Abstract
2,6-Pyridine dicarboxylic acid was immobilized on the surface of nanometer-sized silica to prepare a new solid phase extractant which was applied to extract and preconcentrate trace mercury(II) from aqueous solutions prior to the determination by inductively coupled plasma atomic emission spectrometry. The optimization of some analytical parameters affecting the recovery of the analyte such as acidity, shaking time, eluent condition, sample volume, sample flow rate, and influence of potentially interfering ions were investigated. At pH 3, the maximum uptake capacity for mercury(II) was found to be 92 mg g−1. Quantitative recovery (≥95%) of mercury (II) was achieved by stripping with 2 mL of 0.1 mol L−1 hydrochloric acid and 3% thiourea. The presence of several metal cations and anions, some of them in high excess, did not interfere with the separation of mercury (II) under optimal conditions. An enrichment factor of 175 and a relative standard deviation less than 3.0% (n = 8) were obtained for mercury(II) determinations. The detection limit (3σ) was 0.09 ng mL−1. The method has been validated using certified reference materials (GBW 08303 and GBW 08301), and was applied to the determination of trace mercury(II) in environmental and biological samples with satisfactory results.
Similar content being viewed by others
References
Fang GZ, Tan J, Yan XP (2005) An ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique combined with a sol-gel process for selective solid-phase extraction of cadmium(II). Anal Chem 77:1734
Ray AB, Selvakumar A (2000) Laboratory studies on the remediation of mercury contaminated soils. Remed J 10:49
Yang D, Chang XJ, Liu YW, Wang S (2004) Synthesis and efficiency of a spherical macroporous epoxypolyamide chelating resin for preconcentrating and separating trace noble metal ions. Microchim Acta 147:219
Liu YW, Chang XJ, Wang S, Guo Y, Din BJ, Meng SM (2004) Solid-phase extraction and preconcentration of cadmium(II) in aqueous solution with Cd(II)-imprinted resin (poly-Cd(II)-DAAB-VP) packed columns. Anal Chim Acta 519:173
Sun YC, Mierzwa J, Lan CR (2000) Direct determination of molybdenum in seawater by adsorption cathodic stripping square-wave voltammetry. Talanta 52:417
Himeno S, Kitano E, Kanaya M, Takamoto M (2007) Simultaneous capillary electrophoretic determination of Sc(III) and Y(III) based on the complex-formation with a lacunary Keggin-type [PW11O39]7−complex. Talanta 71:822
Minowa H, Ebihara M (2003) Separation of rare earth elements from scandium by extraction chromatography: application to radiochemical neutron activation analysis for trace rare earth elements in geological samples. Anal Chim Acta 498:25
He Q, Chang XJ, Huang XP, Hu Z (2008) Determination of trace elements in food samples by ICP-AES after preconcentration with p-toluenesulfonylamide immobilized on silica gel and nanometer SiO2. Microchim Acta 160:147
Zhang LJ, Chang XJ, Zhai YH, He Q, Huang XP, Hu Z, Jiang N (2008) Selective solid phase extraction of trace Sc(III) from environmental samples using silica gel modified with 4-(2-morinyldiazenyl)-N-(3-(trimethylsilyl)propyl)benzamide. Anal Chim Acta 629:84
Zhai YH, Liu YW, Chang XJ, Chen SB, Huang XP (2007) Selective solid-phase extraction of trace cadmium(II) with an ionic imprinted polymer prepared from a dual-ligand monomer. Anal Chim Acta 593:123
Zhang LJ, Zhai YH, Chang XJ, He Q, Huang XP, Hu Z (2009) Determination of trace metals in natural samples by ICP-OES after preconcentration on modified silica gel and on modified silica nanoparticles. Microchim Acta 165:319
Lian N, Chang XJ, Zheng H, Wang S, Cui YM, Zhai YH (2005) Application of dithizone-modified TiO2 nanoparticles in the preconcentration of trace chromium and lead from sample solution and determination by inductively coupled plasma atomic emission spectrometry. Microchim Acta 151:81
