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Synthesis, characterization and solid‐phase extraction properties of novel bis (diazo‐azomethine) ligands supported on mesoporous silica
Author(s) -
Uruş Serhan,
Karabörk Muharrem,
Köksal Hüseyin
Publication year - 2018
Publication title -
applied organometallic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.53
H-Index - 71
eISSN - 1099-0739
pISSN - 0268-2605
DOI - 10.1002/aoc.4022
Subject(s) - chemistry , diazo , solid phase extraction , mesoporous material , methylene , extraction (chemistry) , spectroscopy , nuclear chemistry , elemental analysis , inductively coupled plasma , inorganic chemistry , catalysis , chromatography , organic chemistry , physics , plasma , quantum mechanics
The novel mesoporous silica‐supported bis (diazo‐azomethine) compounds have been synthesized and characterized successively. In the first step, 1,3‐phenylenedimethanamine and 4,4′‐diaminodiphenylmethane were diazotized, and the obtained bis (diazonium) cations were coupled with 2,4‐dihydroxybenzaldehyde. The synthesized bis (diazo‐carbonyl) compounds, 5,5′‐((1,3‐phenylenebis(methylene))bis(diazene‐2,1‐diyl))bis(2,4‐dihydroxybenzaldehyde) (A1) and 5,5′‐((methylenebis(4,1‐phenylene))bis(diazene‐2,1‐diyl))bis(2,4‐dihydroxybenzaldehyde) (A2) were chemically supported on amino‐modified silica‐gel (as L1 and L2). Elemental analysis, liquid chromatography‐mass spectroscopy, liquid‐phase NMR ( 1 H and 13 C) and solid‐phase NMR (CP‐MAS 29 Si and 13 C), FT‐IR, TG/DTA, scanning electron microscopy and energy‐dispersive X‐ray spectroscopy techniques were used for characterizations of all the synthesized compounds. The syringe and batch techniques were applied for the solid‐phase extraction properties of Pb(II), Cu(II), Cd(II) and Cr(III) ions using an inductively coupled plasma‐atomic emission spectroscopy instrument. The recoveries of Pb(II), Cu(II), Cd(II) and Cr(III) ions have been achieved to 95–99% with the (RSDs) of ± 2–3% in optimum conditions.