The sun is an abundant and cheap source of energy, harnessing it as storable fuel has the potential for a large societal impact. Organic photoelectrodes (PEs) formed from low molecular weight hydrogels are showing promise as PEs for water splitting. Photoelectrochemical data indicates that the gelation method impacts on the photo-response efficiency. This implies the arrangement and size of the fibres formed during gelation is important in their behaviour as PEs. We propose a GISANS experiment using the SANS2d instrument to measure the structure and alignment of the PEs, particularly close to the conductive substrate surface where the alignment is likely to have the most influence. Comparison between preparation methods and of different depths through the hydrated gel film will be vital, hence TOF-GISANS is the most appropriate technique for the measurements to improve gel PE design.