不同萃取剂下原油样品荧光光谱的实验研究
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摘要
自从上世纪30年代从前苏联传入我国至今,荧光录井先后经历了定性、半定量和定量荧光录井等各个发展阶段。现阶段用于定量石油录井的荧光仪器主要依靠发射光谱荧光强度与原油样品浓度间的相互关系作为计算岩屑或岩芯中含油量的主要依据,但由于二维荧光发射谱存在数据有限、准确度不高、浓度测量范围狭窄等不足而在使用中暴露出一些问题。由中国海洋大学光学光电子实验室建立的基于同步荧光光谱的浓度三维定量分析技术能够有效弥补上述不足,有力的推动了荧光分析技术在石油勘探领域的应用。但目前普遍使用的萃取剂毒性大,使用安全性低,特别是荧光性质不够理想,难以满足定量录井尤其是改进后的浓度三维定量分析技术对定量分析精度的要求。为了弥补这一制约浓度定量计算精度的缺陷,本论文以提高荧光定量分析技术的准确性和精度为目的,提出选择一种性能全方位满足荧光定量分析要求的萃取试剂的设想,并开展了相关实验研究。
论文总体上分为三大部分,采用的是实验对比的研究思路。
第一大部分为相关工作的引入与介绍。首先通过理论阐述和文献综述奠定本论文相关研究内容的理论依据。通过对实验仪器设备、样品来源、试剂以及光谱采集和数据处理的详细介绍,确定了论文相关实验所依赖的技术手段和研究对象,这些内容构成了论文的前三章。
第二大部分是作者的主要工作,包括:不同萃取剂下相同原油样品荧光光谱特征的实验对比和相同萃取剂下不同原油样品荧光光谱特征的实验对比两个大的方面的工作,相关内容构成了论文的第四章和第五章。
一方面,在充分考虑了萃取剂因素对定量荧光分析的影响的基础上,从技术改进的高度,提出选择符合定量荧光录井要求的理想萃取剂的设想,并以岩屑荧光录井发展历程中使用过的十余种各类有机试剂作为研究对象,着重从溶解能力和荧光特性两个方面进行了全面详细的实验对比。在总结实验结果并综合考虑毒性、使用安全性等其它因素的基础上,确定异丙醇在各个方面都比目前普遍使用的萃取剂正己烷更为符合定量荧光分析的要求,可以作为今后进行荧光光谱研究的首选试剂;
另一方面,在采用异丙醇作为荧光光谱研究首选试剂的基础上,分别配制了不同井区相同层段、相同井区不同井号以及物理性质相近的不同种类的原油样品对应不同浓度的萃取液。分别采集不同浓度萃取液的二维荧光发射谱和同步荧光光谱进行光谱特征实验对比。结果表明:原油储藏地域、埋藏时期、地质条件以及物理性质的相似性均不会削弱荧光光谱的差别,从而为日后进行原油种类鉴别的尝试奠定了事实依据。
作论文的最后一部分,第六章在对本论文的工作进行总结的基础上,对下一步工作的努力方向进行了展望,并在本论文研究内容奠定的事实基础上,提出了下一步凭借荧光光谱特征对原油的种类进行鉴别的设想。结合多种全新的数据处理、特征提取、模式识别技术并结合化学计量学的最新成果,提出了实现特定目标的技术路线。
Fluorescence analysis technique,with its special capability of detecting polycyclic aromatic hydrocarbons(PAHs) in crude oil,has been widely used in the field of oil logging.After being introduced into China from former Soviet Union in 1930s,the technique has experienced three development stages:qualitative,semi-quantitative and quantitative analysis stage,with significant improvements on its technical means. But there are still some defects in application of this technique.The measurement of emission spectrum is comparatively easy and fast,but with limited concentration range and lower accuracy.A new method based on synchronous fluorescence spectrum analysis of crude oil has been established by the Optics & Optoelectronics Laboratory of Ocean University of China,which can effectively solve the problem mentioned above,and meet all the need of oil logging on both accuracy and efficiency.
But the extraction agents conventionally used nowadays are with high toxicity and relatively poor fluorescence property,they can hardly meet all the need of quantitative analysis.In order to solve this problem,in this thesis,some relative experimental investigations have been made to find an idea extraction agent with the purpose to improve the accuracy of fluorescence quantitative analysis.
This thesis consists of three main parts and applies the research approach of experimental comparison.
The first part makes introductions of relative contents which provide theoretical foundation,research thought,and experimental method of this thesis.Theoretical explanation and literature review are made first by means of introducing basic theories,relative fluorescence detection techniques,and development of fluorescence analysis method in petroleum exploration as well as usage of extraction agents in oil logging in history.Then an introduction about origin and characters of crude oil samples used in experiments,properties and parameter settings of instruments,data processing and 3D spectra formation is made.
There were more than ten types of organic solvents used in the developing history of fluorescence oil logging,and they are chosen as research objects in this thesis. Comprehensive comparison experiment is made at two aspects of solubility and fluorescence property.Solutions of the same crude oil sample with concentration range from 10g/L to 10~(-4)g/L were prepared using different types of extraction agents. Through the comparison experiments of emission spectrum and synchronous spectrum about fluorescence property of both the extraction agents and solutions, isopropanol is chosen as an idea extraction agent in fluorescence quantitative analysis.
