气相色谱法测定生物柴油中脂肪酸甲酯含量

1、第5期刘祥华等:气相色谱法测定生物柴油中脂肪酸甲酯含量591文章编号:1004-1656(2006)05-0591-02气相色谱法测定生物柴油中脂肪酸甲酯含量刘祥华,刘灿明13,吴苏喜,曾凡佳,胡秋龙211(1.湖南农业大学理学院应用化学系,湖南长沙410128;2.长沙理工大学生物与食品工程系,湖南长沙410076)关键词:气相色谱法;生物柴油;脂肪酸甲脂;菜籽油中图分类号:065717文献标识码:A生物柴油是利用动植物油脂等可再生资源通过酯交换技术制造的可以替代石化柴油的新型清1-3洁安全燃料它的主要成分是脂肪酸甲酯。由于不同油脂原料所生产的生物柴油的脂肪酸甲脂组成不同因而测定时所需的气相

2、色谱条件与方法4-6也不尽相同。本文采用HP-innowax色谱柱,以十三酸甲酯为内标物,籽生物柴油中主要脂肪酸甲酯(甲酯、亚油酸甲酯、和芥酸甲酯),、准确度高、,。的升温速率升至240°C5min;载气:N2,柱头压60kPa;氢气:in;空气:320mL/L,混合脂肪酸min;:11。2、3、4、5、6和7分别为十、油酸甲酯、亚油酸甲酯、亚、花生一烯酸甲酯和芥酸甲酯。1实验部分111材料油菜籽生物柴油(按照动植物油脂脂肪酸甲7酯制备方法自制)112仪器与试剂SP-6890型气相色谱仪;FID检测器;N3000色谱工作站;AL204电子天平;HP-innowax毛细m)。管色谱柱(

3、30m×0125mm×0125十三酸甲酯、棕榈酸甲酯、油酸甲酯、亚麻酸甲酯、花生一烯酸甲酯和芥酸甲酯(均为色谱纯,Sigma公司),其它试剂为分析纯。113生物柴油的预处理及其脂肪酸甲酯含量的计算取一定量的生物柴油样品于1mL的容量瓶中,加入0125mL浓度为8mg/mL的十三酸甲酯,用正己烷定容后,进行气色谱分析。将从标准工作曲线上查得的浓度乘以生物柴油样品的稀释倍数,从而得到生物柴油样品中的脂肪酸甲酯含量。114色谱分析条件汽化室温度280°C;检测温度280°C;柱温采用程度升温:初始温度170°C,保持015min,以5°C/

4、min的升温速率升到200°C,然后以15°C/min收稿日期:2005-11-23;修回日期:2006-02-10基金项目:湖南省科技计划项目(05SK3085)图1标准溶液的气相色谱图Fig.1Gaschromatogramofstandardsolutions图2生物柴油的气相色谱图Fig.2Gaschromatogramofbiodieselsample联系人简介:刘灿明(1955-),男,教授,主要从事天然产物和应用化学研究。Email:liucanming© 1994-2010 China Academic Journal Electronic Pub

5、lishing House. All rights reserved. 592化学研究与应用第18卷2结果与讨论211线性关系的测定表1线性关系实验结果Table1Experimentalresultsonlinerarity标准样品浓度范围(mg/mL)线性回归方程Y=019053X-011549Y=110073X-012586Y=01843X-011178Y=015659X-010361Y=018139X-010923Y=01812X-010717相关系数r019987019963019975019979019986019989棕榈酸甲酯11515油酸甲酯11515亚油酸甲酯11515亚麻

6、酸甲酯0175715花生一烯酸甲酯0175715芥酸甲酯0175715称一定量的棕榈酸甲酯、油酸甲酯、亚油酸甲酯、亚麻酸甲酯、花生一烯酸甲酯和芥酸甲酯标准样品,以正己烷为溶剂,配制成混合脂肪酸甲酯标准贮备液。然后再稀释为10个不同浓度的混合脂肪酸甲酯标准溶液液中,棕榈酸甲酯、参考文献:1JurgenUlrichFranke,etal.Mutageniceffectsofexhaustparticulatemat2terofbiodieselcomparedfossildieselfuelJ.Muta2tionResearch,1998,415(1-2):13-23.2CharlesL.Pete

7、rson,ToddHustrulid.CarbonCycleforRapeseedoilBiodieselFuelsJ.BiomassAndBioener2gy,1998,14(2):91-101.3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.依次为2、4、6、8、10、12、14、16、18、20mg/mL,亚麻酸甲酯、花生一烯酸甲酯和芥酸甲酯的浓度依次为1、2、3、4、5、6、7、8、9、10mg/mL。然后再分别取上述混合标准溶液0175mL于1mL的容量瓶中,加入0125mL浓度为8mg/mL的十三酸甲酯做内标。混合均匀后进行气相

8、色谱分析。得到了各脂肪酸甲酯与内标物的峰面积比Y和浓度比X间的标准工作曲线,结果见表1。212回收率测定取一定量的己知脂肪酸甲酯含量的生物柴油样品于1mL的容量瓶中,加入0125mL浓度为8mg/mL的十三酯甲酯和一定量的棕榈酸甲酯、油酸甲酯、亚油酸甲酯、亚麻酸甲酯、花生一烯酸甲酯和芥酸甲酯标样,进行气相色谱分析,回收率在98%。2131mL的容量瓶中的十三酸甲酯,相对标准偏。4GB/T17377-1998,动植物油脂脂肪酸甲酯的气相色谱分析S.5郭登峰,盛梅,罗士平.气色谱法测定生物柴油中多种脂肪酸甲酯J.中国油脂,2004,29(4):44-46.6方芳,曾虹燕.气相色谱法测定生物柴油中的

9、脂肪酸甲脂J.福建林学院学报,2005,25(1):35-37.7GB/T17376-1998,动植物油脂脂肪酸甲酯制备S.DeterminationoffattyacidmethylestersinbiodieselbygaschromatographyLIUXiang-hua,LIUCan-ming,WUSU-xi,ZENGFan-jia,HUQiu-long1111(1.CollegeofScience,HunanAgriculturalUniversity,Changsha410128,China;2.DepartmentofBiologyandFoodEngineering,Chan

10、gshaUniversityOfScience&Technology,Changsha410076,China)Abstract:TodevelopanaccuratedeterminationmethodoffattyacidmethylestersinbiodieselbyGC,tridecanoicacidmethy1esterwasusedasaninternalstandard.Therecoveriesaredeterminedtobefrom97159%to101142%(m=5)Therelativestandardde2viationsrangefrom1132%to

11、2189%(n=5).Keywords:gaschromatography;biodiesel,fattyacidmethy1ester;rapedeedoil(责任编辑李方)© 1994-2010 China Academic Journal Electronic Publishing House. All rights reserved. CHEMICALRESEARCHANDAPPLICATIONVol.18NO.5May.2006MonthlyReviewsandSummaryAccountsThefactorsfavoringcalciumoxalatedihydratef

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