The objectives of this study are to determine the most significant parameters of Johor River Basin which contribute to river pollution loading and to discover the potential contamination of pollutants and perform the process capability of water quality. The environmetric techniques and statistical process control have been utilize in this study. PCA extracted eight principal components which explaining 77% of total variance. The APCS-MLR model has revealed NH3-N and PO4 as the main parameter which are main pollutants that give highest contribution towards the river. The control charts have been established for NH3-N and PO4 by using SPC to monitor the level of concentration in a timely manner. Thus, continuous monitoring in the area should be done for better improvement of river quality in the Johor River Basin.