Performance and characteristics of a high pressure, high temperature capillary cell with facile construction for operando x-ray absorption spectroscopy

Journal Article · Fri Aug 15 00:00:00 EDT 2014 · Review of Scientific Instruments

DOI:https://doi.org/10.1063/1.4893351· OSTI ID:22314427

Bansode, Atul; Urakawa, Atsushi ^[1]; Guilera, Gemma; Simonelli, Laura; Avila, Marta ^[2]; Cuartero, Vera ^[2]

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1. Institute of Chemical Research of Catalonia (ICIQ), Av. Països Catalans 16, 43007 Tarragona (Spain)
2. ALBA Synchrotron Light Source, Crta. BP 1413, Km. 3.3, 08290 Cerdanyola del Vallès, Barcelona (Spain)

We demonstrate the use of commercially available fused silica capillary and fittings to construct a cell for operando X-ray absorption spectroscopy (XAS) for the study of heterogeneously catalyzed reactions under high pressure (up to 200 bars) and high temperature (up to 280 °C) conditions. As the first demonstration, the cell was used for CO{sub 2} hydrogenation reaction to examine the state of copper in a conventional Cu/ZnO/Al{sub 2}O{sub 3} methanol synthesis catalyst. The active copper component of the catalyst was shown to remain in the metallic state under supercritical reaction conditions, at 200 bars and up to 260 °C. With the coiled heating system around the capillary, one can easily change the length of the capillary and control the amount of catalyst under investigation. With precise control of reactant(s) flow, the cell can mimic and serve as a conventional fixed-bed micro-reactor system to obtain reliable catalytic data. This high comparability of the reaction performance of the cell and laboratory reactors is crucial to gain insights into the nature of actual active sites under technologically relevant reaction conditions. The large length of the capillary can cause its bending upon heating when it is only fixed at both ends because of the thermal expansion. The degree of the bending can vary depending on the heating mode, and solutions to this problem are also presented. Furthermore, the cell is suitable for Raman studies, nowadays available at several beamlines for combined measurements. A concise study of CO{sub 2} phase behavior by Raman spectroscopy is presented to demonstrate a potential of the cell for combined XAS-Raman studies.

• OSTI ID: 22314427
• Journal Information: Review of Scientific Instruments, Vol. 85, Issue 8; Other Information: (c) 2014 AIP Publishing LLC; Country of input: International Atomic Energy Agency (IAEA); ISSN 0034-6748
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ABSORPTION SPECTROSCOPY
ALUMINIUM OXIDES
CAPILLARIES
CARBON DIOXIDE
CATALYSTS
COPPER
HEATING SYSTEMS
HYDROGENATION
METHANOL
PACKED BEDS
PRESSURE RANGE MEGA PA 10-100
RAMAN SPECTROSCOPY
SILICA
TEMPERATURE RANGE 0400-1000 K
THERMAL EXPANSION
X-RAY SPECTROSCOPY
ZINC OXIDES