Surface water is used for a variety of purposes, including agriculture, drinking water, and other services. Therefore, its quality is crucial for irrigation, human welfare, and health. Thus, the main objective is to improve surface water quality assessment and geochemical analysis to evaluate anthropogenic activities’ impact on surface water quality in the Oued Laou watershed, Northern Morocco. Thirteen surface water samples were characterized for 26 physicochemical and biological parameters. In this aspect, emerging techniques such as multivariate statistical approaches (MSA), water quality indices (WQI), irrigation water quality (IWQI), and Geographic Information System (GIS) were employed to identify the sources of surface water pollution, their suitability for consumption, and the distribution of surface water quality. The results showed that the major ion concentrations were reported in the following order: Ca2+, Na+, Mg2+, and K+; and HCO3− > CO32− > Cl− > SO42− > NO3− > F− > PO43− > NO2−. It was also demonstrated that almost all parameters had concentrations lower than World Health Organization (WHO) limits, except for bicarbonate ions (HCO3−) and the biochemical oxygen demand for five days (BOD5), which exceeded the WHO limits at 120 mg/L and 3 mg/L, respectively. Furthermore, the types of Ca2+-HCO3− (Calcium-Bicarbonate) and Ca2+-Mg2+-HCO3− (Calcium-Magnesium-Bicarbonate) predominated in surface water. The Principal Component Analysis (PCA) indicates that the Oued Laou river was exposed to two forms of contamination, the first being attributed to anthropogenic activities such as agriculture, while the second reflects the water-sediment interaction. The Hierarchical Cluster Analysis (HCA), reflecting the mineralization in the study area, has classified the samples into four clusters. The Inverse Distance Weighting (IDW) of the WQI indicates that 7.69% and 38.46% of the surface water represent, respectively, excellent and good quality for drinking. At the same time, the IWQI revealed that 92.30% of the water surface is good for irrigation. As a result, the combination of WQIs, PCA, IWQI, and GIS techniques is effective in providing clear information for assessing the suitability of surface water for drinking and its controlling factors and can also support decision-making in susceptible locations such as the Oued Laou river in northern Morocco. © 2022 by the authors.