麻疯树等生物柴油分析方法研究
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摘要
本文采用GC-MS和毛细管GC-FID-外标法对三种黔产原料油(麻疯树籽油、菜籽油、乌桕梓油)通过酯交换反应得到的生物柴油产品进行定性定量分析。
麻疯树生物柴油中脂肪酸甲酯的主要化学成分由GC-MS的测定结果表明为:亚油酸甲酯(C18:2),油酸甲酯(C18:1),棕榈酸甲酯(C16:0)、硬脂酸甲酯(C18:0)和棕榈油酸甲酯(C16:1),痕量的亚麻酸甲酯(C18:3)和花生酸甲酯(C20:0),同时存在天然作物少见的奇数碳脂肪酸甲酯:十七烷酸甲酯(C17:0),但其含量较少。通过GC-MS鉴定菜籽油生物柴油中脂肪酸甲酯的主要成分为:芥酸甲酯(C18:2)、亚麻酸甲酯(C18:3)、亚油酸甲酯(C18:2)、油酸甲酯(C18:1)、硬脂酸甲酯(C18:0)、棕榈酸甲酯(C16:0)、花生一烯酸甲酯(C20:1),少量棕榈油酸甲酯(C16:1)、花生酸甲酯(C20:0)、花生二烯酸甲酯(C20:2)及二十四烷(烯)甲酯等。通过GC-MS鉴定乌桕梓油生物柴油中脂肪酸甲酯的主要化学成分为:亚麻酸甲酯(C18:3)、亚油酸甲酯(C18:2)、油酸甲酯(C18:1)、硬脂酸甲酯(C18:0)、棕榈酸甲酯(C16:0),2,4-癸二烯酸甲酯(C10:2),少量花生酸甲酯(C20:0)。
采用毛细管GC-FID-外标法测定生物柴油中脂肪酸甲酯的质量百分数,同时考察了方法的准确度、精密度、重现性。实验结果表明:方法线性关系良好,相对标准偏差在2%以内,平均回收率在96%～101%之间。以上结果说明方法灵敏度、准确度和精密度均达到了色谱分析检测的要求。GC法简便、快速、准确率高、重现性好,能准确测定生物柴油中脂肪酸甲酯的质量分数,可作为生物柴油产品质量监控,并为生物柴油产品新配方研究与开发提供有效的参考数据。
In this thesis,the qualitative and quantitative analysis method of biodiesel products,which were made from renewable biological sources,such as Jatropha curcas L.seed oil,rapeseed oil and Chinese tallow kernel oil growing in Guizhou province was established.The main constituents of the Jatropha curcas L.biodiesel, rapeseed biodiesel,and Chinese tallow kernel biodiesel were identified by GC-MS. And the external standard method for quantitative analysis of fatty acid methyl esters was established by capillary GC-FID.
The GC-MS experiment results showed that the main fatty acid methyl esters (FAME) of Jatropha curcas L.biodiesel were methyl palmitate(C16:0),methyl palmitoleate(C16:1),stearic acid methyl ester(C18:0),oleic acid methyl ester (C18:1),methyl linoleate(C 18:2),and trace amount of methyl linolenate(C18:3) and methyl arachidate(C20:0).There is also heptadecane acid methyl ester(C17:0) in Jatropha curcas biodiesel,a kind of odd-carbon fatty acid methyl ester which rarely exists in natural crops.The main FAME of rapeseed biodiesel were methyl palmitate(C16:0),methyl palmitoleate(C16:2),stearic acid methyl ester(C18:0),oleic acid methyl ester(C18:1),methyl linoleate(C18:2),methyl linolenate(C18:3),methyl cis- 11-eicosenoate(C20:1),11,13-eicosenoate(C20:2),methyl erucate(C22:1), tetracosanioc acid methyl ester(C24:0) and etc,which were identified.And the main FAME of Chinese tallow kernel biodiesel were 2,4-decadienoic acid methyl ester methyl palmitate(C10:2),stearic acid methyl ester(C18:0),oleic acid methyl ester(C18:1),methyl linoleate(C18:2),methyl linolenate(C18:3),and trace amount of methyl arachidate(C20:0) by GC-MS.
