气相色谱法和折光率法测定乙醇-正丙醇物系组分含量比对
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摘要
建立了气相色谱氢火焰离子化检测器(FID)测定乙醇-正丙醇物系含量方法,并通过实验拟合得到折光率和乙醇质量分数线性方程y=-4 194.6x+5 792.5(R~2=0.999 5)。比对气相色谱法和折光率法测定乙醇-正丙醇物系中乙醇和正丙醇含量。结果表明,当乙醇含量≥30%,折光率法检测相对误差RE≤3.0%,可以采用折光率法进行快速检测;当乙醇含量<30%,折光率法检测RE>5%,随着乙醇含量降低,RE逐渐升高达到19.50%,而GC检测RE均<2%,建议采用GC进行检测。该方法线性关系良好,乙醇回收率99%～101%,精密度良好,准确度高,耐用性好,溶液稳定,检测限为0.000 77%,定量限为0.002 6%,可用于乙醇-正丙醇物系定量检测。
A GC(FID) method for determination of ethanol-propanol content in basic chemical engineering experiment was established.The linearity relation between refractive index and ethanol content was also obtained as y=-4 194.6x+5 792.5(R~2=0.999 5).It was shown in the comparison of the two methods that when ethanol content is more than 30%,the relative error(RE) of refractive index method is not more than 3.0%.The result showed that when ethanol content is less than 30%,the relative error(RE) of refractive index method is more than 5% and it increases as ethanol content reduces.The relative error(RE) of the refractive index method was even up to 19.50% while the relative error(RE) of the GC method was below 2%.The method is used when ethanol content below 30%.The validation results showed that the GC method has good linearity,precision,robustness,accuracy and stability of the solution.The LOD and LOQ was 0.000 77% and 0.002 6% respectively.It is concluded that the GC method can be applied for the determination of ethanol-propanol content in basic chemical engineering experiment.
A GC(FID) method for determination of ethanol-propanol content in basic chemical engineering experiment was established.The linearity relation between refractive index and ethanol content was also obtained as y=-4 194.6x+5 792.5(R~2=0.999 5).It was shown in the comparison of the two methods that when ethanol content is more than 30%,the relative error(RE) of refractive index method is not more than 3.0%.The result showed that when ethanol content is less than 30%,the relative error(RE) of refractive index method is more than 5% and it increases as ethanol content reduces.The relative error(RE) of the refractive index method was even up to 19.50% while the relative error(RE) of the GC method was below 2%.The method is used when ethanol content below 30%.The validation results showed that the GC method has good linearity,precision,robustness,accuracy and stability of the solution.The LOD and LOQ was 0.000 77% and 0.002 6% respectively.It is concluded that the GC method can be applied for the determination of ethanol-propanol content in basic chemical engineering experiment.
引文
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[3] 张振坤.乙醇-正丙醇物系的折光率-温度-组成的关系模型建立[J].广州化工,2016,44(4):84-86.
[4] 胡育筑,严拯宇.分析化学(上册)[M].北京:科学出版社,2015.
[5] 国家食品药品监督管理局药品认证管理中心.GMP实施指南(质量控制实验室和物料系统)[M].北京:中国医药科技出版社,2011.
[6] 洪薇,符传武,农丽丹.正丙醇作内标气相色谱法测定白酒的酒精度[J].中国酿造,2015,34(1):152-154.
[7] 宋光林,杨昌彪,肖飞,等.内标-气相色谱法分析白酒中的正丙醇含量[J].贵州科学,2012,30(6):70-72.
[8] 李先国.物理化学[M].北京:北京大学出版社,2016.
[9] 刘建兰,张东明.物理化学实验[M].北京:化学工业出版社,2015.