Flow injection on-line minicolumn preconcentration and determination of trace copper ions using an alumina/titanium oxide grafted silica matrix and FAAS
We describe the analytical performance of a hybrid material composed of SiO2, Al2O3 and TiO2. It was prepared by a sol–gel process and can act as an adsorbent in the continuous-flow enrichment of copper. A minicolumn was packed with the material, copper ions are adsorbed at pH 9.13, then eluted with 1.0 mol L−1 nitric acid, and determined by FAAS. The material was characterized by infrared spectroscopy, scanning electron and energy dispersive spectroscopy, energy dispersive X-ray fluorescence analysis, powder X-ray diffraction, and specific surface area analysis. No significant interference was observed for most ions in up to copper/interferent ratios of 1:100 and of 1:500 in case of Ca(II), Ba(II), and Mg(II). The breakthrough capacity is 1.4 mg g−1 under dynamic conditions. The limits of detection and of quantification are 0.50 and 1.4 μg L−1, respectively, and the calibration plot is linear in the range from 5.0 to 245.0 μg L−1 (r = 0.999). The relative standard deviation is 3.20 (for n = 7 and at a Cu(II) concentration of 10 μg L−1). The method was applied to the determination of trace copper ions in water, vegetable and alcohol fuel samples.
KeywordsPreconcentration Copper Silica/Alumina/Titanium Doehlert design Water Alcohol fuel
The authors would like to thank the CNPq (Conselho Nacional de Desenvolvimento Científico e Tecnológico), the CAPES (Coordenação de Aperfeiçoamento de Pessoal de Nível Superior), the FAPERJ (Fundação Carlos Chagas Filho de Amparo à Pesquisa do Estado do Rio de Janeiro), the UFRJ (Universidade Federal do Rio de Janeiro), the Parana Araucaria Foundation (Fundação Araucária do Paraná), the FAEPE-UEL, and the INCT for Bioanalytics (Instituto Nacional de Ciência e Tecnologia de Bioanalítica) for their financial support and fellowships.
- 1.Escudero LA, Cerutti S, Olsina RA, Salonia JA, Gasquez J (2010) Factorial Design of experimental variables in the on-line separation/preconcentration of copper in water samples using solid phase extraction and ICP-OES determination. J Hazard Mater 183:218–223. doi: 10.1016/j.jhazmat.2010.07.014 CrossRefGoogle Scholar
- 3.CONAMA (2005) National Council for the Environment. Resolution Number 357, March, 17. http://www.mma.gov.br/port/conama/legiabre.cfm?codlegi=459.Accessed 03 December 2011
- 6.Chamjangali MA, Bagherian G, Mokhlesian A, Bahramian B (2011) Synthesis and application of chloromethylated polystyrene modified with 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new sorbent for the on-line preconcentration and determination of copper in water, soil, and food samples by FAAS. J Hazard Mater 192:1641–1649. doi: 10.1016/j.jhazmat.2011.06.093 CrossRefGoogle Scholar
- 14.Cui Y, Chang X, Zhu X, Luo H, Hu Z, Zou X, He Q (2007) Chemically modified silica gel with p-dimethylaminobenzaldehyde for selective solid-phase extraction and preconcentration of Cr(III), Cu(II), Ni(II), Pb(II) and Zn(II) by ICP-OES. Microchem J 87:20–26. doi: 10.1016/j.microc.2007.04.004 CrossRefGoogle Scholar
- 17.Zheng H, Gao X, Song L, Guo H, Yang S, Chang X (2011) Preconcentration of trace aluminum (III) ion using a nanometer-sized TiO2-silica composite modified with 4-aminophenylarsonic acid, and its determination by ICP-OES. Microchim Acta 175:225–231. doi: 10.1007/s00604-011-0667-3 CrossRefGoogle Scholar
- 18.Tarley CRT, Ávila TC, Segatelli MG, Lima GF, Peregrino GS, Scheeren CW, Dias SLP, Ribeiro ES (2010) Silica-Alumina-Niobia (SiO2/Al2O3/Nb2O5) matrix obtained by the sol–gel processing method: new material for on-line extraction of zinc ions. J Braz Chem Soc 21:1106–1116. doi: org/10.1590/S0103-50532010000600021 CrossRefGoogle Scholar
- 21.Oliveira FM, Somera BF, Corazza MZ, Yabe MJS, Segatelli MG, Ribeiro ES, Lima EC, Dias SLP, Tarley CRT (2011) Cellulose microfiber functionalized with N,N_-bis (2-aminoethyl)-1,2-ethanediamine as a solid sorbent for the fast preconcentration of Cd(II) in flow system analysis. Talanta 85:2417–2424. doi: 10.1016/j.talanta.2011.07.088 CrossRefGoogle Scholar
- 29.Fang Z (1993) Flow injection separation and preconcentration. VCH, Weinheim, GermanyGoogle Scholar
- 30.Saraçoglu S, Elçi L (2002) Column solid-phase extraction with Chromosorb-102 resin and determination of trace elements in water and sediment samples by flame atomic absorption spectrometry. Anal Chim Acta 452:77–83. doi:http://dx.doi.org/10.1016/S0003-2670(01)01425-8
- 32.Nie R, Chang X, He Q, Hu Z, Li Z (2009) Preparation of p-tert[(dimethylamino)methyl]-calixarene functionalized aminopropylpolysiloxane resin for selective solid-phase extraction and preconcentration of metal ions. J Hazard Mater 169:203–209. doi: 10.1016/j.jhazmat.2009.03.084 CrossRefGoogle Scholar
- 34.Lima GF, Souza PMJ, Segatelli MG, Luccas PO, Tarley CRT (2010) Spectrophotometric flow-injection system using multiwalled carbon nanotubes as solid preconcentrator for copper monitoring in water samples. In: Environanotechnology, 1rd edn. Elsevier, pp 177–198Google Scholar
- 35.Brazil (Agência Nacional do Petróleo): Portaria no.2 of January 16, 2002Google Scholar