Here we report the method of fabrication of supermacroporous monolith sorbents (cryogels) via covalent cross-linking of polyallylamine (PAA) with diglycidyl ether of 1,4-butandiol. Using comparative analysis of the permeability and sorption performance of the obtained PAA cryogels and earlier developed polyethyleneimine (PEI) cryogels, we have demonstrated the advantages and disadvantages of these polymers as sorbents of heavy metal ions (Cu(II), Zn(II), Cd(II), and Ni(II)) in fixed-bed applications and as supermacroporous matrices for the fabrication of composite cryogels containing copper ferrocyanide (CuFCN) for cesium ion sorption. Applying the rate constant distribution (RCD) model to the kinetic curves of Cu(II) ion sorption on PAA and PEI cryogels, we have elucidated the difference in sorption/desorption rates and affinity constants of these materials and showed that physical sorption contributed to the Cu(II) uptake by PAA, but not to that by PEI cryogels. It was shown that PAA cryogels had significantly higher selectivity for Cu(II) sorption in the presence of Zn(II) and Cd(II) ions in comparison with that of PEI cryogels, while irreversible sorption of Co(II) ions by PEI can be used for the separation of Ni(II) and Co(II) ions. Using IR and Mössbauer spectroscopy, we have demonstrated that strong complexation of Cu(II) ions with PEI significantly affects the in situ formation of Cu(II) ferrocyanide nanosorbents leading to their inefficiency for Cs+ ions selective uptake, whereas PAA cryogel was applicable for the fabrication of efficient monolith composites via the in situ formation of CuFCN or loading of ex situ formed CuFCN colloids.
Combined experimental 57Fe Mössbauer and theoretical DFT study of a series of iron(II)-centered (pseudo)macrobicyclic analogs and homologs was performed. The field strength of the corresponding (pseudo)encapsulating ligand was found to...
The continuously increasing flow of toxic heavy metals to the environment due to intensive industrial activity and tightening requirements with regard to the content of metal ions in drinking and discharged waters urges the development of affordable and sensitive devices to the field control of pollutants. Here, we report a new thiated Rhodamine-lactam probe for Hg2+ detection and demonstrate how its sensitivity can be increased via the incorporation of the probe molecules into the optically transparent siloxane-acrylate coatings on polymethyl methacrylate and, alternatively, into the water-dispersible light-harvesting FRET nanoparticles (NPs), in which dye cations are separated by fluorinated tetraphenylborate anions. We have shown that the optimization of the FRET NPs composition had allowed it to reach the antenna effect of ~300 and fabricate “off/on” sensor for Hg2+ ion determination in aqueous solutions with the detection limit of ~100 pM, which is far below the maximum permissible concentration (MPC) of mercury in drinking water recommended by the World Health Organization. Although this work is more proof-of-concept than a ready-to-use analytical procedure, the suggested approaches to fabrication of the FRET NPs based on the popular rhodamine-lactam platform can be used as a background for the development of low-cost portable sensing devices for the extra-laboratory determination of hazardous metal ions.
To understand how polyethyleneimine (PEI), as a ligand, affects structure and properties of the transition metals hexacyanoferrates (HCFs) immobilized in cross-linked PEI matrix, we have synthesized Cu(II), Zn(II), and Fe(III) HCFs via successive ion-exchange reactions with metal salts and K4[FeII(CN)6] or K3[FeIII(CN)6]. The structure and properties of the obtained materials in comparison with the crystalline HCF analogs were investigated with FT-IR, Mössbauer, and UV–Vis spectroscopy. Complete reduction of Fe(III) to Fe(II) by PEI in HCF(III) was confirmed. When synthesis was performed at pH favoring binding of precursor metal ions by PEI, cyano-bridged hybrids rather than polymer—HCFs composites were formed. Although the obtained hybrids did not demonstrate sorption activity toward cesium ions, known for crystalline HCFs, they are of interest for the other applications. SQUID measurements revealed a significant difference in magnetic properties of PEI–HCFs hybrids in comparison with crystalline HCFs. Due to the Fe(III) to Fe(II) reduction in HCF ions, Cu(II) and Fe(III) HCFs(III) lost the molecular magnets properties in PEI matrix, but magnetic ordering, including ferromagnet-antiferromagnet interactions, was observed in all hybrids over the broad temperature range.
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