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• First application of DGA resins in analytical flow systems. • Achieved ppt limit of detection allows environmental and technological applications. • Fast computer controlled procedure with on-line preconcentration for determination of 239Pu. The monitoring of the presence of plutonium isotopes is a very important issue in both nuclear energy industry and environmental protection for human health risk assessment. The developed method for the determination of 239Pu isotope with ICP-QMS detection is based on the use of sequential injection analysis (SIA) system for the pretreatment of samples to be analyzed with the use of a commercial sorbent called diglycolamide (DGA-b) for the analyte preconcentration and separation from 238U, which is the source of the most significant isobaric interference 238U1H+. Optimizing the size of the sorbent bed and the conditions of analyte sorption and elution of plutonium and uranium provides the analytical procedure for 239Pu determination, where at total analysis time of 45 min (at flow rate 10 mL min−1) the evaluated method detection limit (MDL) for 100 mL sample volume was 88 mBq L−1. This is satisfactory detectability for applications in both technological and environmental samples. Image, graphical abstract [ABSTRACT FROM AUTHOR]

Diglycolamide ligands are widely applied in the analysis of radionuclides, especially lanthanides and actinides. They are used in liquid-liquid extraction procedures or in solid-phase extraction sorbents where they are adsorbed on the surface of hydrophobic polymers. The main objective of this study was to synthesize the N , N , N'N ′-tetrahexyl diglycolamide with one vinyl terminating group (vTHDGA) for further covalent immobilization on the polystyrene-divinylbenzene polymeric support. The obtained complexing resin (THDGA) was employed for the mechanized sample pretreatment in the Sequential Injection Analysis - Lab-on-Valve (SIA-LOV) flow system for the determination of 239Pu using ICP-MS detection. The analytical procedure was optimized in terms of selectivity towards several other radionuclides and elements forming potentially isobaric interferences in mass spectrometry. For 100 mL volume of sample to be analyzed, the method detection limit (MDL) was 96 mBq L−1 (42 pg L−1). The developed method was employed for the determination of 239Pu in real samples of a nuclear reactor coolant and spent fuel pool water from a nuclear reactor. Image 1 • Computer-controlled SIA-LOV setup with an exchangeable sorbent bed • New complexing sorbent for actinides • ICP-MS detection with examination of numerous interferences • Pu-239 determination in samples from nuclear industry [ABSTRACT FROM AUTHOR]