A method for the rapid determination of the oxidation rate of naturally occurring pyrite (FeS2) samples is presented. The progress of the oxidation reaction was followed by measurement of the concentration of total dissolved iron using flow injection analysis. Iron was determined using UV–vis detection after reaction with the colorimetric reagent 5-sulfosalicylic acid in the presence of ammonia. The calibration function was linear between 5 and 150 mg L−1, and the detection limit was 0.46 mg L−1. The relative standard deviation was typically less than 1% (n = 10) and the measurement frequency was 60/h. The method was used to quantify the oxidation rate of 10 ground and cleaned pyrite samples (53 μm < x < 106 μm) from various international locations that were subjected to accelerate oxidation in acidic hydrogen peroxide. Results of these experiments showed that there was almost an order of magnitude of difference in oxidation rates of the pyrite samples.