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EN
A new vicinal dioxime ligand (1E,2E)-N 1,N 2-bis(2-formylphenyl)-N c1,Nc2-dihydroxy - ethanediimidamide (H2L) has been synthesized by the rea tion of o-anisidine with dichloroglyoxime. Mononuclear complexes with some transition metal ions have been prepared. This compound forms square-planar metal complexes (M(HL)2), with Ni(II), Co(II) and Cu(II), with a metal ligand ratio of 1:2. Also, the tetrahedral complexes of Hg(II), Cd(II) and Zn(II) have been prepared and were found to have a metal ligand ratio of 1:1. The results indicated that the metal ions are coordinated through two N atoms of the ligand, as do most of the vic-dioximes. H2L forms the binuclear nonplanar N, O co or - dinating complex [(H2L)(OH)2M2] and a metal ligand ratio of 1:1 with M = U(VI)O2. The composition and structural formula of these complexes were confirmed by elemental analysis, IR, MS, and NMR spectroscopic methods.
EN
A new vic-dioxime derivative (2H-1,4-benzolhioazine-2.3(4H)dionedioxime, Oxime I) has been synthesized and investigated as a selective compiexing ligand for homogeneous liquid-liquid extraction and preconcentration of Ni2+ and Cu!2+ ions. Zony l FSA has beenapplied as a phase separation agent. The influence of pH. type, and concentration of water-miscible organic solvent, Zonyl FSA, and Oxime I, as well as the effect of different diverse ions on extraction and determination of Ni2+ and Cu22+ ions has been investigated. Under optimum conditions ([Oxime l]T = 1.2 x 10 mol L-1, [THF]T = 16.7 % v/v, [FSA]T = 3.2 % m/v, pH = 4.5), 5 ng of each Ni2+ and Cu2+ in 5.5 mL aqueous phase was extracted quantitatively into 75 &muL of the precipitated liquid phase. Limit of detection of the proposed method was 0.004 ng mL-1 for Ni2+ and 0.005 ng mL-1for Cu2+. The proposed method has been extended over extraction and determination of Ni:2+ and Cu2+ ions in different synthetic and natural water samples.
PL
Zsyntetyzowano nową pochodną (2H-1,4-benzotiazyno-2,3(4H)dionodioksymu. oksyrn I) i badanoją pod kątem zastosowania jako kompeksującego ligandu do jednorodnej ekstrakcji ciecz-ciecz i wstępnego zateżania jonów Ni2+ i Cu2+. Jako czynnika rodzielającego fazy użyto Zonylu FSA. Badano wpływ pH oraz wpływ rodzaju i stężenia mieszającego się z wodą rozpuszczalnika organicznego. Zonylu FSA i oksymu I, a także wpływ rozmaitych jonów na ekstrakcje i oznacznie Ni2+ i Cu2+t. W optymalnych warunkach ([oksyrn I]T = 12 x 10-3 moL L-1, [THF]T = 16,7 % v/v, [FSA]T = 3.2 % v/v, pH = 4.5), 5 ng Ni2+ i Cu2+ w 5,5 mL-1 fazy wodnej wyekstrahowano do 75 &.L strąconej fazy ciekłej. Granica wykrywalności proponowanej metody wynosi 0.004 ng mL-1 w przypadku Ni2+ i 0,005 ng mL-1 w przypadku Cu2+. Metodę zastosowano do ekstrakcji i oznaczania Ni2+ i Cu+2 w syntetycznych i naturalnych próbkach wód.
EN
The novel Schiff base ligand, 4-methoxysalicyliden-p-aminoacetophenoneoxime (LH) was synthesized starting from p-aminoacetophenoneoxime and 4-methoxysalicylaldehyde. Mononuclear cobalt(II), copper(II) and zinc(II) complexes of the ligand have been prepared by using Co(II), Cu(II) and Zn(II) salt with a metal to ligand ratio of 1:2. The structures of the ligand and its complexes were identified by using elemental analyses, IR, 1H- and 13C-NMR spectra, magnetic susceptibility measurements, UV spectra and thermogravimetric analyses (TGA).
EN
4,6,8-Triaryl-2-oxa-4,6,8-triazabicyclo[3.3.0]octanes (4) and 6,8-diaryl-2,4-dioxa-6,8- diazabicyclo[3.3.0]octanes (5) were synthesized by condensation of arylamines with glyoxal and formaldehyde in CH3CN. Change of the reaction solvent to CH3OH leads to dimethoxy imidazolidine (7). Depending on the reaction conditions, intermediates with different configuration are formed. The X-ray crystal structure determination of 5 shows a cis fusion of the two five-membered rings, in line with two anomeric effect; a strong nN_óC-O * interaction and a weak nO_óC-N * . The compound5 is a rare molecule containing N-C-N and O-C-O units adjacent to N-C-O anomeric moiety. The results show, that in the presence of anomeric unit of N-C-O, the anomeric effect of N-C-N and O-C-O moieties are negligible.
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