气相色谱法测定阳离子表面活性剂合成体系中脂肪烷基二甲基叔胺
|
摘要
选用HP-NINOWax毛细管色谱柱及氢火焰离子化检测器(FID),采用程序升温,建立了4种脂肪烷基二甲基叔胺的分析方法。结果表明,4种脂肪烷基二甲基叔胺质量浓度在0.005～1.0 g/L范围内,其峰面积与质量浓度有良好的线性关系,相关系数(R~2)在0.999 6以上。检出限(LODs,信噪比为3)在0.001～0.002 g/L之间,定量限(LOQs,信噪比为10)在0. 003～0.005 g/L之间,回收率在90%～130%之间,相对标准偏差为1.3%～6.9%(n=6)。方法的线性范围宽、回收率高、选择性好,可用于叔胺的产品质量分析及生产过程控制分析。利用该方法对阳离子表面活性剂合成反应中十六烷基二甲基叔胺进行监测,结果很好地符合双分子亲核取代反应。该方法比滴定分析法更快速、精确,与液相色谱法相比,不需要进行柱前衍生或者使用色谱-质谱联用仪器。
A method to determine fatty alkyl dimethyl tertiary amines by gas chromatography(GC) was set up using HP-INNOWax capillary column, hydrogen flame ionization detector(FID) and temperature programming. The linearities were all excellent in the range of 0.005-1.0 g/L with the correlation coefficients being above 0.999 6. The limits of detection(LODs, S/N=3) of the method were between 0.001 g/L and 0.002 g/L, and the limits of quantification(LOQs, S/N=10) were between 0.003 g/L and 0.005 g/L. The recoveries ranged between 90% and 130% with relative standard deviations of 1.3%-6.9%(n=6). The proposed method has the advantages of wide linear range, higher recovery, and selectivity, which was suitable for the quantitative analysis of fatty alkyl dimethyl tertiary amines and monitoring process control in industrial production. The method was faster and more accurate than titration, and also precluded the need for pre-column derivatization and determination by liquid chromatography-tandem mass spectrometry.
A method to determine fatty alkyl dimethyl tertiary amines by gas chromatography(GC) was set up using HP-INNOWax capillary column, hydrogen flame ionization detector(FID) and temperature programming. The linearities were all excellent in the range of 0.005-1.0 g/L with the correlation coefficients being above 0.999 6. The limits of detection(LODs, S/N=3) of the method were between 0.001 g/L and 0.002 g/L, and the limits of quantification(LOQs, S/N=10) were between 0.003 g/L and 0.005 g/L. The recoveries ranged between 90% and 130% with relative standard deviations of 1.3%-6.9%(n=6). The proposed method has the advantages of wide linear range, higher recovery, and selectivity, which was suitable for the quantitative analysis of fatty alkyl dimethyl tertiary amines and monitoring process control in industrial production. The method was faster and more accurate than titration, and also precluded the need for pre-column derivatization and determination by liquid chromatography-tandem mass spectrometry.
引文
[1]Xu B C,Zhang G J,Han F,et al.Fine Chemicals,2011,28(9):839徐宝财,张桂菊,韩富.精细化工,2011,28(9):839
[2]Geng T.[PhD Dissertation].Taiyuan:Taiyuan University of Technology,2010耿涛.[博士学位论文].太原:太原理工大学,2010
[3]Weisshaar D E,Earl G W,Amolins M W,et al.J Surfactants Deterg,2012,15(2):199
[4]Li G,Xu H B.Yunnan Chemical Technology,2014(3):29李敢,徐惠彬.云南化工,2014(3):29
[5]Zhao S F,Duan H R,Wu S,et al.Biological Chemical Engineering,2018,4(5):83赵松福,段浩然,吴莎,等.生物化工,2018,4(5):83
