ATR-FTIR结合GC-FID快速识别油指纹技术研究

发布时间：2018-03-11 20:18

本文选题：油指纹鉴别　切入点：衰减全反射红外光谱技术　出处：《大连海事大学》2017年硕士论文　论文类型：学位论文

【摘要】：大型物资海上运输和石油资源不断开采导致海上溢油事故频发,造成严重危害,准确快速鉴别溢油源有助于开展清污行动、解决责任归属和争端纷争。目前海上溢油鉴别趋于多方法联合使用,准确度高却耗时耗力,不能满足快速鉴别油指纹的现实需求。因此,本研究提出结合红外光谱法和气相色谱法进行油指纹鉴别,实现两方法优势互补,以期提供一种快速、便捷、准确性高的溢油鉴别技术。本文结合傅里叶变换衰减全反射红外光谱法操作简单、检测速度快和气相色谱法准确度高的优点,分析研究0#柴油、-35#柴油、120#燃料油、大庆原油、内蒙古原油等五种油品中正构烷烃含量及短期风化(风化时间为40天)特性,并通过对两方法相关性分析,对两方法进行关系耦合,实现油指纹快速鉴别。实验结果表明:柴油、原油红外光谱图整体相似,均于约2954 cm-1、约2920 cm-1、约 2850 cm-1、约 1460 cm-1、1376 cm-1、约 720 cm-1 处有特征吸收峰，为烷烃振动频率;120#燃料油红外光谱图于2952 cm-1、2920 cm-1、2851 cm-1、1595 cm-1、1455cm-1、1375cm-1、811cm-1和749cm-1处有特征吸收峰,为烷烃和芳烃振动频率。风化后油品红外光谱图原有特征吸收峰峰位未发生移动,但柴油、原油于约1700 cm-1、约1600 cm-1处出现新特征吸收峰。油品种类不同,其气相色谱图及各碳数正构烷烃浓度分布差异显著,风化后油品总正构烷烃浓度降低,但中碳数正构烷烃浓度增大。柴油、原油官能团区1700 cm-1处吸光度随着风化程度的加深而增强,指纹区720 cm-1处吸光度随相连CH2个数增加而增强,据此对红外光谱法和气相色谱法进行关系耦合,提出一种油指纹快速鉴别方法:基于红外光谱法谱图数据估算油品风化时间,并通过气相色谱、红外光谱和风化时间三者耦合关系式求得气相色谱实验中正构烷烃成分比例,从而通过红外光谱实验间接获取气相色谱实验相关信息,达到快速、准确鉴别油指纹的目的。对该方法进行验证表明关系耦合效果良好。但油品于不同季节风化的风化程度存在差异,对其进行校正后,该方法精确度显著提高。
[Abstract]:Maritime transportation of large materials and continuous exploitation of oil resources lead to frequent oil spills at sea, causing serious harm. Accurate and rapid identification of oil spill sources is helpful for carrying out clean-up operations. At present, the identification of oil spill at sea tends to be used in combination with multiple methods, but the accuracy is high, but time-consuming and labor-consuming, so it can not meet the practical requirements of rapid identification of oil fingerprints. In this study, oil fingerprint identification with infrared spectroscopy and gas chromatography was proposed to realize the complementary advantages of the two methods, in order to provide a rapid and convenient. Combined with the advantages of Fourier transform attenuated total reflectance infrared spectroscopy (FTIR), fast detection speed and high accuracy of gas chromatography, this paper analyzes and studies the fuel oil No.120#, Daqing crude oil. The content of n-alkanes and the characteristics of short-term weathering (weathering time is 40 days) in five kinds of oil such as Inner Mongolia crude oil are analyzed, and the relationship between the two methods is coupled by analyzing the correlation between the two methods. The experimental results show that the infrared spectra of diesel oil and crude oil are similar in whole, and all have characteristic absorption peaks at about 2954 cm-1, about 2920 cm-1, about 2850 cm-1, about 1460 cm-1 and 1376 cm-1, and about 720 cm-1, respectively. For alkane vibrational frequency, the infrared spectrum of 2952 cm ~ (-1) ~ 2920 cm ~ (-1), 2851 cm ~ (-1), 1595 cm ~ (-1), 1455 cm ~ (-1), 1375 cm ~ (-1), 811cm ~ (-1) and 749 cm ~ (-1) have characteristic absorption peaks, which are the vibrational frequencies of alkanes and aromatics. After weathering, the original characteristic absorption peak does not move, but the original characteristic absorption peak does not move in diesel oil. New characteristic absorption peaks appeared in crude oil at about 1700cm-1, about 1600 cm-1. The gas chromatogram and the distribution of n-alkanes of each carbon number varied significantly with different types of oil, and the total n-alkane concentrations of oil products decreased after weathering. However, the concentration of n-alkanes increased. The absorbance at 1700 cm-1 in the functional group region of diesel oil and crude oil increased with the deepening of weathering, and the absorbance at 720 cm-1 in fingerprint region increased with the increase of the number of connected CH2. Based on the relationship between infrared spectrum and gas chromatography, a fast identification method for oil fingerprint was proposed. The method was used to estimate the weathering time of oil products based on the spectrum data of infrared spectrum method, and to estimate the weathering time of oil products by gas chromatography. The coupling relation of infrared spectrum and weathering time is used to obtain the proportion of n-alkane in gas chromatographic experiment, and the relative information of gas chromatographic experiment is obtained indirectly through infrared spectrum experiment. The purpose of accurate identification of oil fingerprinting shows that the relationship coupling effect is good, but the weathering degree of oil products in different seasons is different, and the accuracy of this method is significantly improved after correcting it.
【学位授予单位】：大连海事大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X55;U698.7

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