We have designed a laboratory experiment to illustrate the use of spectroelectrochemical techniques for determination of aqueous iron. The experiment described in this article is applicable to an undergraduate laboratory course in analytical chemistry. Students are asked to fabricate spectroelectrochemical sensors, make electrochemical and optical measurements, and relate the analytical signals to aqueous iron concentrations by constructing a calibration curve. Three optional experiments are also offered, which can be performed during the 2-hour slide-soaking period at the discretion of the instructor. (Contains 5 figures.)