导击穿光谱（LIBS）技术分析脐橙中Pb含量的多元线性回归定量分析模型. 选用脐橙中Ca Ⅱ 393.37 nm与Ca Ⅱ 396.84 nm特征谱线强度之和、Pb I 405.78 nm特征谱线强度、在405.03–405.96 nm范围内Pb元素的谱线积分强度作为自变量，得到了回归关联式，通过方差分析和回归统计验证了关联式的可行性. 结果表明，多元线性回归模型预测值与原子吸收光谱法检测值之间的相对误差最大值为12.99%，平均值为4.87%，并且利用这两种方法得到的结果拟合效果很好，拟合度达到0.995. 这说明多变量的定标法能比较充分地利用光谱中的信息，降低基体效应的影响，从而提高LIBS 定量分析的精确度，并对LIBS技术进一步应用于水果中重金属元素的定量检测提供了实验指导.The detection accuracy of laser induced breakdown spectroscopy (LIBS) is affected by system parameters, ambient gas, matrix effect, sample morphology, calibration methods etc. Heavy metals in Gannan navel orange are determined by LIBS in our laboratory. The experimental parameters are optimized. In this work, multivariate linear regression model is used to predict the concentration of Pb element in navel oranges. The real concentration of Pb is quantitatively determined by atomic absorb spectroscopy (AAS). The concentration is set as dependent variable, while the intensity of Pb I 405.78 nm, the intensity sum of Ca Ⅱ 393.37 nm and Ca Ⅱ 396.84 nm, and the integrated intensity in a range of 405.03-405.96 nm are taken as independent variable. The calibration results indicate that the maximum relative error between the predicted Pb concentration from the multiple linear regression model and the measured one by the AAS is 12.99%, and the average relative error of the samples is 4.87%. And the fitting degree of the results of two methods is 0.995. The result shows that the multivariate calibration method can utilize the information about the spectra and reduce the influence of the matrix effect. The multivariate linear regression model is proved to be feasible in improving the prediction accuracy of LIBS.
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Keywords:
- laser induced breakdown spectroscopy /
- navel orange /
- heavy metals /
- multiple linear regression
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[1] Lin Z X, Li J, Liu L M, Wu J Q 2009 High Power Laser and Particle Beams 21 817 (in Chinese) [林兆祥, 李捷, 刘林美, 吴金泉 2009 强激光与粒子束 21 817]
[2] Du C, Gao X, Shao Y, Song X W, Zhao Z M, Hao Z Q, Lin J Q 2013 Acta Phys. Sin. 62 045202 (in Chinese)[杜闯, 高勋, 邵妍, 宋晓伟, 赵振明, 郝作强, 林景全 2013 62 045202]
[3] Huang J S, Chen Q L, Zhou W D 2009 Spectrosc. Spect. Anal. 29 3126 (in Chinese) [黄基松, 陈巧玲, 周卫东 2009 光谱学与光谱分析 29 3126]
[4] Zhao F, Zhang Q, Xiong W, Rong J B, Li R H 2010 Environ. Sci. Technol. 33 137 (in Chinese) [赵芳, 张谦, 熊威, 容静宝, 李润华2010 环境科学与技术 33 137]
[5] Jiang J, Li G, Li R H, Chen Y Q 2011 High Power Laser and Particle Beams 23 2528 (in Chinese) [姜杰, 李关, 李润华, 陈钰琦 2011强激光与粒子束 23 2528]
[6] Yao S C, Lu J D, Lu Z M, Xie C L, Li J, Pan S H, Jiang M C, Li P 2009 Acta Opt. Sin. 29 1126 (in Chinese) [姚顺春, 陆继东, 卢志民, 谢承利, 李捷, 潘圣华, 蒋梅城, 李娉 2009 光学学报 29 1126]
[7] Cui Z F, Zhang X Y, Yao G X, Wang X L, Xu X S, Zheng X F, Feng E Y, Ji X H 2007 J. Atom. Mol. Phys. 24 25 (in Chinese) [崔执凤, 张先燚, 姚关心, 汪小丽, 许新胜, 郑贤锋, 凤尔银, 季学韩 2007 原子与分子 24 25]
[8] Liu J, Tao H Y, Gao X, Hao Z Q, Lin J Q 2013 Chin. Phys. B 22 044206
[9] Wang C L, Liu J G, Zhao N J, Ma M J, Wang Y, Hu L, Zhang D H, Yu Y, Meng D S, Zhang W, Liu J, Zhang Y J, Liu W Q 2013 Acta Opt. Sin. 33 033002 (in Chinese) [王春龙, 刘建国, 赵南京, 马明俊, 王寅, 胡丽, 张大海, 余洋, 孟德硕, 章炜, 刘晶, 张玉钧, 刘文清2013 光学学报 33 033002]
[10] Sun L X, Yu H B, Xin Y, Cong Z B 2010 Spectrosc. Spect. Anal. 30 3186 (in Chinese) [孙兰香, 于海斌, 辛勇, 丛智博 2010 光谱学与光谱分析 30 3186]
[11] Liu L T, Liu J G, Zhao N J, Chen D, Shi H, Wang C L, Zhang Y J, Liu W Q 2011 Chin. J. Lasers 38 115002 (in Chinese)[刘立拓, 刘建国, 赵南京, 陈东, 石焕, 王春龙, 张玉钧, 刘文清 2011 中国激光 38 115002]
[12] Wang Z, Feng J, Li L, Ni W, Li Z 2011 J. Anal. Atom. Spectrom. 26 2175
[13] Dong M L, Lu J D, Yao S C, Chen K, Li J, Li J Y 2012 J. Eng. Thermophys. 33 175 (in Chinese) [董美蓉, 陆继东, 姚顺春, 陈凯, 李军, 李俊彦 2012 工程热 33 175]
[14] Zhang X, Yao M Y, Liu M H 2013 Acta Phys. Sin. 62 044211 (in Chinese) [张旭, 姚明印, 刘木华 2013 62 044211]
[15] Fan W X, Li X Z, Jing R J 2006 Spectrosc. Spect. Anal. 26 567 (in Chinese) [范文秀, 李新峥, 荆瑞俊 2006 光谱学与光谱分析 26 567]
[16] Yao Y, Chen Y, Wang C, Qi J Y, Zhang P, Wang X N 2008 Food Sci. 29 386
[17] Xu L, Shao X G 2004 Methods of Chemometrics (Beijing: Science Press) p40 (in Chinese) [许禄, 邵学广 2004 化学计量学方法 (北京: 科学出版社) 第40页]
[18] Li Y 2011 Ph. D. Dissertation (Qingdao: Ocean University of China) (in Chinese) [李颖 2011 博士学位论文 (青岛: 中国海洋大学)]
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