A high-pressure and high-temperature gas-loading system for the study of conventional to real industrial sized samples in catalysed gas/solid and liquid/solid reactions

作者：Andrieux Jerome^*; Chabert Christophe; Mauro Anthony; Vitoux Hugo; Gorges Bernard; Buslaps Thomas; Honkimaeki Veijo

来源：Journal of Applied Crystallography, 2014, 47(1): 245-255.

DOI：10.1107/S1600576713030197

A high-pressure-high-temperature gas-loading system (GLS) is described for combined operando X-ray diffraction and mass spectrometry investigations during catalysed gas/solid or liquid/solid reactions. The pressure cell consists of a single-crystal sapphire tube which serves as both high-pressure container and reaction cell, with up to 6 mm inner diameter. The system can operate in two different configurations, under either static high pressure or dynamic pressurized flow. The transportable reaction cell can be filled under inert atmosphere inside a glove box, enabling studies with oxygen-sensitive compounds to be conducted. The five main benefits of this system can be summarized as follows: (i) the temperature, pressure and gas-flow ranges of 2981273 K, 10(-3) mbar-200 bar (0.1-2 x 10(7) Pa) and 0-1 l min(-1), respectively, (ii) the combination of different gases, (iii) the flexibility of the cell design, (iv) the full rotation of the pressurized cell, and (v) the combination of X-ray diffraction and mass spectrometry as analytical tools. These key points open new possibilities for studying the evolution of catalysts or compounds from a fundamental point of view as well as for industrial applications, in both cases in operando conditions.

• 出版日期2014-1