The thermal decompositions of dicitratoborates MI[B(CtHtO7),].nH20 (n=0-2, M' = Rb, K, Li, Nit,,) and MUlB(CtHtO7)z]z .8H20 (M II = Co, Ni, Mn, Cu, Zn, Cd) were investigated by means of TG, DTA and DTG methods. It was found that these thermal decompositions involve three successive stages: dehydration, the endothermal decomposition of the ligand, and oxidation of the residual ~ganic component. The volatile products of decomposition in each stage were detected by means of gas chromatography. The method of TGcurve transformation into the curve dm/d Tvs. m, where m is the loss of weight at each moment of time, was used for a more detailed study of dehydration. The optimal conditions for TG-curve modification were found.The dicitratoborates M~[B(C6H6OT)z].nH20, where n = 0-2, and M ~ = Li, K, NH4, Rb, and Mn[B(C6H6OT)212 9 8H20, where M n = Zn, Cd, Co, Mn, Cu were synthesized earlier [1][2][3]. The complex anion was found to be: