title: Cellulose based macromolecular chelator having pyrocatechol as an anchored ligand: synthesis and applications as metal extractant prior to their determination by flame atomic absorption spectrometry.
abstract: Pyrocatechol is immobilized on cellulose via NHCH(2)CH(2)NHSO(2)C(6)H(4)NN linker and the resulting macromolecular chelator characterized by IR, TGA, CPMAS (13)C NMR and elemental analyses. It has been used for enrichment of Cu(II), Zn(II), Fe(III), Ni(II), Co(II), Cd(II) and Pb(II) prior to their determination by flame atomic absorption spectrometry (FAAS). The pH ranges for quantitative sorption (98.0-99.4%) are 4.0-7.0, 5.0-6.0, 3.0-4.0, 5.0-7.0, 5.0-8.0, 7.0-8.0 and 4.0-5.0, respectively. The desorption was found quantitative with 0.5 mol dm(-3) HCl/HNO(3) (for Pb). The sorption capacity of the matrix for the seven metal ions has been found in the range 85.3-186.2 mumol g(-1). The optimum flow rate of metal ion solution for quantitative sorption of metal onto pyrocatechol functionalized cellulose as determined by column method, is 2-6 cm(3) min(-1), whereas for desorption it is 2-4 cm(3) min(-1). The tolerance limits for NaCl, NaBr, NaI, NaNO(3), Na(2)SO(4), Na(3)PO(4,) humic acid, EDTA, ascorbic acid, citric acid, sodium tartrate, Ca(II) and Mg(II) in the sorption of all the seven metal ions are reported. Ascorbic acid is tolerable up to 0.8 mmol dm(-3) with Cu and Pb where as sodium tartrate does not interfere up to 0.6 mmol dm(-3) with Pb. There is no interference of NaBr, NaCl and NaNO(3) up to a concentration of 0.5 mol dm(-3), in the sorption of Cu(II), Cd(II) and Fe(III) on to the chelating cellulose matrix The preconcentration factors are between 75 and 300 and t(1/2) values </=5 min for all the metal ions. Simultaneous sorption of Cu, Zn, Ni and Co is possible at pH 5.0 if their total concentration does not exceed lowest sorption capacity. The present matrix coupled with FAAS has been used to enrich and determine the seven metal ions in river and tap water samples (relative standard deviation (R.S.D.) 1.05-7.20%) and synthetic certified water sample SLRS-4 (NRC, Canada) with R.S.D. approximately 2.03%. The cobalt present in pharmaceutical vitamin tablets was also preconcentrated on the modified cellulose and determined by FAAS (R.S.D. approximately 1.87%).
authors.affiliation: Department of Chemistry, Indian Institute of Technology, Hauz Khas, New Delhi 110016, India.
authors.forename: Vibha
authors.initials: V
authors.lastname: Gurnani
authors.forename: Ajai K
authors.initials: AK
authors.lastname: Singh
authors.forename: B
authors.initials: B
authors.lastname: Venkataramani