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Improvement of selenium speciation in environmental matrices (water and fish)

Exploitable results

General Information : The main aims of the project are: - To improve the state of the art of Se-specification analyses in water and fish samples for Se(IV) and Se(VI), by organizing one intercomparison. - To prepare two batches of candidate certified reference materials (CRMs) of water to be certified for their contents of Se(IV) and Se(VI) and to organize the certification campaign. - To study the feasibility of preparation of a candidate CRM of fish for the improvement of organic and inorganic Se-species determination by testing the homogeneity and stability of these species in a selected fish material. The development of an analytical method will also be carried out. Achievements : This report describes the preparation of two artificial solutions containing Se(IV) and Se(VI). The homogeneity and stability studies and the analytical work performed for the tentative certification of the contents of total selenium, Se(IV) and Se(VI) are described. The report contains all the results and gives the methods used to determine the contents of total selenium ((13.5 ± 0.4) µg. L-1 in RM 602 and (80.3 ± 1.4) µg.L-1 in RM 603), Se(IV) ((5.9 ± 0.2) µg L-1 in RM 602 and (34.9 ± 0.8) µg.L-1 in RM 603), and Se(VI) ((8.1 ± 0.3) µg.L-1 in RM 602 and (45.1 ± 2.4) µg.L-1 in RM 603). Certification could not be achieved, owing to an instability of the Se-species after 36 months storage in polypropylene bottles. The results of this tentative certification show that (1) the state-of-the-art for Se-specification is good enough for laboratories to obtain comparable data, (2) reference materials containing inorganic Se-species can be stabilized and used over a 12-month period for the purpose of interlaboratory studies or routine quality control checks, (3) work remains to be done to find the optimal storage conditions for candidate CRMs to enable long term stability and availability of the materials. An important aspect of this work is that reference materials can be prepared by laboratories for their own quality control, following the 'cooking recipe' given in this paper; it is obvious that such reference solutions should be used with all necessary care to avoid instability problems and should certainly not be kept over a period longer than 12 months.

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