摘要本文采用磁性分子印迹聚合物法富集、高效液相色谱法检测水体中的壬基酚(NP)。首先对富集条件参数:富集温度、富集时间、盐析效应、pH;高效液相色谱法相关条件参数:进样量、流动相比例、柱温进行研究。确定了磁性分子印迹聚合物法的富集温度为25℃,富集时间为300min,氯化钠的浓度为300mg/L,pH=6;高效液相色谱条件:进样量为150μL,流动相甲醇:水=9:1,柱温为25℃。其检出限为0.285mg/L;测得的1mg/L、20mg/L、50mg/L精密度RSD分别是2.53%、1.16%和2.33%;M-MIP的自来水加标回收率在90%~120%之间;M-NIP的自来水加标回收率在60%~100%。18917
对所采集的环境水样的检测结果显示:在河水和湖水中的M-MIP的加标回收率为94.0%~98.2%,M-NIP的加标回收率为61.2%~92.4%。
关键词 壬基酚 磁性分子印迹聚合物 高效液相色谱法 检测
毕业设计说明书(毕业论文)外文摘要
Title Enrichment And Analysis of Nonylphenol in Water
Abstract
In this paper, Nonylphenol(NP) was enriched using magnetic molecularly imprinted polymer (M-MIP) and was detected by high performance liquid chromatography (HPLC). First, the operating conditions of enrichment were optimized, including temperature, enrichment time, salting-out effect and pH. The related testing conditions of HPLC were tested, including the injection volume, the proportion of the mobile phase and column temperature. And the results showed that the best conditions were 25℃ of enrichment temperature, 300 min of enrichment time , 300mg/L of the concentration of sodium chloride and pH=6.HPLC conditions for injection volume were 150μL, mobile phase of methanol: water =9:1 and column temperature was 25 ℃. The detection limit was 0.285mg/L, precision (RSD, n=7of 1mg/L, 20mg/L, 50mg/L) were 2.53%, 1.16% and 2.33% respectively, spiked recovery of M-MIP in water was 90% ~120% and spiked recovery of M-NIP in water is 60% ~100%.
Then the method was used to determine NP in water samples collected from river and lake. The results showed that the spiked recovery of M-MIP was 94.0%~98.2%, the spiked recovery of M-NIP was 61.2%~92.4%。
Keywords Nonylphenol(NP) HPLC M-MIP Determination
目次
1 引言 1
1.1课题研究的目的、意义及背景 1
1.2壬基酚的富集和检测方法的研究进展 1
1.3研究工作的主要内容 3
2 理论部分 5
2.1磁性分子印迹聚合物 5
2.2高效液相色谱法 6
3 实验部分 7
3.1实验试剂和仪器设备 7
3.1.1实验试剂 7
3.1.2实验设备 7
3.1.3标准系列溶液的制备 8
3.2水样的采集和保存 8
3.3样品的预处理 8
3.4高效液相色谱条件的确定 9
3.4.1流动相比例的确定 9
3.4.2柱温的选择 9
3.4.3进样量的影响 9
3.4.4初始浓度的影响 9
3.5富集条件的确定 9
3.5.1富集温度的选择 9
3.5.2盐析效应的影响 9
3.5.3 pH对实验的影响 10
3.5.4富集时间的影响 10
3.5.5洗脱时间的影响 10
4 实验结果与讨论 11
4.1M-MIP的SEM图 11
4.2实验条件可能性的讨论 11
4.2.1壬基酚的紫外吸收图 11
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