基于臭氧氧化化学发光新体系的海水化学需氧量（COD）现场测量仪研制
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摘要
海水化学需氧量(COD)是表征海水中有机污染物的综合指标,是海洋水质常规监测最重要的项目之一。海水COD数据是海洋污染评估和海洋水质污染灾害预报、预警的基础,加强其成因机制以及监测技术水平,对于全面了解和掌握多介质海洋生态环境的综合质量状况及其变化规律,以缓解海洋经济发展与海洋生态环境污染之间的矛盾尤为重要。
目前海水COD的测量还是以实验室为主,采用国家标准规定的海水COD测量方法一碱性高锰酸钾法,该方法分析过程繁杂,持续时间长,时效性差。另外,我国海洋有机物污染具有相当大的复杂性,一方面污染物质进入海洋以后,在海水中进行复杂的物理、化学和生物过程,通过这三种过程的作用,污染物质在海水中被稀释、吸收、沉降或转化；另一方面污染物质受本身的性质和浓度影响外,还与海岸地形、水文条件、水中微生物的种类和数量、海水温度和含氧状况等环境条件密切相关,因此污染有机物的形态和浓度受时空影响大,这决定了目前海水COD测定方法不能有效的反映海洋现场真实状况,无法胜任现场的COD跟踪,更不适用于大范围内的COD实时调查,测量结果的时效性和代表性不能满足我国海洋生态环境监测与保护的需要。防灾减灾的关键是对灾害性海况进行准确的预报,卓有成效的预报需要及时准确的现场数据,因此高质量数据的获取必须依靠现场、实时测量仪,研制开发海水COD现场测量仪势在必行。
研制现场、实时、快速海水COD测量仪一方面可以帮助广大海洋科学工作者研究海洋COD细微变化程度,了解海洋COD形成和去除机制及与其他海洋生态要素之间的函数关系,为海洋污染评价以及生态环境研究提供重要资料；另一方面能够有效降低海洋调查、海洋监测人员的劳动强度,提高我国对突发海洋污染事件的反应能力。
针对目前海水COD测量方法现状,本论文研制了一种具有现场、实时、快速工作特性的海水COD现场测量仪,并将之应用到了现场COD的测量。主要结论如下：
(1)研制成功了海水COD现场测量仪,该仪器基于臭氧氧化化学发光原理,应用化学发光动力学方法进行海水COD现场测量,仪器具有不产生二次污染,分析响应速度快,可在海洋环境中长期工作,适合于船载、海洋台站、海洋石油平台等场合使用。在布点方式上可采用定点或走航方式对沿海海洋经济带进行现场、实时、连续的测量。该测量仪的研制成功不仅避免了现场采样和实验室分析的繁杂过程,同时也满足了海洋水质污染要素监测的特别需要,能真正反映出海洋现场复杂多变的现状,增强了我国海洋生态环境中COD监测技术水平,同时也提高了现场监测能力和监测速度。
(2)本仪器用VC++高级语言编写了上位机处理软件,包括信号采集以及信号优化处理、分析测量运算、实时监测曲线显示以及人机对话等各种处理程序。仪器能够实现自动控制、实时分析计算、实时监测曲线显示、数据自动存储以及数据图谱回放等各项功能。可以根据实际要求设定各种测量模式,上位机软件协调控制整个仪器各执行部分的动作顺序,在程序指令控制下自动完成测试工作。通过实验室性能测试以及现场实验,上位机软件运行稳定,各项功能执行良好。
(3)通过对所研制的仪器进行系统测试和实验分析,首先确定了工作曲线,y=0.033x+0.0503R2=0.9955,数据表明,工作曲线线性度满足仪器测量要求。在此基础上进行了仪器测量准确度、精密度、检出限试验,通过试验分析,仪器准确度,在海水样品COD值小于1.0mg/L时,土0.1mg/L,在海水样品COD值大于等于1.0mg/L时,土10%；精密度为10%,检出限为0.08mg/L,低于GB17378.4中碱性高锰酸钾法的检出限(0.15mg/L)。海水COD是个条件参数,而仪器采用的原理与国标法有一定的差别,因此又进行了仪器回收率以及线性关系实验,通过添加标准品试验,回收率范围在90%-120%之间,通过现场水样等比例稀释测量,仪器具有很好的线性关系。因此仪器完全满足现场、实时快速分析的要求,数据与国标法具有非常好的线性关系。
(4)通过在青岛胶州湾两次海试,仪器运行平稳,系统工作正常,仪器测量数据与国标法—碱性高锰酸钾法误差处于所研制仪器的正常误差范围内,仪器可以满足现场测量工作,可以为海洋水质监测、海洋生态环境研究、海洋污染预警、预报以及海洋污染评估等方面提供方便快捷的海水COD测量仪器。
Seawater Chemical Oxygen Demand (COD) indicates the contents of organicpollutants in seawater, thus is one of the most important items of routine monitoring.Seawater COD supplies the basis of marine pollution assessment and disasterforecasting. Studying the control factors and monitoring technologies can help fullyunderstand the environment quality and its variation of the multi-media integratedmarine, in order to decrease the contradiction between marine economy developmentand environment pollution.
In the current COD measurement rely on the laboratory technologies, in whichalkaline potassium permanganate method is the national standard COD measurementof seawater. The standard method has a series of complex procedures and consumes along time. However, the organic pollutants in our marine is largely complex for theseries of physical, chemical and biological processes and the influence factors such asthe quality and concentration of organic pollutants, the coastal topography, thehydrological conditions, the microorganisms in water, water temperature and oxygenconditions etc. That is, the type and concentration of organic pollutants vary in thespace and time scales; therefore, the current COD measurement can not meet thein-situ studies at both the small and large scales. In addition, disaster forecasting is theaim of marine environmental monitoring and protection, which rely on the accuratein-situ technologies. Therefore, it is critical to study the in-situ equipment of CODmeasurement.
The instrument of in-situ COD measurement can help the marine scientists tounderstand the COD variation and its control factors, which supply the data forevaluation of the marine environmental pollution and study of the marine ecology. On the other hand, the equipment can effectively reduce the labor intensity in marinesurvey and monitoring and improve the response capabilities on the marine pollutionemergency.
We developed an in-situ measuring instrument of seawater COD based on therecent development on the COD measurement in seawater and apply it in two marinesurveys. The main conclusions are as follows:
(1) the instrument based on the ozonation chemiluminescence theory has nosecondary pollution, analysis rapidly, work in ship, marine stations, offshore oilplatforms for a long-term. The instrument avoids the complex procedures in thesampling, stock, transportation, and laboratory analysis, also realize the in-situmonitoring of COD, enhancing the capabilities of marine environment monitoring.
(2) The PC software is written by VC++, including a variety of processes, suchas signal acquisition and optimization processing, operations of analysis andmeasurement, real-time display of monitoring curves, man-machine dialogue, etc.With the software, the instrument can achieve a set of functions, such as automaticcontrol, real-time analysis and calculation, real-time display of monitoring curve, datastorage and playback, etc. With the software, a variety of measurement modes can beset according to the actual requirements. The testing in the laboratory and fieldshowed that the software is stable and its function performs well.
(3) A working curve (y=0.033x+0.0503, R~2=0.9955) was first developedbased on the system testing and laboratory analysis by the instruments. Resultsshowed that the working curve meet the measurement requirements. Then theinstrument was tested its measurement accuracy, precision, and detection limit.Results showed that the instrument accuracy is±0.1mg/L when the COD in thesample is less than1.0mg/L, and the accuracy is±10%when the COD is greater than1.0mg/L; the precision is10%and the detection limit is0.08mg/L, lower than thedetection limit (0.15mg/L) of the alkaline potassium permanganate method(GB17378.4) the detection limit. COD is a water condition parameters, while theinstrument used in principle with the GB method is different, thus anotherexperiments were used to test the recovery rate and linear relationship between the instrument and the standard method. The recovery rate is in the range of90-120and a high linear relationship was in the instrument. Therefore, the instrument fullymeet the in situ monitoring in that the data measured by the instrument has a highlinear relationship with the national standard method.
(4) The instrument works well during two sea trials in the Jiaozhou Bay. The datadifference between the instrument measurement and the national standard method isin the normal error range. Therefore, the instrument can meet the in-situ survey formarine water quality, marine environment research, marine pollution warning,assessment and forecasting of marine pollution.
目前海水COD的测量还是以实验室为主,采用国家标准规定的海水COD测量方法一碱性高锰酸钾法,该方法分析过程繁杂,持续时间长,时效性差。另外,我国海洋有机物污染具有相当大的复杂性,一方面污染物质进入海洋以后,在海水中进行复杂的物理、化学和生物过程,通过这三种过程的作用,污染物质在海水中被稀释、吸收、沉降或转化；另一方面污染物质受本身的性质和浓度影响外,还与海岸地形、水文条件、水中微生物的种类和数量、海水温度和含氧状况等环境条件密切相关,因此污染有机物的形态和浓度受时空影响大,这决定了目前海水COD测定方法不能有效的反映海洋现场真实状况,无法胜任现场的COD跟踪,更不适用于大范围内的COD实时调查,测量结果的时效性和代表性不能满足我国海洋生态环境监测与保护的需要。防灾减灾的关键是对灾害性海况进行准确的预报,卓有成效的预报需要及时准确的现场数据,因此高质量数据的获取必须依靠现场、实时测量仪,研制开发海水COD现场测量仪势在必行。
研制现场、实时、快速海水COD测量仪一方面可以帮助广大海洋科学工作者研究海洋COD细微变化程度,了解海洋COD形成和去除机制及与其他海洋生态要素之间的函数关系,为海洋污染评价以及生态环境研究提供重要资料；另一方面能够有效降低海洋调查、海洋监测人员的劳动强度,提高我国对突发海洋污染事件的反应能力。
针对目前海水COD测量方法现状,本论文研制了一种具有现场、实时、快速工作特性的海水COD现场测量仪,并将之应用到了现场COD的测量。主要结论如下：
(1)研制成功了海水COD现场测量仪,该仪器基于臭氧氧化化学发光原理,应用化学发光动力学方法进行海水COD现场测量,仪器具有不产生二次污染,分析响应速度快,可在海洋环境中长期工作,适合于船载、海洋台站、海洋石油平台等场合使用。在布点方式上可采用定点或走航方式对沿海海洋经济带进行现场、实时、连续的测量。该测量仪的研制成功不仅避免了现场采样和实验室分析的繁杂过程,同时也满足了海洋水质污染要素监测的特别需要,能真正反映出海洋现场复杂多变的现状,增强了我国海洋生态环境中COD监测技术水平,同时也提高了现场监测能力和监测速度。
(2)本仪器用VC++高级语言编写了上位机处理软件,包括信号采集以及信号优化处理、分析测量运算、实时监测曲线显示以及人机对话等各种处理程序。仪器能够实现自动控制、实时分析计算、实时监测曲线显示、数据自动存储以及数据图谱回放等各项功能。可以根据实际要求设定各种测量模式,上位机软件协调控制整个仪器各执行部分的动作顺序,在程序指令控制下自动完成测试工作。通过实验室性能测试以及现场实验,上位机软件运行稳定,各项功能执行良好。
(3)通过对所研制的仪器进行系统测试和实验分析,首先确定了工作曲线,y=0.033x+0.0503R2=0.9955,数据表明,工作曲线线性度满足仪器测量要求。在此基础上进行了仪器测量准确度、精密度、检出限试验,通过试验分析,仪器准确度,在海水样品COD值小于1.0mg/L时,土0.1mg/L,在海水样品COD值大于等于1.0mg/L时,土10%；精密度为10%,检出限为0.08mg/L,低于GB17378.4中碱性高锰酸钾法的检出限(0.15mg/L)。海水COD是个条件参数,而仪器采用的原理与国标法有一定的差别,因此又进行了仪器回收率以及线性关系实验,通过添加标准品试验,回收率范围在90%-120%之间,通过现场水样等比例稀释测量,仪器具有很好的线性关系。因此仪器完全满足现场、实时快速分析的要求,数据与国标法具有非常好的线性关系。
(4)通过在青岛胶州湾两次海试,仪器运行平稳,系统工作正常,仪器测量数据与国标法—碱性高锰酸钾法误差处于所研制仪器的正常误差范围内,仪器可以满足现场测量工作,可以为海洋水质监测、海洋生态环境研究、海洋污染预警、预报以及海洋污染评估等方面提供方便快捷的海水COD测量仪器。
Seawater Chemical Oxygen Demand (COD) indicates the contents of organicpollutants in seawater, thus is one of the most important items of routine monitoring.Seawater COD supplies the basis of marine pollution assessment and disasterforecasting. Studying the control factors and monitoring technologies can help fullyunderstand the environment quality and its variation of the multi-media integratedmarine, in order to decrease the contradiction between marine economy developmentand environment pollution.
