Electroless NiP films, with 12 to 16 wt % P, were deposited from a moderately acid solution. Thermogravimetric analysis indicates the presence of occluded hydrogen in the layers, which desorbs upon heating. The amount of incorporated hydrogen decreases when the pH of the solution or the nickel sulfate concentration is increased; by contrast it increases with hypophosphite concentration. Cyclic voltammetry, using an electrochemical quartz crystal microbalance, confirms the existence of parasitic reactions, namely the reduction of protons of the solvent during the cathodic process and oxidation of hydrogen during the dissolution of the layers. This behaviour is in qualitative agreement with the proposed reaction scheme.