Linear alkyl sulfonates (LAS) constitute a large fraction of the surfactants used in cleaning processes in households, trade and industry Despite the industrial significance and the possible environmental impact of these compounds, the fast and inexpensive determination of LAS concentrations is still a difficult task. In this study, near infrared (NIR) spectroscopy which is a rapid spectroscopic analysis method compared with a traditional analytical method for the measurement of LAS concentration such as HPLC, GC and standard wet chemistry method. NIR spectra of LAS between 0.313 and 25.0% (w/v) in water were utilized to develop a calibration model. The best results (R ＝ 0.998, SEP ＝ 0.244% (w/v)) obtained by using partial least-squares regression with spectral data treatment and 2nd derivatization were comparable to the results (SEC ＝ 0.186% (w/v), SEP ＝ 0.206% (w/v)) obtained by using multiple linear least-squares regression (MLR). However, models based on derivative spectra have no significant advantage with MLR.