Exploring catalytic solid/liquid interfaces by in situ attenuated total reflection infrared spectroscopy.

In situ attenuated total reflection Fourier transform infrared (ATR-FT-IR) spectroscopy has gained considerable attention as a powerful tool for exploring processes occurring at solid/liquid and solid/liquid/gas interfaces as encountered in heterogeneous catalysis and electrochemistry. Understanding of the molecular interactions occurring at the surface of a catalyst is not only of fundamental interest but constitutes the basis for a rational design of heterogeneous catalytic systems. Infrared spectroscopy has the exceptional advantage to provide information about structure and environment of molecules. In the last decade, in situ ATR-FT-IR has been developed rapidly and successfully applied for unraveling processes occurring at solid/liquid interfaces. Additionally, the kinetics of complex reactions can be followed by quantifying the concentration of products and reactants simultaneously in a non-destructive way. In this tutorial review we discuss some key aspects which have to be taken into account for successful application of in situ ATR-FT-IR to examine solid/liquid catalytic interfaces, including different experimental aspects concerned with the internal reflection element, catalyst deposition, cell design, and advanced experimental methods and spectrum analysis. Some of these aspects are illustrated using recent examples from our research. Finally, the potential and some limitations of ATR will be elucidated.

[1]  W. A. Pliskin,et al.  Infrared Spectra of Chemisorbed Carbon Monoxide , 1954 .

[2]  N. Harrick Study of Physics and Chemistry of Surfaces from Frustrated Total Internal Reflections , 1960 .

[3]  Theodore Kuwana,et al.  Observation of electrode-solution interface by means of internal reflection spectrometry , 1966 .

[4]  B. S. Pons,et al.  An in situ Spectrophotometric Method for Observing the Infrared Spectra of Species at the Electrode Surface During Electrolysis. , 1966 .

[5]  R. Greenler Infrared Study of Adsorbed Molecules on Metal Surfaces by Reflection Techniques , 1966 .

[6]  K. Kunimatsu Potential dependence of infrared reflection absorption spectrum of the adsorbed carbon monoxide produced by chemisorption of methanol on a smooth plati , 1982 .

[7]  R. Sorbello,et al.  The metal-surface selection rule for infrared spectra of molecules adsorbed on small metal particles , 1982 .

[8]  W. Sproul,et al.  Physical vapor deposition tool coatings , 1996 .

[9]  A. Baiker Progress in asymmetric heterogeneous catalysis: Design of novel chirally modified platinum metal catalysts , 1997 .

[10]  John Arul Phillips,et al.  In Situ Monitoring of an Escherichia coli Fermentation Using a Diamond Composition ATR Probe and Mid‐infrared Spectroscopy , 1999, Biotechnology progress.

[11]  Richard G. Brereton,et al.  Introduction to multivariate calibration in analytical chemistry , 2000 .

[12]  Harris,et al.  In situ adsorption studies at silica/solution interfaces by attenuated total internal reflection fourier transform infrared spectroscopy: examination of adsorption models in normal-phase liquid chromatography , 2000, Analytical chemistry.

[13]  D. Ferri,et al.  An in situ attenuated total reflection infrared study of a chiral catalytic solid-liquid interface: cinchonidine adsorption on pt. , 2001, Journal of the American Chemical Society.

[14]  D. Ferri,et al.  Pt and Pt/Al2O3 thin films for investigation of catalytic solid-liquid interfaces by ATR-IR spectroscopy: CO adsorption, H2-induced reconstruction and surface enhanced absorption , 2001 .

[15]  C. H. Bartholomew Mechanisms of catalyst deactivation , 2001 .

[16]  J. Ryczkowski IR Spectroscopy in Catalysis , 2001 .

[17]  D. Bousfield,et al.  In situ Infrared Technique for Studying Adsorption onto Particulate Silica Surfaces from Aqueous Solutions , 2001 .

[18]  A. Baiker,et al.  In Situ Infrared Spectroscopy of Catalytic Solid−Liquid Interfaces Using Phase-Sensitive Detection: Enantioselective Hydrogenation of a Pyrone over Pd/TiO2 , 2002 .

