摘要
在不经过任何预分离的情况下,结合紫外光谱法和化学计量学方法建立了水样中苯甲酸、苯酚、苯胺的同时测定方法。配制了在0~70 mg·L^-1范围内不同浓度的三组分混合水样共48份,其中70%的样本构成训练集,其余样本为独立测试集,在240~400 nm波长范围内测定各样品的紫外光谱。分别考察了四种光谱预处理方法、四种特征筛选方法及三种多元校正方法,最终确定苯甲酸、苯酚、苯胺的分析方法为:预处理分别采用Savitzky-Golay平滑、一阶导数及标准化;特征筛选方法分别为移动窗口偏最小二乘法(MWPLS)、无信息变量剔除法(UVE)及变量结合种群分析法(VCPA);多元校正方法均采用偏最小二乘法(PLS)。结果在独立测试集上三组分的预测误差均方根(RMSEP)分别为0.9716、0.7938、0.7652;将最佳模型用于水样加标回收,结果回收率为97.8%~103.8%,RSD<3%。紫外光谱法结合化学计量学方法可作为水样中多组分同时测定的一种简便、有效、快速的方法。
A simultaneous determination strategy of utilizing UV spectroscopy coupled with chemometrics was developed,through which the benzoic acid,phenol and aniline can be rapidly determined without any pre-separation.48 of samples were prepared in which the concentration of benzoic acid,phenol and aniline were ranged from 0 to 70 mg·L^-1,70%of the samples built the training set in the Monte Carlo sampling manner and the others formed independent test set,the UV spectra of the samples were measured in wavelength range of 240 nm^400 nm.For data analysis,4 of spectra preprocessing methods,4 of feature selection methods and 3 of multivariate calibration methods were investigated respectively.The optimum methods for benzoic acid,phenol and aniline data analysis were:Savitzky-Golay smoothing,first derivative and standardization for spectra preprocessing,Moving Window Partial Least Squares(MWPLS),Uninformative Variable Elimination(UVE)and Variable Combination Population Analysis(VCPA)for feature selection,and Partial Least Squares(PLS)for modeling methods on the 3 data sets,respectively.As results,the Root Mean Square Error of Prediction(RMSEPs)for the 3 components on independent test set was 0.9716,0.7938 and 0.7652.The optimum models were used for recovery test,the recovery of water sample is 97.8~103.8%,the RSDs of all elements are less than 3.0%.UV spectroscopy coupled with chemometrics may be used as simple,effective and rapid strategy for environment monitoring.
作者
张世芝
张明锦
ZHANG Shi-zhi;ZHANG Ming-jin(School of Chemistry and Chemical Engineering,Qinghai Nationalities University,Xining 810007,China;Key Laboratory of National Ethnic Affairs Commission of Resource Chemistry and Ecological Environment Protection on Qinghai-Tibet Plateau,Xining 810007,China;School of Chemistry and Chemical Engineering,Qinghai Normal University,Xining 810016,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2020年第11期1967-1972,共6页
Chemical Research and Application
基金
国家自然科学基金项目(51963018)资助。
关键词
苯系物
紫外光谱
化学计量学
同时测定
benzene series
ultraviolet spectroscopy
chemometrics
simultaneous determination
