By energy-dispersive X-ray microanalysis (EDX) in scanning electron microscopy, we studied the calcification of the inner-basic lamellas of a cow bone and the coronal cementum of a horse tooth treated with sodium hypochlorite (NaOCl). These tissues were divided into 4 groups with a combination of NaOCl treatment and polyester-resin embedding including, [A]: non-NaOCl + Resin, [B]: non-NaOCl + non-resin, [C]: NaOCl + Resin, and [D]: NaOCl + non-Resin. From the Ca and P values by EDX analysis, it was suggested that the natural porous spaces of [B] were higher than those of [A], and both the natural and NaOCl-soluble porous spaces were highest in [D]. However, [A] had the lowest porous spaces in both the tissues because the micropores formed 3-dimensionally by NaOCl treatment might be incompletely filled with the resin. The backscattered electron microscopy and the difference of the Ca/P ratios indicated that the NaOCl treatment of the calcified tissues caused some minerals besides organic materials to dissolve. Thus, the sample preparation of [B] is suitable for the quantitative EDX of calcified tissues, whereas the data of [C] except for the Ca/P ratio may be used to approximate the Ca and P contents.