Synchrotron-radiation-induced total reflection x-ray fluorescence (SR-TXRF) analysis was used for x-ray absorption near edge structure (XANES) measurements for the speciation of arsenic in cucumber (Cucumis sativus L.) xylem sap. The objective of the presented work was to exploit the advantages of the TXRF geometry for XANES analysis. Measurements were accomplished at the bending magnet beamline L of HASYLAB, Hamburg, Germany, using a Si(111) double crystal monochromator and a silicon drift detector (SDD). Experiments were performed by growing cucumber plants in hydroponics containing arsenite [As(III)] or arsenate [As(V)] in order to identify the arsenic species of the collected xylem saps by K-edge SR-TXRF XANES. Cucumber xylem saps, as well as nutrient solutions containing arsenic in the two above-mentioned species, were analyzed and compared with arsenate and arsenite standard solutions. Arsenic speciation in xylem sap down to 30 ng/ml (30 ppb) was achieved, and no alteration of the oxidation state was observed during the measurements. Analysis of xylem saps showed that As(V) taken up from the nutrient solution was reduced to As(III). As(III) contained in the nutrient solutions was found to be partially oxidized to As(V). These results confirmed the preliminary measurements obtained with flow injection analysis (FIA) and high-performance liquid chromatography-high resolution inductively coupled plasma mass spectrometry (HPLC-HR-ICP-MS) and showed the competitive capability of SR-TXRF XANES analysis for this application.
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