Calcium fructoborate solid materials of formula Ca(C6H10O6BO)2 ·3.5H2O were prepared by chemical wet technique. The neutral trigonal form of boron organic ester with fructose, under the solid form, is prepared and modified in solution in the anionic tetrahedral form; the borate compound is investigated by XRD spectroscopy. An ideal strong amorphous forming material is obtained upon modification with ZnCO3 or CaCO3. 11B NMR solids and solution and Raman spectroscopy were developed to determine different types and the amount of borate derivative present in products. The modifier portion from calcium carbonate and fructose are consumed for boron transformation from three to four coordinated units. Raman spectra of pure B2O3 confirm the presence of the borate boroxol ring as the main structural units. But different borate units are formed upon modification by calcium carbonate and fructose. Modification by ZnCO3 had a few effects on boron transformation. The chemical shift of 11 B NMR spectra is remaining unchanged upon its addition.