A cell/microreactor is develop and fully characterized to perform diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) experiments to investigate heterogeneously catalyzed surface reactions. The experimental setup allows the simultaneous acquisition of time-resolved infrared spectra at high quality and the gas phase quantification by a mass spectrometer connected at the outlet of the cell. The cell behaves as a true plug-flow microreactor while allows the infrared radiation to sense the lateral part of the catalyst bed. The selected geometry allows a better correlation between the evolution of infrared signals from surface species and the gas concentration at the exit of the cell, that is, for strict Operando experimentation. The mass and heat transport phenomena were characterized using well established criteria to determine the operative limitations under steady state and fast transient experiments, e.g. during concentration-modulation excitation spectroscopy (c-MES). The performance of the cell is validated by studying the CO oxidation on a Au/CeO₂ catalyst. Identification and quantification of active surface species under reaction conditions are obtained combining modulation approach with phase sensitive detection (PSD) analysis and step experiments.

开发了一种细胞/微反应器，并对其进行了全面表征，以进行漫反射红外傅里叶变换光谱（DRIFTS）实验，以研究非均相催化的表面反应。实验设置允许同时获取高质量的时间分辨红外光谱，并通过连接在电池出口的质谱仪进行气相定量分析。该电解槽的行为就像一个真正的活塞流微反应器，同时允许红外辐射感测催化剂床的侧面部分。选定的几何形状允许从表面物种发出的红外信号的演变与单元出口处的气体浓度之间有更好的相关性，也就是说，对于严格的Operando实验而言。使用公认的标准对质量和传热现象进行表征，以确定稳态和快速瞬态实验（例如在浓度调制激发光谱法（c-MES）期间）下的操作局限性。通过研究Au / CeO上的CO氧化来验证电池的性能₂催化剂。结合调制方法与相敏检测（PSD）分析和分步实验，获得了反应条件下活性表面物种的鉴定和定量分析。