分析化学在时空上的延伸
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摘要
本文通过灵敏的现代光谱分析方法—遥感傅里叶变换红外光谱和原子发射光谱，分别对它们在温度测量及大气有机污染物监测中的应用开展了较为深入的研究。本文研究了遥感傅里叶变换红外发射光谱在研究火焰燃烧特性中的应用，应用分子转振光谱理论，研究了高红外活性的固体推进剂燃烧火焰的光谱辐射绝对能量分布，测定了火焰的温度，探讨了仪器响应函数受黑体温度的影响，并定量分析了燃烧产物的浓度；建立了一个由四种化学计量学方法组成的大气有机污染物多组分分析平台，并讨论了人工神经网络在十组分大气污染物监测中的应用，比较了等间距取点和特征吸收峰取点方式的预测结果；应用开路FTIR遥感监测大气中的有毒易挥发有机化合物(VOCs)，分别对含有二、三、四和五组分的模拟泄漏源体系进行了监测，并得到了各物质沿光路的积分浓度随时间的变化规律；另外，对于大范围内的大气VOCs，在准稳定状态下，描述了污染物的空间浓度分布；此外，应用原子发射光谱多谱线法测定了等离子体的激发温度和电子密度，并讨论了光谱参数的选择对测定结果的影响。该项研究将对复杂的温度测定和大气污染物监测起到关键作用。本文的主要内容如下：
1．FTIR遥测固体推进剂的燃烧特性
本文发展了基于分子转振红外发射谱线强度理论的温度计算方程式。将遥感FTIR与分子转振光谱测温法和分子发射光谱最大强度谱线测温法相结合，对固体推进剂Ⅰ和固体推进剂Ⅱ的燃烧温度及其随时间的变化进行了连续实时的测定，两种方法测得的结果相当一致。另外，本文校正了遥感FTIR光谱仪的光路系统，对仪器响应函数的概念及意义作了介绍和分析，实时地测定了固体推进剂燃烧火焰的绝对光谱能量分布，并定量分析了燃烧产物的浓度。
2．化学计量学方法在大气有毒VOCs测定中的应用
本文建立了一个由4种能克服多种大气易挥发有机化合物谱带混叠干扰的，多组分同时测定的化学计量学分析平台。所包含的四种多变量校准方法是：经典最小二乘法(CLS)，偏最小二乘法(PLS)，卡尔曼滤波法(KFM)和人工神经网络法(ANN)，在1，3-butadiene，benzene，o-xylene，chlorobenzene和acrolein五组
博士论文
分析化学在时空上的延伸
分大气VOCS的定量测定中，对四种方法的预测误差比较，偏最小二乘法显示了
较为稳健的能力。另外，对于存在未知干扰物的五组分体系，采用改进型的偏最
小二乘法，成功地鉴别出了干扰物，校正了光谱，得到了已知组分的浓度。本文
还将人工神经网络应用到十种大气VOCs的多组分定量研究中，结果表明，采用
特征吸收峰取点的数据处理方法，预测结果优于等间距取点的方法。
3.FTIR遥测泄漏气体的浓度一时间分布
本文利用人工神经网络法与遥感FTIR光谱仪联用分别对含有二、三、四和五
种有毒易挥发有机化合物混合物的模拟泄漏源进行了研究，所研究的有机化合物
包括ehloroform，methylene chioride，aeetone，methanol，hexane和butanol，采用
三层反向传播人工神经网络(BP一ANN)对各组分进行了定量，得到了各组分沿光
路的积分浓度随时间的变化规律，误差小。
4.遥感FTIR测定泄漏气体的二维空间浓度分布
本文发展了一种遥感FTIR对泄漏气体的浓度分布进行二维空间描述的方法，
分别从垂直方向和水平方向上对污染物浓度的分布做了遥感测定。在光路高度分
别为0.36m，o.6lm和o.86m时，遥测了固定泄漏源挥发的VOCs:Toluene，hexane
和acetone，结果表明，当对固定的泄漏源挥发气体进行浓度测定时，红外光源光
路的高度对测定结果的影响很大，当光路的高度为o.6lm时，测量值最大。
在面积为 100m2，光路高度为1.som的二维平面上，在稳定状态下，测定了
chloroform和methanol沿不同光路的积分浓度，并重构了它们的二维空间浓度分
布曲面图和等浓度图，找到了浓度的最大值分别为5.2ppm和12.’7ppm，峰值位置
在坐标(6m，7m)。遥感FTIR对大范围内的气体污染物进行二维空间浓度分布的实
时监测，速度快，可靠性强，有很强的应用潜力。
5.原子发射光谱法测定电热等离子体的激发温度和电子密度
当用原子发射光谱Boltzmann法测量电热高密度等离子体的温度和电子密度
时，目前，国际上都应用eu原子在510.554，515.324.521.820，529250，570.020和
578.213nln处的六条中性原子光谱线测量，产生很大的误差，高达25%，甚至更
高。国际上著名科学家BOLlxham和Kohel等人都认为“偏离Boltzmanll曲线的原
博士论文
分析化学在时空上的延伸
因是由于高光密度等离子体内的自吸，或由于辐射原子态内固有非热粒子流造成
的”。在我们的研究中发现，产生这样大误差的原因，并不是像他们所说的那样，
而是由于他们在计算温度时，采用了错误的光谱参数，如:谱线上能级统计权重g、
跃迁几率A和上能级能量E‘的原因。我们认为，只有在正确选择和应用了这些光
谱参数后，才能得到正确的和实验可信度极高的温度测量数据。在我们的实验结
果中，我们将实验的可信度从89一94%提高到了98一99.5%，实验误差从士16一20%降
低到了士6.5%。我们的这一发现?
This paper presented the advantages of modern spectroscopy applications of remote sensing Fourier Transform Infrared (FTIR) spectroscopy and atomic emission spectroscopy in temperature measurements and air organic pollutants monitoring as a sensitive technology, especially combined with other analytical methods. The applications of remote sensing FTIR coupled with molecular spectra theory in combustion characteristics under high temperature and high pressure were investigated for the determination of combustion temperature of solid propellant. The influence of Blackbody temperature on the instrumental response function was studied to measure the energy distribution of the infrared emission spectra