THERMAL-BEHAVIOR AND CHARACTERIZATION OF SOME NOVEL IRON(III)-O-PHTHALATES

Citation
V. Vancina et al., THERMAL-BEHAVIOR AND CHARACTERIZATION OF SOME NOVEL IRON(III)-O-PHTHALATES, Thermochimica acta, 246(1), 1994, pp. 199-212
Citations number
16
Categorie Soggetti
Chemistry Analytical
Journal title
ISSN journal
00406031
Volume
246
Issue
1
Year of publication
1994
Pages
199 - 212
Database
ISI
SICI code
0040-6031(1994)246:1<199:TACOSN>2.0.ZU;2-Z
Abstract
Several polynuclear iron(III)-o-phthalates precipitated from acid and alkaline solutions were characterized by chemical and thermogravimetri c analysis, and infrared, Mossbauer and magnetic measurements. Compoun ds prepared in acid solutions contain the trimer unit Fe3O and, althou gh different in chemical composition and in thermal decomposition beha viour, show very similar IR, Mossbauer and magnetic characteristics. T he variable temperature magnetic susceptibility measurements of these compounds were fitted to a theoretical expression derived from a spin Hamiltonian, taking into account two different exchange pathways along inequivalent sides of an isosceles triangle, yielding J(12)/cm(-1) = -35.4 and J(13)/cm(-1) = -21.1. The Mossbauer spectra of this group of samples could be satisfactorily fitted by considering the superpositi on of two quadrupole split doublets with different relative areas. Sam ples prepared in highly alkaline solution show a characteristic band i n the infrared spectra at 890 cm(-1), assigned to the asymmetric Fe-O- Fe stretch. Their Mossbauer spectra taken in the temperature region 77 -300 K reveal superparamagnetic behaviour of small particles or cluste rs. Magnetic susceptibility measurements of these polynuclear iron(III ) species show T-max/K = 10 and 25, respectively. Zero field-cooled, f ield-cooled and torque measurements were used to prove their spin glas s behaviour in the low temperature region.