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This study focuses on the feasibility of a spectroscopic multivariate method for monitoring the concentration of phenol and its main degradation products during heterogeneous photocatalysis. Phenolic compounds were chosen as model to evaluate the degradation process due to their toxicity and persistence in the environment and also their well-known degradation pathway. The predictive capability of the multivariate method developed by partial least squares regression (PLSR) over the spectral range of 200-350 nm was satisfactory, allowing mean predicted errors below 5.0 % in the simultaneous determination of the target compounds using six latent variables and smoothing spectra. Suitable results were reported for the simultaneous determination of hydroquinone, resorcinol, pyrocatechol, and p-benzoquinone in accordance to the chromatographic method. Characteristics such as simplicity, low cost, and fast data acquisition are remarkable in this procedure, which makes it appropriate for this type of analytical control.

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