We examined LEDs as a cheap and test lamp source to simulate monochromatic laser radiation to help us cost out optics while evaluating materials for renewable fuels. The light source spectrum was recorded using a fiber optic spectrophotometer and a calibrated silicon photodiode was used to determine the intensity. Photon flux from the LEDs was recorded using actinometry. We chose CdS and Fe 3O 4 as photocatalysts. The as-prepared and annealed samples were characterised using X-Ray Diffraction, UV-Visible spectroscopy, UV-Visible Diffuse reflectance spectroscopy, Fourier Transform Infra-red spectroscopy, Attenuated Total Reluctance-FTIR spectroscopy, Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). CdS and Fe 3O 4 were evaluated for hydrogen evolution using DI water, sacrificial agents and an electron donor (methyl viologen) using three light sources (LEDs, sunlight and mercury vapour lamp). Products were collected by an inverted burette (Generation 1), balloons with a B-14 adapter (Generation2) and septum cells (Generation3). Developing an analytical technique to quantify products continues to remain a challenge. © 2011 Materials Research Society.