光声光谱微量气体检测技术及其应用研究
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摘要
种类繁多的气体不仅在工农业生产中扮演着重要角色,更关系到人类自身的健康和生命安全,对气体的定量分析技术已成为现代分析测量技术的一个重要分支。光声光谱技术具有检测灵敏度高、选择性好、响应速度快等特点,是实现多种气体实时监测的理想方法。本文针对火灾预警和现场检测的需要研制了紧凑结构光声光谱仪,针对血液透析过程中利用呼气监测疗效的需要研制了高灵敏度光声光谱仪,并提出了氢气的光声光谱间接测量方法,其主要内容包括以下几个方面：
通过分析光声信号产生机理深入讨论了经典理论在光声光谱仪设计中的指导意义,详细论述了辐射源选择、光声池设计、传声器匹配等系统设计的核心问题。获得热辐射光源激发非共振光声池并匹配大尺寸传声器构成紧凑结构光声光谱仪的方案,以及激光光源驱动共振式光声池并匹配小尺寸传声器构成高灵敏度光声光谱仪的方案,并指出利用光声信号相位、频率等信息实现氢气间接测量的可能性。
在研制基于热辐射光源和非共振光声池的紧凑结构光声光谱仪过程中,根据光源辐射谱和滤光片透过特性对多组分气体的吸收谱进行了综合数值分析。依此确定CO、NO和H2S检测所需带通滤光片的中心波长分别为4650nm、5350nm和3700nm,实现了气体吸收效率和抗交叉干扰性的兼顾。
通过实验测定了非共振光声池和传声器相配合的工作频率曲线,得到其在35Hz的光源调制频率下能够获得光声信号激发效率和拾取效率的最佳匹配。进而对仪器性能的评定结果表明,其对CO、NO和H2S三种气体的循环检测时间小于60s,极限检测灵敏度分别达到1.5ppm、4.5ppm和400ppm,且表现出良好的线性度。
在研制基于CO2激光器和共振光声池的高灵敏度光声光谱仪过程中,对气体分子与固体材料表面间的微观作用机理和NH。分子在光声池内壁上吸附解吸附过程的宏观表现进行了深入分析。依此选取低表面能Teflon材料设计加工了以共振管中央切线方向进气结构为典型特征的低流量快速响应一阶纵向共振式光声池,其在100SCCM的流量下对低浓度NH3标准气响应时间且极限检测灵敏度达0.86ppb。
设计了能够有效降低混合气体中CO2含量的深冷分离方法,使得光声光谱仪在N2、O2、CO2和H2O占绝对优势的多组分呼出气中实现对微量NH3的高灵敏度检测成为可能。实测血液净化中心两名志愿者HD治疗前呼出气中NH3含量分别为4.73ppm和3.54ppm,与其他学者的前期实验结果基本一致。
为克服光声光谱技术应用于变压器油溶解气检测的局限性,提出了利用共振频率变化来检测H2含量的方法,并通过在原系统中增加光源调制频率扫描功能实现了对共振频率的精确测量。实验测得共振频率变化量与H2含量的变化关系与理论预期相同,极限检测灵敏度约为220ppm,且经温度补偿后可获得进一步提高。
利用LabVIEW软件平台所提供的虚拟仪器技术和多线程技术对系统软件和硬件进行了全面优化。虚拟仪器技术的应用使仪器硬件的控制、测量能力和计算机的数据处理能力得以紧密结合,简化了硬件构成并增强了智能控制、信号分析、显示储存等方面的功能,同时多线程技术的应用使复杂的仪器控制和数据采集任务得以简化,降低了编程难度并有效提高了系统的运行效率。
本论文研制的基于红外热辐射光源的紧凑结构光声光谱仪和基于CO2激光器的高灵敏度、快速响应微量气体光声光谱仪在火灾气体探测、电力系统大型变压器运行状态监测和故障诊断以及医学领域的临床呼吸气体监测方面具有广阔应用前景。
There is a wide range of gases not only playing important role in agriculture and industry, but also relating to public health and safety. The trace gases detection techniques have become an impotant branch of the modern analysis technologies. Trace gas measurements with photoacoustic spectroscopy (PAS) provide highly sensitive and selective detection in continuous-flow mode, suitable for online multicomponent trace gas analysis. In this dissertation, photoacoustic spectrometers for fire detection and for exhalation diagnosis are developed respectively, also a method for hydrogen detection is proposed. The main research works are outlined as follows:
The guide for photoacoustic spectrometer design including IR sources, photoacoustic cells and microphones is discussed in detail by analyzing the photoacoustic signal generation process. Photoacoustic spectrometers based on thermal emitter, nonresonant PA cell and large microphone are compact and suitable for multicomponent gas detection, while photoacoustic spectrometers based on laser, resonant PA cell and small microphone are rather sensitve and suitable for trace gas detection. The phase and frequency information make it possible to detect gases without light absorption in IR band.
In the development process of compact photoacoustic spectrometer, the integrated absorption coefficients of absorption gases at different absorption band are compared, thus the optimum parameters of the IR filters are determined:center wavelength of 4650nm,5350nm and 3700nm for CO, NO and H2S respectively. The light absorption efficiency and the cross interference are both considered.
The operating frequency of 35Hz is determined based on the measured frequency curve, that ensures the PA signal excitation and detection most effective. Experimental results show that the detection limits of 1.6ppm,4.5ppm and 400ppm for CO, NO and H2S can be obtained respectively in less than 60s. The repeatability and linearity tested for CO in the concentration range of 0-987ppm are also fairly satisfactory.
In the development process of highly sensitive photoacoustic spectrometer, the adsorption-desorption process caused by ammonia exchange between the cell surface and the gas phase is deeply analyzed, thus an H-type first longitudinal resonant PA cell made of Teflon is proposed. The sample gas is directed at tangent into the inlet located at center of the resonant cell and forced flowing in spiral along the surface. Experimental results show that the response time ofτPTFE 90%≈5 min and detection limit of 0.86ppb is achieved at 100SCCM sample flow rate.
The method of cryogenic separation is used to separate CO2 in exhalation, which ensure the CO2 laser based photoacoustic spectrometer achieve high sensitivity for ammonia measurement. Experimental results of two volunteers before HD show that the exhaled ammonia concentrations are 4.73ppm and 3.54ppm respectively, which are in agreement with the results obtained in previous experiments by other scholars.
A method for hydrogen detection is proposed, that makes it possible to measure all the seven types of gas in dissolved gas analysis by PAS. Experimental results show that the relation between resonant frequency change and hydrogen concentration in binary gas mixture is consistent with the theoretical expectation. The detection limit is about 200ppm, which can be further improved through temperature compensation.
The hardware and software of the photoacoustic spectrometers are fully optimized based on virtual instrument technique combined with multitasking program provided by LabVIEW platform. The control and measurement ability of hardware is closely combined with the computer data processing, and complex tasks are organized efficiently.
In summary, the capability to monitor multicomponent trace gas is provided by the IR rhermal emitter based compact photoacoustic spectrometerfor and the CO2 laser based sensitive photoacoustic spectrometer developed in this dissertation. The potential applications as fire gas detection, condition measurement of power transformers and breath gas analysis in medicine are also discussed.
通过分析光声信号产生机理深入讨论了经典理论在光声光谱仪设计中的指导意义,详细论述了辐射源选择、光声池设计、传声器匹配等系统设计的核心问题。获得热辐射光源激发非共振光声池并匹配大尺寸传声器构成紧凑结构光声光谱仪的方案,以及激光光源驱动共振式光声池并匹配小尺寸传声器构成高灵敏度光声光谱仪的方案,并指出利用光声信号相位、频率等信息实现氢气间接测量的可能性。
在研制基于热辐射光源和非共振光声池的紧凑结构光声光谱仪过程中,根据光源辐射谱和滤光片透过特性对多组分气体的吸收谱进行了综合数值分析。依此确定CO、NO和H2S检测所需带通滤光片的中心波长分别为4650nm、5350nm和3700nm,实现了气体吸收效率和抗交叉干扰性的兼顾。
通过实验测定了非共振光声池和传声器相配合的工作频率曲线,得到其在35Hz的光源调制频率下能够获得光声信号激发效率和拾取效率的最佳匹配。进而对仪器性能的评定结果表明,其对CO、NO和H2S三种气体的循环检测时间小于60s,极限检测灵敏度分别达到1.5ppm、4.5ppm和400ppm,且表现出良好的线性度。
在研制基于CO2激光器和共振光声池的高灵敏度光声光谱仪过程中,对气体分子与固体材料表面间的微观作用机理和NH。分子在光声池内壁上吸附解吸附过程的宏观表现进行了深入分析。依此选取低表面能Teflon材料设计加工了以共振管中央切线方向进气结构为典型特征的低流量快速响应一阶纵向共振式光声池,其在100SCCM的流量下对低浓度NH3标准气响应时间且极限检测灵敏度达0.86ppb。
设计了能够有效降低混合气体中CO2含量的深冷分离方法,使得光声光谱仪在N2、O2、CO2和H2O占绝对优势的多组分呼出气中实现对微量NH3的高灵敏度检测成为可能。实测血液净化中心两名志愿者HD治疗前呼出气中NH3含量分别为4.73ppm和3.54ppm,与其他学者的前期实验结果基本一致。
为克服光声光谱技术应用于变压器油溶解气检测的局限性,提出了利用共振频率变化来检测H2含量的方法,并通过在原系统中增加光源调制频率扫描功能实现了对共振频率的精确测量。实验测得共振频率变化量与H2含量的变化关系与理论预期相同,极限检测灵敏度约为220ppm,且经温度补偿后可获得进一步提高。
利用LabVIEW软件平台所提供的虚拟仪器技术和多线程技术对系统软件和硬件进行了全面优化。虚拟仪器技术的应用使仪器硬件的控制、测量能力和计算机的数据处理能力得以紧密结合,简化了硬件构成并增强了智能控制、信号分析、显示储存等方面的功能,同时多线程技术的应用使复杂的仪器控制和数据采集任务得以简化,降低了编程难度并有效提高了系统的运行效率。
本论文研制的基于红外热辐射光源的紧凑结构光声光谱仪和基于CO2激光器的高灵敏度、快速响应微量气体光声光谱仪在火灾气体探测、电力系统大型变压器运行状态监测和故障诊断以及医学领域的临床呼吸气体监测方面具有广阔应用前景。
