Multielement Solid Phase Preconcentration Using a Chelating Resin of Styrene Divinylbenzene Copolymer and Application for the Analysis of Seawater and Fish Otoliths by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

Abstract

A new chelating resin was synthesized by immobilizing 4–(2–thiazolylazo) resorcinol (TAR) on to a styrene divinylbenzene copolymer. This material was examined for on-line solid phase extraction/preconcentration of Cd, Co, Cu, Ni, Pb, and Zn in seawater and fish otoliths for determination by inductively plasma mass spectrometry (ICP-MS). A volume of 5.0 mL sample solution was loaded on to a mini-column of the resin at 2.0 mL min⁻¹ via a sequential injection system. The optimum pH for multielement preconcentration was around pH 5.5. Recoveries were better than 96% in artificial seawater. Elution was achieved with 1.0 mL of 0.75 mol L⁻¹ HNO₃. The resin possesses a large sorption capacity ranging from 82.0 µmol g⁻¹ for Pb to 319 µmol g⁻¹ for Cu. The detection limits (3σ) varied between 0.0016 µg L⁻¹ (Cd) and 0.015 µg L⁻¹ (Zn) for preconcentration of 5.0 mL blank solutions (pH 5.5). Relative standard deviation for three replicate runs was between 0.3% (Cd) and 6% (Zn) at the 1.0 µg L⁻¹ level. The procedure was validated by analysis of a nearshore seawater and a fish otoliths certified reference material, and employed for coastal seawater and estuarine water samples.

Keywords:

• Fish otolith
• ICP-MS
• Immobilized resin
• Seawater
• Solid phase extraction

Acknowledgments

This project was supported by grants from the National Center for Research Resources (5 G12 RR013459–15), the National Institute on Minority Health and Health Disparities (8 G12 MD007581–15), and the Research Initiative for Scientific Enhancement (2 R25 GM067122) from the National Institutes of Health. The views expressed herein are those of authors and do not necessarily represent the official views of the NIH and any of its sub-agencies. The authors also acknowledge financial support from the Turkish Higher Education Council to Dr. Vedat Yilmaz during the course of this project.

Notes

Note: Values are given as average ± standard deviation for given replicate analyses.

Note: Values are given as average ± standard deviation for five replicate analyses (n = 5).

^a Yoshinaga et al. (2000).

^b Arslan and Paulson (2002).

^c Yoshinaga et al. (1999).