The presented work applies mid-infrared attenuated total reflection (ATR) spectroscopy to the measurment of hydrogen peroxide in aqueous matrices. The performance of different ATR crystals mounted in flow cells was investigated in the presence of aqueous hydrogen peroxide solutions. Quantitative determination has been achieved by evaluation of specific OH stretching and deformation vibrations with linear correlation between peak areas or peak heights and hydrogen peroxide concentration in the range of 1–10% (weight in water). Important aspects such as chemical stability of the waveguide material and influences of pH and ionic strength on the performance are discussed. Feasibility for the investigation of real world samples is demonstrated by measuring industrial bleaching solutions with known concentrations of hydrogen peroxide fitting well with calibration graphs established with neat hydrogen peroxide solutions. The presented sensor system is capable of determining hydrogen peroxide within complex matrices and clearly corroborates the potential of providing an <i>in situ</i> measurement concept for on-line hydrogen peroxide detection.
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