Journal of Membrane Science 354 (2010) 32–39 Contents lists available at ScienceDirect Journal of Membrane Science journal homepage: www.elsevier.com/locate/memsci Novel high throughput equipment for membrane-based gas separations Asim Laeeq Khan, Subhankar Basu, Angels Cano-Odena, Ivo F.J. Vankelecom Centre for Surface Chemistry and Catalysis, Faculty of Bioengineering Sciences, Katholieke Universiteit Leuven, Kasteelpark Arenberg 23, 3001 Leuven, Belgium article info Article history: Received 4 September 2009 Received in revised form 15 February 2010 Accepted 27 February 2010 Available online 6 March 2010 Keywords: Gas separation High throughput Pressure-driven membrane processes Constant volume system abstract The design and fabrication of a high throughput (HT) gas permeation system will be described. In order to test large sets of membranes, a HT-gas separation module was developed, allowing gas permeation and selectivity testing of 16 membranes simultaneously at different feed pressure and temperature. A variable temperature controller and adjustable upstream pressure controller permit measurements of low-permeability membranes and evaluation of temperature related phenomena. The potential of the developed equipment and the HT-screening concept in general was validated by demonstrating the reproducibility of experimental flux and selectivity data for a lab-made dense Matrimid and a commercial asymmetric membrane at all 16 positions. Permeate flux was measured with increased permeate pres- sure as function of time in a constant volume auxiliary cylinder. An on-line compact gas chromatograph was used for fast gas selectivity measurements. The reproducibility of the data was highly encouraging, proving that this HT approach can be a useful tool to rapidly screen a large array of operational param- eters in membrane processes and of synthesis parameters in the development of new high-performing membranes. © 2010 Elsevier B.V. All rights reserved. 1. Introduction High throughput (HT) synthesis and screening is a powerful tool for rapid preparation and processing of a large variety of material. The discovery process of new materials can indeed be reduced con- siderably by their synthesis and performance-testing in a HT way. Such techniques have been used over the years in pharmaceutical and biotechnological research [1–3]. They have thus contributed significantly to the discovery of drugs but also more recently to that of new solid-state materials [4,5], such as polymers, catalysts, and membranes among others [6,7]. Membrane technology is an attractive area for HT exploration. Membranes have shown tremendous potential for a variety of separations, ranging from rough separations, like in waste water treatment, to separations of gases or liquids at molecular level [8,9]. There are constantly new applications of membrane technology appearing which require exploration of materials, operational con- ditions, membrane synthesis procedures etc. Selection of the most suitable material or conditions for these applications requires per- formance screening, which is a time consuming and laborious task. In recent years, there have been considerable improvements in the design of standard single gas permeation cells. Tabe-Muhammadi et al. designed and constructed a gas permeation system based on a constant volume system for the measurement of gas permeation Corresponding author. Tel.: +32 16 321594; fax: +32 16 321998. E-mail address: ivo.vankelecom@biw.kuleuven.be (I.F.J. Vankelecom). rates as low as 1 × 10 -8 cm 3 /s [10]. Damle and Koros developed a new type of membrane masking technique in the permeation cell suitable for working in high-pressure applications [11]. Moore et al. further reduced the leak rate of atmospheric gases in the perme- ation cell by designing an O-ring based system coupled with film masking procedures that could be used for more brittle polymers [12]. However, all these involve testing of only one membrane at a time. The availability of fast and efficient HT equipment will result in the reduction of time and cost, leading to a faster development and better optimization of membranes and membrane processes respectively. Membranes for gas separation purposes are typically screened in a standard single gas permeation cell. Mainly due to the more complicated, hence expensive, on-line analysis, the more interest- ing mixed gas selectivities are much scarcer in literature. In previous studies, our research group reported a HT equip- ment for testing solvent resistant nanofiltration (SRNF) membranes [13,14]. The equipment was designed in-house and was the first high throughput set-up in the field of membrane technology. This new study reports the first expansion of HT equipment to membrane-based gas separation (HTGS). It allows on-line selec- tivity and permeability analysis of 16 membranes simultaneously with variable mixed gas feeds. 2. Calculations The permeability of gases through most polymeric membranes follows the solution-diffusion mechanism [15]. Permeabilities of 0376-7388/$ – see front matter © 2010 Elsevier B.V. All rights reserved. doi:10.1016/j.memsci.2010.02.069