title: Enrichment of iron(III), cobalt(II), nickel(II), and copper(II) by solid-phase extraction with 1,8-dihydroxyanthraquinone anchored to silica gel before their determination by flame atomic absorption spectrometry.
abstract: A chelating matrix prepared by immobilizing 1,8-dihydroxyanthraquinone on silica gel modified with 3-aminopropyltriethoxysilane has been characterized by use of cross-polarization magic angle spinning (CPMAS) NMR, diffuse reflectance infrared Fourier transformation (DRIFT) spectroscopy, and thermogravimetric analysis and used to preconcentrate Fe(III), Co(II), Ni(II), and Cu(II) before their determination by flame atomic absorption spectrometry. The optimum pH ranges for quantitative sorption are 6.5-8.0, 6.0-7.0, 6.0-8.0, and 7.0-8.5 for Cu, Fe, Co, and Ni, respectively. All the metal ions can be desorbed with 2 mol L(-1) HCl or HNO3. The sorption capacity ( micromol g(-1) matrix) and preconcentration factor were 226.6, 250; 365.6, 300; 101.8, 150; and 109.0, 250 for Cu, Fe, Co, and Ni, respectively. The lowest concentration for quantitative recovery was 4.0, 3.3, 6.6, and 4.0 ng mL(-1), respectively for the four metal ions. The limits up to which electrolytes NaNO3, NaCl, NaBr, Na2SO4, and Na3PO4 and cations Ca(II) and Mg(II) can coexist with the four metal ions during their sorption without adverse effect are reported. The simultaneous enrichment and determination of all the four metals is possible if the total load of metal ions is less than the sorption capacity. Flame AAS was used to determine the metal ions in underground, tap, and river water samples (RSD<or=7.1%) after their enrichment with the matrix. The cobalt content of pharmaceutical samples (multivitamin tablet) preconcentrated by use of this silica gel matrix and determined by FAAS was found to be 2.00 microg g(-1), with RSDtilde;1.7% (reported concentration level, 1.99 microg g(-1)).
authors.affiliation: Department of Chemistry, Indian Institute of Technology, New Delhi 110016, India.
authors.forename: Anupama
authors.initials: A
authors.lastname: Goswami
authors.forename: Ajai K
authors.initials: AK
authors.lastname: Singh
mesh_terms: D000880:Anthraquinones / Q000737:chemistry; D002413:Cations, Divalent; D002614:Chelating Agents / Q000737:chemistry; D002850:Chromatography, Gel; D003035:Cobalt / Q000032:analysis*; D003300:Copper / Q000032:analysis*; D005290:Ferric Compounds / Q000032:analysis*; D009532:Nickel / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000032:analysis; D058428:Silica Gel; D012822:Silicon Dioxide / Q000737:chemistry; D013054:Spectrophotometry, Atomic / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D000880:Anthraquinones; D002413:Cations, Divalent; D002614:Chelating Agents; D005290:Ferric Compounds; D004364:Pharmaceutical Preparations; D014874:Water Pollutants, Chemical; D003035:Cobalt; D058428:Silica Gel; D012822:Silicon Dioxide; D003300:Copper; D009532:Nickel; C004315:danthron