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ATR-FTIR結(jié)合GC-FID快速識(shí)別油指紋技術(shù)研究

發(fā)布時(shí)間:2018-03-11 20:18

  本文選題:油指紋鑒別 切入點(diǎn):衰減全反射紅外光譜技術(shù) 出處:《大連海事大學(xué)》2017年碩士論文 論文類型:學(xué)位論文


【摘要】:大型物資海上運(yùn)輸和石油資源不斷開(kāi)采導(dǎo)致海上溢油事故頻發(fā),造成嚴(yán)重危害,準(zhǔn)確快速鑒別溢油源有助于開(kāi)展清污行動(dòng)、解決責(zé)任歸屬和爭(zhēng)端紛爭(zhēng)。目前海上溢油鑒別趨于多方法聯(lián)合使用,準(zhǔn)確度高卻耗時(shí)耗力,不能滿足快速鑒別油指紋的現(xiàn)實(shí)需求。因此,本研究提出結(jié)合紅外光譜法和氣相色譜法進(jìn)行油指紋鑒別,實(shí)現(xiàn)兩方法優(yōu)勢(shì)互補(bǔ),以期提供一種快速、便捷、準(zhǔn)確性高的溢油鑒別技術(shù)。本文結(jié)合傅里葉變換衰減全反射紅外光譜法操作簡(jiǎn)單、檢測(cè)速度快和氣相色譜法準(zhǔn)確度高的優(yōu)點(diǎn),分析研究0#柴油、-35#柴油、120#燃料油、大慶原油、內(nèi)蒙古原油等五種油品中正構(gòu)烷烴含量及短期風(fēng)化(風(fēng)化時(shí)間為40天)特性,并通過(guò)對(duì)兩方法相關(guān)性分析,對(duì)兩方法進(jìn)行關(guān)系耦合,實(shí)現(xiàn)油指紋快速鑒別。實(shí)驗(yàn)結(jié)果表明:柴油、原油紅外光譜圖整體相似,均于約2954 cm-1、約2920 cm-1、約 2850 cm-1、約 1460 cm-1、1376 cm-1、約 720 cm-1 處有特征吸收峰,為烷烴振動(dòng)頻率;120#燃料油紅外光譜圖于2952 cm-1、2920 cm-1、2851 cm-1、1595 cm-1、1455cm-1、1375cm-1、811cm-1和749cm-1處有特征吸收峰,為烷烴和芳烴振動(dòng)頻率。風(fēng)化后油品紅外光譜圖原有特征吸收峰峰位未發(fā)生移動(dòng),但柴油、原油于約1700 cm-1、約1600 cm-1處出現(xiàn)新特征吸收峰。油品種類不同,其氣相色譜圖及各碳數(shù)正構(gòu)烷烴濃度分布差異顯著,風(fēng)化后油品總正構(gòu)烷烴濃度降低,但中碳數(shù)正構(gòu)烷烴濃度增大。柴油、原油官能團(tuán)區(qū)1700 cm-1處吸光度隨著風(fēng)化程度的加深而增強(qiáng),指紋區(qū)720 cm-1處吸光度隨相連CH2個(gè)數(shù)增加而增強(qiáng),據(jù)此對(duì)紅外光譜法和氣相色譜法進(jìn)行關(guān)系耦合,提出一種油指紋快速鑒別方法:基于紅外光譜法譜圖數(shù)據(jù)估算油品風(fēng)化時(shí)間,并通過(guò)氣相色譜、紅外光譜和風(fēng)化時(shí)間三者耦合關(guān)系式求得氣相色譜實(shí)驗(yàn)中正構(gòu)烷烴成分比例,從而通過(guò)紅外光譜實(shí)驗(yàn)間接獲取氣相色譜實(shí)驗(yàn)相關(guān)信息,達(dá)到快速、準(zhǔn)確鑒別油指紋的目的。對(duì)該方法進(jìn)行驗(yàn)證表明關(guān)系耦合效果良好。但油品于不同季節(jié)風(fēng)化的風(fēng)化程度存在差異,對(duì)其進(jìn)行校正后,該方法精確度顯著提高。
[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.
【學(xué)位授予單位】:大連海事大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:X55;U698.7

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本文編號(hào):1599735


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