高温气相色谱法测定费-托合成蜡的碳数分布
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摘要
采用柱上进样技术,使用DB-HT-SimDis色谱柱,通过高温气相色谱-火焰离子化检测法,对含高碳数产物的费-托合成蜡的碳数分布进行了快速准确的测定。对载气流量、柱箱升温程序、进样量、进样浓度等实验参数进行了考察。在最佳实验条件下,可在60min内准确测定费-托合成蜡C_(21)~C_(101)的碳数分布,所得C_(21)~C_(74)相邻碳数化合物分离度高于1.5,C_(74)~C_(101)之间相邻碳数化合物分离度高于1.2。从C_(57)至C_(101),ln(W/n)与对应碳数的线性关系良好,相关系数为0.999 3,可计算得到实验用费-托合成产物的链增长因子α值为0.928。所建方法操作简便、分离效率高、测定结果准确,对各种蜡产物的品质分析有重要的意义。
A high temperature gas chromatography coupled with cold-on-column inlet and flame ionization detector(FID)was used to rapidly determine the carbon number distribution of Fischer-Tropsch wax.The experimental parameters,such as column flow,oven temperature program,injection volume and sample concentration,were studied by DB-HT-SimDis column.Under the optimized GC conditions,the carbon number distribution of Fischer-Tropsch wax between C_(21) and C_(101) can be verified accurately within 60 min.The GC resolutions are higher than 1.5 and 1.2 for C_(21) to C_(74) and C_(74) to C_(101),respectively.The linear correlation coefficient value between ln(W/n)and carbon number in the range of C_(57) and C_(101) is 0.999 3 and the chain growth probability(αvalue)of 0.928 is calculated.
A high temperature gas chromatography coupled with cold-on-column inlet and flame ionization detector(FID)was used to rapidly determine the carbon number distribution of Fischer-Tropsch wax.The experimental parameters,such as column flow,oven temperature program,injection volume and sample concentration,were studied by DB-HT-SimDis column.Under the optimized GC conditions,the carbon number distribution of Fischer-Tropsch wax between C_(21) and C_(101) can be verified accurately within 60 min.The GC resolutions are higher than 1.5 and 1.2 for C_(21) to C_(74) and C_(74) to C_(101),respectively.The linear correlation coefficient value between ln(W/n)and carbon number in the range of C_(57) and C_(101) is 0.999 3 and the chain growth probability(αvalue)of 0.928 is calculated.
引文
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[18]Vander Laan G P,Beenackers A.Kinetics and selectivity of the Fischer-Tropsch synthesis[J].Catalysis Reviews—Science and Engineering,1999,41(3/4):255-318
[19]江云辉.锆改性钴基催化剂费-托合成反应性能研究[D].天津:天津大学,2013
[2]孙予罕,陈建刚,王俊刚,等.费-托合成钴基催化剂的研究进展[J].催化学报,2010,30(8):919-927
[3]郑申棵.反应条件对钴基费-托合成催化剂产物分布影响的氘同位素示踪研究[D].武汉:中南民族大学,2007
[4]Fu Tingjun,Jiang Yunhui,LüJing,et al.Effect of carbon support on Fischer-Tropsch synthesis activity and product distribution over Co-based catalysts[J].Fuel Processing Technology,2013,110(1):141-149
[5]Jiang Yunhui,Fu Tingjun,LüJing,et al.Zirconnium modified Co/SiO2Fischer-Tropsch catalyst prepared by dielectric-barrier discharge plasma[J].Journal of Energy Chemistry,2013,22(3):506-511
[6]陈宜俍,凡俊琳,郭士岭,等.F-T合成产物分布影响因素的研究进展[J].现代化工,2007,27(1):74-79
[7]蒋莹,吕蝶,李自运,等.费-托合成反应产物的气相色谱法全分析[J].石油学报(石油加工),2011,27(6):935-940
[8]Hawthorne S B,Miller D J.Analysis of commercial waxes using capillary supercritical fluid chromatography-mass spectrometry[J].Journal of Chromatography,1987,388(2):397-409
[9]Tsubaki N,Fujimoto K.Product control in Fischer-Tropsch synthesis[J].Fuel Processing Technology,2000,62:173-186
[10]杨海鹰.气相色谱在石油化工中的应用[M].北京:化学工业出版社,2005:235-243
[11]Kumar S,Gupta A K,Agrawal K M.Study on carbon number distribution of high melting microcrystalline waxes[J].Petroleum Science and Technology,2003,21(7/8):1253-1263
[12]周云琪.高熔点蜡中正、异构烷烃碳数分布的高温气相色谱法[J].色谱,1996,14(5):403-404
[13]Regert M,Langlois J,Colinart S.Characterisation of wax works of art by gas chromatographic procedures[J].Journal of Chromatography A,2005,1091(1/2):124-136
[14]Ludwig Sr F J.Gas chromatography of petroleum-derived waxes and high-molecular-mass liner alcohols and acids[J].Journal of Chromatography A,1995,718(1):119-129
[15]Bawase M A,Reve S D,Shete S V,et al.Carbon number distribution by gas chromatography for identification of outlying diesel sample[C]//2nd National Conference of Metrology Society of India on Advances in Metrology(AdMet),2012,CM003:1-7
[16]Villalanti D C,Raia J C,Maynard J B.Encyclopedia of Analytical Chemistry[M].Chichester,2000:6726-6741
[17]郑立辉,盛奎龙,潘金亮.石油蜡的生产及深加工[M].北京:化学工业出版社,2008:27-30
[18]Vander Laan G P,Beenackers A.Kinetics and selectivity of the Fischer-Tropsch synthesis[J].Catalysis Reviews—Science and Engineering,1999,41(3/4):255-318
[19]江云辉.锆改性钴基催化剂费-托合成反应性能研究[D].天津:天津大学,2013