This research explain the study about compound of 5,11,17,26,27,arene (TBCA) that will be used as adsorption material for heavy metal cations. Adsorption using immersion method with variations such as the value of acidity (pH), time of exposure and initial concentration of metal cations have been conducted. The results of each investigation showed that the optimum pH of adsorption was at pH = 5 for metal cations of Pb(II) and Fe (III). The observation results showed the optimum time exposure of cation adsorption of Pb(II) and Fe(III) was 90 minutes. Study about kinetic adsorption of Pb(II) metal cations of the adsorbent refered the Ho kinetic model, pseudo second order with rate constant of adsorption 143x10 -3 g.mol -1 .min -1 and Fe(III) refered the Lagergren kinetics model, pseudo first order with the rate constant of 9.21 x 10 -3 min -1 . The observation of the study showed that the isotherms adsorption for metal cations of Pb(II) and Fe(III) refered the pattern trend of Langmuir isotherm models. The value of the optimum capacity for metal cation adsorption Pb(II) and Fe(III) each was 128.46 mg/g and 156.09 mg/g respectively. Adsorption energy for Pb(II) and Fe(III) was 5.81 k.J/mol and 7.01 kJ / mol, respectively. …………………………………………………………………………………………………….... Introduction:-The existence of the metal cations can endanger human health as heavy metals if enter into the body, because the heavy metals are toxic/poison. Heavy metals are chemical elements with a specific gravity greater than 5 g/cm 3 that located in the lower right corner of the periodic table system. Iron or Ferrum (Fe) is a silvery-white metal, clay, and can be formed. It has been conducted a study of adsorption of metal cations Fe(III) in aqueous systems using zeolite, in the determination of adsorption of metal cations Fe +3 performed at pH area between 1-6 [1]. Lead was widely used in the paint factory, fuel, battery industry and ammunition bullets. Lead is toxic which very influenced toward children, because the paint is widely used in residences. If the metal contains in the blood up to 10 mg/mL, it can cause illness symtoms and Pb(II) concentrations in the water does not depend on the season, but on the depth. Lead ions contained in the water can get into the body of the fish and other aquatic animals [2]. Siswanta research resulted that the adsorbent Calix[4]resorcinarene, hybrid or Calix[4]resorcinarene-chitosan and chitosan can be applied to eliminate the Pb(II) metal ions. The results of the investigation explained that the value of adsorption capacity was Calix[4]resorcinaren > Chitosan > Calix [4] resorcinarene-chitosan (hybrid) [3]. Prabawati, reported that it can be synthesized compounds of p-t.butyl-37-monoallyloxy-38,39,40,41,42-pentahidroxycalix[6]arene and p-t.butyl-