红外水中油分析仪的全自动化研究

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摘要

在水资源日益紧缺的今天，水体受各种污染越来越严重。其中，油类污染所

带来的危害非常巨大，仅次于 CODCr，我国每年有近 8万多吨的油类污染物排放，

给自然生态环境以及人类造成了严重的危害。利用现有的技术实现对水中油类物

质的监测，及时掌握水质状况，对保护水体具有十分重要的意义。以各类测油方

法为原理的测油仪给测油提供了现实基础，其中以国家标准方法——红外分光光

度法为原理的测油仪最为普遍。大部分红外测油仪只提供测量的功能，在测量之

前，需要人工萃取或者使用自动萃取仪萃取。人工萃取过程不但费时费力，四氯

化碳的挥发还很容易侵害人体，而自动萃取过程中四氯化碳损耗很大，对环境不

利。因此，本课题致力于研究一种全自动红外测油仪，利用最新的膜萃取分离技

术，设计多级萃取模块，实现四氯化碳和水样的自动微量萃取并测量。

本文按照仪器开发流程进行设计，硬件设计包括电路到光路的设计和元器件

的选择；软件设计包括上位机和下位机的程序编写以及通信协议的编制。最后将

流路系统整合到硬件结构中，实现仪器的自动进样、萃取、分离和测量。研究讨

论各种影响萃取分离效果的因素，包括萃取管和分离模块的设计，优化了萃取分

离的最佳条件，保证了四氯化碳对水样的充分萃取，使测量结果准确可靠。

通过质量控制试验，得到仪器的最小检出限为 0.26mg/L，精密度 RSD<5%，

样品加标回收率为 79%～102%，相关系数为 0.9998(4cm 比色池)，可用于实际水

样的测量。

全自动红外水中油分析仪通过膜萃取分离技术和红外测油仪的结合，实现了

水中油的全自动化测量，开创了水中油类物质在线监测仪器研发的新思路，在环

境自动在线监测领域有良好的应用前景。

关键词：水中油红外分光法三波长全自动膜萃取分离

ABSTRACT

Water was polluted by all kinds of pollutants more seriously in today with the

increasing shortage of water resources. Oils had great harm to natural ecological

environment and humans only next to CODCr, about 80000 tons of oils were discharged

each year in China. It’s full of meaning for water protection by using existing

technologies to monitor oils in water and grasp water quality conditions in time. Oil

metering instruments based-on various of oils’ measure methods provided a realistic

foundation for measurement of oils in water. Instruments, based-on infrared

spectrophotometric method which was a national standard method, were commonly

used. Most infrared metering device only provided the measurement function, artificial

extraction or automatic extraction apparatus were need before measurement. Artificial

extraction was laborious and time consuming, also harm to human bodies due to the

volatilization of carbon tetrachloride. Carbon tetrachloride was wasted in the process of

the automatic extraction and harm to environment. Therefore, the paper was committed

to research a kind of automatic infrared metering device, used the latest technology of

membrane extraction separation, designed a kind of multi-stage extraction module,

realized automatic trace of carbon tetrachloride and water extraction and measurement.

The paper designed the instrument according to the development process. The

hardware design included designing circuits and light path and selecting components.

The software design included the programming of upper machine and lower machine

and establishing communication protocol. Finally the flow system and the hardware

structure were integrated to realize automatic sampling, extraction, separation and

measurement. The paper also discussed various factors affecting extraction separation,

including the extraction tubes and separation module design, optimized the best

conditions of extraction separation, which ensured the sufficient extraction of carbon

tetrachloride and water samples, to make the measurement results accurate and reliable.

With the quality control tests, the detection limit of instrument was 0.26mg/L, the

precision was less than 5% and the sample recovery rate ranged from 79% to 102%. The

correlation coefficient was 0.9998(4cm cuvette). The instrument could be used to

determine actual water samples.

Automatic infrared oils-in-water analyzer combined the membrane extraction

separation technology and infrared oils-measuring instrument, realized the full

automatic measurement of oils in water, created a new idea for automatic and online

instruments monitoring oils in water and had a good application prospect.

