Abstract. This research objectives to study post treatment on Ca-Mg-Al-Layered Double Hydroxide (Ca-Mg-Al-LDH) slurry which was prepared from brine water by cooling treatment. The cooling rate was varied from 1 to 3 °C/min by using stirring and without stirring, and the cooling time was done at 0, 30 minutes and 24 hours. The quantitative X-ray diffraction (QXRD) was employed on Ca-Mg-Al-LDH using Le Bail refinement method. The refinement results found another Mg-Al-LDH and Ca-Al-LDH phases, such as Mg(OH) 2 , Al(OH) 3 and CaCO 3 . The highest phase composition on material Ca-Mg-Al-LDH using Le Bail refinement was showed by Al(OH) 3 .