Polymer free calix[4]arene nanofibers were prepared via new electrospinning method with metal ion adsorption capacity. Two different calix[4]arene derivatives (compound 2 and 3) containing amide functionalities were used in this study, which were fully characterized by HNMR, FTIR and elemental analysis. Calix[4]arene nanofibers were analyzed with different surface characterization techniques such as SEM, TEM and AFM. SEM images of compound 2 and 3 nanofibers reveals there are non-bonded randomly grown fibers with average fiber diameter (AFD) was in the range of 237 to 307 nm for compoud 2 and 203–280 nm for compound. Adsorption study show the SEM-EDX mapping show adsorption of different metal ions (Hg+2, Pb+2, Cu+2, Co+2, Cd+2, Ni+2) on nanofibers. The the adsorption study show Hg+2, Pb+2 and Cu+2 adsorbed on nanofibers particularly at high pH. The maximum adsorption (98 %) was observed at pH 2 for Hg+2.