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Recent advances in imaging and monitoring of heterogeneous catalysts with Raman spectroscopy. Catalysis is a complex multidisciplinary science that enables efficient performance in energy, automotive, chemical and pharmaceutical industries; most chemical reactions are catalyzed and it is a science that cannot be understood without spectroscopy. Spectroscopy is the enabling tool for knowledge-based design of highly efficient and stable catalysts. This review presents the progress of operando Raman spectroscopy during reaction and temperature-programmed treatments for heterogeneous catalysts solid-gas and solid-liquid , with particular emphasis on the combination with other techniques, by extending it to space-resolved analyses and as a tool for mechanism investigation and monitoring in the liquid phase. Operando techniques are a key tool to understand catalysis and for monitoring and controlling catalytic processes. We summarize the most relevant research lines where Raman spectroscopy is applied in catalysis, challenges, hurdles and opportunities. This review outlines the versatility of Raman spectroscopy, for real-time analyses, in situ variable-programmed investigations and reaction studies. Spectroscopic information can be enhanced in a quantitative or qualitative manner, i. This compilation outlines the posibilities of signal enhancement by resonance or SERS, and expanding it to mapping. We also comment developments for Raman imaging of profiles during catalyst synthesis and during reaction. Finally, this review summarizes the progress made in the liquid phase, to study catalyst synthesis, to monitor and investigate reaction mechanism and progress. The simultaneous combination of Raman with other complementary techniques is presented for these three lines of development. The current scenario presents an extraordinary perspective on opportunities for future developments. Catalysis cannot be understood without spectroscopy. Spectroscopic techniques for characterization of catalysts in the working state are powerful, because they provide fundamental information about catalyst structures, including surface structures, under the appropriate conditions. Such characterizations have permitted major advances in catalysis, as they can be the basis for the design or discovery of new catalysts. Catalysis has gained importance and popularity in chemical technology since it enables the determination of relationships between catalytic activity and catalyst structure at the atomic scale. The need for characterization of catalysts during reaction has been highlighted and demonstrated by several authors. Time-resolved transient temperature or pressure response experiments can be also carried out by Raman spectroscopy and reaction kinetics data can be measured directly and correlated with the spectroscopic data. In addition, catalytic reactors are easily accessible to spectroscopy using quartz fiber optics. The Raman experiments can be carried out with static controlled atmosphere or under flowing mixtures of gases to mimic the conditions in a catalytic reactor. It is also possible to study reactions in the liquid phase or under supercritical conditions. Operando spectroscopic techniques are suitable for studying, monitoring and controlling homogeneous and heterogeneous catalysts in real-time under working conditions such as high pressures and temperatures in the gas and liquid phase, so that they are kept at its optimum performance. The operando methodology combines in situ spectroscopy during reaction with simultaneous activity measurement in a cell that meets the requirements of both, in situ cell and catalytic reactor. They are nowadays commonly used to obtain mechanistic insight into the active site and the related reaction mechanism. Thus, operando spectroscopic methodologies have now become efficient tools for the design of advanced catalytic materials. This would result in much higher product selectivity and typically longer catalyst operation time since relatively aggressive regeneration cycles is avoided; for instance thermal peaks during coke calcination. New instrumental developments combining multiple spectroscopic techniques into one operando set-up have emerged during the last years, giving ample opportunities to reach a more detailed understanding of many relevant catalytic systems. In the present paper, an overview of the literature on the most representative examples of using Raman operando as a single-technique as well as those relating to combining Raman operando with other spectroscopic techniques are presented. Its application for imaging and monitoring during catalytic operation or catalyst synthesis is also presented. A large number of monographs and review articles on Raman spectroscopy in heterogeneous catalysis have been published to date so this work is not aiming at bringing a thorough review, but presents current progress and opportunities for Raman spectroscopy based on the significant progress of in situ and operando studies during the last decade for both liquid and gas phase reactions. In situ spectroscopic methodologies bring an insight on the state of catalytic materials, their structure, surface structure and adsorbed species under controlled environment. As the experimental facilities progress, there is an evident evolution