Sorption of As (III) and Se (IV) from aqueous solutions for subsequent determination by total reflection X-ray fluorescence

An approach to the simultaneous isolation of As (III) and Se (IV) from solutions on a new S,N-containing sorbent followed by determination of the analyte in the sorbent phase using total reflection X-ray fluorescence (TXRF) has been proposed. To match the goal, a sorbent with a branched structure was synthesized on the base of polyacrylamide modified with formaldehyde and hydrogen sulfide. This is a heteroatomic copolymer containing sulfide bridges in the chain and crosslinking by a tertiary amine. Conditions for the quantitative co-extraction of As (III) and Se (IV), i.e., sorption in solutions of 1 M HNO₃ with calcium ions present, heating to 60°C and phase contact time of 1 h were determined. The mechanism of sorption interaction of the analytes under specified conditions is discussed. It is shown that a 100-fold excess of iron, zinc and copper does not interfere with the extraction of analytes, thus providing the possibility of As (III) and Se (IV) isolation from different types of raw materials and processed products using the synthesized sorbent. A method for the direct XRF quantification of arsenic and selenium with sr 0.09 and 0.08, respectively, in the sorbent phase has been developed. The correctness of the results was confirmed by the ICP-MS method in analysis of aqueous reference solution after dissolution of the sorbate in HNO₃ (1:1).

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