title: 2,3-Dihydroxypyridine-loaded cellulose: a new macromolecular chelator for metal enrichment prior to their determination by atomic absorption spectrometry.
abstract: New macromolecular chelators have been synthesized, by loading 2,3-dihydroxypyridine (DHP) on cellulose via linkers -NH-CH(2)-CH(2)-NH-SO(2)-C(6)H(4)-N=N- and -SO(2)-C(6)H(4)-N=N-, and characterized by elemental analysis, TGA, IR, and CPMAS (13)C NMR spectra. The cellulose with DHP anchored by the shorter linker had better sorption capacity (between 69.7 and 431.1 micromol g(-1)) for Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Pb(II), and Fe(III)) than the other (51.9-378.1 micromol g(-1)); the former was therefore studied in detail as a solid extractant for these metal ions. The optimum pH ranges for quantitative sorption (recovery 97.6-99.8%) on this matrix were: 7.0-9.0, 6.0-9.0, 3.0-8.0, 6.0-8.0, 6.0-9.0, 6.0-7.0, and 2.0-6.0 respectively. Desorption was quantitative with 0.5 mol L(-1) HCl and 0.5 mol L(-1) HNO(3) (for Pb). Simultaneous sorption (at pH 7.0) of all metal ions other than Fe(III) was possible if their total concentration did not exceed the sorption capacity (lowest value). The recovery of seven metal ions from their mixture at pH 6.0 was nearly quantitative when the concentration level of each metal ion was 0.2 microg mL(-1). The optimum flow rate of metal ion solutions for quantitative sorption of metal onto a column packed with DHP-modified cellulose was 2-7 mL min(-1), whereas for desorption the optimum flow rate for the acid solution was 2-4 mL min(-1). The time needed to reach 50% of the total loading capacity ( t(1/2)) was <5 min for all the metal ions except Ni and Pb. The limit of detection (blank+3 s) was from 0.70 to 4.75 microg L(-1) and the limit of quantification (blank+10 s) was between 0.79 and 4.86 microg L(-1). The tolerance limits for NaCl, NaBr, NaI, NaNO(3), Na(2)SO(4), Na(3)PO(4,) humic acid, EDTA, Ca(II), and Mg(II) for sorption of all metal ions are reported. The column packed with DHP-anchored cellulose can be reused at least 20 times for enrichment of metal ions in water sample. It has been used to enrich all the metal ions in pharmaceutical and water samples before their determination by flame AAS. RSD for these determinations was between 1.1 and 6.9%.
authors.affiliation: Department of Chemistry, Indian Institute of Technology, 110 016, New Delhi, 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
mesh_terms: D002412:Cations / Q000737:chemistry; D002482:Cellulose; D002614:Chelating Agents / Q000737:chemistry*; D003035:Cobalt / Q000032:analysis; D004573:Electrolytes / Q000737:chemistry; D005618:Fresh Water / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D007700:Kinetics; D015394:Molecular Structure; D004364:Pharmaceutical Preparations / Q000737:chemistry; D011725:Pyridines / Q000737:chemistry*; D013054:Spectrophotometry, Atomic / Q000379:methods*; D013997:Time Factors; D014881:Water Supply
chemical_list: D002412:Cations; D002614:Chelating Agents; D004573:Electrolytes; D004364:Pharmaceutical Preparations; D011725:Pyridines; D003035:Cobalt; C035877:2,3-dihydroxypyridine; D002482:Cellulose