on in situ studies that get closer and closer to the catalytic event. This evolution has become more apparent in the literature after the term 'operando' that was first published in Since this term were coined as described elsewhere. A qualitative change has become apparent in the last decade to further consolidate in situ spectroscopy of the working catalyst. The term 'operando' is a common term in literature, but it is appropriate to put its concept in perspective. The term 'in situ,' Latin for 'on site,' implies that the sample is analyzed at the location the cell where it has been treated or is being treated. In situ is quite a versatile term and several levels of such experiments are described in literature Fig. In many in situ studies, though, the temperature or gas phase may have changed at the moment of acquisition. Temperature-programmed processes are a typical case, like TPR-Raman spectroscopy, in which Raman spectra characterize the reduction of a sample, TPO-Raman spectroscopy, or any temperature-programmed reaction with an adsorbate or a probe molecule TPSR. In the last few years, a powerful variant of variable-conditions 'in situ' spectroscopy is becoming increasingly important: modulation excitation; in this case, the signal-to-noise and time resolution can be significantly improved. This is an increasingly important approach to assess the state of the catalyst during reaction. However, in this approach, no online activity measurement is typically made, or if it is, activity values are significantly lower that it should correspond to the system. This is due to the fact that spectroscopic criteria dominate in the design of the in situ cell. On occasions, there are significant temperature gradients, or the catalyst is as a wafer for reactions runs on powder catalysts, and many other possible cases. Thus, it is possible to demonstrate that the spectra correspond to an operating catalyst. Due to simultaneous quantitative analysis of the reaction progress, structure and activity can be correlated. The term 'operando' is Latin for 'working'. In the operando methodology, the operando cell must be a cell that delivers reaction kinetics data that match those obtained in the corresponding conventional reactor and be adequate for simultaneous spectroscopic analyses. Since it was first proposed, a key requirement was that the operando cell would be kinetically relevant thus comparisons with conventional reactor activity data or Arrhenius plots were reported using operando cells. Meunier has reported detailed analyses of kinetic aspects of many operando cells. While 'operando' is a rather new term, several groups had already executed experimental approaches using the ideas of this concept. For instance, an operando EPR cells was presented in by Fehrmann et col. Treating the organometallic compound in reaction feed for butadiene hydrogenation or for crotonaldehyde hydrogenation, it is possible to observe how the organometallic compounds based on carbonyl ligands progressive decomposes, releasing CO. DRIFT spectra show the progressive transformation into a metallic surface based on the IR bands of carbonyl ligands, that shift from frequencies characteristic of CO ligands, to those of chemisorbed CO on a metal surface. Such structural transformation runs parallel to the rise of hydrogenation catalytic activity, thus, to the birth of an active metal catalyst out of an inert organometallic compound. That DRIFT cell was modified to be able to obtain quantitative conversion values, like those obtained in a fixed-bed microreactor; alas, such changes are only briefly commented in those papers. Fortunately, a very detailed description and much more thorough study on how to obtain quantitative conversion modifying com- mercial DRIFT cells was recently reported by Meunier. In the case of Raman spectroscopy, the first paper using the operando approach was reported by Hill et al. Interestingly their first papers using the term 'operando' were also for Raman spectroscopy and for ammoxidation reaction, in these cases, it was for the gas-phase ammoxidation of propane into acrylonitrile. Many authors have demonstrated the need for characterization of catalysts at work; its progress has been summarized in three recent volumes of Advances in Catalysis and in the compilation in Chemical Society Reviews. In particular, Raman is one of the most powerful tools for operando study of working catalysts. Raman experiments can be carried out at virtually any temperature and pressure, without interference from the gas phase, with increasingly higher time-resolutions. Thus, reaction kinetic data can be measured directly and correlated with the spectroscopic data. A number of monographs and review articles on Raman spectroscopy in heterogeneous catalysis have been published and have been reviewed. Very recently several exciting reviews address specific areas of progress for in situ Raman spectroscopy. Raman spectroscopy can be used to investigate the state of the catalyst its bulk and surface structure , of the reactants and of the adsorbed molecules. When reactions happen in the liquid phase, Raman can be used as an efficient tool for monitoring reaction progress. Detailed revisions of variable-programmed in situ and operando Raman studies has been done recently, so we will only present representative studies as well as their