[19]  D. Ferri,et al.  Probing Catalytic Solid‐Liquid Interfaces by Attenuated Total Reflection Infrared Spectroscopy: Adsorption of Carboxylic Acids on Alumina and Titania , 2002 .

[20]  A. Baiker,et al.  VCD spectroscopy of chiral cinchona modifiers used in heterogeneous enantioselective hydrogenation: conformation and binding of non-chiral acids , 2002 .

[21]  Carol J. Hirschmugl,et al.  Frontiers in infrared spectroscopy at surfaces and interfaces , 2002 .

[22]  J. Grunwaldt,et al.  High pressure view-cell for simultaneous in situ infrared spectroscopy and phase behavior monitoring of multiphase chemical reactions , 2003 .

[23]  A. Baiker,et al.  Interaction between ketopantolactone and chirally modified Pt investigated by attenuated total reflection IR concentration modulation spectroscopy. , 2003, Journal of the American Chemical Society.

[24]  A. Baiker,et al.  Epoxidation on titania–silica aerogel catalysts studied by attenuated total reflection Fourier transform infrared and modulation spectroscopy , 2003 .

[25]  A. Urakawa,et al.  ATR-IR Flow-Through Cell for Concentration Modulation Excitation Spectroscopy: Diffusion Experiments and Simulations , 2003 .

[26]  A. Baiker,et al.  Probing Enantiospecific Interactions at Chiral Solid−Liquid Interfaces by Absolute Configuration Modulation Infrared Spectroscopy , 2003 .

[27]  C. Williams,et al.  In situ investigation of solid-liquid catalytic interfaces by attenuated total reflection infrared spectroscopy , 2003 .

[28]  C. Domingo,et al.  Surface-Enhanced Infrared Spectroscopy , 2004, Applied spectroscopy.

[29]  A. Baiker,et al.  Absolute configuration modulation attenuated total reflection ir spectroscopy: an in situ method for probing chiral recognition in liquid chromatography. , 2004, Analytical chemistry.

[30]  J. Moulijn,et al.  Real-time in situ ATR-FTIR analysis of the liquid phase hydrogenation of -butyrolactone over Cu-ZnO catalysts: A mechanistic study by varying lactone ring size , 2004 .

[31]  J. Moulijn,et al.  Operando ATR-FTIR analysis of liquid-phase catalytic reactions: can heterogeneous catalysts be observed? , 2004 .

[32]  A. Baiker,et al.  Epoxidation of cyclic allylic alcohols on titania–silica aerogels studied by attenuated total reflection infrared and modulation spectroscopy , 2004 .

[33]  Combined in situ attenuated total reflection infrared and UV–vis spectroscopic study of alcohol oxidation over Pd/Al2O3 , 2005 .

[34]  J. Grunwaldt,et al.  Benzyl alcohol oxidation in supercritical carbon dioxide: spectroscopic insight into phase behaviour and reaction mechanism. , 2005, Physical chemistry chemical physics : PCCP.

[35]  In situ ATR-IR spectroscopic and reaction kinetics studies of water-gas shift and methanol reforming on Pt/Al2O3 catalysts in vapor and liquid phases. , 2005, The journal of physical chemistry. B.

[36]  In situ Attenuated Total Reflection Infrared Spectroscopy of Catalysts , 2005 .

[37]  D. Ferri,et al.  On the role of CO formation during the aerobic oxidation of alcohols on Pd/Al2O3: an in situ attenuated total reflection infrared study , 2005 .

[38]  D. Ferri,et al.  Unraveling the surface reactions during liquid-phase oxidation of benzyl alcohol on Pd/Al2O3: an in situ ATR-IR study. , 2005, The journal of physical chemistry. B.

[39]  H. Assender,et al.  Quantitative ATR-IR Analysis of Anisotropic Polymer Films: Surface Structure of Commercial PET , 2005 .

[40]  D. Ferri,et al.  Supercritical carbon dioxide: an inert solvent for catalytic hydrogenation? , 2005, The journal of physical chemistry. B.

[41]  S. Kazarian,et al.  Fourier transform infrared imaging for high-throughput analysis of pharmaceutical formulations. , 2005, Journal of combinatorial chemistry.

