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New Knudsen effusion apparatus with simultaneous gravimetric and quartz crystal microbalance mass loss detection
Authors:Luís MNBF Santos  Luís M Spencer S Lima  Carlos FRAC Lima  Fernão D Magalhães  Manuel C Torres  Bernd Schröder  Manuel AV Ribeiro da Silva
Institution:1. Centro de Investigação em Química, Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade do Porto, Rua do Campo Alegre, 687, P-4169-007 Porto, Portugal;2. LEPAE, Departamento de Engenharia Química, Faculdade de Engenharia, Universidade do Porto, Rua Roberto Frias, P-4200-465 Porto, Portugal
Abstract:A new Knudsen effusion apparatus, enabling simultaneous gravimetric and quartz crystal microbalance mass loss detection, is described. This device allows the measurement of vapour pressures of small sample mass (50 to 100) mg over a wide temperature range (350 to 650) K using very short effusion time intervals. The performance of the apparatus was checked by measuring the vapour pressures of anthracene, benzanthrone, and 1,3,5-triphenylbenzene, between (0.1 and 1) Pa, over temperature intervals of 20 K. The derived standard molar enthalpies of sublimation and vapour pressures are in excellent agreement with the mean of the available literature values and with the recommended values. The new working methodology and design of this apparatus allows the measurement of high quality vapour pressure data due to: accurate temperature measurement and control; improvement in vacuum thermal contact between the effusion cell and the oven metal block; optimisation of the quartz crystal sensor head microbalance position; efficient temperature control of the quartz crystal microbalance head; accurate measurement of the resonance crystal frequency using an impedance circuit analyser methodology.
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