基于荧光光谱分析的石油类污染物识别测量方法及其实验研究
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摘要
石油是重要的能源和工业原料，在石油的勘探、开采、运输、加工乃至消费过程中，有大量的原油或石油产品被泄漏或排放至自然环境中，由石油引起的环境污染日益严重，甚至导致生态灾难。针对石油类污染物的识别和含量测量是环境监测和治理的重要内容。
论文以荧光光谱分析为主要方法，在深入分析了石油类污染物成分特点的基础上，提出了结合荧光光谱分析与平行因子分析理论的混合体系中石油类污染物整体识别测量方法，并进行了实验论证。
由光致发光理论，结合石油化学相关数据，论证应用荧光方法整体测量原油或石油产品等石油类污染物的可行性、适用性。研究实验仪器特性和散射现象对荧光光谱测量的影响，实验确定消除影响的方法。综合考虑被测物成分组成、散射消除等问题，选定激发与发射测量范围，对选定样品进行荧光光谱测量，获得样品三维荧光光谱与各维度投影光谱，分析光谱特征。
测量样品有机溶液荧光光谱，研究了其与纯样品光谱的差异。研究多元校正与平行因子分析理论及方法，确定应用平行因子分析方法作为石油类污染物多成分混合体系中成分识别与测量的基本手段。以不同被测样品的四氯化碳溶液稀释混合构造共存体系实验样本集；根据被测物的光谱特征判定平行因子分析的因子数，进而辨识溶液成分特征光谱并实现定量测量；设定一种样品为干扰成分，研究其对混合体系中主要成分识别与定量测量的影响。经过实验，分别识别了各预测样本集中主要成分并测得它们的含量。
研究表面活性剂胶束溶液在荧光测量分析中的应用原理与方法，测量石油类样品在十二烷基硫酸钠胶束溶液中光谱，验证使用胶束增敏荧光方法测量水中复杂组分石油类污染物含量的方法。实验确定被测石油类样品应用胶束方法有效测量范围；将溶液稀释与混合制成共存体系样本集，然后通过分析浓度模式因子载荷曲线，确定因子数，辨识表征样品含量的因子，估计预测样本集中各成分含量。对于光谱重叠程度较高的样本集，首先使用局部光谱结合平行因子分析方法测定部分成分含量；然后使用不含已知成分的校正样本集光谱数据重构三维数据矩阵，重复应用平行因子分析方法实现对其它成分的定量测量。实验表明在一定浓度范围内，胶束增敏荧光方法结合平行因子分析可以实现对混合体系内的石油类污染物成分的识别与定量测量。
Petroleum is an important energy source and industrial raw material. Large quantitiesof crude oil and oil products are leaked or spilled to the natural environment during oilexploration, mining, transportation, processing and consumption. The environmentpollution caused by petroleum is increasingly serious and the pollution may even lead toan ecological disaster. Therefore, identifying and concentration measurement of petroleumpollutants are the important content of environmental monitoring and management.
This paper employs fluorescence spectroscopy as primary means. Based on theanalysis of the petroleum pollutant components characteristics, the paper presents anidentification and measurement method for petroleum pollutant components in mixedsystem. The method combines the three-dimensional fluorescent spectroscopy with theparallel factor analysis, and is tested by experiments.
This paper demonstrates the feasibility and applicability of fluorescence methodoverall measurement in crude oil and petroleum products pollutant according lightelectroluminescent theory and related data of petrochemistry.
The experiment instruments characteristics and fluorescence spectra measurementinfluence resulted in scattering phenomenon are researched, and then the method ofremoval the influence is studied. The excitation and emission scan range is selectedconsidering of substances composition and elimination of scattering. Three dimensionalfluorescence spectrum and projection spectra of each dimension of samples are acquiredand spectral features are analyzed through the fluorescence spectrum measurement of theselected samples.
Through measuring the fluorescence spectrum of sample organic solution, thespectrum difference between the solution and pure sample is researched. Through theresearch of multivariate calibration and parallel factor analysis theory and methods, thispaper applies parallel factor analysis method as the basic means for measurement andidentification of petroleum pollutants composition mixed system. Experimental sample setis consisted by dilution and blend of CCl4solutions of different samples. First, the numberof parallel factor analysis factors is determined according to spectral features of analyte. Then, the identification of characteristic spectra and quantitative measurement are realized.A sample is set as interference composition, and its influence on spectrum resolution andquantitative measurement of the main components is studied in the mixed system. Byexperiments, primary components of each predicted sample set are identified and theirconcentrations are measured.
Application principle and method of surfactant micelle solution in the measurementand analysis of fluorescence are researched. Spectrums of petroleum samples in sodiumdodecyl sulfate micelle solutions are measured. The method of measuring complicatedcomponents petroleum pollutant content in the water with micelle sensitizing fluorescencemethod is verified. In this paper, the effective range of micelle method applying topetroleum samples is determined by experiment. Then coexistence system sample is madethrough dilution and mix, and the components of system are measured at the same time byapplying the parallel factor analysis method. The factor number is determined andconcentrations of each component in the prediction samples are estimated and the factorswhich represent sample content are identified through the analysis of the mode ofconcentration factor curve of load. For the samples which spectra are highly overlapped,local spectrum combined with the method of parallel factor analysis is used to estimatesectional component content firstly. The concentration of the other samples are estimatedby applying parallel factor analysis after reconstruction of correction samples withsamples exclude known component finally. The experiments show that in a certain rangeof concentration, micelle sensitizing fluorescence analysis and parallel factor analysis canrealize the identification and quantitative measurement of petroleum pollutant componentsin mixed system.
