离子色谱法测定生物柴油中甲酸、乙酸、丙酸含量的研究
|
摘要
研究了离子色谱法测定生物柴油中的甲酸、乙酸、丙酸含量。结果表明:采用离子色谱法检测甲酸、乙酸、丙酸含量时,其相关系数均在0. 999以上,相关性较好;检出限分别为0. 001、0. 002 mg/L和0. 003 mg/L,均小于0. 02 mg/L,满足离子色谱检定规程对电导检测器最小可检测浓度的要求;色谱峰面积的相对标准偏差分别为1. 0%、2. 0%和1. 5%,均小于3%,精密度高;加标回收率为87%～99%,说明油样前处理方法是有效的。地沟油生物柴油和小桐子生物柴油中甲酸含量分别为7. 010、7. 133 mg/kg,乙酸含量分别为8. 955、1. 390 mg/kg,丙酸含量分别为9. 283、0 mg/kg,表明生物柴油中甲酸、乙酸、丙酸含量可受生物柴油种类的影响。采用超声波辅助管式反应器碱催化法和集热式恒温加热磁力搅拌器碱催化法制备的小桐子生物柴油中甲酸含量分别为7. 153、5. 701mg/kg,乙酸含量分别为1. 500、0. 752 mg/kg,丙酸含量分别为0. 158、0 mg/kg,表明生物柴油中甲酸、乙酸、丙酸含量受其制备方法的影响。
The determination of contents of formic acid,acetic acid and propionic acid by ion chromatography was studied. The results showed that the correlation coefficients of formic acid,acetic acid and propionic acid determined by ion chromatography were above 0. 999 and the correlation was good. The detection limits were 0. 001,0. 002 mg/L and 0. 003 mg/L respectively,less than 0. 02 mg/L,meeting the requirements of ion-chromatographic verification rules for the minimum detectable concentration of the conductance detector. The relative standard deviations of chromatographic peak area were 1. 0%,2. 0% and 1. 5% respectively,less than 3%,with high precision. The recovery rate of the standard was87%-99%,indicating that the pre-treatment method of the oil sample was effective. The formic acid contents in swill-cooked dirty oil biodiesel and Jatropha curcas L. biodiesel were 7. 010,7. 133 mg/kg,acetic acid contents were 8. 955,1. 390 mg/kg,and the propionic acid contents were 9. 283,0 mg/kg,respectively. It indicated that the contents of formic acid,acetic acid and propionic acid in biodiesel were affected by the types of biodiesel. The formic acid contents in Jatropha curcas L. biodiesels produced by alkali catalytic method in tube reactor assisted by ultrasound and alkali catalytic method of magnetic stirrer with collector constant temperature heating were 7. 153,5. 701 mg/kg,the acetic acid contents were 1. 500,0. 752 mg/kg,and the propionic acid contents were 0. 158,0 mg/kg,respectively. It indicated that the contents of formic acid,acetic acid and propionic acid in biodiesel were affected by the preparation method.
The determination of contents of formic acid,acetic acid and propionic acid by ion chromatography was studied. The results showed that the correlation coefficients of formic acid,acetic acid and propionic acid determined by ion chromatography were above 0. 999 and the correlation was good. The detection limits were 0. 001,0. 002 mg/L and 0. 003 mg/L respectively,less than 0. 02 mg/L,meeting the requirements of ion-chromatographic verification rules for the minimum detectable concentration of the conductance detector. The relative standard deviations of chromatographic peak area were 1. 0%,2. 0% and 1. 5% respectively,less than 3%,with high precision. The recovery rate of the standard was87%-99%,indicating that the pre-treatment method of the oil sample was effective. The formic acid contents in swill-cooked dirty oil biodiesel and Jatropha curcas L. biodiesel were 7. 010,7. 133 mg/kg,acetic acid contents were 8. 955,1. 390 mg/kg,and the propionic acid contents were 9. 283,0 mg/kg,respectively. It indicated that the contents of formic acid,acetic acid and propionic acid in biodiesel were affected by the types of biodiesel. The formic acid contents in Jatropha curcas L. biodiesels produced by alkali catalytic method in tube reactor assisted by ultrasound and alkali catalytic method of magnetic stirrer with collector constant temperature heating were 7. 153,5. 701 mg/kg,the acetic acid contents were 1. 500,0. 752 mg/kg,and the propionic acid contents were 0. 158,0 mg/kg,respectively. It indicated that the contents of formic acid,acetic acid and propionic acid in biodiesel were affected by the preparation method.
引文
[1]王加云.浅谈我国生物柴油的发展现状[J].工程技术(全文版),2016(10):220-221.
[2]YILMAZ N.Performance and emission characteristics of a diesel engine fuelled with biodiesel-ethanol and biodieselmethanol blends at elevated air temperatures[J].Fuel,2012,94(1):440-443.
[3]SHARMA Y C,SINGH V.Microalgal biodiesel:a possible solution for India’s energy security[J].Renew Sust Energ Rev,2017,67:72-88.
[4]郑依凡.微生物油脂的分离提取工艺研究[D].北京:北京化工大学,2016.
[5]KIMMING M,SUNDBERG C,NORBERG,et al.Replacing fossil energy for organic milk production-potential biomass sources and greenhouse gas emission reductions[J].J Clean Prod,2015,106:400-407.
[6]金鑫.棕榈油生物柴油低温流动性及其改进[D].安徽淮南:安徽理工大学,2015.
[7]MOSER B R.Impact of fatty ester composition on low temperature properties of biodiesel-petroleum diesel blends[J].Fuel,2014,115(1):500-506.
[8]王学春,方建华,陈波水,等.生物柴油中不饱和脂肪酸甲酯对内燃机油摩擦学性能的影响[J].润滑与密封,2015,40(9):78-82.
[9]李法社.小桐子生物柴油的超临界两步法制备及其抗氧化耐低温性的研究[D].昆明:昆明理工大学,2011.
[10]ELBOULIFI N,BOUAID A,MARTINEZ M,et al.Optimization and oxidative stability of biodiesel production from rice bran oil[J].Renewa Energ,2013,53:141-147.
[11]王浩,贾燕红,曹世理.不同生物柴油对柴油机材料的性能影响研究[J].河南科技,2014(10):73.
[12]SILVEIRA E L C,DE CALAND L B,TUBINO M.Simultaneous quantitative analysis of the acetate,formate,chloride,phosphate and sulfate anions in biodiesel by ion chromatography[J].Fuel,2014,124:97-101.
[13]冯宗红.生物柴油中离子含量的试验研究[D].昆明:昆明理工大学,2017.
[14]LI F S,FENG Z H,WANG C Z,et al.Simultaneous quantitative of inorganic anions in commercial waste-oil biodiesel using suppressed ion exchange chromatography[J].Bulg Chem Commun,2016,48:30-35.
[15]FENG Z H,LI F S,HUANG Y D,et al.Simultaneous quantitative analysis of six cations in three biodiesel and their feedstock oils by an ion-exchange chromatography system without chemical suppression[J].Energ Fuel,2017,31(4):3921-3928.
[2]YILMAZ N.Performance and emission characteristics of a diesel engine fuelled with biodiesel-ethanol and biodieselmethanol blends at elevated air temperatures[J].Fuel,2012,94(1):440-443.
[3]SHARMA Y C,SINGH V.Microalgal biodiesel:a possible solution for India’s energy security[J].Renew Sust Energ Rev,2017,67:72-88.
[4]郑依凡.微生物油脂的分离提取工艺研究[D].北京:北京化工大学,2016.
[5]KIMMING M,SUNDBERG C,NORBERG,et al.Replacing fossil energy for organic milk production-potential biomass sources and greenhouse gas emission reductions[J].J Clean Prod,2015,106:400-407.
[6]金鑫.棕榈油生物柴油低温流动性及其改进[D].安徽淮南:安徽理工大学,2015.
[7]MOSER B R.Impact of fatty ester composition on low temperature properties of biodiesel-petroleum diesel blends[J].Fuel,2014,115(1):500-506.
[8]王学春,方建华,陈波水,等.生物柴油中不饱和脂肪酸甲酯对内燃机油摩擦学性能的影响[J].润滑与密封,2015,40(9):78-82.
[9]李法社.小桐子生物柴油的超临界两步法制备及其抗氧化耐低温性的研究[D].昆明:昆明理工大学,2011.
[10]ELBOULIFI N,BOUAID A,MARTINEZ M,et al.Optimization and oxidative stability of biodiesel production from rice bran oil[J].Renewa Energ,2013,53:141-147.
[11]王浩,贾燕红,曹世理.不同生物柴油对柴油机材料的性能影响研究[J].河南科技,2014(10):73.
[12]SILVEIRA E L C,DE CALAND L B,TUBINO M.Simultaneous quantitative analysis of the acetate,formate,chloride,phosphate and sulfate anions in biodiesel by ion chromatography[J].Fuel,2014,124:97-101.
[13]冯宗红.生物柴油中离子含量的试验研究[D].昆明:昆明理工大学,2017.
[14]LI F S,FENG Z H,WANG C Z,et al.Simultaneous quantitative of inorganic anions in commercial waste-oil biodiesel using suppressed ion exchange chromatography[J].Bulg Chem Commun,2016,48:30-35.
[15]FENG Z H,LI F S,HUANG Y D,et al.Simultaneous quantitative analysis of six cations in three biodiesel and their feedstock oils by an ion-exchange chromatography system without chemical suppression[J].Energ Fuel,2017,31(4):3921-3928.