Abstract

To establish a method for sensitive, accurate, and precise determination of Se in real samples, isotope dilution analysis using high-power nitrogen microwave-induced plasma mass spectrometry (N 2 MIP-IDMS) was conducted. In this study, freeze-dried human blood serum (Standard Reference Material, NIES No. 4) provided by NIES (National Institute for Environmental Studies) was used as a real sample. The measured isotopes of Se were 78 Se and 80 Se which are the major isotopes of Se. The appropriate amount of a Se spike solution was theoretically calculated by using an error multiplication factor (F) and was confirmed experimentally for the isotope dilution analysis. The mass discrimination effect was corrected for by using a standard Se solution for the measurement of Se isotope ratios in the spiked sample. However, the sensitivity for the detection of Se was not so good and the precision of the determination was not improved (2-3%) by N 2 MIP-IDMS with use of the conventional nebulizer. Therefore, a hydride generation system was connected to N 2 MIP-IDMS as a sample introduction system (HG-N 2 MIP-IDMS) in order to establish a more sensitive detection and a more precise determination of Se. A detection limit (3σ) of 10 pg mL -1 could be achieved, and the RSD was less than 1% at the concentration level of 5.0-10.0 ng mL -1 by HG-N 2 MIP-IDMS. The analytical results were found to be in a good agreement with those obtained by the standard addition method using conventional Ar ICPMS. It is well-known that Se is an essential element for all mammals. Se deficiency leads to deficiency syndromes, for example, Keshan disease, which is known for cardiac insufficiency that occurred in children and pregnant women in China. Problems also occur if the concentration of Se is too high; for example, gastroenteric disorders, dermatitis, and neurotic disorders are caused by excessive intake of Se. Moreover, it is well-known that the range of permissive intake amounts of Se is very narrow for human beings. Therefore, it is restricted as a toxic element in environmental standards. There are several sources of environmental Se pollution: the processes of Se refinement and the production processes of Se-containing products. For these reasons, the accurate and precise determination of trace levels of Se in environmental and biological samples is required, and studies of Se determination have been reported by several groups. [1][2][3][4][5][6][7][8][9][10][11] Because Ar ICPMS can measure multiple elements at a concentration range from ng mL -1 to fg mL -1 , it has widespread use in the determination of trace elements in various samples. 12-25 However

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