The present work assesses the possibility of using spectrophotometry in the near-mid-ultraviolet and visible wavelength ranges (282–790 nm) for the direct monitoring of treatment performance in municipal wastewater treatment plants (WWTPs). Principal component analysis (PCA) was used to analyze spectral data from samples collected along three WWTP process lines with different primary and secondary treatment units. The clustering observed in PCA score plots was mainly attributed to the suspended solids fraction present in the wastewater and highlighted differences in solids quality between plants and along the treatment lines. Thus, satisfactory partial least squares (PLS) calibration models to estimate total suspended solids (TSS) values from the acquired spectra could only be established per plant. The PLS models were established using 1–2 factors, with root mean error of cross-validation and coefficient of determination values in the 50–86 mg TSS L<sup>–1</sup> and 82–95% ranges, respectively.
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