We examined the use of near infrared (NIR) spectroscopy as a rapid technique for the evaluation of sewage quality. Influent water samples, primary sedimentation tank water samples, and final effluent water samples were collected from sewage treatment facilities in Nagoya, Japan and their NIR spectra obtained. Partial least squares (PLS) models for total phosphate (TP), total nitrogen (TN), biochemical oxygen demand (BOD), total organic carbon (TOC), and turbidity of sewage water were constructed from the NIR data. The models provided good correlation between measurements obtained conventionally and those predicted from spectroscopy. Spectral variation induced by background interference in samples affected accuracy. Loading plots and score plots derived from PLS regression analysis resolved the background interference and allowed highly accurate predictions. Spectral variation induced by contamination in the sewage was a main predictor of sewage quality. These results show that NIR spectroscopy shows potential for in-line, non-destructive measurement of sewage quality.