Apparatus for the investigation of high-temperature, high-pressure gas-phase heterogeneous catalytic and photo-catalytic materials

Alvino, Jason F.; Bennett, Trystan; Kler, Rantej; Hudson, Rohan J.; Aupoil, Julien; Nann, Thomas; Golovko, Vladimir B.; Andersson, Gunther G.; Metha, Gregory F.

doi:10.1063/1.4982350

Cited by 6 publications

(8 citation statements)

References 57 publications

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“…Photocatalytic D 2 evolution from heavy water (D 2 O) was carried out in the gas phase using a batch reactor described in detail previously [14]. D 2 O was investigated to ensure products were not derived from sacrificial reagents or the catalyst itself.…”

Section: Photocatalysismentioning

confidence: 99%

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Pt Nanocluster Co-Catalysts for Photocatalytic Water Splitting

Shearer

Alvino

Batmunkh

et al. 2018

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Degussa P25 is a benchmark form of TiO 2 used worldwide in photocatalysis studies. Currently, no such benchmark exists for co-catalysts, which are essential for many photocatalytic reactions. Here, we present the preparation of Pt nanocluster co-catalysts on TiO 2 using an unmodified commercial source and equipment that is commonly available. Transmission electron microscopy reveals that the procedure produces TiO 2 decorated with Pt atoms and nanoclusters (1-5 atoms). Optical reflectance and X-ray diffraction measurements show that the procedure does not affect the TiO 2 polymorph or ultraviolet-visible (UV-Vis) absorbance. Gas phase photocatalytic splitting of heavy water (D 2 O) shows that the Pt nanocluster-decorated TiO 2 outperforms Pt nanoparticle (produced by photodeposition) decorated TiO 2 in D 2 production. Pt nanoclusters, produced directly from a commercial source, with high co-catalyst activity, are prime candidates to be used in benchmark photocatalytic reactions.

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Section: Photocatalysismentioning

confidence: 99%

“…The sample reaction cell is then evacuated for 30 min before the process is repeated 2 or more times with the same sample. The recorded values from the RGA are converted into moles produced from calibration procedures and is described in detail elsewhere [14].…”

Section: Photocatalysismentioning

confidence: 99%

Pt Nanocluster Co-Catalysts for Photocatalytic Water Splitting

Shearer

Alvino

Batmunkh

et al. 2018

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“…Photocatalytic heavy water (D2O) splitting was carried out in the gas phase using a batch reactor described in detail previously [14]. The general procedure for each experiment was to load the photocatalyst (on the microfibre disc) into the reaction cell, evacuate to high vacuum under heating to 150 o C for 1 h before isolating the cell from vacuum.…”

Section: Photocatalysismentioning

confidence: 99%

Pt Nanocluster Co-Catalysts for Photocatalytic Water Splitting

Shearer¹,

Alvino²,

Batmunkh³

et al. 2018

Preprint

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Degussa P25 is a benchmark form of TiO2 used worldwide in photocatalysis studies. Currently no such benchmark exists for co-catalysts, which are essential for many photocatalytic reactions. Here, we present the preparation of Pt nanocluster co-catalysts on TiO2 using an unmodified commercial source and equipment that is commonly available. Transmission electron microscopy reveals that the procedure produces TiO2 decorated with Pt atom and nanoclusters (1-5 atoms). Optical reflectance and X-ray diffraction measurements show that the procedure does not affect the TiO2 polymorph or UV-Vis absorbance. Gas phase photocatalytic splitting of heavy water (D2O) shows that the Pt nanocluster decorated TiO2 outperforms Pt nanoparticle (produced by photodeposition) decorated TiO2 in D2 production. Pt nanoclusters, produced directly from a commercial source, with high co-catalyst activity are prime candidates to be used in benchmark photocatalytic reactions.

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“…Of which, MS typically serves as a faster detection method even for the unknown products. Although various studies and applications of the quantitative gas analysis using MS have been published, [9][10][11] the quantitative product analysis by means of MS for a continuous heterogeneously catalytic reaction, such as the CO 2 hydrogenation reaction, was not yet reported. Recently, Alvino et al demonstrated a quantitative gas analysis method by means of MS via a pressure controlled vacuum chamber.…”

Section: Introductionmentioning

confidence: 99%

“…Recently, Alvino et al demonstrated a quantitative gas analysis method by means of MS via a pressure controlled vacuum chamber. 11 In their setup, which is equipped with a batch reactor with a sapphire window for photocatalytic experiments, the reaction gas from the reactor was injected into a pressure controlled vacuum chamber with a pulsed nozzle valve. The MS then sampled the gas from the vacuum chamber, which was held at constant pressure for the calibration and the experiments.…”

Section: Introductionmentioning

confidence: 99%

Fast real time and quantitative gas analysis method for the investigation of the CO2 reduction reaction mechanism

Mutschler

Luo

Moioli

et al. 2018

Review of Scientific Instruments

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We present a new fast real time and quantitative gas analysis method by means of mass spectrometry (MS), which has approximately an order of magnitude faster sampling rate in comparison with a traditional gas chromatography. The method is presented and discussed on the example of the CO 2 reduction reaction. The advantages of the method are the possibility to analyze the reaction kinetics, where the kinetically determined reaction range is often only tens of degrees wide. Furthermore, due to the fast sampling rate, the experiments are much shorter and effects due to possible aging of the catalyst are significantly reduced. The quantification of the gas partial pressures is achieved by calibrating the Faraday detector in the quadrupole MS for the expected reactants and products. One major challenge to achieve a quantitative measurement with the MS is to correct for the pressure fluctuations over the probing capillary over the course of the experiment. This fluctuation is compensated in the analysis by normalizing the sum of all calculated partial pressures to the measured reaction pressure for every measured spectrum. With that, a precise, fast, and quantitative gas analysis is achieved. This is the fundament for, e.g., the kinetic reaction analysis where a high data point density is required. The method is discussed on the example of the CO 2 hydrogenation reaction to CH 4 on a commercial Ru/Al 2 O 3 catalyst. Additionally, the key features of the gas controlling and analysis setup built for the CO 2 hydrogenation reaction are described.

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Apparatus for the investigation of high-temperature, high-pressure gas-phase heterogeneous catalytic and photo-catalytic materials

Cited by 6 publications

References 57 publications

Pt Nanocluster Co-Catalysts for Photocatalytic Water Splitting

Pt Nanocluster Co-Catalysts for Photocatalytic Water Splitting

Pt Nanocluster Co-Catalysts for Photocatalytic Water Splitting

Fast real time and quantitative gas analysis method for the investigation of the CO2 reduction reaction mechanism

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