煤焦油沥青中致癌多环芳烃含量气相色谱法测定研究  

Study of contents determination of polycyclic aromatic hydrocarbons in coal tar pitch with gas chromatography

作　　者：张秋民[1] 黄杨柳[1] 关珺[1] 何德民[1] 赵树昌[1] 

机构地区：[1]大连理工大学化工学院,辽宁大连116012

出　　处：《大连理工大学学报》2010年第4期481-485,共5页Journal of Dalian University of Technology

基　　金：国家自然科学基金资助项目(90610004)

摘　　要：介绍了煤焦油沥青中致癌多环芳烃(PAHs)的测定方法及分布.对典型煤焦油和煤焦油沥青中的14种PAHs的含量进行了研究.实验采用煤焦油沥青溶剂萃取—萃取物柱色层层析—层析液芳烃分气相色谱分析三步骤.用萘、菲、屈、二苯并[a,h]蒽做内标物体系测定了14种PAHs标准物的保留指数用于定性鉴别;用三苯甲烷、9,10-二苯蒽做内标物体系测定了其相对校正因子并用内标法测定了原料中14种PAHs的含量.用标准物混合物试验,结果表明:SE-54毛细管柱能够很好地分离绝大部分PAHs标准物,只有对苯并[k]荧蒽和苯并[b]荧蒽两种沸点很接近的异构体分离效果稍差.鉴别和测定准确可靠:对芴、菲等沸点较低的PAHs含量测定,其标准偏差范围为0.02～0.08;对茚并[1,2,3-cd]芘等高沸点PAHs的测定,其标准偏差范围为0.11～0.29.根据煤沥青PAHs组成及各个PAH相对苯并[a]芘致癌性的当量系数计算了煤沥青的苯并[a]芘当量含量.The content of cancerogenic polycyclic aromatic hydrocarbons （PAHs） in coal tar pitch and coal tar is researched by introducing the determination method and distribution of PAHs in coal tar pitch. There are three steps：extracting coal tar employing solvent — separating extract phase by column chromatography — analyzing aromatics of extract phase by gas chromatography. Using naphthalene,phenanthrene,chrysene,dibenzo[a,h] anthracene as internal standards,the retention indices of 14 PAHs＇ standards were determined for quality determination. And using triphenylmethane,9,10-diphenylanthrancene as internal standards,their relative adjustment factors were determined. Then,the contents of 14 PAHs in raw were determined by the internal standard method. The results indicate that SE-54 capillary column can separate most of PAHs very well,except benzo[k] fluoranthene and benzo[b] fluoranthene which have the close boiling points. The identification and determination of PAHs in raw are accurate and reliable：for the determination of lower boiling point PAHs such as phenanthrene,fluoranthene and so on,its standard deviation is 0.02-0.08; and for high boiling point PAHs such as indeno [1,2,3-cd] pyrene,its standard deviation is 0.11-0.29. While,BaP cancerogenic equivalency contents of coal tar pitch were calculated according to contents of PAHs and BaP cancerogenic equivalency factors.

关 键 词：多环芳烃 煤焦油沥青 气相色谱法 

分 类 号：TQ53[化学工程—煤化学工程]