氣相色譜法測(cè)定生物柴油中脂肪酸甲酯含量

1、第5期劉祥華等:氣相色譜法測(cè)定生物柴油中脂肪酸甲酯含量591文章編號(hào):1004-1656(2006)05-0591-02氣相色譜法測(cè)定生物柴油中脂肪酸甲酯含量劉祥華,劉燦明13,吳蘇喜,曾凡佳,胡秋龍211(1.湖南農(nóng)業(yè)大學(xué)理學(xué)院應(yīng)用化學(xué)系,湖南長(zhǎng)沙410128;2.長(zhǎng)沙理工大學(xué)生物與食品工程系,湖南長(zhǎng)沙410076)關(guān)鍵詞:氣相色譜法;生物柴油;脂肪酸甲脂;菜籽油中圖分類號(hào):065717文獻(xiàn)標(biāo)識(shí)碼:A生物柴油是利用動(dòng)植物油脂等可再生資源通過酯交換技術(shù)制造的可以替代石化柴油的新型清1-3潔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產(chǎn)的生物柴油的脂肪酸甲脂組成不同因而測(cè)定時(shí)所需的氣相

2、色譜條件與方法4-6也不盡相同。本文采用HP-innowax色譜柱,以十三酸甲酯為內(nèi)標(biāo)物,籽生物柴油中主要脂肪酸甲酯(甲酯、亞油酸甲酯、和芥酸甲酯),、準(zhǔn)確度高、,。的升溫速率升至240°C5min;載氣:N2,柱頭壓60kPa;氫氣:in;空氣:320mL/L,混合脂肪酸min;:11。2、3、4、5、6和7分別為十、油酸甲酯、亞油酸甲酯、亞、花生一烯酸甲酯和芥酸甲酯。1實(shí)驗(yàn)部分111材料油菜籽生物柴油(按照動(dòng)植物油脂脂肪酸甲7酯制備方法自制)112儀器與試劑SP-6890型氣相色譜儀;FID檢測(cè)器;N3000色譜工作站;AL204電子天平;HP-innowax毛細(xì)m)。管色譜柱(

3、30m×0125mm×0125十三酸甲酯、棕櫚酸甲酯、油酸甲酯、亞麻酸甲酯、花生一烯酸甲酯和芥酸甲酯(均為色譜純,Sigma公司),其它試劑為分析純。113生物柴油的預(yù)處理及其脂肪酸甲酯含量的計(jì)算取一定量的生物柴油樣品于1mL的容量瓶中,加入0125mL濃度為8mg/mL的十三酸甲酯,用正己烷定容后,進(jìn)行氣色譜分析。將從標(biāo)準(zhǔn)工作曲線上查得的濃度乘以生物柴油樣品的稀釋倍數(shù),從而得到生物柴油樣品中的脂肪酸甲酯含量。114色譜分析條件汽化室溫度280°C;檢測(cè)溫度280°C;柱溫采用程度升溫:初始溫度170°C,保持015min,以5°C/

4、min的升溫速率升到200°C,然后以15°C/min收稿日期:2005-11-23;修回日期:2006-02-10基金項(xiàng)目:湖南省科技計(jì)劃項(xiàng)目(05SK3085)圖1標(biāo)準(zhǔn)溶液的氣相色譜圖Fig.1Gaschromatogramofstandardsolutions圖2生物柴油的氣相色譜圖Fig.2Gaschromatogramofbiodieselsample聯(lián)系人簡(jiǎn)介:劉燦明(1955-),男,教授,主要從事天然產(chǎn)物和應(yīng)用化學(xué)研究。Email:liucanming© 1994-2010 China Academic Journal Electronic Pub

5、lishing House. All rights reserved. 592化學(xué)研究與應(yīng)用第18卷2結(jié)果與討論211線性關(guān)系的測(cè)定表1線性關(guān)系實(shí)驗(yàn)結(jié)果Table1Experimentalresultsonlinerarity標(biāo)準(zhǔn)樣品濃度范圍(mg/mL)線性回歸方程Y=019053X-011549Y=110073X-012586Y=01843X-011178Y=015659X-010361Y=018139X-010923Y=01812X-010717相關(guān)系數(shù)r019987019963019975019979019986019989棕櫚酸甲酯11515油酸甲酯11515亞油酸甲酯11515亞麻

6、酸甲酯0175715花生一烯酸甲酯0175715芥酸甲酯0175715稱一定量的棕櫚酸甲酯、油酸甲酯、亞油酸甲酯、亞麻酸甲酯、花生一烯酸甲酯和芥酸甲酯標(biāo)準(zhǔn)樣品,以正己烷為溶劑,配制成混合脂肪酸甲酯標(biāo)準(zhǔn)貯備液。然后再稀釋為10個(gè)不同濃度的混合脂肪酸甲酯標(biāo)準(zhǔn)溶液液中,棕櫚酸甲酯、參考文獻(xiàn):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,張冠杰.國(guó)內(nèi)外生物柴油研究生產(chǎn)現(xiàn)狀及發(fā)展趨勢(shì)J.化工時(shí)刊,2004,18(1):23-27.依次為2、4、6、8、10、12、14、16、18、20mg/mL,亞麻酸甲酯、花生一烯酸甲酯和芥酸甲酯的濃度依次為1、2、3、4、5、6、7、8、9、10mg/mL。然后再分別取上述混合標(biāo)準(zhǔn)溶液0175mL于1mL的容量瓶中,加入0125mL濃度為8mg/mL的十三酸甲酯做內(nèi)標(biāo)?；旌暇鶆蚝筮M(jìn)行氣相

8、色譜分析。得到了各脂肪酸甲酯與內(nèi)標(biāo)物的峰面積比Y和濃度比X間的標(biāo)準(zhǔn)工作曲線,結(jié)果見表1。212回收率測(cè)定取一定量的己知脂肪酸甲酯含量的生物柴油樣品于1mL的容量瓶中,加入0125mL濃度為8mg/mL的十三酯甲酯和一定量的棕櫚酸甲酯、油酸甲酯、亞油酸甲酯、亞麻酸甲酯、花生一烯酸甲酯和芥酸甲酯標(biāo)樣,進(jìn)行氣相色譜分析,回收率在98%。2131mL的容量瓶中的十三酸甲酯,相對(duì)標(biāo)準(zhǔn)偏。4GB/T17377-1998,動(dòng)植物油脂脂肪酸甲酯的氣相色譜分析S.5郭登峰,盛梅,羅士平.氣色譜法測(cè)定生物柴油中多種脂肪酸甲酯J.中國(guó)油脂,2004,29(4):44-46.6方芳,曾虹燕.氣相色譜法測(cè)定生物柴油中的

9、脂肪酸甲脂J.福建林學(xué)院學(xué)報(bào),2005,25(1):35-37.7GB/T17376-1998,動(dòng)植物油脂脂肪酸甲酯制備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(責(zé)任編輯李方)© 1994-2010 China Academic Journal Electronic Publishing House. All rights reserved. CHEMICALRESEARCHANDAPPLICATIONVol.18NO.5May.2006MonthlyReviewsandSummaryAccountsThefactorsfavoringcalciumoxalatedihydratef

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