Cui YM, Chang XJ, Zhu XB, Jiang N, Hu Z, Lian N (2007) Nanometer SiO2 modified with 5-sulfosalicylic acid as selective solid-phase extractant for Fe(III) determination by ICP-AES from biological and natural water samples. Microchemical J 86:23
Zhu XB, Yang D, Chang XJ, Cui YM, Hu Z, Zou XJ (2008) Selective solid-phase extraction of trace Fe(III) from biological and natural water samples using nanometer SiO2 modified with acetylsalicylic acid. Microchim Acta 161:115
Sun DX (2007) Preparation and token of nano-silica. Nanoscience & Nanotechnology 3:35 Chinese
Guo Y, Din BJ, Liu YW, Chang XJ, Meng SM, Liu JH (2004) Preconcentration and determination of trace elements with 2-aminoacetylthiophenol functionalized amberlite XAD-2 by inductively coupled plasma-atomic emission spectrometry. Talanta 62:209
Miranda CES, Reis BF, Baccan N, Packer AP, Giné MF (2002) Automated flow analysis system based on multicommutation for Cd, Ni and Pb on-line pre-concentration in a cationic exchange resin with determination by inductively coupled plasma atomic emission spectrometry. Anal Chim Acta 453:301
Chang XJ, Jiang N, Zheng H, He Q, Li ZH, Zhai YH, Cui YM (2007) Solid-phase extraction of iron(III) with an ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique. Talanta 71:38
Shen XQ, Yao HC, Yang R, Li ZJ, Zhang HY (2008) Synthesis, structure and thermal properties of polynuclear complexes with a new multidentate ligand, N, N′-bis(5-ethyl-1, 3, 4-thiadiazol-2-yl)-2, 6-pyridinedicarboxamide. Polyhedron 27:203
Dev K, Rao GN (1995) Preparation and analytical properties of a chelating resin containing bicine groups. Talanta 42:591
Jiang HM, Hu B, Jiang ZC, Qin YC (2006) Microcolumn packed with YPA4 chelating resin on-line separation/preconcentration combined with graphite furnace atomic absorption spectrometry using Pd as a permanent modifier for the determination of trace mercury in water samples. Talanta 70:7
Zhai YH, Chang XJ, Cui YM, Lian N, Lai SJ, Zheng H, He Q (2006) Selective determination of trace mercury(II) after preconcentration with 4-(2-pyridylazo) resorcinol-modified nanometer-sized SiO2 particles from sample solutions. Microchim Acta 154:253
Mahmoud ME, Osman MM, Amer ME (2000) Selective pre-concentration and solid phase extraction of mercury(II) from natural water by silica gel-loaded dithizone phases. Anal Chim Acta 415:33
Dakova I, Karadjova I, Georgieva V, Georgiev G (2009) Ion-imprinted polymethacrylic microbeads as new sorbent for preconcentration and speciation of mercury. Talanta 78:523
Huang CZ, Hu B (2008) Silica-coated magnetic nanoparticles modified with γ-mercaptopropyltrimethoxysilane for fast and selective solid phase extraction of trace amounts of Cd, Cu, Hg, and Pb in environmental and biological samples prior to their determination by inductively coupled plasma mass spectrometry. Spectrochim Acta, Part B 63:437
Li ZH, Chang XJ, Zou XJ, Zhu XB, Nie R, Hu Z, Li RJ (2009) Chemically-modified activated carbon with ethylenediamine for selective solid-phase extraction and preconcentration of metal ions. Anal Chim Acta 632:272
Author information
Authors and Affiliations
Corresponding author
Electronic supplementary material
Below is the link to the electronic supplementary material.
ESM 1
(DOC 38066 kb)
Rights and permissions
About this article
Cite this article
Zhang, L., Chang, X., Hu, Z. et al. Selective solid phase extraction and preconcentration of mercury(II) from environmental and biological samples using nanometer silica functionalized by 2,6-pyridine dicarboxylic acid. Microchim Acta 168, 79–85 (2010). https://doi.org/10.1007/s00604-009-0261-0
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00604-009-0261-0