气相色谱-氧选择性火焰离子检测器在煤焦油酚类化合物分析研究中的应用
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摘要
利用气相色谱-氧选择性火焰离子检测器(GC-OFID)建立了煤焦油中酚类物质的测定方法,该方法可以鉴定出低级酚单体(苯酚、甲基苯酚、C_2苯酚)的含量和高级酚总含量。所建方法的重复性较好,相对标准偏差RSD小于5%,加标回收率在97%～104%之间、线性相关系数R~2>0.99;单个物质的氧质量分数检测下限为10μg/g,符合色谱分析的一般要求。中低温煤焦油中的酚类物质基本存在于小于300℃的馏分油中,低级酚含量较高,并且以苯酚、甲基苯酚、乙基苯酚和2,5-二甲基苯酚为主,高级酚物质种类多但含量较低。
A method for the determination of phenols in coal tar was established by gas chromatography-oxygen selective flame ionization detector(GC-OFID).The method has good repeatability and can identify the content of lower phenol monomers(phenol,methylphenol,C_2 phenol)and the total content of higher phenols.The RSD was less than 5%,the standard recovery was between 97% and 104%,and the linear correlation coefficient R~2 was 0.99.The lower limit of oxygen mass fraction of a single substance was 10 μg/g,which met the general requirements of chromatographic analysis.Phenolic substances exist in the coal tar distillate less than 300 ℃.Low phenol content was higher,in which phenol,methyl phenol,phenol and 2,5-dimethyl ethyl phenol was principal,while senior phenolic substances had more variety but lower content.
A method for the determination of phenols in coal tar was established by gas chromatography-oxygen selective flame ionization detector(GC-OFID).The method has good repeatability and can identify the content of lower phenol monomers(phenol,methylphenol,C_2 phenol)and the total content of higher phenols.The RSD was less than 5%,the standard recovery was between 97% and 104%,and the linear correlation coefficient R~2 was 0.99.The lower limit of oxygen mass fraction of a single substance was 10 μg/g,which met the general requirements of chromatographic analysis.Phenolic substances exist in the coal tar distillate less than 300 ℃.Low phenol content was higher,in which phenol,methyl phenol,phenol and 2,5-dimethyl ethyl phenol was principal,while senior phenolic substances had more variety but lower content.
引文
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[2] 任洪凯,邓文安,李传,等.中/低温煤焦油酚类化合物的组成研究 [J].煤炭转化,2013,36(2):67-70
[3] 耿层层,李术元,岳长淘,等.神木低温煤焦油中含氧化合物的分析与鉴定 [J].石油学报(石油加工),2013,29(1):130-136
[4] 文峰.焦油萃取提酚新工艺的开发[J].上海化工,2017,42(3):20-23
[5] 李宇,乔海燕,石薇薇,等.煤焦油萃取分离及产品性质[J].石油炼制与化工,2017,48(3):58-62
[6] 邵润梅.测定轻煤焦油中酚的含量[J].当代化工,2012,41(3):315-316
[7] 史军歌,吴梅,田松柏,等.电位滴定法测定煤焦油中的有机弱酸含量[J].石油炼制与化工,2015,46(8):96-100
[8] 张生娟,高亚男,李晓宏,等.煤焦油组分分离与分析技术研究进展[J].煤化工,2017,45(1):45-49
[9] 高平强,乔再立,张岩,等.超声萃取中低温煤焦油轻质油中酚类化合物研究[J].洁净煤技术,2016,22(2):54-58,63