Analytical Sciences

Abstract − Analytical Sciences, 22(5), 731 (2006).

Determination of Cadmium, Chromium, Copper and Lead in Sediments and Soil Samples by Electrothermal Atomic Absorption Spectrometry Using Zirconium Containing Chemical Modifiers
Orhan ACAR
TAEA, Saraykoy Ankara Nukleer Arastirma ve Egitim Merkezi, 06100 Ankara, Turkey
A method for direct determination of cadmium, chromium, copper and lead in sediments and soil samples by electrothermal atomic absorption spectrometry using Zr, Ir, etylenediamine acetic acid (EDTA), Zr + EDTA, Ir + EDTA, Zr + Ir and Zr + Ir + EDTA as chemical modifiers in 0.5% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture used as diluent was developed. The effects of mass and mass ratio of modifiers on analytes in sample solutions were studied. The optimum masses and mass ratios of modifiers: 20 µg of Zr, 4 µg of Ir, 100 µg of EDTA and 20 µg of Zr + 4 µg of Ir + 100 µg of EDTA, were used to enhance the analyte signals. Pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, and detection limits of analytes in samples were compared in the presence or absence of a modifier. The detection limits and characteristic masses of analytes in a 0.5% (m/v) dissolved sample (dilution factor of 200 ml g-1) obtained with Zr + Ir + EDTA are 8.0 ng g-1 and 1.2 pg for Cd, 61 ng g-1 and 4.3 pg for Cr, 32 ng g-1 and 23 pg for Cu, and 3.4 ng g-1 and 19 pg for Pb, respectively. The Zr + Ir + EDTA modifier mixture was found to be preferable for the determination of analytes in sediment and soil-certified and standard reference materials. Depending on the sample type, the percent recoveries of analytes were increased from 81 to 103% by using the proposed modifier mixture; the results obtained are in good agreement with the certified values.