from the combustion flame, thereby quantified the combustion products concentrations. A multi-component analytical platform including Classical Least Squares (CLS), Partial Least Squares (PLS), Kalman Filter Method (KFM) and Artificial Neural Network (ANN) was established to overcome the overlaps between the spectral bands of each component in air Volatile Organic Compounds (VOCs) monitoring. The Open-Path real time air pollutant monitoring of remote sensing FTIR was conducted for the two-, three- four-and five- component system, herein the Path-Integrated Concentrations (PIC) of the desired VOCs leaking from the simulated source vs. the leaking time were obtained. Moreover, the concentrations of chloroform and methanol were spatially mapped in the vertical direction and on the horizontal plane during the quasi-steady state. The atomic emission spectroscopy with multiple spectral lines was used to measure the electro-thermal plasma temperatures and electronic density, and the influence of spectral parameters on the measurement accuracy was evaluated. This study will play significant influence on techniques of temperature measurement and air contaminant monitoring. The major content was described as follows:
1. The Real Time Measurement of Combustion Characteristics of Solid Propellant by Remote Sensing FTIR
The superiority of theory of molecular rotation-vibration emission spectra for the temperature measurement was verified. The in-situ combustion temperatures of solid propellant I and II were measured by Remote sensing FTIR combined with molecular
rotation-vibration emission spectra method and maximum spectral line intensity method. The results of molecular rotation-vibration emission spectra method and maximum spectral line intensity method were hi great agreement. Moreover, the optics of remote sensing FTIR used was calibrated, and the instrumental response function (IRF) was introduced and analyzed. Thus, the energy distribution of infrared emission spectra of the solid propellant combustion flame was measured.
2. Studies of Four Chemometrics in the Simultaneous Determination of Air Toxic VOCs
A chemometrics analytical platform was established to overcome the spectra interference and overlaps between the spectral bands of each component when doing multicomponent analysis of 1, 3-butadiene, benzene, o-xylene, chlorobenzene and acrolein. The methods included CLS, PLS, KFM and ANN. PLS was found to be the most potential method by comparing the prediction errors of each method. As for prediction samples, in which some unknown interferents exist, the modified PLS method successfully identified the interferents and corrected the spectrum, thus the concentrations of each desired component was quantified successfully. Moreover, ANN was applied to a ten-component system, results showed that the characteristic peak selection method was better than the equi-spaced wavenumber selection method when composing the analytical samples.
