An undergraduate laboratory experiment for the volumetric quantitative analysis of ascorbic acid and iron in dietary supplement tablets is presented. Powdered samples of the dietary supplement tablets were volumetrically titrated against electrolytically generated reagents, and the mass of dietary reagent in the tablet was determined from the volume of potassium hydrogen phthalate solution used as a primary standard. Proposed electrolysis cell was directly powered by a 9 V battery eliminating the requirement of a coulometer. Students use this method to quantify the active ingredient in dietary supplement tablets: iron and ascorbic acid (vitamin C). The experiment is suitable for the undergraduate quantitative analysis laboratory.