A novel method of preparing AgCl nanoparticles by mixing AgCl powder and a microemulsion consisting of dioctyldimethylammonium chloride/n-decanol/water/isooctane is introduced. This new method was discovered during the preparation of AgCl nanoparticles in single microemulsions by direct reaction with the dioctyldimethylammonium chloride surfactant counterion. The effect of the following variables on the concentration of the colloidal AgCl nanoparticles (the nanoparticle uptake) and the particle size were studied: (1) operating variables, including mixing and temperature; and (2) microemulsion variables, including surfactant and cosurfactant concentration, and water to surfactant mole ratio. Manipulating these variables provides an insight into the role of the surfactant surface layer rigidity on the phenomenon. The results were explained by the effect of these variables on reaction rates and the colloidal nanoparticle stability. Mixing had a significant effect on the nanoparticle uptake. At 300 rpm an equilibrium AgCl nanoparticle uptake was achieved in about 1 h, while without mixing only 5% of the equilibrium value was reached even after 24 h. An optimum temperature was found for which a maximum nanoparticle uptake was obtained. At higher temperatures, the nanoparticle uptake declined. The nanoparticle uptake increased linearly with the surfactant concentration, and the particle size increased as well. A monotonic decrease in the nanoparticle uptake accompanied by an increase in the particle size was observed when increasing n-decanol concentration or the water to surfactant mole ratio.