The design and operation of a new kind of high pressure/high temperature stirred IR cell is described. The cell is a stand-alone autoclave made of Hastelloy and effective stirring and gas diffusion are provided by a magnetically driven Teflon shaft. The length of the optical path can be regulated without the need of calibrated spacers and the problem of the sealing of the windows to the cell body has been solved by employing FEP (fluorinated ethylene propylene) encapsulated Viton O-rings, which, upon adapting to the cell when warmed, provide an excellent seal that is also tolerant of all standard solvents. The use of this kind of O-rings allows taking advantage of the chemical resistance of Teflon without needing to mechanically stress the fragile windows as it would be required if bulk Teflon O-rings were employed.

Design and Use of a High‐Pressure Stirred IR Cell for Operando Studies in Homogeneous Catalysis / C. Crotti, F. Ferretti, F. Ragaini. - In: CHEMISTRY METHODS. - ISSN 2628-9725. - 1:9(2021), pp. 415-420. [10.1002/cmtd.202100048]

Design and Use of a High‐Pressure Stirred IR Cell for Operando Studies in Homogeneous Catalysis

F. Ferretti
Secondo
;
F. Ragaini
Ultimo
2021

Abstract

The design and operation of a new kind of high pressure/high temperature stirred IR cell is described. The cell is a stand-alone autoclave made of Hastelloy and effective stirring and gas diffusion are provided by a magnetically driven Teflon shaft. The length of the optical path can be regulated without the need of calibrated spacers and the problem of the sealing of the windows to the cell body has been solved by employing FEP (fluorinated ethylene propylene) encapsulated Viton O-rings, which, upon adapting to the cell when warmed, provide an excellent seal that is also tolerant of all standard solvents. The use of this kind of O-rings allows taking advantage of the chemical resistance of Teflon without needing to mechanically stress the fragile windows as it would be required if bulk Teflon O-rings were employed.
Carbonylation; High Pressure Spectroscopy; Homogeneous Catalysis; IR Spectroscopy; Operando techniques
Settore CHIM/03 - Chimica Generale e Inorganica
2021
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/2434/870815
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