Quantitative analysis of iron oxides using Fourier transform infrared spectrophotometry

In this study, a systematic approach based on the application of Fourier transform infrared spectrophotometry (FTIR) was taken, in order to quantitatively analyze the corrosion products formed in the secondary cycle of pressurized water reactors (PWR). Binary mixtures of iron oxides were prepared with known compositions containing pure commercial magnetite (Fe3O4), maghemite (γ-Fe2O3), and hematite (α-Fe2O3) for calibration purposes. Calcium oxide (lime) was added to all samples as a standard reference in obtaining the calibration curves. Using regression analysis, relationships were developed for intensity versus concentration for absorption bands corresponding to each of the phases in their corresponding FTIR spectrum. Correlation coefficients, R2, of 0.82, 0.87, and 0.86 were obtained for maghemite–magnetite, hematite–magnetite, and hematite–maghemite systems, respectively. The calibration curves generated were used to quantify phases in multi-component unknown field samples that were obtained from different components (moisture separators, condensers, and high- and low- pressure heaters) of the two units (units 1 and 2) of the secondary cycle of the Comanche Peak PWR.