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摘要本论文检测PAEs中较常见的四种：邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二(2-乙基己基)酯（DEHP），采用固相微萃取（SPME）和固相萃取（SPE）法对水样进行预处理，采用GC-ECD法进行检测。首先对预处理条件进行探索，再确定ECD检测器的条件。通过混合标准系列溶液（内标法定量）的测定，建立起不同预处理方法下的标准曲线，相关性较好，相关系数达到0.99以上。根据实验数据测得SPME法和SPE法的检出限、精密度、准确度，并将两者进行对比。结果表明，SPME法比SPE法的精密度和准确度都略高。采集紫霞湖和秦淮河的水样进行检测，测得紫霞湖中DMP含量8.137457~8.847777μg/L，DEP含量11.09521~12.27μg/L，DBP含量7.490424~7.61214μg/L，DEHP含量32.25796~35.6669μg/L；秦淮河中DMP含量5.784444~6.097905μg/L，DEP含量11.265295
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~13.28083μg/L，DBP含量17.91991~18.5242μg/L，DEHP含量15.211994~17.76818μg/L。与国家标准及其他水体中含量进行比较，发现紫霞湖和秦淮河水体中PAEs的含量较高，需引起相关部门的注意。8785
关键词：邻苯二甲酸酯，HS-SPME-GC-ECD，SPE-GC-ECD，检测
毕业设计说明书（论文）外文摘要
Title Study on the Detection Methods of Phthalic Acid Esters in Water
Abstract
Four common PAEs: Dibutyl phthalate (DBP), Diethyl phthalate (DEP), Dimethyl phthalate (DMP) and Di 2-Ethyl Hexyl Phthalate (DEHP) were detected in this experiment. The samples were pretreated by using SPME and SPE, and determined by using GC-ECD. First, the operating conditions of pretreatment were determined. Then the related testing conditions of GC-ECD were tested. By detecting the blended standard solutions (quantified by internal standard method), standard curves under defferent pretreatments with high correlation up to 99 percent were built. Compared the detection limits, precisions and accuracies. of defferent pretreatments based on the experimental data, it turned out that the precision and accuracy of SPME was higher than that of SPE.
The water samples from Zixia lake and Qinhuai river were detected. The concentrations of DMP,DEP,DBP and DEHP in Zixia lake were 8.137457~8.847777μg/L, 11.09521~12.27μg/L, 7.490424~7.61214μg/L and 32.25796~35.6669μg/L. The concen -trations of DMP, DEP, DBP and DEHP in Qinhuai river were 5.784444~6.097905μg/L, 11.265295~13.28083μg/L, 17.91991~18.5242μg/L and 15.211994~17.76818μg/L. Compared the results with the national standard and the data of other waters, it was found out that the concentrations of PAEs in the Zixia lake and Qinhuai river were higher. The related departments should pay attention to this situation.
Keywords: PAEs, HS-SPME-GC-ECD, SPE-GC-ECD, Detection
目 次
1 绪论 1
1.1 研究背景 1
1.2 邻苯二甲酸酯检测分析方法的研究进展 2
1.3 本课题的研究内容与意义 4
2 实验原理 6
2.1 预处理方法 6
2.2 检测方法 7
3 实验部分 9
3.1 试剂与仪器 9
3.2 HS-SPME-GC-ECD过程 10
3.3 SPE-GC-ECD过程 12
4 实验结果与讨论 14
4.1 实验条件的确定 14
4.2 定性分析 20
4.3 标准曲线 22
4.4 方法的检出限 29
4.5 精密度 30
4.6 准确度 32
4.7 实际水样的测定 33