Hydrogen detection during photocatalytic water splitting: A tutorial

The increasing interest in the usage of clean technologies pointed toward the photocatalytic evolution of hydrogen. Consequently, an appropriate analytical procedure becomes mandatory to detect and quantify the produced hydrogen in different photocatalytic systems so that the quantification, as well as the photocatalytic experiment is reliable and repeatable. Herein, this work represents a first-of-the-kind approach proposing guidelines for a robust detection and quantification of hydrogen evolved from photocatalytic reaction systems together with standard operation procedures to consider when performing photocatalytic hydrogen evolution reactions. Gas chromatography with thermal conductivity detector (GC-TCD) was chosen as the analytical tool for the detection and quantification through the preparation of calibration curves carried out emulating the reaction conditions i.e. introducing hydrogen into a reactor containing electrolyte solution and sealed with a silicon septum for gas tight assurance. Validation parameters were calculated and linearity of the calibration curves obtained with the proposed methodology was proved.