Determination of the total and extractable mass fractions of cadmium and lead in mineral feed by using isotope dilution inductively coupled plasma mass spectrometry

This paper describes the determination of the total and extractable mass fractions of Cd and Pb in mineral feed test sample distributed by the Community Reference Laboratory for Heavy Metals in Feed and Food (CRL-HM), in the frame of the fifth interlaboratory comparison for the European Union National Reference Laboratories (NRL).The developed in this study protocol for the total and extractable mass fractions of Pb and Cd in mineral feed sample is based on isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The applied dual spiking approach reduced by 50% the number of analytical steps. The addition of hydrofluoric acid in the digestion step was found necessary to ensure a full decomposition and complete isotope equilibration. Quadrupole inductively coupled plasma mass spectrometer equipped with collision reaction interface (CRI) was employed for the measurements of Cd and Pb. Two methods for the determination of Cd were applied and compared. In the first one the high molybdenum content was reduced by introduction of matrix separation step followed by standard ICP-MS mode measurement, whereas in the second one CRI mode was used for the determination of Cd without preliminary matrix separation. The estimation of the combined uncertainty was performed according to the ISO guidelines. Uncertainty propagation was used as a tool for validation of proposed analytical procedure. Contributions from the correction for moisture content, sample homogeneity, procedural blank, instrumental background and dead time effects were evaluated in both cases. The largest uncertainty contributors for Cd and Pb is due to the within bottle homogeneity of the mineral feed sample – 50.3% and 90% respectively. The IUPAC data for isotope composition are the second major contributor to the combined uncertainty of the result for the total mass fraction of Cd in mineral feed – 43.3%. However, the ID ICP-MS results achieved from the two series of samples (partial and total extraction) were in excellent agreement within uncertainty, irrespective of the method used for extraction.The ID ICP-MS results for the total and extractable mass fractions of Cd and Pb in feed sample were compared with the results obtained with external calibration approach and routinely applied in the daily analytical practice of the Belgium National Reference Laboratory for trace elements in food and feed.

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► The protocol for the total and extractable mass fractions of Pb and Cd in mineral feed sample based on isotope dilution inductively coupled plasma mass spectrometry is developed.
► The ID ICP-MS method for the total and extractable mass fractions of Cd and Pb in feed sample is used for the validation of external calibration method for both elements in feed matrix.
► Two methods for the determination of Cd were developed: matrix separation of Cd followed by standard ICP-MS measurement in CRI mode without preliminary matrix separation.