色谱2017,Vol.35Issue(11):1204-1209,6.DOI:10.3724/SP.J.1123.2017.07022
固相萃取-气相色谱法测定甲醇制烯烃副产汽油及甲醇制汽油产物中的含氧化合物
Determination of oxygenates in methanol-to-olefin gasoline byproducts and methanol-to-gasoline product with solid phase extraction-gas chromatography
田文卿 1李继文 1王川1
作者信息
- 1. 上海石油化工研究院,绿色化工与工业催化国家重点实验室,上海201208
- 折叠
摘要
Abstract
Silica solid phase extraction ( SPE ) column was used for sample pretreatment to enrich the target analytes and simplify background. Due to its high efficiency, reliability and simplicity, the technique has been widely used in many fields. The byproduct gasoline of methanol-to-olefin (MTO) and the product of methanol-to-gasoline (MTG) mainly consist of hydrocarbons along with small amounts of oxygenates. Trace amounts of oxygenates are hard to identify because of their complex hydrocarbon components. With the SPE technique, the sam-ples were separated into two major classes, oxygenates and hydrocarbons. Oxygenates were then determined with gas chromatography-mass spectrometry ( GC-MS) . The elution conditions of the silica solid phase extraction column were optimized with the standard sample. Under the optimized elution conditions, the hydrocarbons were first eluted from the SPE column with 5 mL dichloromethane, the oxygenates were then eluted with 3 mL acetonitrile. The recoveries of standard samples were tested before and after pretreatment. The standard recoveries were 87. 7%-95. 3%. The oxygenates except methanol and ethanol were then quantified by gas chromatography-flame ionization detection ( GC-FID) and internal standard method. Methanol and ethanol were then quantified by extracting characteristic ion chromatograms and external standard method. The results show that the oxygenates of MTO byproduct gasoline and MTG product mainly consist of ketones and aldehydes. The method improves the sensitivities of the target compounds and reduces the interference of the background.关键词
固相萃取/气相色谱/质谱/火焰离子化检测/含氧化合物/甲醇制烯烃副产汽油/甲醇制汽油产物/硅胶小柱Key words
solid phase extraction ( SPE )/gas chromatography ( GC )/mass spectrometry ( MS)/flame ionization detection ( FID)/oxygenates/methanol-to-olefin byproduct/methanol-to-gasoline product/silica cartridge分类
化学化工引用本文复制引用
田文卿,李继文,王川..固相萃取-气相色谱法测定甲醇制烯烃副产汽油及甲醇制汽油产物中的含氧化合物[J].色谱,2017,35(11):1204-1209,6.