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Acetic acid was supplied by Sigma and ethanol and ethyl acetate were supplied by Merck. The components were degassed ultrasonically,dried over molecular sieves (type4A,Aldrich),and kept in an inert argon with a maximum water content of 2*10-6mass fraction. Their mass fraction purities were>99 mass% for acetic acid and>99.8 mass% for methanol,ethanol and ethyl acetate. The water was bidistillated and deionized. The catalyst used was an ion-exchange resin Amberlyst 15 supplied by Supelco.The catalyst was washed with ethanol and water to remove impurities and dried at 363.15K. Mean diameter of the resin beads,obtained by scanning electron microscopy, is 7.6*10-3m. A Hewlett-Packard 6890GC chromatograph was used to determine the composition of the samples.The gas chromatograph column was HP-FFAP polyethylene glycol TPA equipped with series of connected thermal conductivity and flame ionization detectors to detect water and the other compounds in the same run.Helium was used as carrier at a flow rate of 6.8 *10-8m-3 s-1 . Injector, detectors and oven temperature were 473.15,503.15 and 423.15K,respectively.To know the composition of these quaternary mixtures it is necessary to have quaternary patrons of known composition,so 249 quaternary mixtures were prepared by mass and were measured by gas chromatography. The experiments were performed in a stirred glass reactor with a volume of 1.5*10-4m 3. The temperature in the reactor was maintained within+0.1K. The acetic acid and the catalyst were heated at reaction temperature,ethanol was heated separately.When temperature reaction is reached,the second reactant was added to the mixture in the reactor and this was considered the starting time of the reaction.During each experiment, samples of about 5*10-7m3 were taken and cooled to avoid vaporization before analyzing. The homogeneous reactions, esterification or hydrolysis,are catalyzed by the acetic acid.Table1 summarizes the experiments made at 303.15, 323.15 and 353.15K. The duration of each experiment to reach chemical equilibrium is indicated in the third column. |
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dwaww(金币+1): 2011-03-20 19:47:58
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A Hewlett-Packard 6890GC chromatograph was used to determine the composition of the samples.The gas chromatograph column was HP-FFAP polyethylene glycol TPA equipped with series of connected thermal conductivity and flame ionization detectors to detect water and the other compounds in the same run.Helium was used as carrier at a flow rate of 6.8 *10-8m-3 s-1 . Injector, detectors and oven temperature were 473.15,503.15 and 423.15K,respectively.To know the composition of these quaternary mixtures it is necessary to have quaternary patrons of known composition,so 249 quaternary mixtures were prepared by mass and were measured by gas chromatography. Hewlett-Packard 6890型气相色谱测定样品的组成成分。在相同的分析测试中，用配备系列热导检测器和火焰离子检测器的HP-FFAP 型聚乙二醇TPA 色谱柱测定水分和其它组分。低流速（6.8 *10-8m-3 s-1）的氦气作载气。进样器温度、检测器温度以及柱温分别为473.15,503.15和423.15K。为能知道这些四元混合物的组成，有必要建立一个已知成分的四元混合物标准模型。所以，按质量比配制一249四元混合物并用气相色谱测定其含量。 |
6楼2011-03-19 20:58:16
2楼2011-03-19 12:48:25
3楼2011-03-19 13:53:33
dwaww(金币+1, 翻译EPI+1): 谢啦 可是只有一段呀 2011-03-20 19:44:38
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Acetic acid was supplied by Sigma and ethanol and ethyl acetate were supplied by Merck. The components were degassed ultrasonically,dried over molecular sieves (type4A,Aldrich),and kept in an inert argon with a maximum water content of 2*10-6mass fraction. Their mass fraction purities were>99 mass% for acetic acid and>99.8 mass% for methanol,ethanol and ethyl acetate. The water was bidistillated and deionized. 醋酸由Sigma公司提供，乙醇和乙酸乙酯为Merck公司产品。这些原料经超声脱除空气、分子筛（4A型，Aldrich公司产品）干燥，然后保存在内充氩气的干燥器中（里面水含量最大不超过2*10-6质量分数）。醋酸的质量分数纯度大于99%，而乙醇和乙酸乙酯的质量分数超过99.8%。水为二次蒸馏、去离子水。 |
4楼2011-03-19 20:33:52
简单回复
Mally8913楼
2011-03-20 11:45
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