Key Word：oils in water, infrared spectrophotometry, three-wavelength,

full-automatic, membrane separation

中文摘要

ABSTRACT

第一章绪论 .................................................................................................................... 1

1.1 研究背景 ................................................................................................................ 1

1.2 水中油类污染概述 ................................................................................................ 2

1.2.1 水中油类的定义 ............................................................................................. 2

1.2.2 水中油类污染的来源 ..................................................................................... 2

1.2.3 水中油类污染的危害 ..................................................................................... 2

1.3 水中油类的分析方法 ............................................................................................ 3

1.3.1 重量法 ............................................................................................................. 3

1.3.2 比重瓶法 ......................................................................................................... 3

1.3.3 气相色谱法 ..................................................................................................... 4

1.3.4 紫外分光光度法 ............................................................................................. 4

1.3.5 荧光法 ............................................................................................................. 4

1.3.6 非色散红外光度法 ......................................................................................... 5

1.3.7 红外分光光度法 ............................................................................................. 5

1.4 国内外监测现状 .................................................................................................... 6

1.4.1 国内外测油仪现状 ......................................................................................... 6

1.4.2 红外测油仪的发展历程 ................................................................................. 7

1.4.3 实现测油自动化的意义 ................................................................................. 9

1.5 研究内容及创新点 .............................................................................................. 10

1.5.1 研究内容 ....................................................................................................... 10

1.5.2 创新点 ........................................................................................................... 10

第二章全自动红外油分仪设计概述 ........................................................................... 11

2.1 红外法测量原理 ................................................................................................... 11

2.2 红外测油仪的结构 .............................................................................................. 12

2..2.1 光学系统 ...................................................................................................... 12

2.2.2 电学系统 ....................................................................................................... 13

2.3 全自动化设计 ...................................................................................................... 14

2.3.1 设计思路 ....................................................................................................... 14

2.3.2 设计原理 ....................................................................................................... 14

2.3.3 设计的优势 ................................................................................................... 15

第三章全自动化硬件和软件设计 .............................................................................. 17

3.1 全自动化硬件设计 .............................................................................................. 17

3.1.1 单片机 ........................................................................................................... 18

3.1.2 电磁阀 ........................................................................................................... 19

3.1.3 蠕动泵 ........................................................................................................... 19

3.1.4 分光系统 ....................................................................................................... 21

3.1.5 电路设计 ....................................................................................................... 21

3.1.6 通信串口 ....................................................................................................... 21

3.2 全自动化软件设计 .............................................................................................. 24

3.2.1 单片机程序设计 ........................................................................................... 24

3.2.2 上位机程序设计 ........................................................................................... 28

3.2.3 通信程序设计 ............................................................................................... 31

第四章全自动化流路设计和讨论 .............................................................................. 36

4.1 进液的动力设计 .................................................................................................. 36

4.1.1 泵头和泵管 ................................................................................................... 36

4.1.2 进液速度控制 ............................................................................................... 36

4.2 自动萃取的设计 .................................................................................................. 37

4.2.1 自动萃取原理 ............................................................................................... 37

4.2.2 萃取管的管径与长度 ................................................................................... 38

4.3 自动分离的设计 .................................................................................................. 39

4.3.1 自动分离原理 ............................................................................................... 39

4.3.2 分离模块的设计 ........................................................................................... 40

4.3.3 影响分离效果的因素 ................................................................................... 40

4.4 萃取比例的控制 .................................................................................................. 43

4.4.1 泵管比例与萃取比的关系 ........................................................................... 43

4.4.2 多级萃取 ....................................................................................................... 45

第五章结果与讨论 ...................................................................................................... 47

5.1 仪器检出限 .......................................................................................................... 47

5.2 全程空白试验 ...................................................................................................... 48

5.3 精密度 .................................................................................................................. 49

5.4 准确度 .................................................................................................................. 49

5.5 相关系数 .............................................................................................................. 50

第六章结论与展望 ...................................................................................................... 52

6.1 结论 ...................................................................................................................... 52

6.2 展望 ...................................................................................................................... 52

参考文献 ........................................................................................................................ 53

在读期间公开发表的论文和承担科研项目及取得成果 ............................................ 57

致谢 ............................................................................................................................ 58

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