Readily Constructed Glass Piston Pump for Gas Recirculation

The recirculation of gases in a sealed reactor system is a broadly useful method in catalytic and electrocatalytic studies. It is especially relevant when a reactant gas reacts slowly with respect to residence time in a catalytic reaction zone and when mass transport control through the reaction zone is necessary. This need is well illustrated in the field of electrocatalytic N₂ reduction, where the need for recirculation of ¹⁵N₂ has recently become more apparent. Herein, we describe the design, fabrication, use, and specifications of a lubricant-free, readily constructed recirculating pump fabricated entirely from glass and inert polymer (poly(ether ether ketone) (PEEK), poly(tetrafluoroethylene) (PTFE)) components. Using these glass and polymer components ensures chemical compatibility between the piston pump and a wide range of chemical environments, including strongly acidic and organic electrolytes often employed in studies of electrocatalytic N₂ reduction. The lubricant-free nature of the pump and the presence of components made exclusively of glass and PEEK/PTFE mitigate contamination concerns associated with recirculating gases saturated with corrosive or reactive vapors for extended periods. The gas recirculating glass pump achieved a flow rate of >500 mL min^-1 N₂ against atmospheric pressure at 15 W peak power input and >100 mL min^-1 N₂ against a differential pressure of +6 in. H₂O (∼15 mbar) at 10 W peak power input.