A series of Layered Double Hydroxides (LDHs) - Hydrotalcite with varying ratio of Mg/Al (2,3,4) were prepared by the co-precipitation method with the solution of Mg2+ and Al3+ in the medium containing different anions (CO3- and NO3-) and synthesis conditions (aqueous ammonium solution or sodium hydroxide to control pH of the reaction) followed by the calcinations at different temperature (350-550°C). The samples were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and infi'ared spectroscopy (FTIR). The XRD patterns shown that pure Hydrotalcite phase were obtained for all samples and layered structure is still maintained up to 350°C. However further heating at higher temperature the collapse of the layered structure was taken. The effect of the intercalated anion (NO3, CO3) and Mg/Al ratio on the structural and textural properties have been investigated. It was shown that the nitrate form Hydrotalcite MgAl-NO) has higher basal spacing compared with the carbonate form about 0.5 Aat the same Mg/Al ratio. The crystalline size calculated by Sheerer's equation for all prepared samples was below 10 mn. The particle sheet size of Hydrotalcite with carbonate intercalated anion was smaller than that of nitrate anion. The PZC of the obtained Hydrotalcite has mainly similar value (10-11) for the both form at the same Mg/Al ratio. This is indicated that the synthesis condition and nature of intercalate anion NO3 and CO3 have no significant effect on PZC. The lower Mg/Al ratio the higher value of PZC. The calcined hydrotalcite can be restructured easy in the anionic solution.