Various techniques and approaches have been designed to synthesize precipitated calcium carbonate. We used a continuous sprayed-mist technique that induced spontaneous precipitation reaction of the droplets with the higher surface area when in contact with the gas. The effects of optimum reactant concentration, gas flow rate, and reactant feeding rate including reaction conditions were investigated. The effectiveness of the techniques was scrutinized by analyzing the resultant PCC characteristics, especially the particle phase morphology and size distribution using XRD, FTIR, and SEM. The variation of initial concentration of milk of lime with different gas flow rate was studied. Experimental results, as well as XRD and FTIR, indicated that all the products produced were favorable for the formation of calcite. SEM revealed that the morphologies of PCC were all rhombohedral and tended to adhere to each other (twinning). It was found that production of PCC by using spray-mist method is suitable for lower initial concentration of Ca(OH)2 and higher gas flow rate only.