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Experimental Section Materials and Analysis The chemicals used for the kinetic study were of analytical grade (rectapur); Amberlyst 15 and concentrated sulphuric acid were selected as catalysts. For the reactive distillation experiments, the chemicals were of reaction grade (99.5%) and sulphuric acid was the catalyst. All samples were analysed by gas chromatography (Varian 3800) using cross-linked polyethylene glycol CP-WAX 52 CB 30 m 0.32 mm column with FID detector. For the homogeneously catalyzed kinetic runs, the acetic acid concentration has been determined using titration; additional titrations were performed with a METTLER DL 35 Karl¨CFischer-Titrator to measure the quantity of water formed during the reaction. A data reconciliation process was led in order to appreciably increase reliability and consistency of results: the elimination of aberrant measurements is performed on the base of the atomic conservation (Fillon et al., 1995). An accuracy of molar fractions of 3% can thus be expected. |
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±¦MMC(½ð±Ò+15, ·ÒëEPI+1): лл 2011-05-23 14:06:37
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Experimental Section Materials and Analysis ʵÑ鲿·Ö£º²ÄÁϺͷÖÎö·½·¨ The chemicals used for the kinetic study were of analytical grade (rectapur); Amberlyst 15 and concentrated sulphuric acid were selected as catalysts.¶¯Á¦Ñ§Ñо¿ËùÓÃÊÔ¼Á¾ùΪ·ÖÎö´¿£»Ñ¡Óôó¿×Ê÷Ö¬15ºÍŨÁòËáΪ´ß»¯¼Á¡£ For the reactive distillation experiments, the chemicals were of reaction grade (99.5%) and sulphuric acid was the catalyst. ÔÚÕôÁó·´Ó¦ÊµÑéÖУ¬ËùÓÃÊÔ¼ÁΪ·´Ó¦¼¶£¨99.5%£©£¬´ß»¯¼ÁΪÁòËá¡£All samples were analysed by gas chromatography (Varian 3800) using cross-linked polyethylene glycol CP-WAX 52 CB 30 m 0.32 mm column with FID detector. È«²¿ÑùÆ·ÒÔÆøÏàÉ«Æ×£¨ÍßÀï°²3800£©½øÐзÖÎö£º½»Áª¾ÛÒÒ¶þ´¼CP-WAX 52 CB 30 m 0.32 mm ·ÖÎöÖù£»Çâ»ðÑæÀë×Ó»¯¼ì²âÆ÷¡£For the homogeneously catalyzed kinetic runs, the acetic acid concentration has been determined using titration; additional titrations were performed with a METTLER DL 35 Karl¨CFischer-Titrator to measure the quantity of water formed during the reaction.¾ùÏà´ß»¯¶¯Á¦Ñ§·ÖÎöÖУ¬ÒÒËáŨ¶Èͨ¹ýµÎ¶¨È·¶¨£»·´Ó¦ÆÚ¼äÉú³ÉË®µÄÁ¿Í¨¹ýÃ·ÌØÀÕDL 35¿¨¶û-·ÑÉá¶ûµÎ¶¨ÒDzⶨ¡£ A data reconciliation process was led in order to appreciably increase reliability and consistency of results: the elimination of aberrant measurements is performed on the base of the atomic conservation (Fillon et al., 1995). An accuracy of molar fractions of 3% can thus be expected.Êý¾Ý¼ÓÒԺ˶ÔÒÔÌá¸ß½á¹ûµÄ¿É¿¿ÐÔºÍÒ»ÖÂÐÔ£ºÔÚÔ×ÓÊØºãµÄ»ù´¡ÉÏÌÞ³ýÁ˲¿·ÖÆ«»ûÊý¾Ý(Fillon et al., 1995)¡£Ô¤ÆÚ׼ȷ¶ÈΪĦ¶û·ÖÊý3%¡£ |
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