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采用共轴双脉冲激光诱导击穿光谱（DP-LIBS）技术对3种植物油中的重金属铬（Cr）含量进行定量分析.对实验配制的24个样品，采用桐木木片对其中的Cr进行富集，烘干后进行LIBS试验.选取Cr I 425.39 nm为定量分析谱线，CN分子谱线（421.49 nm）、Ca原子谱线（422.64 nm）以及它们谱线强度之和为内标线，分别建立了Cr的基本定标法、单谱线内标法和双谱线内标法的定标曲线，并用验证样品对它们进行检验.研究结果表明，3种植物油的基本定标曲线的拟合度R2在0.97以上，低浓度验证样品预测的相对误差较大；采用单谱线内定标法时，定标曲线拟合度R2在0.98以上，验证样品预测的相对误差较基本定标法有所降低；采用双谱线内标时，大豆油、花生油和玉米油的内定标曲线拟合度R2分别为0.995，0.992和0.996，2个验证样品预测的相对误差分别为12.81%，1.73%，9.19%，6.05%和6.23%，6.69%.由此可见，采用双谱线内标法能有效减小定量分析误差，提高LIBS对植物油中Cr元素的预测能力.
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关键词:
- 双脉冲激光诱导击穿光谱 /
- 内定标法 /
- 植物油 /
- 铬
The safety quality of vegetable oil is very important for human life. The objective of this research is to determine the content of heavy metal chromium (Cr) in each of three kinds of vegetable oils (soybean oil, peanut oil, and corn oil) quantitatively by collinear double pulse laser-induced breakdown spectroscopy (DP-LIBS). In this study, a total of 24 vegetable oil samples are prepared, and each kind of vegetable oil has 8 samples. Fortune paulownia wood chips with a diameter of 20 mm and thickness of 3 mm are placed into the vegetable oil samples to collect the Cr element. After that, the 24 samples (fortune paulownia wood chips that have enriched Cr element) are dried in the oven, and the LIBS spectra of samples are acquired in a wavelength range of 206.28-481.77 nm by a dual-channel high-precision spectrometer. The spectral line of Cr (Cr I 425.39 nm) is chosen as the quantitative analysis spectral line, while CN (CN 421.39 nm) molecular spectral line, Ca (Ca I 422.64 nm) atomic spectral line and the sum of their spectral line intensities are selected as the internal standard lines. Then the calibration curves of Cr are obtained by the basic calibration method, single-line internal standard method (CN 421.39 nm or Ca I 422.64 nm as the internal standard line) and dual-line internal standard method (CN 421.39 nm and Ca I 422.64 nm as the internal standard lines). Finally, the validation samples are used to verify the performances of the calibration curves of Cr element. The results show that the values of fitting degree (R2) of the basic calibration curves for three kinds of vegetable oils are all above 0.97, and the relative errors of validation samples with low concentration are bigger than those with high concentration. The values of (R2) of calibration curves obtained by single-line internal standard method are above 0.98, and the relative errors of validation samples are lower than those obtained using basic calibration method. And the values of (R2) of calibration curves for soybean oils, corn oils and peanut oils are 0.995, 0.992 and 0.996, respectively, with using dual-line internal standard method. The relative errors between the two validation samples are 12.8%, 1.73%, 9.19%, 6.05% and 6.23%, 6.69%, respectively. And the results obtained by the dual-line internal standard method are better than those obtained by the basic calibration method and single-line internal standard method. Thus it can be seen that the dual-line internal standard method can reduce the error of quantitative analysis effectively and improve the predicting ability of LIBS technique for Cr element detection in vegetable oil.-
Keywords:
- double pulse laser-induced breakdown spectroscopy /
- internal standard method /
- vegetable oil /
- chromium
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[1] Yao Z Q 2011Studi.Trace Elem.Heal. 28 67(in Chinese)[姚智卿2011微量元素与健康研究28 67]
[2] Wu J M, Cheng S G 2009Modern Preven.Medic. 36 4610(in Chinese)[吴继明, 程胜高2009现代预防医学36 4610]
[3] Sweetapple M T, Tassios S 2015Am.Mineral. 100 2141
[4] Hu L, Zhao N J, Liu W Q, Fang L, Wang Y, Meng D S, Yu Y, Gu Y H, Wang Y Y, Ma J M, Xiao X, Wang Y, Liu J G 2015Acta Opt.Sin. 35 0630001(in Chinese)[胡丽, 赵南京, 刘文清, 方丽, 王寅, 孟德硕, 余洋, 谷艳红, 王园园, 马明俊, 肖雪, 王煜, 刘建国2015光学学报35 0630001]
[5] Liu Y F, Ding Y J, Peng Z M, Huang Y, Du Y J 2014Acta Phys.Sin. 63 205205(in Chinese)[刘玉峰, 丁艳军, 彭志敏, 黄宇, 杜艳君2014 63 205205]
[6] Hu Z Y, Zhang L, Yin W B, Ma W G, Dong L, Jia S T 2013J.Atmo.Environ.Optics 8 26(in Chinese)[胡志裕, 张雷, 尹王保, 马维光, 董磊, 贾锁堂2013大气与环境光学学报8 26]
[7] Yuan T B, Wang Z, Li Z, Ni W D, Liu J M 2014Anal.Chim.Acta 807 29
[8] Ma F Y, Dong D M 2014Food Anal.Method 7 1858
[9] Gondal M A, Hussain T, Yamani Z H, Baig M A 2006Talanta 69 1072
[10] Wu J L, Fu Y X, Li Y, Lu Y, Cui Z F, Zheng R R 2008Spectrosc.Spect.Anal. 28 1979(in Chinese)[吴江来, 傅院霞, 李颖, 卢渊, 崔执凤, 郑荣儿2008光谱学与光谱分析28 1979]
[11] Zhao F, Zhang Q, Xiong W, Rong J B, Li R H 2010Environ.Sci.Tech. 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]
[12] Xu Y, Yao M Y, Liu M H, Lei Z J, Peng Q M, Zhang X, Chen T B 2011Acta Opt.Sin. 31 1230002(in Chinese)[徐媛, 姚明印, 刘木华, 雷泽剑, 彭秋梅, 张旭, 陈添兵2011光学学报31 1230002]
[13] Xu L, Wang L, Yao G X, Wang C H, Ji X H, Zhang X, Cui Z F 2012J.Anhui Normal Univ.(Nat.Sci.) 35 438(in Chinese)[徐丽, 王莉, 姚关心, 王传辉, 季学韩, 张先, 崔执凤2012安徽师范大学学报(自然科学版)35 438]
[14] Wu Y Q, Sun T, Liu X H, Mo X X, Liu M H 2016Laser Optoelectro.Progress 53 043001(in Chinese)[吴宜青, 孙通, 刘秀红, 莫欣欣, 刘木华2016激光与光电子学进展53 043001]
[15] Mousavi S J, Farsani M H, Darbani S M R, Asadorian N, Soltanolkotabi M, Majd A E 2015Appl.Opt. 54 1713
[16] Angel F B, Tomas D, Patricia L, Laserna J J 2013Spect.Acta Part B 89 77
[17] Liu M H 2011Technology and Application of Optical Nondestructive Inspecting Quality and Safety for Agricultural Products(Wuhan:Huazhong University of Science and Technology press) pp70-71(in Chinese)[刘木华2011农产品质量安全光学无损检测技术及应用(武汉:华中科技大学出版社)第70-71页]
[18] Liu L 2015Laser Tech. 39 90(in Chinese)[刘莉2015激光技术39 90]
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