The external standard method for quantitative analysis of fatty acid methyl esters was established by capillary GC-FID.At the same time the accuracy,precision and reproducibility were reviewed and the results showed that good linear relationship were abtained,and the relative standard deviations were lower than two percent,and the average recovery rates were in the range of 96%to 101%.These results illustrated that the sensitivity,accuracy and precision were in accordance with the requirements of chromatographic analysis.The experimental results also showed that the GC-FID analysis method was effective,quick,stable,and reproducible with high accuracy.It can be qualified in determining the constituents of the fatty acid methyl esters in the biodiesel and can be applied in the quality control of biodiesel products.More importantly,it can provide an effective reference for the new formulation and development of biodiesel products.
麻疯树生物柴油中脂肪酸甲酯的主要化学成分由GC-MS的测定结果表明为:亚油酸甲酯(C18:2),油酸甲酯(C18:1),棕榈酸甲酯(C16:0)、硬脂酸甲酯(C18:0)和棕榈油酸甲酯(C16:1),痕量的亚麻酸甲酯(C18:3)和花生酸甲酯(C20:0),同时存在天然作物少见的奇数碳脂肪酸甲酯:十七烷酸甲酯(C17:0),但其含量较少。通过GC-MS鉴定菜籽油生物柴油中脂肪酸甲酯的主要成分为:芥酸甲酯(C18:2)、亚麻酸甲酯(C18:3)、亚油酸甲酯(C18:2)、油酸甲酯(C18:1)、硬脂酸甲酯(C18:0)、棕榈酸甲酯(C16:0)、花生一烯酸甲酯(C20:1),少量棕榈油酸甲酯(C16:1)、花生酸甲酯(C20:0)、花生二烯酸甲酯(C20:2)及二十四烷(烯)甲酯等。通过GC-MS鉴定乌桕梓油生物柴油中脂肪酸甲酯的主要化学成分为:亚麻酸甲酯(C18:3)、亚油酸甲酯(C18:2)、油酸甲酯(C18:1)、硬脂酸甲酯(C18:0)、棕榈酸甲酯(C16:0),2,4-癸二烯酸甲酯(C10:2),少量花生酸甲酯(C20:0)。
采用毛细管GC-FID-外标法测定生物柴油中脂肪酸甲酯的质量百分数,同时考察了方法的准确度、精密度、重现性。实验结果表明:方法线性关系良好,相对标准偏差在2%以内,平均回收率在96%～101%之间。以上结果说明方法灵敏度、准确度和精密度均达到了色谱分析检测的要求。GC法简便、快速、准确率高、重现性好,能准确测定生物柴油中脂肪酸甲酯的质量分数,可作为生物柴油产品质量监控,并为生物柴油产品新配方研究与开发提供有效的参考数据。
In this thesis,the qualitative and quantitative analysis method of biodiesel products,which were made from renewable biological sources,such as Jatropha curcas L.seed oil,rapeseed oil and Chinese tallow kernel oil growing in Guizhou province was established.The main constituents of the Jatropha curcas L.biodiesel, rapeseed biodiesel,and Chinese tallow kernel biodiesel were identified by GC-MS. And the external standard method for quantitative analysis of fatty acid methyl esters was established by capillary GC-FID.
The GC-MS experiment results showed that the main fatty acid methyl esters (FAME) of Jatropha curcas L.biodiesel were methyl palmitate(C16:0),methyl palmitoleate(C16:1),stearic acid methyl ester(C18:0),oleic acid methyl ester (C18:1),methyl linoleate(C 18:2),and trace amount of methyl linolenate(C18:3) and methyl arachidate(C20:0).There is also heptadecane acid methyl ester(C17:0) in Jatropha curcas biodiesel,a kind of odd-carbon fatty acid methyl ester which rarely exists in natural crops.The main FAME of rapeseed biodiesel were methyl palmitate(C16:0),methyl palmitoleate(C16:2),stearic acid methyl ester(C18:0),oleic acid methyl ester(C18:1),methyl linoleate(C18:2),methyl linolenate(C18:3),methyl cis- 11-eicosenoate(C20:1),11,13-eicosenoate(C20:2),methyl erucate(C22:1), tetracosanioc acid methyl ester(C24:0) and etc,which were identified.And the main FAME of Chinese tallow kernel biodiesel were 2,4-decadienoic acid methyl ester methyl palmitate(C10:2),stearic acid methyl ester(C18:0),oleic acid methyl ester(C18:1),methyl linoleate(C18:2),methyl linolenate(C18:3),and trace amount of methyl arachidate(C20:0) by GC-MS.
