The synthesis and application of silver nanoparticles are increasingly becoming attractive. Hence, a critical examination of the various factors needed for the synthesis of silver nanoparticles as well as the characterization is imperative. In light of this, we addressed in this chapter, the nitty-gritty on the operational parameters (factors) and characterization relevant to synthesis of silver nanoparticle. The following characterization protocols were discussed in the context of silver nanoparticle synthesis. These protocols include spectroscopic techniques such as ultraviolet visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), X-ray fluorescence (XRF), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS).