液液萃取-气相色谱-氧选择性检测法测定柴油中的酚类化合物  

DETEEMINATION OF PHENOLIC COMPOUNDS IN DIESELS USING LIQUID-LIQUID EXTRACTION AND GC-OXYGEN SELECTIVE DETECTOR

作　　者：李长秀[1] 钱钦[1] 金珂[1] 吴梅[1] 孔翠萍[1] Li Changxiu;Qian Qin;Jin Ke;Wu Mei;Kong Cuiping(SINOPEC Research Institute of Petroleum Processing,Beijing 100083)

机构地区：[1]中国石化石油化工科学研究院,北京100083

出　　处：《石油炼制与化工》2018年第1期83-87,共5页Petroleum Processing and Petrochemicals

摘　　要：建立了液液萃取结合气相色谱-氧选择性检测器(GC-OFID)测定柴油样品中微量酚类化合物的方法。待测试样经10%的氢氧化钠溶液萃取,水相经稀盐酸调至pH为5~6后,用二氯甲烷反萃取其中的酚类化合物,挥发溶剂后得到浓缩的酚类富集物,然后进行GC-MS和GC-OFID检测。通过与GC-MS检测结果对比,结合各酚类组分的沸点和色谱峰保留规律,确定了GC-OFID上54个(组)色谱峰对应酚类化合物的结构或类型。在酚类富集物中加入已知量的苯甲醇作内标物,采用内标法进行定量。在样品量为50mL时,测定苯酚、2,5-二甲基苯酚、2,3,5-三甲基苯酚的检测限分别为0.5,1.0,1.5mg/L,在质量浓度8~40mg/L范围内连续5次重复性测定结果的相对标准偏差均小于8.0%,可以用于柴油中酚类化合物的测定。A method for determination of phenolic compounds in diesels was established by using liquid li quid extraction combined with gas chromatograph equipped with oxygen selective flame ionization detector(GC-OFID)Diesel samples were first extracted with10%sodium hydroxide.The extracted water phase was neutralized to pH5-6with dilute hydrochloric acid and then re extracted with dichloromethane.The phenolic compounds containing dichloromethane were evaporated to get concentrated phenolic compounds and were then detected by GC MS and GO OFID The structures or types of54peaks or groups of phenolic compounds were identified by GC MS,chromatography retention time and boiling points.Benzyl alcohol was added into the concentrated samples as internal standard for quantification test.When50mL diesel sample is treated,the detection limits of phenol,2,5dimethyl phenol and2,3,5trimethyl phenol are05,10,15mg/L respectively.The relative standard deviations of five consecutive results are less than80%in the phenolic compound concentration range of8-40mgL,which meet the requirement of routine analysis.

关 键 词：酚类化合物 柴油 氧选择性检测器 气相色谱 

分 类 号：O657.71[理学—分析化学] TE626.24[理学—化学]