High-pressure adsorption differential volumetric apparatus (HP-ADVA) for accurate equilibrium measurements

The volumetric system is a commonly used experimental method for gas adsorption measurements. Starting from the conventional volumetric system (single-branched), the development of differential (double-branched) apparatus has been proposed to overcome some criticalities connected to the original design. The following study is focused on the assessment of the high-pressure differential volumetric apparatus (HP-ADVA) built at the University of Edinburgh in order to discover and characterise system peculiarities at different experimental conditions, in terms of temperature and pressure. To do this, an integrated approach is proposed: an initial experimental campaign has been performed to take confidentiality with the apparatus, then, the experimental results were the starting point for the development of a sensitivity and error analysis aimed at describing the effect of each operating parameter into the final result. In this regard, a different analytical approach, compared to the ones commonly proposed in literature, has been proposed to closely reproduce the real system. Beyond having obtained promising results, some criticalities, matching what originally hypothesized from the experimental campaign, have been noted: valve volume effect and temperature control and measurements have been discovered being crucial aspects, and, supposedly, source of errors leading to explain the unexpected results obtained by the experimental campaign. Moreover, the importance of symmetry maintenance among the branches has been repeatedly confirmed in the analysis. Some recommendations aimed at improving the system set-up have been moved regarding the installation of a temperature control system and more accurate temperature measurement devices. Additionally, an accurate assessment and characterisation of pneumatically-actuated valves, as well as of the differential pressure transducer used for pressure measurement, before the installation, could be useful to reduce inaccuracies.