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首页> 外文期刊>The Analyst >Establishing a new conductance stopped-flow apparatus to investigate the initial fast step of reaction between 1,1,1-trichloro-3-methyl-3-phospholene and methanol under a dry inert atmosphere
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Establishing a new conductance stopped-flow apparatus to investigate the initial fast step of reaction between 1,1,1-trichloro-3-methyl-3-phospholene and methanol under a dry inert atmosphere

机译：建立一种新的电导停止流装置，以研究在干燥的惰性气氛下1,1,1-三氯-3-甲基-3-膦与甲醇之间反应的初始快速步骤

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摘要

In the present work, for the first time, investigation of the initial fast step of reaction betweenn1,1,1-trichloro-3-methyl-3-phospholene (TCMP) and methanol was studied under a dry inertnatmosphere by a newly constructed CSF apparatus by means of a further development in thenconfiguration of the previous stopped-flow spectrophotometer (SFS). Hence, it was necessary to makenmany changes to the stopped-flow apparatus: replacement of the spectrophotometer amplifier withna conductance amplifier and the use of a conductivity cell to replace the optical one. The conductivityncell was made of polyethylene capillary tube (1 mm internal diameter; i.d.) and its inside dimensionsnwere 1 mm i.d. u0002 3 mm long. Two tube electrodes which are made of stainless steel (0.8 mm i.d. u0002n14 mm long) were fixed at opposite ends of the observation cell and their outer surfaces were connectednto the conductivity bridge amplifier by the two lead wires. The mixer was a 3-way Teflon valve and thendistance between the mixer and the end of the observation cell was 30 mm. For each run, at least 24 mLnof solution was required for a typical trace with a dead time of about 5 ms. Because of the extremensensitivity of TCMP to moisture, the stopped-flow (CSF) apparatus was used inside a glove bag underna dry nitrogen atmosphere. Kinetic parameters for pseudo first-order reaction involving kobs ?30 su00031 atn22 u0004C and activation energy Ea ?13.55 KJ molu00031 were successfully calculated for the initial fast step ofnthe reaction between TCMP and methanol at 22 u0004C.
机译：在本工作中，首次使用新型CSF设备在干燥惰性气氛下研究了n1,1,1-三氯-3-甲基-3-膦（TCMP）与甲醇之间的反应的初始快速步骤。通过对先前的停流分光光度计（SFS）进行进一步的配置。因此，有必要对停流设备进行任何更改：用电导放大器替换分光光度计放大器，并使用电导池替换光学传感器。导电单元由聚乙烯毛细管（内径1mm；内径）制成，其内部尺寸为内径1mm。 u0002 3毫米长。两个由不锈钢制成的管形电极（长0.8毫米，内径为u0002n14毫米）固定在观察池的相对两端，其外表面通过两条导线连接到电导桥放大器上。混合器是三通铁氟龙阀，然后混合器与观察池末端之间的距离为30 mm。对于每次运行，典型的迹线至少需要24 mLnof的溶液，死区时间约为5 ms。由于TCMP对水分的极端敏感性，因此在干燥氮气气氛下的手套袋内使用了停流（CSF）设备。对于在22 u0004C下TCMP和甲醇之间反应的初始快速步骤，成功地计算了涉及Kobs≥30 su00031 atn22 u0004C和活化能Ea≤13.55KJ molu00031的拟一级反应的动力学参数。

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  • 来源
    《The Analyst》 |2011年第8期|p.1713-1721|共9页
  • 作者

    Sayyed Mostafa Habibi Khorassani Ali Ebrahimi Malek Taher Maghsoodlou Mehdi Shahraki and Dennis Price;

  • 作者单位

    aDepartment of Chemistry, Faculty of Science, The University of Sistanand Baluchestan, P.O. Box 98135-674, Zahedan, Iran. E-mail:smhabibikhorassani@yahoo.com, Fax: +98 541 244655, Tel: +98 541244655bDepartment of Chemistry and Applied Chemistry, The University ofSalford, Salford, UK† This paper is dedicated to Dr A. K. Davies for his constant adviceduring my study at the Salford University.,;

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