The external standard method for quantitative analysis of fatty acid methyl esters was established by capillary GC-FID.At the same time the accuracy,precision and reproducibility were reviewed and the results showed that good linear relationship were abtained,and the relative standard deviations were lower than two percent,and the average recovery rates were in the range of 96%to 101%.These results illustrated that the sensitivity,accuracy and precision were in accordance with the requirements of chromatographic analysis.The experimental results also showed that the GC-FID analysis method was effective,quick,stable,and reproducible with high accuracy.It can be qualified in determining the constituents of the fatty acid methyl esters in the biodiesel and can be applied in the quality control of biodiesel products.More importantly,it can provide an effective reference for the new formulation and development of biodiesel products.
引文
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[2]曾建立,王晓东,赵兵,王玉春.高温气相色谱分析油脂转酯反应[J].中国油脂,2007,32(7):66-69.
[3]张恬,袁银南.生物柴油的环境效益与社会经济效益[J].能源环境保护,2005,19(2):16-19.
[4]朱建良,张冠杰.国内外生物柴油研究生产现状及发展趋势[J].化工时刊,2004,18(1):23-27.
[5]方芳,曾虹燕.气相色谱法测定生物柴油中的脂肪酸甲酯[J].福建林学院学报,2005,25(1):1-4.
[6]何东平,张世宏,齐玉掌.我国生物柴油的发展与展望[J].粮食加工与食品机械,2004,(9):10-12.
[7]张大华,李丽霞.液相色谱法测定生物柴油中多种脂肪酸甲酯[J].粮食与油脂,2007,(12):41-43.
[8]李长秀,唐忠.气相色谱法测定生物柴油样品中脂肪酸甲酯和脂肪酸甘油酯的含量[J].分析测试学报,2005,24(5):66-68.
[9]黄庆德,黄凤洪.郭萍梅.生物柴油生产技术及其开发意义[J].粮食与油脂,2002,(9):8-10.
[10]唐建设,项丽.毛细管电泳在农药残留检测上的应用[J].分析测试技术与仪器,2005,11(3):215-220.
[11]谭天伟,土芳,邓立.生物柴油的生产和应用[J].现代化工,2002,22(2):4-6.
[12]蒲晓斌,蒋梁材,张锦芳.生物柴油——一类可再生清洁燃料[J].四川农业科技,2004,(8):6-7.
[13]冀星.生物柴油——点亮北京奥运[J].中关村,2004,(5):35.
[14]邬国英,巫淼鑫,林西平.植物油制备生物柴油[J].江苏石油化工学院学报,2002,14(3):8-11.
[15]Ackman,R.G.The choice of chromatography column for analysis biodiesel[J].Journal of American Oil Chemists' Society,1989,66(3):290-293.
[15]Abdulkadir,S.;Tsuchiya;Makoto.One-step method for quantitative and qualitative analysis of fatty acids in marine animal samples[J].Journal of Experimental Marine Biology and Ecology,2008,354(1):1-8.
[17]Bamwal,B.K.;Sharma,M.P.Prospects of biodiesel production from vegetable oils in India[J].Renewable and Sustainable Energy Reviews,2005,9(4):363-378.
[18] Bender, M. Economic feasibility review for community-scale farmer cooperatives for biodiesel [J]. Bioresource Technology, 1999, 70(1): 81～87.
[19] Bonan, S.; Mosca, G.; Vamerali, T. Oil crops for biodiesel production to Italy [J]. Renewable Energy, 1999,(16): 1053-1056.
[20] Carraretto, C.; Macor, A.; Mirandola, A. Biodiesel as alternative fuel: experimental analysis and energetic evaluations [J]. Energy, 2004, 29(12-15): 2195-2211.
[21] Cock, S. Analysis for Fatty Acid Methyl Esters by Using Supercritical Fluid Chromatography with Mass Evaporative Light Scattering Detection [J]. Analytical Process, 1991,28(1): 11.
[22] Darnoko, D.; Cheryan, M.; Perkins, E.G. Analysis of Vegetable Oil Transesterification Products by Gel Permeation Chromatography [J]. The Journal of Liquid Chromatography & Related Technologies, 2000, 23: 2327-2335.
[23] Eder, K. Gas chromatographic analysis of fatty acid methyl esters [J]. Journal of Chromatography B: Biomedical Sciences and Applications , 1995, 671(1-2): 113-131.
[24] Encinar, J. M. Biodiesel Fuels from Vegetable Oils: Transesterificationof Cynara Cardunculus L Oils with Ethanol [J]. Energy and Fuels, 2002, 7(5(2): 443.
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