Silver as internal standard for simultaneous determination of Cd and Pb in whole blood by electrothermal atomic absorption spectrometry

Abstract

The use of internal standardization for simultaneous atomic absorption spectrometry (SIMAAS) was investigated for Cd and Pb determination in whole blood. The comparison of thermochemical and physico-chemical parameters allowed the selection of Ag, Bi, and Tl as internal standard candidates. Correlation graphs, plotted from the normalized absorbance signals (n = 20) of internal standard (axis y) versus analyte (axis x), precision and accuracy were used to select Ag as the most appropriate internal standard. Blood samples were diluted (1 + 9) with 0.11% (m/v) Triton X-100 + 1.1% (v/v) HNO₃ + 0.28% (m/v) NH₄H₂PO₄ + 10 µg L⁻¹ Ag⁺. Pyrolysis and atomization temperatures for the optimized heating program were 550 and 1700 °C, respectively. Characteristic masses based on integrated absorbance were 1.68 ± 0.01 pg for Cd and 30.3 ± 0.1 pg for Pb. The detection limits (DL) were 0.095 ± 0.001 µg L⁻¹ and 0.86 ± 0.01 µg L⁻¹ for Cd and Pb, respectively. The mean RSD for all determinations was the same for Cd (13 ± 9%) with or without Ag as internal standard (IS). On the other hand, the use of Ag as IS improved the RSD for Pb from 3.6 ± 4.0% to 2.2 ± 2.0%. An effective contribution of the internal standard Ag was verified in the recoveries of spiked samples (0.5 µg L⁻¹ Cd²⁺ and 5.0 µg L⁻¹ Pb²⁺). The mean recoveries were 81 ± 8% and 91 ± 4% for Cd, and 80 ± 11% and 93 ± 6% for Pb without and with IS correction, respectively. This is the first application of IS for a simultaneous determination by SIMAAS.