【作者】 闫兴菊；

【导师】 法焕宝；

【作者基本信息】 重庆大学 ， 化学， 2010， 硕士

【摘要】 随着人类活动和工业的迅速发展,大量的废水、废气、废渣排放到环境中,同时大量的农药、难分解物、重金属离子等也被排放到土壤、水层之中,环境污染正一步步影响着人们的生活质量。2008年中国三鹿奶粉事件风靡全球;而重金属离子也是一类对人类有害的污染物;这些污染物都是在含量很低时就会对人体造成巨大的危害。因此,对三聚氰胺、重金属离子建立痕量检测水平分析有着很大的必要性和重要性。紫外可见分光光度法具有操作简便、灵敏度高、利于回收、检测限低等优点,是常用的痕量分析手段之一。卟啉是一类有着优良光电性能的有机半导体材料,在近代化学研究中受到了广大科研工作者的广泛关注。目前已被应用到各个领域。特别在光化学分析中,卟啉有灵敏度高、选择性好、稳定性高等优点。在本课题的研究中,我们首先以苯甲醛、对羟基苯甲醛、新蒸吡咯等为原料,利用Alder一步合成法合成了组成相似而结构和功能不同的meso位系列羟基卟啉。并用柱层析成功分离了不同数目的羟基卟啉,探索并找到了合适的洗脱剂配比。通过紫外、红外、核磁、元素分析等对系列羟基卟啉的结构进行了表征确认,探索有机合成的机理和分离方法。在成功合成并分离系列羟基卟啉后,我们利用系列羟基卟啉为显色剂,用紫外分光光度法对三聚氰胺、重金属铅、汞离子做了痕量检测。研究了表面活性剂、显色剂、温度以及时间等对显色反应的影响,找到了各自的最低检测限,建立了良好的线性关系。对比分析数据,找出各自的检测范围和检测效果最好的卟啉显色剂。紫外检测具有操作简便、利于回收、数据重复性好等优点,实验为其他农药残留、重金属检测等提供了理论依据和数据参考。更多还原

【Abstract】 A large number of wastewater, waste gas and waste residue were discharged to the environment with human activities and the rapid development; and now the pollution is affecting the quality of people’s life seriously. A lot of harmful pollutants such as pesticides ,difficult decomposed products and heavy metal ions are released into the soil and the rivers at the same time. China’s Sanlu milk powder is known by the world in 2008. Heavy metal ions are potentially harmful and important pollutants, and it can cause environmental pollution even at low level. So it is a great significance to establish the trace analysis determination technology of melamine and heavy metal ions. UV-visible spectrophotometry is commonly used to trace analysis for the advantages of its high sensitivity, high recovery, low detection and simple operation.The porphyrin compounds are organic semiconductor materials that have excellent optical properties. It has been widespread attended in modern chemical research by more and more scientists. They have been applied to various fields especially in the photochemical analysis because of high sensitivity, good selectivity and high stability.In our researchs, we synthesized six kinds of different porphyrins by using of benzaldehyde, p-hydroxybenzaldehyde and the new steamed pyridyl. These six differert kinds of compounds have similar structures but different characters. And then we separate and purify them through column chromatography. At last we characterized six compounds by elemental analysis, 1HNMR, UV-vis and IR,spectrum, respectively, which proved that these compounds are the target products.We explored the mechanism of organic synthesis and separation methods through column chromatography.The complexing reaction of melamine and metal ions (lead and mercury) with six different porphyrins were studied with spectrophotometric analysis method. The affection of the Tween-80, NaOH, tempertrue and time of the reactions were studied. The detection limits of melamine ,lead and mercury were calculated and the results also obeyed the Beer’s law.The data would provid a beneficial reference in the detection of pesticide residuses and metal ions.更多还原