A general formula of hydrotalcite like Mg-Al layered double hydroxide (LDH) is expressed as [Mg1-x2+Alx3+ (OH) 2] x+ [Anx/nn-] ·yH2O. An oxidative decomposition method of EDTA-Metal chelate with hydrogen peroxide was investigated in order to prepare LDH. Effects of H2O2 concentrations and Mg/Al mole ratio (R1) in the reaction solution on the Mg/Al mole ratio (Rs) in LDH were investigated to find an optimum synthesis conditions. LDH was successfully obtained by allowing to react the solution with R1=6 and pH = 10 for 6 h. The Rs values were influenced with the R1 value. The Rs values were the range of 1.4-2.3. The (003) basal spacing of the products was spread to the range of 0.758 nm to 0.770 nm with increasing Rs The (003) basal spacing of the ethylene glycol-intercarated LDH was 1.36-1.40 nm. However, it spread only to 0.78 nm on the Rs value being 2.3.