十通阀双柱切换技术高灵敏检测汽油中甲缩醛和酯类
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摘要
建立了十通阀双柱切换技术的气相色谱法测定汽油中非法添加的甲缩醛和酯类(乙酸仲丁酯、碳酸二甲酯)含量。将待测物导入装有两根柱子及一个电磁阀的色谱系统。组分首先进入极性TCEP预切换柱,将轻烃放空,并保留甲缩醛、酯类化合物和较重烃组分。在甲缩醛流出之前将阀切换至反吹位置,使甲缩醛、酯类化合物进入HP-1非极性毛细管柱分离。甲缩醛、酯类化合物依沸点顺序分离并通过火焰离子化检测器检测,根据各组分色谱峰的保留时间对组分进行定性,采用内标法定量。结果表明,采用HP-1非极性毛细管柱(30m×0.53mm×5μm)分离,在1.0%～5%浓度范围内,加标回收率为96%～101%,重现性试验的相对标准偏差≤1.0%,甲缩醛和酯类化合物的检出限为0.1%。该方法准确、重现性好,可用于日常检验。
The method for the determination of illegal addition of methylformaldehyde and esters in gasoline by means of gas chromatography with double column switching of ten way valves was established.The pending object was imported into a chromatographic system with two columns and an electromagnetic valve.The components first entered the polarity TCEP precut column,released the light hydrocarbon,and retained the acetal,ester and the heavier hydrocarbon components.The valve was switched to the anti-blowing position before the acetal outflow,so that the methyl aldehyde and ester compounds were separated into the wall coated open tubalar column non-polar capillary column.Methylal and ester compounds were separated by boiling point and detected by flame ionization detector.The composition was qualitatively determined according to the retention time of each component.Results showed that in the mass fraction concentration range of 1.0%-0.5%,standard addition recoveries were 96%-101%,the relative standard deviations were not more than 1.0%,the detection limit of methylal and ester compounds were 0.1% mass fraction.The method can be used for daily test.
The method for the determination of illegal addition of methylformaldehyde and esters in gasoline by means of gas chromatography with double column switching of ten way valves was established.The pending object was imported into a chromatographic system with two columns and an electromagnetic valve.The components first entered the polarity TCEP precut column,released the light hydrocarbon,and retained the acetal,ester and the heavier hydrocarbon components.The valve was switched to the anti-blowing position before the acetal outflow,so that the methyl aldehyde and ester compounds were separated into the wall coated open tubalar column non-polar capillary column.Methylal and ester compounds were separated by boiling point and detected by flame ionization detector.The composition was qualitatively determined according to the retention time of each component.Results showed that in the mass fraction concentration range of 1.0%-0.5%,standard addition recoveries were 96%-101%,the relative standard deviations were not more than 1.0%,the detection limit of methylal and ester compounds were 0.1% mass fraction.The method can be used for daily test.
引文
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[4] XING A H,ZHANG M Q,HE Z M,ZHANG J P.Chinese Journal of Analytical Chemistry(邢爱华,张敏卿,何志敏,张建平.分析化学),2005,33(8):1147.
[5] ZHAO Y,XU D Y,LIN H X,etal.Chinese Journal of Chromatography(赵彦,徐董育,林浩学,等.色谱),2014,32(6):662.
[6] WEN H,XU L,LH M,et al.Petrochemical Technology(闻环,徐玲,吕焕明,等.石油化工),2015,44(5):630.
[7] GAO Z R,LI J W,WANG C.Petrochemical Technology(高枝荣,李继文,王川.石油化工),2013,42(2):230.
[8] ZHANG Y,CAI Z B,LIU L.Chinese Journal of Health Laboratory Technolgy(张英,蔡志斌,刘丽.中国卫生检验杂质),2010,20(6):1341.
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[12]LI C X,WANG Y M,JIN K.Petroleum Processing and Petrochemicals(李长秀,王亚敏,金珂.石油炼制与化工),2016,47(8):102.