A mass production of nitrate type Mg/Al layered double hydroxide was examined by co-precipitation from solution by the titration of concentrated solution of metal salts with ammonium hydroxide under ambient atmosphere. The influence of the suspension pH and post precipitation aging on the products was studied. Over five grams of single-phase nitrate type Mg/Al layered double hydroxide was obtained from a hundred-milliliter suspension (initial concentration of metal salt solution of 1.6 M), which corresponded to 97% yield from the metal ion consumption. Well-defined platy particles of nitrate type Mg/Al layered double hydroxide nanoparticles were obtained by applying post precipitation aging at 80 °C under ambient atmosphere. The sample preparation has been carried out without any caution to remove carbonate contamination to obtain nitrate type Mg/Al layered double hydroxide.