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In this book, silver and zinc oxide nanoparticles were synthesized in-situ within the gum acacia/poly (acrylate) hydrogel network using reduction and hydrothermal approaches respectively. The synthesized metal nanoparticles were characterized by Surface plasmon resonance (SPR), X-Ray diffraction (XRD) analysis, Fourier transform infrared (FTIR) spectroscopy Transmission electron microscopy (TEM) , Thermogravimetric analysis (TGA) and Scanning electron microscopy (SEM). The water absorption behavior of Ag and ZnO loaded GA/poly(SA) hydrogels was investigated in the phosphate buffer saline (PBS) of pH 7.4 at 37 C.The water uptake data were analyzed with the help of various kinetic models. Finally, the antimicrobial action of nanocomposites was studied using E. coli as model bacteria.