3. Temporally Monitoring Air Toxic VOCs by Remote Sensing FTIR and ANN
The simulated leaking sources composed of two-, three, four- and five VOCs were monitored by remote sensing FTIR with ANN as a quantification tool. The measured VOCs include chloroform, methylene chloride, acetone, methanol, hexane and butanol, etc. The plot of Path-Integrated Concentrations
1．FTIR遥测固体推进剂的燃烧特性
本文发展了基于分子转振红外发射谱线强度理论的温度计算方程式。将遥感FTIR与分子转振光谱测温法和分子发射光谱最大强度谱线测温法相结合，对固体推进剂Ⅰ和固体推进剂Ⅱ的燃烧温度及其随时间的变化进行了连续实时的测定，两种方法测得的结果相当一致。另外，本文校正了遥感FTIR光谱仪的光路系统，对仪器响应函数的概念及意义作了介绍和分析，实时地测定了固体推进剂燃烧火焰的绝对光谱能量分布，并定量分析了燃烧产物的浓度。
2．化学计量学方法在大气有毒VOCs测定中的应用
本文建立了一个由4种能克服多种大气易挥发有机化合物谱带混叠干扰的，多组分同时测定的化学计量学分析平台。所包含的四种多变量校准方法是：经典最小二乘法(CLS)，偏最小二乘法(PLS)，卡尔曼滤波法(KFM)和人工神经网络法(ANN)，在1，3-butadiene，benzene，o-xylene，chlorobenzene和acrolein五组
博士论文
分析化学在时空上的延伸
分大气VOCS的定量测定中，对四种方法的预测误差比较，偏最小二乘法显示了
较为稳健的能力。另外，对于存在未知干扰物的五组分体系，采用改进型的偏最
小二乘法，成功地鉴别出了干扰物，校正了光谱，得到了已知组分的浓度。本文
还将人工神经网络应用到十种大气VOCs的多组分定量研究中，结果表明，采用
特征吸收峰取点的数据处理方法，预测结果优于等间距取点的方法。
3.FTIR遥测泄漏气体的浓度一时间分布
本文利用人工神经网络法与遥感FTIR光谱仪联用分别对含有二、三、四和五
种有毒易挥发有机化合物混合物的模拟泄漏源进行了研究，所研究的有机化合物
包括ehloroform，methylene chioride，aeetone，methanol，hexane和butanol，采用
三层反向传播人工神经网络(BP一ANN)对各组分进行了定量，得到了各组分沿光
路的积分浓度随时间的变化规律，误差小。
4.遥感FTIR测定泄漏气体的二维空间浓度分布
本文发展了一种遥感FTIR对泄漏气体的浓度分布进行二维空间描述的方法，
分别从垂直方向和水平方向上对污染物浓度的分布做了遥感测定。在光路高度分
别为0.36m，o.6lm和o.86m时，遥测了固定泄漏源挥发的VOCs:Toluene，hexane
和acetone，结果表明，当对固定的泄漏源挥发气体进行浓度测定时，红外光源光
路的高度对测定结果的影响很大，当光路的高度为o.6lm时，测量值最大。
在面积为 100m2，光路高度为1.som的二维平面上，在稳定状态下，测定了
chloroform和methanol沿不同光路的积分浓度，并重构了它们的二维空间浓度分
布曲面图和等浓度图，找到了浓度的最大值分别为5.2ppm和12.’7ppm，峰值位置
在坐标(6m，7m)。遥感FTIR对大范围内的气体污染物进行二维空间浓度分布的实
时监测，速度快，可靠性强，有很强的应用潜力。
5.原子发射光谱法测定电热等离子体的激发温度和电子密度
当用原子发射光谱Boltzmann法测量电热高密度等离子体的温度和电子密度
时，目前，国际上都应用eu原子在510.554，515.324.521.820，529250，570.020和
578.213nln处的六条中性原子光谱线测量，产生很大的误差，高达25%，甚至更
高。国际上著名科学家BOLlxham和Kohel等人都认为“偏离Boltzmanll曲线的原
博士论文
分析化学在时空上的延伸
因是由于高光密度等离子体内的自吸，或由于辐射原子态内固有非热粒子流造成
的”。在我们的研究中发现，产生这样大误差的原因，并不是像他们所说的那样，
而是由于他们在计算温度时，采用了错误的光谱参数，如:谱线上能级统计权重g、
跃迁几率A和上能级能量E‘的原因。我们认为，只有在正确选择和应用了这些光
谱参数后，才能得到正确的和实验可信度极高的温度测量数据。在我们的实验结
果中，我们将实验的可信度从89一94%提高到了98一99.5%，实验误差从士16一20%降
低到了士6.5%。我们的这一发现?
