气相色谱法测定合成气厌氧发酵液中挥发性脂肪酸
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摘要
建立了PEG-20M固定液毛细管柱气相色谱法直接测定合成气厌氧发酵液中挥发性脂肪酸(VFAs,乙醇、乙酸、丙酸、丁酸、戊酸、己酸和辛酸)的方法;在对样品预酸化处理(pH=3)后,对比程序升温和恒温两种色谱条件对VFAs的分离时间,并确定了恒温条件下方法的线性范围、检出限、精密度及回收率;结果表明:在恒温条件下,分离C6以内(乙醇、乙酸、丙酸、丁酸、戊酸和己酸) VFAs的总时长在5 min左右,仅辛酸出峰时间在9. 8 min;全部7种化合物所在线性范围内,相关系数r均大于0. 993 7,线性良好;检出限在0. 4～1. 1 mg/L之间;实际样品不同质量浓度的加标回收,其回收率在94. 5%～109. 3%之间,相对标准偏差小于10. 4%。
The Gas Chromatography has been applied to the direct determination of volatile fattyacids( VFAs,ethanol,acetic acid,propionic acid,butyric acid,pentanoic acid,caproic acid and octanoic acid) in the anaerobic fermentation liquid of synthesis gas. Two gas chromatographic conditions of order temperature hoist and constant temperature were investigated,followed by acidification of the sample( p H = 3) and GC analysis,with PEG-20 M stationary liquid capillary column and flame ionization detector( FID). The optimum conditions( constant temperature) including the detection limits,precisions and recoveries have been analyzed. The results show that under constant temperature,the total time for separating VFAs including ethanol,acetic acid,propionic acid,butyric acid,pentanoic acid and caproic acid is about 5 minutes but the time for separating octanoic acid is 9. 8 minutes.The linear range of VFAs were good linearity with the correlation coefficients r≥0. 993 7,the detection limits were in range of 0. 4—1. 1 mg/L. The recoveries of the actual sample with different concentrations were between 94. 5—109. 3% and the relative standard deviations were less than 10. 4%.
The Gas Chromatography has been applied to the direct determination of volatile fattyacids( VFAs,ethanol,acetic acid,propionic acid,butyric acid,pentanoic acid,caproic acid and octanoic acid) in the anaerobic fermentation liquid of synthesis gas. Two gas chromatographic conditions of order temperature hoist and constant temperature were investigated,followed by acidification of the sample( p H = 3) and GC analysis,with PEG-20 M stationary liquid capillary column and flame ionization detector( FID). The optimum conditions( constant temperature) including the detection limits,precisions and recoveries have been analyzed. The results show that under constant temperature,the total time for separating VFAs including ethanol,acetic acid,propionic acid,butyric acid,pentanoic acid and caproic acid is about 5 minutes but the time for separating octanoic acid is 9. 8 minutes.The linear range of VFAs were good linearity with the correlation coefficients r≥0. 993 7,the detection limits were in range of 0. 4—1. 1 mg/L. The recoveries of the actual sample with different concentrations were between 94. 5—109. 3% and the relative standard deviations were less than 10. 4%.
