title: Solid phase extractive preconcentration of trace metals using p-tert-butylcalix[4]arene-1,2-crown-4-anchored chloromethylated polymeric resin beads.
abstract: 5,11,17,23-Tetrakis(1,1-dimethylethyl)-25,26-dihydroxy-27,28-crown-4-calix[4]arene in the cone conformation was synthesized. This p-tert-butylcalix[4]arene-1,2-crown-4 compound was then anchored with Merrifield chloromethylated resin beads. The modified polymeric resin was characterized by (1)H NMR, FT-IR and elemental analysis and used successfully for the separation and preconcentration of Cu(II), Cd(II), Co(II), Ni(II) and Zn(II) prior to their determination by FAAS. Effective extraction conditions were optimized in both batch and column methods. The resin exhibits good separating ability with maximum between pH 6.0-7.0 for Cu(II), pH 6.0 for Cd(II), pH 5.0 for Co(II), pH 4.0-4.5 for Ni(II), and pH 4.5 for Zn(II). The elution studies were carried out with 0.5 mol L(-1) HCl for Cu(II), Co(II) and Co(II), 1.0 mol L(-1) HCl for Cd(II) and Zn(II). The sorption capacity, preconcentration factor and distribution coefficient of each metal ion were determined. The detection limits were 1.10, 1.25, 1.83, 1.68 and 2.01 microg L(-1) for Cu(II), Cd(II), Co(II), Ni(II) and Zn(II). The influence of several ions on the resin performance was also investigated. The validity of the proposed method was checked for these metal ions in NIST standard reference material 2709 (San Joaquin Soil) and 2711 (Montana Soil).
authors: Dokuz Eylul University, Faculty of Science and Arts, Chemistry Department, 35160 Izmir, Turkey.
authors: Serap
authors: S
authors: Seyhan
authors: Mehmet
authors: M
authors: Colak
authors: Melek
authors: M
authors: Merdivan
authors: Nadir
authors: N
authors: Demirel
mesh_terms: D000327:Adsorption; D047250:Calixarenes / Q000737:chemistry*; D043844:Crown Ethers / Q000737:chemistry*; D006851:Hydrochloric Acid / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D007700:Kinetics; D019216:Metals, Heavy / Q000032:analysis / Q000737:chemistry*; D017942:Nitric Acid / Q000737:chemistry; D012117:Resins, Synthetic / Q000138:chemical synthesis* / Q000737:chemistry; D052616:Solid Phase Extraction
chemical_list: C519380:5,11,17,23-tetrakis(1,1-dimethylethyl)-25,26-bis(3-hydroxy-2-oxopropoxy)-27,28-crown-4-calix(4)arene; D043844:Crown Ethers; D019216:Metals, Heavy; D012117:Resins, Synthetic; D047250:Calixarenes; D017942:Nitric Acid; D006851:Hydrochloric Acid