This paper presented the advantages of modern spectroscopy applications of remote sensing Fourier Transform Infrared (FTIR) spectroscopy and atomic emission spectroscopy in temperature measurements and air organic pollutants monitoring as a sensitive technology, especially combined with other analytical methods. The applications of remote sensing FTIR coupled with molecular spectra theory in combustion characteristics under high temperature and high pressure were investigated for the determination of combustion temperature of solid propellant. The influence of Blackbody temperature on the instrumental response function was studied to measure the energy distribution of the infrared emission spectra from the combustion flame, thereby quantified the combustion products concentrations. A multi-component analytical platform including Classical Least Squares (CLS), Partial Least Squares (PLS), Kalman Filter Method (KFM) and Artificial Neural Network (ANN) was established to overcome the overlaps between the spectral bands of each component in air Volatile Organic Compounds (VOCs) monitoring. The Open-Path real time air pollutant monitoring of remote sensing FTIR was conducted for the two-, three- four-and five- component system, herein the Path-Integrated Concentrations (PIC) of the desired VOCs leaking from the simulated source vs. the leaking time were obtained. Moreover, the concentrations of chloroform and methanol were spatially mapped in the vertical direction and on the horizontal plane during the quasi-steady state. The atomic emission spectroscopy with multiple spectral lines was used to measure the electro-thermal plasma temperatures and electronic density, and the influence of spectral parameters on the measurement accuracy was evaluated. This study will play significant influence on techniques of temperature measurement and air contaminant monitoring. The major content was described as follows:
1. The Real Time Measurement of Combustion Characteristics of Solid Propellant by Remote Sensing FTIR
The superiority of theory of molecular rotation-vibration emission spectra for the temperature measurement was verified. The in-situ combustion temperatures of solid propellant I and II were measured by Remote sensing FTIR combined with molecular
rotation-vibration emission spectra method and maximum spectral line intensity method. The results of molecular rotation-vibration emission spectra method and maximum spectral line intensity method were hi great agreement. Moreover, the optics of remote sensing FTIR used was calibrated, and the instrumental response function (IRF) was introduced and analyzed. Thus, the energy distribution of infrared emission spectra of the solid propellant combustion flame was measured.
2. Studies of Four Chemometrics in the Simultaneous Determination of Air Toxic VOCs
A chemometrics analytical platform was established to overcome the spectra interference and overlaps between the spectral bands of each component when doing multicomponent analysis of 1, 3-butadiene, benzene, o-xylene, chlorobenzene and acrolein. The methods included CLS, PLS, KFM and ANN. PLS was found to be the most potential method by comparing the prediction errors of each method. As for prediction samples, in which some unknown interferents exist, the modified PLS method successfully identified the interferents and corrected the spectrum, thus the concentrations of each desired component was quantified successfully. Moreover, ANN was applied to a ten-component system, results showed that the characteristic peak selection method was better than the equi-spaced wavenumber selection method when composing the analytical samples.