Then as an idea extraction agents,isopropanol is used to prepare solution of different crude oil samples with concentration range from 10g/L to 10~(-4)g/L.Samples from different well districts or different well numbers and samples with similar physical characteristics were chosen to ensure the representativeness of the comparison experiment.It is found that the fluorescence spectra of various crude oil are obviously different,and these differences are not affected by the similarities of districts,burial time,geological conditions and physical characteristics.This means it's feasible to identify different kinds of crude oil by means of analyzing their fluorescence spectral with proper data processing method.These contents compose of main work in the second part of this thesis.
At the last part of this thesis,summarizes of all the work are made and some possible future developments are brought forward to make certain improvements in data processing and feature extraction include new information extracting method, pattern recognition techniques and new achievements of chemometrics.With these improvements,the newly developed methods may become a useful means in petroleum logging.
论文总体上分为三大部分,采用的是实验对比的研究思路。
第一大部分为相关工作的引入与介绍。首先通过理论阐述和文献综述奠定本论文相关研究内容的理论依据。通过对实验仪器设备、样品来源、试剂以及光谱采集和数据处理的详细介绍,确定了论文相关实验所依赖的技术手段和研究对象,这些内容构成了论文的前三章。
第二大部分是作者的主要工作,包括:不同萃取剂下相同原油样品荧光光谱特征的实验对比和相同萃取剂下不同原油样品荧光光谱特征的实验对比两个大的方面的工作,相关内容构成了论文的第四章和第五章。
一方面,在充分考虑了萃取剂因素对定量荧光分析的影响的基础上,从技术改进的高度,提出选择符合定量荧光录井要求的理想萃取剂的设想,并以岩屑荧光录井发展历程中使用过的十余种各类有机试剂作为研究对象,着重从溶解能力和荧光特性两个方面进行了全面详细的实验对比。在总结实验结果并综合考虑毒性、使用安全性等其它因素的基础上,确定异丙醇在各个方面都比目前普遍使用的萃取剂正己烷更为符合定量荧光分析的要求,可以作为今后进行荧光光谱研究的首选试剂;
另一方面,在采用异丙醇作为荧光光谱研究首选试剂的基础上,分别配制了不同井区相同层段、相同井区不同井号以及物理性质相近的不同种类的原油样品对应不同浓度的萃取液。分别采集不同浓度萃取液的二维荧光发射谱和同步荧光光谱进行光谱特征实验对比。结果表明:原油储藏地域、埋藏时期、地质条件以及物理性质的相似性均不会削弱荧光光谱的差别,从而为日后进行原油种类鉴别的尝试奠定了事实依据。
作论文的最后一部分,第六章在对本论文的工作进行总结的基础上,对下一步工作的努力方向进行了展望,并在本论文研究内容奠定的事实基础上,提出了下一步凭借荧光光谱特征对原油的种类进行鉴别的设想。结合多种全新的数据处理、特征提取、模式识别技术并结合化学计量学的最新成果,提出了实现特定目标的技术路线。
Fluorescence analysis technique,with its special capability of detecting polycyclic aromatic hydrocarbons(PAHs) in crude oil,has been widely used in the field of oil logging.After being introduced into China from former Soviet Union in 1930s,the technique has experienced three development stages:qualitative,semi-quantitative and quantitative analysis stage,with significant improvements on its technical means. But there are still some defects in application of this technique.The measurement of emission spectrum is comparatively easy and fast,but with limited concentration range and lower accuracy.A new method based on synchronous fluorescence spectrum analysis of crude oil has been established by the Optics & Optoelectronics Laboratory of Ocean University of China,which can effectively solve the problem mentioned above,and meet all the need of oil logging on both accuracy and efficiency.
But the extraction agents conventionally used nowadays are with high toxicity and relatively poor fluorescence property,they can hardly meet all the need of quantitative analysis.In order to solve this problem,in this thesis,some relative experimental investigations have been made to find an idea extraction agent with the purpose to improve the accuracy of fluorescence quantitative analysis.
This thesis consists of three main parts and applies the research approach of experimental comparison.
The first part makes introductions of relative contents which provide theoretical foundation,research thought,and experimental method of this thesis.Theoretical explanation and literature review are made first by means of introducing basic theories,relative fluorescence detection techniques,and development of fluorescence analysis method in petroleum exploration as well as usage of extraction agents in oil logging in history.Then an introduction about origin and characters of crude oil samples used in experiments,properties and parameter settings of instruments,data processing and 3D spectra formation is made.
There were more than ten types of organic solvents used in the developing history of fluorescence oil logging,and they are chosen as research objects in this thesis. Comprehensive comparison experiment is made at two aspects of solubility and fluorescence property.Solutions of the same crude oil sample with concentration range from 10g/L to 10~(-4)g/L were prepared using different types of extraction agents. Through the comparison experiments of emission spectrum and synchronous spectrum about fluorescence property of both the extraction agents and solutions, isopropanol is chosen as an idea extraction agent in fluorescence quantitative analysis.
Then as an idea extraction agents,isopropanol is used to prepare solution of different crude oil samples with concentration range from 10g/L to 10~(-4)g/L.Samples from different well districts or different well numbers and samples with similar physical characteristics were chosen to ensure the representativeness of the comparison experiment.It is found that the fluorescence spectra of various crude oil are obviously different,and these differences are not affected by the similarities of districts,burial time,geological conditions and physical characteristics.This means it's feasible to identify different kinds of crude oil by means of analyzing their fluorescence spectral with proper data processing method.These contents compose of main work in the second part of this thesis.
At the last part of this thesis,summarizes of all the work are made and some possible future developments are brought forward to make certain improvements in data processing and feature extraction include new information extracting method, pattern recognition techniques and new achievements of chemometrics.With these improvements,the newly developed methods may become a useful means in petroleum logging.
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