煤基合成轻质汽油中三种金属抗爆剂和两种苯胺类化合物的测定
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摘要
建立了一种采用气质联用法分析煤基合成轻质汽油中三种金属抗爆剂(二茂铁、甲基环戊二烯三羰基锰(MMT)、环戊二烯三羰基锰(CMT)和两种苯胺类化合物(包括苯胺、N,N-二甲基苯胺)的方法。采用强极性INNOWax毛细管色谱柱较好的实现了轻烃和芳烃(C3-C12)组分与三种金属抗爆剂和两种苯胺类化合物的准确分离。采用外标法定量,三种金属抗爆剂在1～50mg·L~(-1)范围内线性关系良好,两种苯胺类化合物在5. 00～250mg·L~(-1)范围内线性关系良好,线性相关系数均达到0. 999,标准样品6次重复性测定的相对标准偏差(RSD)均小于1. 0%,回收率在99. 4%～106. 2%之间,三种金属抗爆剂和两种苯胺类化合物方法测定下限(S/N=3)为0. 016mg·L~(-1)。该方法不需要进行样品前处理,具有操作简单,准确高效的特点,是煤基合成轻质汽油中金属抗爆剂和苯胺类化合物测定的理想分析方法。
A simple and efficient method based on the technique of GC-MS was established for the analysis of the three metal antiknocking agents( including cyclopentadiene manganese tricarbonyl,methylcyclopentadienyl manganesetricarbonyl,ferrocene) and the two phenylamine compouds( includingphenylamine,N,N-DiMethylaniline) in a lightweight oil made from coal.With the use of a INNOWax,we successfully separated the components in a lightweight oil made from coal.In this method,externa standard method was applied for quantification.As a result,good linear relation-ships existed among the three metal anti-knocking agents in the range of1mg·L~(-1)to 50mg·L~(-1)and among the two phenylamine compouds in the range of 5mg·L~(-1)to 250mg·L~(-1),all of the Line-ar correlation coefficient were 0. 999. The relative standard dviations( RSDs) of standard samples in six continuous tests were within1. 0%.The recoveries were between 99. 4%and 106. 2%. The minimum quantitative detection limit( S/N = 3) was 0. 016mg·L~(-1).No pretreatment accurate,quick as well as efficient,and can be used as an ideal method for the analysis of the three metal anti-knocking agents and the two phenylamine compouds in a lightweight oil made from coal.
A simple and efficient method based on the technique of GC-MS was established for the analysis of the three metal antiknocking agents( including cyclopentadiene manganese tricarbonyl,methylcyclopentadienyl manganesetricarbonyl,ferrocene) and the two phenylamine compouds( includingphenylamine,N,N-DiMethylaniline) in a lightweight oil made from coal.With the use of a INNOWax,we successfully separated the components in a lightweight oil made from coal.In this method,externa standard method was applied for quantification.As a result,good linear relation-ships existed among the three metal anti-knocking agents in the range of1mg·L~(-1)to 50mg·L~(-1)and among the two phenylamine compouds in the range of 5mg·L~(-1)to 250mg·L~(-1),all of the Line-ar correlation coefficient were 0. 999. The relative standard dviations( RSDs) of standard samples in six continuous tests were within1. 0%.The recoveries were between 99. 4%and 106. 2%. The minimum quantitative detection limit( S/N = 3) was 0. 016mg·L~(-1).No pretreatment accurate,quick as well as efficient,and can be used as an ideal method for the analysis of the three metal anti-knocking agents and the two phenylamine compouds in a lightweight oil made from coal.
引文
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[9]中国石油化工股份有限公司石油化工科学研究院.SH/T 0711—2002汽油锰含量测定法(原子吸收光谱法)[S].北京:中国石化出版社,2002.
[10]林玉,李怪,何承耀.电感耦合等离子体原子发射光谱法测定汽油中的铁、锰、铅[J].理化检验:化学分册,2009,45(1):1380-1382.
[11]邓全道,许光,林冠春,等.微波消解-电感耦合等离子体发射光谱法同时测定汽油中的锰、铜、铁、铅、磷[J].科技通报,2012,28(3):119-121.
[12]程正军,张运陶,杨志松.模拟汽油中铁锰二组分同时测定实验条件探索[J].西华师范大学学报:自然科学版,2005,26(4):410-413.
[13]王谦,王群威,张建波,等.汽油中微量元素的X射线荧光光谱分析[J].石油学报:石油加工,2008,24(3):360-364.
[14]石丹云.关于车用汽油中甲基苯胺质量检测方法的探讨[J].理化检验:化学分册,2016,(5):20-21.
[15]张月琴.汽油中氮化物的定性定量方法研究与应用[J].石油炼制与化工,2016,47(4):91-95.
[16]HJ168-2010《环境监测分析方法标准制修订技术导则》[S].
[2]Gulson B,Mizon K,Taylor A,et al.Changes in manganese and lead in the environment and young children associated with the introduction of methylcyclopentadienyl manganese tricarbonyl in gasoline-preliminary results[J]. Environ,2006,100(1):100-114.
[3]王充,徐雷,郑琳.汽油抗爆剂甲基环戊二烯三羰基锰对广州大气污染的评价[J].现代预防医学,200734(7):1300-1302.
[4]江国华,高孝洪,吕林,等.汽油中金属成分对发动机性能和排放的影响分析[J].内机,2006,(1):46-49
[5]段鸿杰,马彪,郝亚,等.含锰抗爆剂对发动机的影响及其缓解措施[J].车辆与动力技术,2009,(1):34-39.
[6]全国石油产品和润滑剂标准化技术委员会. GB17930—2011车用汽油[S].北京:中国标准出版社,2011.
[7]中国石油化工股份有限公司石油化工科学研究院.GB/T 8020—1987汽油铅含量测定法(原子吸收光谱法)[S].北京:中国标准出版社,1987.
[8]中国石油化工股份有限公司石油化工科学研究院.SH/T 0712—2002汽油铁含量测定法(原子吸收光谱法)[S].北京:中国石化出版社,2002.
[9]中国石油化工股份有限公司石油化工科学研究院.SH/T 0711—2002汽油锰含量测定法(原子吸收光谱法)[S].北京:中国石化出版社,2002.
[10]林玉,李怪,何承耀.电感耦合等离子体原子发射光谱法测定汽油中的铁、锰、铅[J].理化检验:化学分册,2009,45(1):1380-1382.
[11]邓全道,许光,林冠春,等.微波消解-电感耦合等离子体发射光谱法同时测定汽油中的锰、铜、铁、铅、磷[J].科技通报,2012,28(3):119-121.
[12]程正军,张运陶,杨志松.模拟汽油中铁锰二组分同时测定实验条件探索[J].西华师范大学学报:自然科学版,2005,26(4):410-413.
[13]王谦,王群威,张建波,等.汽油中微量元素的X射线荧光光谱分析[J].石油学报:石油加工,2008,24(3):360-364.
[14]石丹云.关于车用汽油中甲基苯胺质量检测方法的探讨[J].理化检验:化学分册,2016,(5):20-21.
[15]张月琴.汽油中氮化物的定性定量方法研究与应用[J].石油炼制与化工,2016,47(4):91-95.
[16]HJ168-2010《环境监测分析方法标准制修订技术导则》[S].
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