氣相色譜法測定車用汽油中含氧化合物和苯胺類化合物
發(fā)布時間:2018-03-05 11:09
本文選題:氣相色譜 切入點:中心切割 出處:《色譜》2017年05期 論文類型:期刊論文
【摘要】:利用中心切割技術和雙毛細管色譜柱系統(tǒng),采用兩次進樣的方式,建立了氣相色譜測定車用汽油中含氧化合物和苯胺類化合物的分析方法。第一次進樣分析,組分首先進入非極性DB-1色譜柱(30 m×0.32 mm×1.0μm),按沸點由低到高的順序分離,通過電磁閥切換將沸點小于2-己酮的組分切割至強極性GS-OxyPLOT色譜柱(10 m×0.53 mm×10μm)或CP-Lowox色譜柱(10 m×0.53 mm×10μm),其余重烴組分通過阻尼柱進入FID檢測器。在GS-OxyPLOT或CP-Lowox色譜柱上,烴類組分與含氧化合物分離并進入檢測器檢測,消除了大量的烴類組分對含氧化合物測定的影響。第二次進樣分析,設定電磁閥切換時間為間-甲基苯胺從非極性色譜柱流出的時間,苯胺類化合物在GS-OxyPLOT或CP-Lowox色譜柱上與烴類和含氧化合物分離并進入檢測器檢測。以乙二醇二甲基醚為內標化合物進行內標法定量。實現(xiàn)了在一套系統(tǒng)上同時測定車用汽油中添加的甲基叔丁基醚(MTBE)、甲醇、甲縮醛、乙酸仲丁酯、乙酸乙酯、苯胺、鄰/間/對-甲基苯胺和N-甲基苯胺的含量,各組分的檢測范圍為0.01%~10%(質量分數(shù)),回收率為86.0%~102.6%。該法可以為車用汽油的質量控制提供有效的檢測手段。
[Abstract]:A method for the determination of oxygenated compounds and aniline compounds in gasoline by gas chromatography was established by means of central cutting technique and double capillary column system. The components first entered the nonpolar DB-1 column (30 m 脳 0.32 mm 脳 1.0 渭 m) and separated in the order of boiling point from low to high. The components with boiling point less than 2-hexanone were cut to a strong polar GS-OxyPLOT column (10 m 脳 0.53 mm 脳 10 渭 m) or CP-Lowox column (10 m 脳 0.53 mm 脳 10 渭 m) by solenoid valve. The rest of the heavy hydrocarbon components entered the FID detector by damping column. The separation of hydrocarbon components from oxygenated compounds and their entry into the detector eliminates the influence of a large number of hydrocarbon components on the determination of oxygenated compounds. Setting the switching time of the solenoid valve for the outflow of m-methylaniline from the non-polar column, Aniline compounds were separated from hydrocarbons and oxygenated compounds on GS-OxyPLOT or CP-Lowox column and detected by detector. The internal standard quantity was determined by using ethylene glycol dimethyl ether as internal standard compound. Methyl tert-#china_person0# ether (MTBEBEN) and methanol were added to gasoline. Contents of methylal, secondary butyl acetate, ethyl acetate, aniline, o-m-p-methylaniline and N-methylaniline, The detection range of each component is 0. 01% and 10%. The recovery rate is 86. 0% and 10. 6%. This method can provide an effective method for the quality control of automobile gasoline.
【作者單位】: 中國石油化工股份有限公司石油化工科學研究院;
【基金】:國家標準化管理委員會標準化項目(20131688-T-469)~~
【分類號】:O657.71;TE626.21
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