Coupling of a scanning flow cell with online electrochemical mass spectrometry for screening of reaction selectivity.

In this work the online coupling of a miniaturized electrochemical scanning flow cell (SFC) to a mass spectrometer is introduced. The system is designed for the determination of reaction products in dependence of the applied potential and/or current regime as well as fast and automated change of the sample. The reaction products evaporate through a hydrophobic PTFE membrane into a small vacuum probe, which is positioned only 50-100 μm away from the electrode surface. The probe is implemented into the SFC and directly connected to the mass spectrometer. This unique configuration enables fast parameter screening for complex electrochemical reactions, including investigation of operation conditions, composition of electrolyte, and material composition. The technical developments of the system are validated by initial measurements of hydrogen evolution during water electrolysis and electrochemical reduction of CO2 to various products, showcasing the high potential for systematic combinatorial screening by this approach.

[1]  M. Koper,et al.  On-line mass spectrometry system for measurements at single-crystal electrodes in hanging meniscus configuration , 2006 .

[2]  K. Mayrhofer,et al.  Dissolution of Platinum: Limits for the Deployment of Electrochemical Energy Conversion?** , 2012, Angewandte Chemie.

[3]  Angel A Topalov,et al.  Development and integration of a LabVIEW-based modular architecture for automated execution of electrochemical catalyst testing. , 2011, The Review of scientific instruments.

[4]  H. Baltruschat.  Differential electrochemical mass spectrometry , 2004, Journal of the American Society for Mass Spectrometry.

[5]  Ioannis Katsounaros,et al.  Oxygen electrochemistry as a cornerstone for sustainable energy conversion. , 2014, Angewandte Chemie.

[6]  K. Mayrhofer,et al.  Coupling of a high throughput microelectrochemical cell with online multielemental trace analysis by ICP-MS , 2011 .

[7]  H. Baltruschat,et al.  Quantitative DEMS study of ethanol oxidation: effect of surface structure and Sn surface modification. , 2012, Physical chemistry chemical physics : PCCP.

[8]  K. Mayrhofer,et al.  A Scanning Flow Cell System for Fully Automated Screening of Electrocatalyst Materials , 2012 .

[9]  Y. Hori,et al.  Electrochemical CO 2 Reduction on Metal Electrodes , 2008 .

[10]  S. Bruckenstein,et al.  Use of a porous electrode for in situ mass spectrometric determination of volatile electrode reaction products [14] , 1971 .

[11]  Aleksandar R. Zeradjanin,et al.  Rational design of the electrode morphology for oxygen evolution – enhancing the performance for catalytic water oxidation , 2014 .

[12]  R. Behm,et al.  Composition and activity of high surface area PtRu catalysts towards adsorbed CO and methanol electrooxidation: A DEMS study , 2002 .

[13]  Thomas F. Jaramillo,et al.  New insights into the electrochemical reduction of carbon dioxide on metallic copper surfaces , 2012 .

[14]  Nathan S. Lewis,et al.  Powering the Planet , 2007 .

[15]  H. Baltruschat,et al.  New Cell for DEMS Applicable to Different Electrode Sizes , 2012, Electrocatalysis.

[16]  O. Wolter,et al.  Differential Electrochemical Mass Spectroscopy (DEMS) — a New Method for the Study of Electrode Processes , 1984 .

[17]  M. Arenz,et al.  Comparative DEMS study on the electrochemical oxidation of carbon blacks , 2012 .

[18]  M. Koper,et al.  Electrochemical reduction of carbon dioxide on copper electrodes , 2017 .

[19]  Aleksandar R. Zeradjanin,et al.  Gold dissolution: towards understanding of noble metal corrosion , 2013 .

[20]  G. Mul,et al.  Electrochemical CO2 reduction on Cu2O-derived copper nanoparticles: controlling the catalytic selectivity of hydrocarbons. , 2014, Physical chemistry chemical physics : PCCP.