摘要
用GC-14B气相色谱仪测定了水-异丙醚-苯酚体系在319K和329K的等温截面相图.经实验筛选,选择保留时间恰当和分离度较好的乙酰丙酮作为内标物,正丁醇作溶剂.实验测定了除水以外各组分的保留时间以及相对于乙酰丙酮的校正因子.测试了恒温振荡和静止时间对平衡浓度测定的影响.分别进行了回收率测量,确证本实验数据具有相当的可信度.用内标法测定了319K和329K两个等温截面的两相液液平衡实验数据,并给出了相应的相图示意图.对于319K,与以前用外标法测定的实验结果作了比较,内标法实验精确度提高,数据可信度提高.其主要相图特征是类似的.原来用外标法曾估计在异丙醚摩尔分数小于4%时,可能存在另一两相区域,是不正确的.用内标法测定的数据确切表明不存在另一两相区域.最后对实验误差进行了讨论.
Under normal pressure, the isothermal LLE data of water-isopropyl ether-phenol （ H2O-（ CH3 ）2 CHOCH （CH3）2-C6H5OH） system at 319.15K and 329.15K were measured respectively, by using the gas chromatograph method, The inner-scaling method was used to determine the concentration of（ CH3）2CHOCH（CH3）2 and C6H5OH in this ternary system. Acetylacetone （ CH3COCH2COCH3） was chosen as the inner-scaling sample because of its small measurement error and good precision. During measurement, the n-butyl alcohol（n-C4H9OH） was chosen as the diluent. The retaining time of（ CH3）2 CHOCH（CH3 ）2, CH3COCH2COCH3 and C6H5OH are 1.495 min, 2. 383 min and 4.843min respectively, and the relative correcting factors of（ CH3）2CHOCH（ CH3）2 and C6H5OH to CH3COCH2COCH3 are 0.575 and 0.445.
The mean reclaiming ratio for isopropyl ether is 95.9%, and its root-mean-square error is 1.4%. The mean reclaiming ratio for phenol is 101.1% , and its root-mean-square error is 4.6%.
The measured LLE data at two given temperatures mentioned above and their corresponding isothermal section diagrams were given. There was an isothermal section diagram at 319K for the ternary system published in 2003, which was measured with working curve method. The comparison shows that the mean feature is similar to each other, but the results of the inner-scaling method are more reliable than the results of the working curve method. There was a wrong eatimation about two dual-phase co-existing areas in the result of the working curve method. According to the result of the inner-scaling method, there is only one dual-phase co-existing area.
出处
《常熟理工学院学报》
2008年第4期68-72,共5页
Journal of Changshu Institute of Technology
关键词
水-异丙醚-苯酚
液液平衡
气相色谱
内标法
外标法
water-isopropyl ether-phenol
liquid-liquid equilibrium （LLE）
gas chromatograph
inner-scalingmethod, working curve method