In the current COD measurement rely on the laboratory technologies, in whichalkaline potassium permanganate method is the national standard COD measurementof seawater. The standard method has a series of complex procedures and consumes along time. However, the organic pollutants in our marine is largely complex for theseries of physical, chemical and biological processes and the influence factors such asthe quality and concentration of organic pollutants, the coastal topography, thehydrological conditions, the microorganisms in water, water temperature and oxygenconditions etc. That is, the type and concentration of organic pollutants vary in thespace and time scales; therefore, the current COD measurement can not meet thein-situ studies at both the small and large scales. In addition, disaster forecasting is theaim of marine environmental monitoring and protection, which rely on the accuratein-situ technologies. Therefore, it is critical to study the in-situ equipment of CODmeasurement.
The instrument of in-situ COD measurement can help the marine scientists tounderstand the COD variation and its control factors, which supply the data forevaluation of the marine environmental pollution and study of the marine ecology. On the other hand, the equipment can effectively reduce the labor intensity in marinesurvey and monitoring and improve the response capabilities on the marine pollutionemergency.
We developed an in-situ measuring instrument of seawater COD based on therecent development on the COD measurement in seawater and apply it in two marinesurveys. The main conclusions are as follows:
(1) the instrument based on the ozonation chemiluminescence theory has nosecondary pollution, analysis rapidly, work in ship, marine stations, offshore oilplatforms for a long-term. The instrument avoids the complex procedures in thesampling, stock, transportation, and laboratory analysis, also realize the in-situmonitoring of COD, enhancing the capabilities of marine environment monitoring.
(2) The PC software is written by VC++, including a variety of processes, suchas signal acquisition and optimization processing, operations of analysis andmeasurement, real-time display of monitoring curves, man-machine dialogue, etc.With the software, the instrument can achieve a set of functions, such as automaticcontrol, real-time analysis and calculation, real-time display of monitoring curve, datastorage and playback, etc. With the software, a variety of measurement modes can beset according to the actual requirements. The testing in the laboratory and fieldshowed that the software is stable and its function performs well.
(3) A working curve (y=0.033x+0.0503, R~2=0.9955) was first developedbased on the system testing and laboratory analysis by the instruments. Resultsshowed that the working curve meet the measurement requirements. Then theinstrument was tested its measurement accuracy, precision, and detection limit.Results showed that the instrument accuracy is±0.1mg/L when the COD in thesample is less than1.0mg/L, and the accuracy is±10%when the COD is greater than1.0mg/L; the precision is10%and the detection limit is0.08mg/L, lower than thedetection limit (0.15mg/L) of the alkaline potassium permanganate method(GB17378.4) the detection limit. COD is a water condition parameters, while theinstrument used in principle with the GB method is different, thus anotherexperiments were used to test the recovery rate and linear relationship between the instrument and the standard method. The recovery rate is in the range of90-120and a high linear relationship was in the instrument. Therefore, the instrument fullymeet the in situ monitoring in that the data measured by the instrument has a highlinear relationship with the national standard method.
(4) The instrument works well during two sea trials in the Jiaozhou Bay. The datadifference between the instrument measurement and the national standard method isin the normal error range. Therefore, the instrument can meet the in-situ survey formarine water quality, marine environment research, marine pollution warning,assessment and forecasting of marine pollution.
引文
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