interplay with other complementary approaches. Investigation of the state of catalysts under variable-programmed conditions brings insight under several kind of treatments. The Raman studies connect typical profiles e. For instance, the anomalous reduction profiles of dispersed vanadium oxide on silica at vanadia coverage close to its dispersion limit. These are due to the different behavior of dispersed vanadium oxide species due to the presence of neighboring vanadium sites. These, reduce at low coverage, however, reduction at higher coverage triggers structural rearrangement of surface vanadium oxide species. Upon removal of oxide ions, surface vanadium oxide species rearrange and aggregate into nanocrystalline V2O5 Fig. Such transformation occurs at a temperature lower than at which highly dispersed vanadia reduces. The aggregation of dispersed vanadia into nano-V2O5 would facilitate their reduction, since the removal of a V-O-Si bond upon reduction which releases H2O would be compensated by the rearrangement of a neighboring V-O-Si bond into a V-O-V bond. Since, silica does not stabilize polymerized surface vanadium oxide species, this rearrangement leads to segregated V2O5 nanocrystals. V2O5 nanocrystals eventually reduce as temperature increases during reduction; then, dispersed vanadium oxide that did not rearrange, reduces. Such a scenario does not occur at lower coverages, and has been uncovered with TPR-Raman measurement. TPR-Raman may also bring detailed insight on other phenomena occurring during reduction. For instance, Lewandowska et al. In that occasion, the catalysts prepared with vanadyl sulfate exhibited a very sharp reduction peak. This would indicate that surface vanadium oxide species are particularly well dispersed on alumina with this precursor, and that it would render a pretty narrow distribution of states of surface vanadium oxide species. Most interestingly, the on-line mass spectrometer confirms that H2S is concomitantly produced to water Fig. This is indicative that the reduction of both, surface sulfate species and surface vanadium oxide species occur in the same temperature range. It could not have been told in the absence of simultaneous spectroscopic confirmation on the reduction of vanadium species and online analysis of effluent gases. The evolution of reduced S-species from these catalysts during TPR has also been reported by Auroux's group. Purchase options and add-ons. Report an issue with this product. Previous slide of product details. Publication date. Print length. See all details. Next slide of product details. From the Back Cover Over papers are published in the field of catalysis each year. While the majority appear within a handful publications, keeping up with the literature can be difficult. Now in its 24th volume, the Specialist Periodical Report on Catalysis presents critical and comprehensive reviews of the hottest literature published over the last twelve months. Highlights within this volume include Miguel Baneres and Vanesa Calvino-Casilda discussing recent advances in Raman imaging of heterogeneous catalysts. Olaf Deutschmann examines recent studies in catalytic reforming of logistic fuels. The coverage-dependent adsorption properties of late transition metals are discussed by John Kitchin and colleagues. Green oxidation catalysis with metal complexes is discussed by Christina Friere. Cavani et al consider innovative approaches with the selective oxidation of o-xylene. Miguel Yus reviews the Morita-Baylis-Hillman reaction, while Rafael Luque's team examines the catalytic applications of mesoprous silica-based materials. With chapters detailing specific areas within the field, this series is a comprehensive reference for anyone working in Catalysis and an essential resource for any Chemistry Library. All rights reserved. Spivey, M. Kitchin, 83, Green oxidation catalysis with metal complexes: from bulk to nano recyclable hybrid catalysts Cristina Freire, Clara Pereira and Susana Rebelo, , Selective oxidation of o-xylene to phthalic anhydride: from conventional catalysts and technologies toward innovative approaches Fabrizio Cavani, Aurora Caldarelli, Silvia Luciani, Carlotta Cortelli and Federico Cruzzolin, , Asymmetric organocatalyzed Morita-Baylis-Hillman reactions Gabriela Guillena, Diego J. Martinez de la Hoz and Perla B. Balbuena, , CHAPTER 1 Recent advances in imaging and monitoring of heterogeneous catalysts with Raman spectroscopy Catalysis is a complex multidisciplinary science that enables efficient performance in energy, automotive, chemical and pharmaceutical industries; most chemical reactions are catalyzed and it is a science that cannot be understood without spectroscopy. Excerpted from Catalysis Volume 24 by J. Excerpted by permission of The Royal Society of Chemistry. No part of this excerpt may be reproduced or reprinted without permission in writing from the publisher. Excerpts are provided by Dial-A-Book Inc. Read more. Customer reviews. How are ratings calculated? Instead, our system considers things like how recent a review is and if the reviewer bought the item on Amazon. It also analyses reviews to verify trustworthiness. Images in this review. No customer reviews. Your recently viewed items and featured recommendations. Back to top. Get to Know Us. Connect with Us. 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