论文以荧光光谱分析为主要方法，在深入分析了石油类污染物成分特点的基础上，提出了结合荧光光谱分析与平行因子分析理论的混合体系中石油类污染物整体识别测量方法，并进行了实验论证。
由光致发光理论，结合石油化学相关数据，论证应用荧光方法整体测量原油或石油产品等石油类污染物的可行性、适用性。研究实验仪器特性和散射现象对荧光光谱测量的影响，实验确定消除影响的方法。综合考虑被测物成分组成、散射消除等问题，选定激发与发射测量范围，对选定样品进行荧光光谱测量，获得样品三维荧光光谱与各维度投影光谱，分析光谱特征。
测量样品有机溶液荧光光谱，研究了其与纯样品光谱的差异。研究多元校正与平行因子分析理论及方法，确定应用平行因子分析方法作为石油类污染物多成分混合体系中成分识别与测量的基本手段。以不同被测样品的四氯化碳溶液稀释混合构造共存体系实验样本集；根据被测物的光谱特征判定平行因子分析的因子数，进而辨识溶液成分特征光谱并实现定量测量；设定一种样品为干扰成分，研究其对混合体系中主要成分识别与定量测量的影响。经过实验，分别识别了各预测样本集中主要成分并测得它们的含量。
研究表面活性剂胶束溶液在荧光测量分析中的应用原理与方法，测量石油类样品在十二烷基硫酸钠胶束溶液中光谱，验证使用胶束增敏荧光方法测量水中复杂组分石油类污染物含量的方法。实验确定被测石油类样品应用胶束方法有效测量范围；将溶液稀释与混合制成共存体系样本集，然后通过分析浓度模式因子载荷曲线，确定因子数，辨识表征样品含量的因子，估计预测样本集中各成分含量。对于光谱重叠程度较高的样本集，首先使用局部光谱结合平行因子分析方法测定部分成分含量；然后使用不含已知成分的校正样本集光谱数据重构三维数据矩阵，重复应用平行因子分析方法实现对其它成分的定量测量。实验表明在一定浓度范围内，胶束增敏荧光方法结合平行因子分析可以实现对混合体系内的石油类污染物成分的识别与定量测量。
Petroleum is an important energy source and industrial raw material. Large quantitiesof crude oil and oil products are leaked or spilled to the natural environment during oilexploration, mining, transportation, processing and consumption. The environmentpollution caused by petroleum is increasingly serious and the pollution may even lead toan ecological disaster. Therefore, identifying and concentration measurement of petroleumpollutants are the important content of environmental monitoring and management.
This paper employs fluorescence spectroscopy as primary means. Based on theanalysis of the petroleum pollutant components characteristics, the paper presents anidentification and measurement method for petroleum pollutant components in mixedsystem. The method combines the three-dimensional fluorescent spectroscopy with theparallel factor analysis, and is tested by experiments.
This paper demonstrates the feasibility and applicability of fluorescence methodoverall measurement in crude oil and petroleum products pollutant according lightelectroluminescent theory and related data of petrochemistry.
The experiment instruments characteristics and fluorescence spectra measurementinfluence resulted in scattering phenomenon are researched, and then the method ofremoval the influence is studied. The excitation and emission scan range is selectedconsidering of substances composition and elimination of scattering. Three dimensionalfluorescence spectrum and projection spectra of each dimension of samples are acquiredand spectral features are analyzed through the fluorescence spectrum measurement of theselected samples.
Through measuring the fluorescence spectrum of sample organic solution, thespectrum difference between the solution and pure sample is researched. Through theresearch of multivariate calibration and parallel factor analysis theory and methods, thispaper applies parallel factor analysis method as the basic means for measurement andidentification of petroleum pollutants composition mixed system. Experimental sample setis consisted by dilution and blend of CCl4solutions of different samples. First, the numberof parallel factor analysis factors is determined according to spectral features of analyte. Then, the identification of characteristic spectra and quantitative measurement are realized.A sample is set as interference composition, and its influence on spectrum resolution andquantitative measurement of the main components is studied in the mixed system. Byexperiments, primary components of each predicted sample set are identified and theirconcentrations are measured.
Application principle and method of surfactant micelle solution in the measurementand analysis of fluorescence are researched. Spectrums of petroleum samples in sodiumdodecyl sulfate micelle solutions are measured. The method of measuring complicatedcomponents petroleum pollutant content in the water with micelle sensitizing fluorescencemethod is verified. In this paper, the effective range of micelle method applying topetroleum samples is determined by experiment. Then coexistence system sample is madethrough dilution and mix, and the components of system are measured at the same time byapplying the parallel factor analysis method. The factor number is determined andconcentrations of each component in the prediction samples are estimated and the factorswhich represent sample content are identified through the analysis of the mode ofconcentration factor curve of load. For the samples which spectra are highly overlapped,local spectrum combined with the method of parallel factor analysis is used to estimatesectional component content firstly. The concentration of the other samples are estimatedby applying parallel factor analysis after reconstruction of correction samples withsamples exclude known component finally. The experiments show that in a certain rangeof concentration, micelle sensitizing fluorescence analysis and parallel factor analysis canrealize the identification and quantitative measurement of petroleum pollutant componentsin mixed system.
引文
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