论文总字数：15867字

摘 要

在挥发酚测定领域，4-氨基安替比林分光光度法具有显色条件简单，使用试剂无毒等优点被广泛应用，但直接用手工实验不仅操作繁琐，如果能结合连续流动分析技术，不仅能简化实验操作步骤，消除人为误差，更能同时检测多个试样，极大提高重现性和灵敏度。本文旨在研发一种在线蒸馏装置，并将其应用于挥发酚的测定。具体工作内容包括以下两个部分：

1. 采用国标方法测定五组水样。首先分别采用直接和萃取分光光度法测定不同浓度的酚标准溶液，绘制标准曲线，然后测定实际样品。其中，用直接分光光度法测定两组炼油厂废水中的挥发酚含量，萃取分光光度法测定三组南工大湖水中的挥发酚含量。
2. 研制在线蒸馏装置，并做手工方法与装置实验的对比实验，得到实验结果误差在±3%以内，无明显差异。可以认为研发的在线蒸馏装置表现良好，适用于测定挥发酚含量的流动分析仪器。

关键词：连续流动分析 挥发酚 4-氨基安替比林 在线蒸馏分离装置

Abstract

In the field of volatile phenol determination, the spectrophotometric method of 4-aminoantipyrine has the advantages of simple color reaction condition and nontoxic reagent, but direct manual experiment is not only complicated, but also can be combined with continuous flow analysis technology. It not only simplifies the operation of the experiment, eliminates the artificial error, but also can detect many samples at the same time, and greatly improves the reproducibility and sensitivity. In this paper, an on-line distillation unit was developed and applied to the determination of volatile phenol. The specific work consists of the following two parts:

1. Five groups of water samples were determined by national standard method. The standard solution of phenol with different concentrations was determined by direct and extraction spectrophotometry, then the standard curve was drawn, and then the actual sample was determined. The content of volatile phenol in wastewater of two groups of refineries was determined by direct spectrophotometry, and the content of volatile phenol in water of three groups of Nanchongda Lake was determined by extraction spectrophotometry.

（2）The on-line distillation unit was developed and compared with the experiment of manual method and device experiment. The error of the experimental results was within 3%, and there was no obvious difference. It can be considered that the developed on-line distillation unit has good performance and is suitable for the flow analysis instrument for determining the content of volatile phenol.

Key Words: Continuous Flow Analysis Volatile phenol 4-aminoantipyrine On-line distillation separation unit

目 录

摘 要…………………………………………………………………………………I

ABSTRACT………………………………………………………………………II

第一章 绪 论 1

1.1挥发酚概况 1

1.1.1挥发酚的检测 1

1.1.2水质挥发酚的排放情况 2

1.2国内外全自动水质分析仪 2

1.2.1国内全自动水质分析仪 2

1.2.2国外流动注射分析全自动水质分析仪 3

1.3挥发酚的测定方法 5

1.3.1测定方法 5

1.3.2水样中挥发酚的测定方法 5

1.3.3水中挥发酚检测的具体方法及比较 5

1.4本文的研究目的及内容 6

第二章 实验部分 7

2.1前言 7

2.2试剂与仪器 7

2.2.1试剂 7

2.2.2仪器 7

2.3溶液配制 8

2.4样品的采集和制备 8

2.4.1样品的采集和保存 8

2.4.2样品的制备 9

2.5实验步骤 9

2.5.1标准曲线的绘制 10

2.5.2样品测定 10

2.6结果讨论 10

2.6.1标准曲线 10

2.6.2样品测试结果 12

2.6.3结果讨论 13

2.7结论 13

第三章 在线蒸馏装置的研制 14

3.1装置设计 14

3.1.1分析方法原理 14

3.1.2 分析流路设计 14

3.1.3 关键部件的设计 15

3.2设计说明 15

3.2.1装置优势和创新 16

3.3 装置实验 16

3.3.1 最大吸收波长的扫描 17

3.3.2标准曲线的绘制 17

3.3.3 结论 19

第四章 结论与展望 20

4.1结论 20

4.2展望 20

参考文献 21

致谢 23

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