This presentation will deal with the development of new materials and operando methods for electrocatalysis in alkaline media. The presentation will begin with a brief overview of the methods employed with emphasis on the use of X-ray based methods and transmission electron microscopy (TEM) under active potential control. The utility of these methods will be illustrated with selected examples focusing on non-precious metal oxides and nitrides as electrocatalysts for the oxygen reduction reaction (ORR), and Ni based systems for the HOR. Fuel cell (MEA) testing of integrated systems employing non-precious metal electrocatalysts will also be discussed. The presentation will conclude with an assessment of future directions.