[42]  D. Ferri,et al.  Discrimination of active palladium sites in catalytic liquid-phase oxidation of benzyl alcohol. , 2006, The journal of physical chemistry. B.

[43]  D. Ferri,et al.  ATR-IR spectroscopy of pendant NH2 groups on silica involved in the Knoevenagel condensation. , 2006, Langmuir : the ACS journal of surfaces and colloids.

[44]  CO adsorption and oxidation at the catalyst-water interface: an investigation by attenuated total reflection infrared spectroscopy. , 2006, Langmuir : the ACS journal of surfaces and colloids.

[45]  Laurent Pilon,et al.  Effective optical properties of non-absorbing nanoporous thin films , 2006, Thin Solid Films.

[46]  D. Ferri,et al.  Cinchonidine adsorption on gold and gold-containing bimetallic platinum metal surfaces: an attenuated total reflection infrared and density functional theory study. , 2006, The journal of physical chemistry. B.

[47]  T. Bürgi,et al.  Probing chiral interfaces by infrared spectroscopic methods. , 2007, Physical chemistry chemical physics : PCCP.

[48]  J. Moulijn,et al.  Bottom-mounted ATR probes : Pitfalls that arise from gravitational effects , 2007 .

[49]  D. Ferri,et al.  Combined liquid-phase ATR-IR and XAS study of the Bi-promotion in the aerobic oxidation of benzyl alcohol over Pd/Al2O3 , 2007 .

[50]  Ronei J. Poppi,et al.  Second- and third-order multivariate calibration: data, algorithms and applications , 2007 .

[51]  D. Ferri,et al.  Role of guiding groups in cinchona-modified platinum for controlling the sense of enantiodifferentiation in the hydrogenation of ketones. , 2007, Journal of the American Chemical Society.

[52]  Enantioselective interactions at the solid-liquid interface of an HPLC column under working conditions. , 2008, Analytical chemistry.

[53]  A. Urakawa,et al.  Sensitivity enhancement and dynamic behavior analysis by modulation excitation spectroscopy: Principle and application in heterogeneous catalysis , 2008 .

[54]  J. Grunwaldt,et al.  Mn(III)(salen)-catalyzed synthesis of cyclic organic carbonates from propylene and styrene oxide in “supercritical” CO2 , 2008 .

[55]  D. Ferri,et al.  Advances in Infrared Spectroscopy of Catalytic Solid–Liquid Interfaces: The Case of Selective Alcohol Oxidation , 2009 .

[56]  A. Urakawa,et al.  Selective blocking of active sites on supported gold catalysts by adsorbed thiols and its effect on the catalytic behavior: A combined experimental and theoretical study , 2009 .

[57]  A. Baiker,et al.  A green pathway for hydrogenations on ionic liquid-stabilized nanoparticles , 2009 .

[58]  A. Urakawa,et al.  Design and performance of a flow-through polarization-modulation infrared reflection-absorption spectroscopy cell for time-resolved simultaneous surface and liquid phase detection under concentration and temperature perturbations. , 2009, The Review of scientific instruments.

[59]  A. Urakawa,et al.  Polarization-modulation infrared reflection-absorption spectroscopy affording time-resolved simultaneous detection of surface and liquid phase species at catalytic solid-liquid interfaces. , 2009, The Analyst.

[60]  D. Ferri,et al.  Chemical Availability and Reactivity of Functional Groups grafted to Magnetic Nanoparticles monitored In situ by ATR-IR Spectroscopy , 2009 .

[61]  A. Baiker,et al.  Tracing the Acetalization of Cyclohexanone in CO2-Expanded Alcohols by Attenuated Total Reflection Infrared Spectroscopy , 2009, Applied spectroscopy.

[62]  A. Urakawa,et al.  In Situ PM-IRRAS Study of Liquid-Phase Benzyl Alcohol Oxidation on Palladium , 2009 .

[63]  DFT and In-Situ Spectroelectrochemical Study of the Adsorption of Fluoroacetate Anions at Gold Electrodes , 2009 .

[64]  A. Baiker,et al.  Simple in Situ Monitoring of a Complex Catalytic Reaction Network at High Pressure by Attenuated Total Reflection Fourier Transform Infrared Spectroscopy , 2010, Applied spectroscopy.