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摘要本毕业论文采用顶空固相微萃取(HS-SPME)、气相色谱电子捕获型检测器(GC-ECD)的方法检测环境水体中的壬基酚（NP）和双酚A（BPA）。首先对HS-SPME的条件参数：萃取温度、萃取时间、盐析效应、pH；衍生化的条件参数：衍生剂用量、衍生化时间；GC-ECD的相关条件参数：进样口温度、解析时间进行了研究。确定了HS-SPME的萃取温度为65℃，萃取时间为40min，NaCl投加量为6g，pH=2；衍生化的衍生剂用量为15µL，衍生时间为5min；GC-ECD的进样口温度为280℃，解析时间为5min。使用确定的方法及参数检测水中的NP和BPA，其检出限分别为NP 0.07µg/L，BPA 2.43µg/L。加标回收率为91.95%～121.85%。相对标准偏差为5.47%～6.17%。8659
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对所采集的环境水样的检测结果显示，紫霞湖、秦淮河和实验室自来水样品中，NP的含量范围为1.58～4.55µg/L，BPA的含量范围为：2.70～3.64µg/L。
此外，本文还进行了非对称场离子迁移谱（FAIMS）对于NP和BPA检测的可行性研究。
关键词：壬基酚 双酚A HS-SPME-GC-ECD FAIMS 检测
毕业设计说明书（论文）外文摘要
Title Study on the Determination of NP and BPA in Water
Abstract
NP and BPA in water sample were determined by using HS-SPME-GC-ECD. First, the operating conditions of SPME were optimized, including extraction temperature, extraction time, salting-out effect and pH. The conditional parameters of derivatization including derived dosage and derivatization time were also determined. Furthermore, the related testing conditions of GC-ECD were tested, including temperature of injection port and desorption time. And the results show that the best conditions of SPME are extraction temperature 65℃, extraction time 40 min, amount of NaCl 6g ,and pH=2:The concentrated endocrine chemicals were chemically derived by 15µL BSTFA for 5 min: and the testing conditions of GC-ECD were: injection port temperature 280℃,and desorption time 5 min. The detection limits for NP and BPA are 0.07µg/L, 2.43µg/L respectively. Standard deviation of them is within 5.47% and 6.17%.
Then the method was used to determine NP and BPA in water samples collected from Zixia river, Qinhuai river and tap water. The results show that the concentration of NP is from 1.58µg/L to 4.55µg/L and the concentration of BPA is from 2.70µg/L to 3.64µg/L.
In addition, the possibility of determining NP and BPA by high-field asymmetric ion mobility spectrometry (FAIMS) was also studied in this paper.
Keywords Nonylphenol (NP) Bisphenol A (BPA) HS-SPME-GC-ECD
FAIMS Determination
目 次
1 绪论 1
1.1 课题研究的目的、意义及背景 1
1.2 目前壬基酚，双酚A的研究进展 2
1.3 研究工作的主要内容 5
2 实验原理 6
2.1 衍生化试剂（BSTFA）反应机理 6
2.2 顶空-固相微萃取(HS-SPME)原理 6
2.3 GC/ECD原理 8
2.4 FAIMS检测原理 10
3 实验部分 12
3.1 实验试剂及仪器设备 12
3.1.1 实验试剂 12
3.1.2 仪器设备 12
3.1.3 混合标准系列溶液的制备 13
3.2 水样的采集与保存 13