A new glycylcalix[6]arene is synthesized by the reaction of glycine ethyl ester hydrochloride with acid chloride of p-carboxycalix[6]arene. Its physical properties, void volume, density, swelling, cation exchange capacity and t(1/2) have been determined. The glycylcalix[6]arene is used as resin and its metal ion exchange capacities are determined. Mn(II), Fe(II), Co(II), Cu(II), Ni(II) and Zn(II) were absorbed at 5.5, 4.5, 6.0, 4.0, 4.8 and 5.0 pH, respectively. These were eluted with NaF, H2SO4, acetic acid, tartrate and HCl. The chromatographic separation of Mn(II), Fe(II) Co(II), Ni(II), Cu(II) and Zn(II) from each other was studied. These metals were preconcentrated on resin and determined in blood plasma and in the environment samples.