There is a wide range of gases not only playing important role in agriculture and industry, but also relating to public health and safety. The trace gases detection techniques have become an impotant branch of the modern analysis technologies. Trace gas measurements with photoacoustic spectroscopy (PAS) provide highly sensitive and selective detection in continuous-flow mode, suitable for online multicomponent trace gas analysis. In this dissertation, photoacoustic spectrometers for fire detection and for exhalation diagnosis are developed respectively, also a method for hydrogen detection is proposed. The main research works are outlined as follows:
The guide for photoacoustic spectrometer design including IR sources, photoacoustic cells and microphones is discussed in detail by analyzing the photoacoustic signal generation process. Photoacoustic spectrometers based on thermal emitter, nonresonant PA cell and large microphone are compact and suitable for multicomponent gas detection, while photoacoustic spectrometers based on laser, resonant PA cell and small microphone are rather sensitve and suitable for trace gas detection. The phase and frequency information make it possible to detect gases without light absorption in IR band.
In the development process of compact photoacoustic spectrometer, the integrated absorption coefficients of absorption gases at different absorption band are compared, thus the optimum parameters of the IR filters are determined:center wavelength of 4650nm,5350nm and 3700nm for CO, NO and H2S respectively. The light absorption efficiency and the cross interference are both considered.
The operating frequency of 35Hz is determined based on the measured frequency curve, that ensures the PA signal excitation and detection most effective. Experimental results show that the detection limits of 1.6ppm,4.5ppm and 400ppm for CO, NO and H2S can be obtained respectively in less than 60s. The repeatability and linearity tested for CO in the concentration range of 0-987ppm are also fairly satisfactory.
In the development process of highly sensitive photoacoustic spectrometer, the adsorption-desorption process caused by ammonia exchange between the cell surface and the gas phase is deeply analyzed, thus an H-type first longitudinal resonant PA cell made of Teflon is proposed. The sample gas is directed at tangent into the inlet located at center of the resonant cell and forced flowing in spiral along the surface. Experimental results show that the response time ofτPTFE 90%≈5 min and detection limit of 0.86ppb is achieved at 100SCCM sample flow rate.
The method of cryogenic separation is used to separate CO2 in exhalation, which ensure the CO2 laser based photoacoustic spectrometer achieve high sensitivity for ammonia measurement. Experimental results of two volunteers before HD show that the exhaled ammonia concentrations are 4.73ppm and 3.54ppm respectively, which are in agreement with the results obtained in previous experiments by other scholars.
A method for hydrogen detection is proposed, that makes it possible to measure all the seven types of gas in dissolved gas analysis by PAS. Experimental results show that the relation between resonant frequency change and hydrogen concentration in binary gas mixture is consistent with the theoretical expectation. The detection limit is about 200ppm, which can be further improved through temperature compensation.
The hardware and software of the photoacoustic spectrometers are fully optimized based on virtual instrument technique combined with multitasking program provided by LabVIEW platform. The control and measurement ability of hardware is closely combined with the computer data processing, and complex tasks are organized efficiently.
In summary, the capability to monitor multicomponent trace gas is provided by the IR rhermal emitter based compact photoacoustic spectrometerfor and the CO2 laser based sensitive photoacoustic spectrometer developed in this dissertation. The potential applications as fire gas detection, condition measurement of power transformers and breath gas analysis in medicine are also discussed.
引文
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