...
  • 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >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
【24h】

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-膦与甲醇之间的反应的初始快速步骤

获取原文
获取原文并翻译 | 示例
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

摘要

In the present work, for the first time, investigation of the initial fast step of reaction between 1,1,1-trichloro-3-methyl-3-phospholene (TCMP) and methanol was studied under a dry inert atmosphere by a newly constructed CSF apparatus by means of a further development in the configuration of the previous stopped-flow spectrophotometer (SFS). Hence, it was necessary to make many changes to the stopped-flow apparatus: replacement of the spectrophotometer amplifier with a conductance amplifier and the use of a conductivity cell to replace the optical one. The conductivity cell was made of polyethylene capillary tube (1 mm internal diameter; i.d.) and its inside dimensions were 1 mm i.d. × 3 mm long. Two tube electrodes which are made of stainless steel (0.8 mm i.d. × 14 mm long) were fixed at opposite ends of the observation cell and their outer surfaces were connected to the conductivity bridge amplifier by the two lead wires. The mixer was a 3-way Teflon valve and the distance between the mixer and the end of the observation cell was 30 mm. For each run, at least 24 L of solution was required for a typical trace with a dead time of about 5 ms. Because of the extreme sensitivity of TCMP to moisture, the stopped-flow (CSF) apparatus was used inside a glove bag under a dry nitrogen atmosphere. Kinetic parameters for pseudo first-order reaction involving k _(obs) = 30 s~(-1) at 22 °C and activation energy E a = 13.55 KJ mol~(-1) were successfully calculated for the initial fast step of the reaction between TCMP and methanol at 22 °C.
机译：在本工作中，首次通过新构建的方法研究了在干燥的惰性气氛下研究1,1,1-三氯-3-甲基-3-膦烯（TCMP）与甲醇之间的初始快速反应步骤的过程。通过对先前的停流分光光度计（SFS）进行配置的进一步改进，CSF设备得以实现。因此，有必要对停流设备进行许多更改：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。电导池是由聚乙烯毛细管（内径1毫米;内径）制成的，其内部尺寸为内径1毫米。 ×3毫米长。将两个由不锈钢制成的管形电极（内径0.8毫米×14毫米长）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。混合器是三通铁氟龙阀，混合器与观察池末端之间的距离为30 mm。对于每次运行，典型痕迹至少需要24 L溶液，死区时间约为5 ms。由于TCMP对湿气非常敏感，因此在干燥氮气气氛下在手套袋内使用了停流（CSF）设备。成功地计算了22°C时k _（obs）= 30 s〜（-1）和活化能E a = 13.55 KJ mol〜（-1）的拟一级反应动力学参数。在22°C下TCMP与甲醇之间的反应。

著录项

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号