3. Temporally Monitoring Air Toxic VOCs by Remote Sensing FTIR and ANN
The simulated leaking sources composed of two-, three, four- and five VOCs were monitored by remote sensing FTIR with ANN as a quantification tool. The measured VOCs include chloroform, methylene chloride, acetone, methanol, hexane and butanol, etc. The plot of Path-Integrated Concentrations
引文
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66．Zhou Xinli(周新利)，Li Yan(李燕)，Liu Zuliang(刘祖亮)，Zhu Changjiang(朱长江)，Wang Junde(王俊德)，Lü Chunxu(吕春绪)．Combustion Temperature Measurement Of Pyrotechnic Composition using Remote Sensing Fourier Transform Infrared Spectrometry(FTIR遥测红外药剂的燃烧温度)． Spectroscopy and Special Analysis(光谱学与光谱分析)，2002，22：764-768
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71．Wang Junde(王俊德)．Applications of remote Sensing FTIR In Gases Determination(遥感傅里叶变换红外光谱在气体测定上的应用)．Lin C．(林水水)，Wu P．P．(吴平平)，Zhou W．M．(周文敏)，Wang J．D．(：王俊德)主编．Practical Fourier Transform Infrared Spectrometry(实用傅里叶变换红外光谱学)．Beijing(北京)：Chinese Environment Press(中国环境科学出版社)，1991，466-483
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116． Li Yan (李燕), Wang Junde (王俊德). Spatially Investigation of Remote Sensing FTIR for the Quantitative Determination of Air Toxic VOCs (在不同空间高度下遥感FTIR定量测定大气中的某些VOCs). Spectroscopy and Spectral Analysis (光谱学与光谱分析), in press
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120． Gu Binghe, Wang Junde, Zhou Xuetie, Wu Xuan, Liu Fang, Li Yan. Comparison of Multivariate Calibration Methods for Quantitative Analysis of Multicomponent Mixture of Air Toxic Organic Compounds by FTIR. J. Environ. Sci. & Health, 1998, A33: 1419-1436
121． Li Yan (李燕), Wang Junde (王俊德), Chen Zuoru (陈作如), Zhou Xuetie (周学铁). Comparison of Four Multivariate Calibration Methods in Simultaneous Determination of Air Toxic Organic Compounds with FTIR Spectroscopy (四种多变量校准方法在FTIR多组分分析中的性能比较). Spectroscopy and Spectral Analysis (光谱学与光谱分析), 2002,22: 758-760
122． Gu Binghe, Wang Lianjun, Wang Junde, Li Yan, Liu Fang, Chen Zuoru, Luo Yunhua. Elimination of Interferents Influence in Simultaneous Determination of Organic Gases Using PLS with FTIR Spectroscopy. Spectrosc. Lett., 1998, 31: 1451-1467
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125．Liu Fang(刘芳)，Wang Junde(王俊德)．Information Subtraction of Remote Sensing FTIR Spectra by Wavelet Method(运用小波变换对遥感FTIR光谱进行信息提取)．Spectroscopy and Spectral Analyses(光谱学与光谱分析)，in press
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128．Liu Fang(刘芳)，Wang Junde(王俊德)．Genetic Algorithms and Its Application in Infrared Spectral interpretation(遗传算法及其在谱图解析中的应用)． Spectroscopy and Spectral Analyses(光谱学与光谱分析)，2001，21：331-335
129．Liu Fang(刘芳)，Wang Junde(王俊德)．Quantitative Analyses of FTIR Spectra by Genetic Algorithm(遗传算法用于傅里叶变换红外光谱的定量解析)． Spectroscopy and Spectral Analyses(光谱学与光谱分析)，2001，21：607-610
130．Liu Fang(刘芳)，Wang Junde(王俊德)．Spectrum Search by Genetic Algorithms in FTIR Spectral Library(应用遗传算法在FTIR图谱库中进行谱图检索)． Spectroscopy and Spectral Analyses(光谱学与光谱分析)，2002，22：239-240
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142．Li Yan(李燕)，Wang Junde(王俊德)，Meng Guangzheng(孟广政)．Artificial Neural Network and Its Application in Spectral Analysis(人工神经网络及其在光谱分析中的应用)．Spectroscopy and Spectral Analysis(光谱学与光谱分析)，1999，19：844-849
143．Li Yan(李燕)，Wang Junde(王俊德)，Wang Lianjun(王连军)．Artificial Neural Network for the Identification of Infrared Spectra(人工神经网络法鉴别红外光谱)．Spectroscopy and Spectral Analysis(光谱学与光谱分析)，2000，20：477-479
144．Li Yan(李燕)，Sun)(iuyun(孙秀云)，Wang Junde(王俊德)．Determination of Five Component Infrared Spectra System with Artificial Neural Network (人工神经网络法测定五组分红外光谱体系)．Spectroscopy and Spectral Analysis(光谱学与光谱分析)，2000，20：773-776
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