Institute of Surface Chemistry and Catalysis, Ulm University, D-89069 Ulm, Germany.
Anal Chem. 2012 Jul 3;84(13):5479-83. doi: 10.1021/ac203276f. Epub 2012 Jun 13.
We report on a novel approach for complete quantitative online product analysis in electrocatalytic reactions, combining electron impact ionization mass spectrometry (EI-MS) and electrospray ionization mass spectrometry (ESI-MS) for simultaneous detection of both volatile and nonvolatile reaction products. The potential of this method is demonstrated using continuous methanol oxidation in a flow cell. The overall reaction rate was followed via the Faradaic current; CO(2) formation was monitored mass spectrometrically via a membrane inlet system, and formaldehyde and formic acid were detected by ESI-MS after a derivatization-extraction-separation procedure introduced recently (Zhao, W.; Jusys, Z.; Behm, R. J. Anal. Chem.2010, 82, 2472-2479) providing quantitative data on the product distribution. In a more general sense, this approach is applicable for a wide range of reactions at the solid-liquid interface or in liquid phase.
我们报告了一种新的方法，用于电催化反应中的完全定量在线产物分析，结合电子轰击电离质谱（EI-MS）和电喷雾电离质谱（ESI-MS），同时检测挥发性和非挥发性反应产物。该方法的潜力通过在流动池中连续甲醇氧化来证明。通过法拉第电流跟踪总反应速率；通过膜入口系统通过质谱法监测 CO(2)形成，并且通过最近引入的衍生化-提取-分离程序（Zhao，W.；Jusys，Z.；Behm，R. J. Anal. Chem.2010，82，2472-2479）检测甲醛和甲酸，提供产物分布的定量数据。更一般地说，该方法适用于固液界面或液相中的广泛反应。
