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Response surface methodology (RSM) and artificial neural network (ANN) were used to generate a model for the optimization of fluoride removal using chemically activated Dalbergia sissoo sawdust (CADS). The single and collective effects of process parameters, i.e., solution pH, CADS dose, initial fluoride concentration, and contact time, were studied. The point of zero charge was found to be 4.2 with zeta potential analysis. In the first phase, a single-parameter study was performed to reveal dependency of fluoride removal on a particular