Thermal and spectroscopic analysis of Co(II)–Fe(III) polyglyoxylate obtained through the reaction of ethylene glycol with metal nitrates

• Published in: Journal of thermal analysis and calorimetry 2018, Vol.131 (1), p.127-136
• Main Authors: Niculescu, Mircea, Pascariu, Mihai-Cosmin, Muntean, Cornelia, Sasca, Viorel, Lupa, Lavinia, Milea, Marius-Silviu, Birzescu, Mihail
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Anions; Cations; Chemical analysis; Chemical industry; Chemical synthesis; Chemistry; Chemistry and Materials Science; Cobalt; Cobalt ferrites; Dilution; Electron microscopy; Ethylene glycol; Fourier transforms; Glyoxylic acid; Hematite; Infrared analysis; Infrared spectroscopy; Inorganic Chemistry; Iron; Ligands; Measurement Science and Instrumentation; Metal nitrates; Nitrates; Oxidation; Physical Chemistry; Physical properties; Polymer Sciences; Spectrum analysis; Thermal analysis; Thermal decomposition
• ISSN: 1388-6150; 1588-2926
• DOI: 10.1007/s10973-016-6079-1

The synthesis and thermal and spectroscopic studies of a new Co II –Fe III heteropolynuclear coordination compound are presented. The in situ oxidation product of ethylene glycol plays the role of ligand. Under specific working conditions, the reaction of ethylene glycol with Fe III and Co II nitrates in dilute acid solutions occurs with the oxidation of the former to glyoxylic acid, coordinated to the Co II and Fe III cations as glyoxylate anion (C 2 H 2 O 4 2− ), with simultaneous isolation of the heteropolynuclear coordination compound. In order to separate and identify the ligand, the synthesized coordination compound, having the composition formula Co 4 Fe 10 ( L ) 9 (OH) 20 (H 2 O) 32 ·14H 2 O, where L is the glyoxylate anion, has been treated with R–H cationite (Purolite C-100). After the retention of the metal cations, the resulting glyoxylic acid was confirmed by measuring its physical constants, by specific reactions and through spectroscopic methods. The synthesized coordination compound was characterized by physical–chemical analysis, electronic spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD) and thermal analysis. Cobalt ferrite impurified with ferric oxide was obtained following the thermal decomposition of Co II –Fe III polyhydroxoglyoxylate. The oxides obtained through thermolysis were studied by FTIR, XRD, scanning electron microscopy (SEM) and elemental analysis.