[6]Earl G W,Weisshaar D E,Paulson D,et al.J Surfactants Deterg,2005,8(4):325
[7]Tang W Y,Geng T,Jiang Y J.Fine Chemicals,2015,32(10):1106唐伟月,耿涛,姜亚洁,等.精细化工,2015,32(10):1106
[8]Zheng G L,Ding T M,Tian H S.Chemical Reagents,2015,37(12):1131郑甘霖,丁同梅,田恒水.化学试剂,2015,37(12):1131
[9]Dong Z L,Geng T,Jiang Y J,et al.Fine Chemicals,2015,32(7):746董子良,耿涛,姜亚洁,等.精细化工,2015,32(7):746
[10]GB/T 15045-2013
[11]QB 1915-93
[12]GB/T 5174-2004
[13]Wang X,Ma Y,Zheng J,et al.Journal of Nanjing University of Information Science&Technology:Natural Science Edition,2015,7(1):31王兴,马嫣,郑军,等.南京信息工程大学学报:自然科学版,2015,7(1):31
[14]Xu X,Xiao Y C,Geng D D,et al.Chinese Journal of Chromatography,2016,34(4):422许旭,肖远灿,耿丹丹,等.色谱,2016,34(4):422
[15]Zhang B Y,Cai X R,Yin Y Y,et al.Chinese Journal of Chromatography,2017,35(3):344张冰宇,蔡晓蓉,尹艳艳,等.色谱,2017,35(3):344
[16]Zhao Y Z,Yang P,Qian S.Chinese Journal of Chromatography,2015,33(5):508赵云芝,杨坪,钱蜀.色谱,2015,33(5):508
[17]Liu F X,Bi X H,Ren Z F,et al.Chinese Journal of Analytical Chemistry,2017,45(4):477刘凤娴,毕新慧,任照芳,等.分析化学,2017,45(4):477
[18]GB/T 15045-1994
[19]Chen Y W.Fine Chemicals,1990,7(4/5):95谌英武.精细化工,1990,7(4/5):95
[20]Li G,Chen Y,Xia J B.Chinese Journal of Organic Chemistry,2018,38(8):1949李刚,陈烨,夏纪宝.有机化学,2018,38(8):1949
[2]Geng T.[PhD Dissertation].Taiyuan:Taiyuan University of Technology,2010耿涛.[博士学位论文].太原:太原理工大学,2010
[3]Weisshaar D E,Earl G W,Amolins M W,et al.J Surfactants Deterg,2012,15(2):199
[4]Li G,Xu H B.Yunnan Chemical Technology,2014(3):29李敢,徐惠彬.云南化工,2014(3):29
[5]Zhao S F,Duan H R,Wu S,et al.Biological Chemical Engineering,2018,4(5):83赵松福,段浩然,吴莎,等.生物化工,2018,4(5):83
[6]Earl G W,Weisshaar D E,Paulson D,et al.J Surfactants Deterg,2005,8(4):325
[7]Tang W Y,Geng T,Jiang Y J.Fine Chemicals,2015,32(10):1106唐伟月,耿涛,姜亚洁,等.精细化工,2015,32(10):1106
[8]Zheng G L,Ding T M,Tian H S.Chemical Reagents,2015,37(12):1131郑甘霖,丁同梅,田恒水.化学试剂,2015,37(12):1131
[9]Dong Z L,Geng T,Jiang Y J,et al.Fine Chemicals,2015,32(7):746董子良,耿涛,姜亚洁,等.精细化工,2015,32(7):746
[10]GB/T 15045-2013
[11]QB 1915-93
[12]GB/T 5174-2004
[13]Wang X,Ma Y,Zheng J,et al.Journal of Nanjing University of Information Science&Technology:Natural Science Edition,2015,7(1):31王兴,马嫣,郑军,等.南京信息工程大学学报:自然科学版,2015,7(1):31
[14]Xu X,Xiao Y C,Geng D D,et al.Chinese Journal of Chromatography,2016,34(4):422许旭,肖远灿,耿丹丹,等.色谱,2016,34(4):422
[15]Zhang B Y,Cai X R,Yin Y Y,et al.Chinese Journal of Chromatography,2017,35(3):344张冰宇,蔡晓蓉,尹艳艳,等.色谱,2017,35(3):344
[16]Zhao Y Z,Yang P,Qian S.Chinese Journal of Chromatography,2015,33(5):508赵云芝,杨坪,钱蜀.色谱,2015,33(5):508
[17]Liu F X,Bi X H,Ren Z F,et al.Chinese Journal of Analytical Chemistry,2017,45(4):477刘凤娴,毕新慧,任照芳,等.分析化学,2017,45(4):477
[18]GB/T 15045-1994
[19]Chen Y W.Fine Chemicals,1990,7(4/5):95谌英武.精细化工,1990,7(4/5):95
[20]Li G,Chen Y,Xia J B.Chinese Journal of Organic Chemistry,2018,38(8):1949李刚,陈烨,夏纪宝.有机化学,2018,38(8):1949
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |