Flow analysis methodology is presented for the determination of micromolar levels of aqueous hydrogen peroxide by luminol chemiluminescence. Adjustment of the pH to alkaline conditions and addition of the luminophore are implemented using in-line flow-through beds containing crystalline media. The requirement for a homogeneous catalyst is eliminated by electrochemical initiation of luminescence. Traditional laboratory reagents are replaced by packed beds containing solid phase basification media, and crystalline luminol. The methodology is suitable for application in both continuous flow and flow injection analysis configurations.