Calcium hydrogen phosphate was synthesized by reacting calcium chloride and sodium hydrogen phosphate solution in this study. It is well known that the particle size and yield o f calcium hydrogen phosphate produced is greatly affected by the synthetic conditions such as the reactant concentration, reaction temperature, reacting fine, mole ratio and drying temperature, etc. The purpose of this study is to investigate the optimum synthesis condition from the viewpoint of yield and sedimentation volume of the prepared calcium hydrogen phosphate powder according to a randomized complete block design proposed by G.E.P. Box and K.B. Wilson. It was found that the optimum synthetic conditions of calcium hydrogen phosphate were as follows: It was found that optirnum temperature range of reactant solutions was $28-38^{circ}C$ and $32-42^{circ}C$ respectively, on the viewpoint of yield and sedimentation volume. The optimum concentration range of reactant solutions was 5.5-10.0% and 6.9-7.4% respectively, on the viewpoint of yield and sedimentation volume. The optimum mole ratio of $CaCl_2$ to $Na_2HPO_4$ was in the range of 1.2-2.0 and the optimum reacting time range was 8.5-11.0 minutes. The optimum drying temperature range was $39-41^{circ}C$ from the viewpoint of yield, but it was $39-43^{circ}C$ on the basis of sedimentation volume. Crystallographic analysis to X-ray diffraction patterns of commercially available ecalcium hydrogen phosphate and calcium hydrogen phosphate samples prepared in this study suggested that all samples tested belonged to monoclinic crystal system characteristic of $CaHP0_4{cdot}2H_20$ crystals.