综合试验报告.docVIP

综合实验报告 题目：阿司匹林的合成，表征及含量的测定 姓名：裴 童 专业班级：工业分析02班 学号：0906060215 同组者：杨盼 张笑颖 指导老师：万其进 李伟 2011年10月3日 目录 摘要 ················································· 1 中文摘要············································· 2 英文摘要············································· 3 前言 ················································· 4 阿司匹林简介 ······································· 5 阿司匹林性质········································ 6 阿司匹林常见的合成方法····························· 7 本实验中采用的合成法······························· 8 部分实验原理 ······································ 9 实验内容 ········································· 10 实验仪器与设计····································· 11 阿司匹林的合成步骤································· 12 阿司匹林的熔点测定································· 13 红外光谱法鉴定产物································ 14 紫外分光光度法制定阿司匹林的含量················· 15 酸碱滴定法测定阿司匹林含量························ 16 结果与讨论 ·····································17 熔点测定表征产物··································· 18 红外光谱法表征产物································· 19 紫外分光光度法测定阿司匹林含量··················· 20 酸碱滴定法测定阿司匹林含量························ 21 结论与建议 ···································· 22 参考文献 ········································ 23 摘要：在浓硫酸介质中，水杨酸和乙酸酐发生乙酰化发硬生成乙酰水杨酸（阿司匹林），副产物品可采用饱和NaHCO3溶液洗涤及乙酸乙酯重结晶而除去。乙酰水杨酸具有一系列特殊结构，在红外光谱图可出现多个特征振动频率。比较产品和标准的红外光谱图，同时结合产品的熔点，可对合成的产品进行鉴定。水杨酸含有苯环，在紫外光照射下会产生芳香族化合物的特征吸收B带和E带。其中E2带由于共轭效应红移。此外，水杨酸还含有羧基和羟基，可以产生K带和R 带吸收。谱图中可以出现K带R带和B带吸收，K带吸收最强，位于290~300nm处。在醋酸-氯仿介质中，选择特定的激发波长，阿司匹林可发射较强的荧光，该荧光光谱的荧光强度在一定条件下，与阿司匹林的浓度成线性关系，因此，在合适条件下，可用荧光分析法测定阿司匹林的含量。此外乙酰水杨酸的分子中含有羧基，在溶液中能离解出一个质子。用NaOH标准溶液直接滴定，用酚酞做指示剂可分析其含量。操作中控制温度10℃一下，在中性乙醇溶液中用NaOH标准溶液滴定，可以有效防止乙酰水杨酸水解，得到较为理想的结果。 关键字：阿司匹林；合成；红外光谱；测定；熔点；酸碱滴定； Abstract: In concentrated sulfuric acid, salicylic acid and anhydride acetylation occurred stiff acetyl salicylic (Aspirin), by-product washed by saturated sodium bicarbonate solution and recrystallized with ethyl acetate to remove. Acetyl salicylic acid has a special structure, it occurs in the infrared spectra of se