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  • SI-traceable certification of the amount content of cadmium below the ng g(-1) level in blood samples by isotope dilution ICP-MS applied as a primary method of measurement


The present paper describes the development and implementation of a method for the certification of cadmium in blood samples at low to sub ng g{-1} level. The analytical procedure is based on inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) applied as a primary method of measurement. For the decomposition of the samples, two different sample digestion methods, an optimised microwave digestion procedure using HNO(3)/H(2)O(2) as oxidizing agents and a high pressure asher digestion procedure, were developed and compared. The very high salt content of the digests and the high molybdenum content, which can cause oxide-based interference on the Cd isotopes, were reduced by a chromatographic matrix separation step using an anion exchange resin. All isotope measurements were performed by a quadruple ICP-MS equipped with an ultrasonic nebulizer with membrane desolvator. This sample introduction set up was used to increase sensitivity and to minimize the formation of oxides in order to further decrease any possible MoO{+} interference present on the Cd isotopes.

Due to the very low Cd concentrations in the samples and the resulting need to minimize the procedural blank as much as possible, all sample processing steps were performed in a clean room environment. Detection limits of 0.005 ng g{-1} Cd were achieved using sample weights of 2.7 g. The described method was applied to re-certify the cadmium amount content in three different reference materials of reconstituted bovine blood from the Community Bureau of Reference (BCR) of the European Commission. Cadmium concentrations ranged between 0.2 ng g{-1} and 12 ng g{-1}. For these materials, SI-traceable certified values including total uncertainty budgets according to ISO and EURACHEM guidelines were established. .

Additional information

Authors: DIEMER J ET AL, JRC, IRMM, Geel (BE)
Bibliographic Reference: An article published in: Fresenius Journal of Analytical Chemistry, Vol.370 (2001), pp.492-498
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