引文
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[11]冯琳.顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸[J].理化检验(化学分册),2011,47(1):86-89FENG L.GC Determination of Volatile Fatty Acids in Waste Water with HS-SPME[J].Physical Testing and Chemical Analysis(Chemical Analysis),2011,47(1):86-89(in Chinses)
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[14]赵兴涛,徐桂转,刘杰博,等.气相色谱法测定厌氧发酵液中挥发性脂肪酸的研究[J].河南农业大学学报,2013,47(5):584-591ZHAO X T,XU G Z,LIU J B,et al.Study on VFAs Content in the Anaerobic Fermentation Liquid by Gas Chromatography[J].Journal of Henan Agricultural University,2013,47(5):584-591(in Chinses)
[15]朱灵峰,张楠,苏彩丽,等.气相色谱法测定厌氧发酵产氢过程中产生的挥发性脂肪酸[J].江苏农业科学,2012,40(6):296-297ZHU L F,ZHANG N,SU C L,et al.Determination of Volatile Fatty Acids in Anaerobic Fermentation of Hydrogen by Gas Chromatography[J].Jiangsu Agricultural Sciences,2012,40(6):296-297(in Chinses)
[2]STMAS A H.Microbiology of Synthesis Gas Fermentation for Biofuel Production[J].Curr Opin Biotechno,2017,18(3):200-206
[3]ABUBACKAR H N,VEIGA M C,KENNES C.Biological Conversion of Carbon Monoxide:Rich Syngas or Waste Gases to Bioethanol[J].Biofuels,Bioproducts and Biorefining,2011,5(1):93-114
[4]MSSONL B,MURTO M,JANTSCH T G,et al.Evaluation of New Methods for the Monitoring of Alkalinity Dissolved Hydrogen and the Microbial Community in Anaerobic Digestion[J].Water Research,2001,35(12):2833-2840
[5]顾福权,徐红娟,柳展飞,等.气相色谱法测定废水中6种挥发性脂肪酸含量[J].能源环境保护,2014,28(3):62-64GU F Q,XU H J,LIU Z F,et al.Content of 6 Volatile Fatty Acidsof Waste Water by Gas Chromatography[J].Energy Environmental Protection,2014,28(3):62-64(in Chinses)
[6]刘只欣.气相色谱法测定污水厌氧消化过程产生的挥发性脂肪酸[J].中国给水排水,2014,30(24):144-146LIU Z X.Determination of Volatile Fatty Acids Produced in Anaerobic Digestion Process of Wastewater by Gas Chromatography[J].China Water&Wastewater,2014,30(24):144-146(in Chinses)
[7]ULAH M A,KIM K,SZULEJKO J E,et al.The Gas Chromatographic Determination of Volatile Fatty Acids in Wastewater Samples:Evaluation of Experimental Biases in Direct Injection Method against Thermal Desorption Method[J].Analytica Chimica Acta,2014,820(11):159-167
[8]刘艳玲,任南琪,刘敏,等.气相色谱法分析厌氧反应器中的挥发性脂肪酸(VFA)[J].哈尔滨建筑大学学报.2000,33(6):31-34LIU Y L,REN N Q,LIU M,et al.Analysis of Volatile Fatty Acid(VFA)in Anaerobic Bio-reactor by Gas Chromatography[J].Journal of Harbin University of Civil Engineering and Architecture,2000,33(6):31-34(in Chinses)
[9]GHIDOTTI M,FABBRI D,TORRI C,et al.Determination of Volatile Fatty Acids in Digestate by Solvent Extraction with Dimethyl Carbonate and Gas Chromatography-Mass Spectrometry[J].Analytica Chimica Acta,2018,1034(30):92-101
[10]FENG L,HUANG Y M,WANG H.Solid-Phase Microextraction in Combination with GC-FID for Quantification of the Volatile Free Fatty Acids in Wastewater from Constructed Wetlands[J].J Chromatogr Sci,2008,46(7):577-584
[11]冯琳.顶空固相微萃取-气相色谱法测定废水中挥发性脂肪酸[J].理化检验(化学分册),2011,47(1):86-89FENG L.GC Determination of Volatile Fatty Acids in Waste Water with HS-SPME[J].Physical Testing and Chemical Analysis(Chemical Analysis),2011,47(1):86-89(in Chinses)
[12]VAN L J.DEWULF G W H.Determination of Acetic Acid in Aqueous Samples by Water-Phase Derivatisation Solid-Phase Microextraction and Gas Chromatography[J].Journal of Chromatography A,2000,874(2):225-234
[13]JURADO S,BALLESTEROS E,GALLEGO M.Determination of Carboxylic Acids in Water by Gas Chromatography-Mass Spectrometry after Continuous Extraction and Derivatisation[J].Talanta,2012,93(15):224-232
[14]赵兴涛,徐桂转,刘杰博,等.气相色谱法测定厌氧发酵液中挥发性脂肪酸的研究[J].河南农业大学学报,2013,47(5):584-591ZHAO X T,XU G Z,LIU J B,et al.Study on VFAs Content in the Anaerobic Fermentation Liquid by Gas Chromatography[J].Journal of Henan Agricultural University,2013,47(5):584-591(in Chinses)
[15]朱灵峰,张楠,苏彩丽,等.气相色谱法测定厌氧发酵产氢过程中产生的挥发性脂肪酸[J].江苏农业科学,2012,40(6):296-297ZHU L F,ZHANG N,SU C L,et al.Determination of Volatile Fatty Acids in Anaerobic Fermentation of Hydrogen by Gas Chromatography[J].Jiangsu Agricultural Sciences,2012,40(6):296-297(in Chinses)
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