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Available online on http://www.rspublication.com/ijst/index.html ISSN 2249-9954
INTRODUCTION:
Our literature Survey indicates that the study of ammonium salts of metallo oxalates is
limited as compared to the potassium salts the thermal investigation of sodium and ammonium
metallodicarboxilates of metals like Mn(II),Fe(II), Fe(III), Co(II),Ni(II), Cu(II),Zn(II) and Cd(II)
with ligand oxalate has been reported1. Also study of metallo oxalates of Ni(II), Cu(II),Zn(II) has
been reported2.
Using information given in earlier reports, the study of synthesis, analysis and thermo
gravimetry of ammonium salts of metallo-oxalates of Ni(II), Mn(II), Co(II) is carried out. The
compositions have been ascertained from the analysis of metals (by titrimetry), ammonium (by
potentiometry), oxalate (by permagnometry) as well as metal and water(by TGA), from this
study we gain experience about the preparation of complex, standard titrimetric estimation of all
constituents and use of thermogravimetric analysis.
Present investigation:
EQUATIONS:
Estimation of oxalate
Standardization of KMnO4
Metal complex
Standardization of EDTA
Back titration of excess (unused) EDTA with standard Zn2+ ion solution
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International Journal of Advanced Scientific and Technical Research Issue 3 volume 6, Nov.-Dec. 2013
Available online on http://www.rspublication.com/ijst/index.html ISSN 2249-9954
Blank titration
Estimation of NH4+
Standardization of NaOH
Decomposition of metallo-oxalates
EXPREMENTAL:
Analysis of metal-oxalates.
Estimation of Ammonium
Thermogravimetry
Result table:
Estimation of Ni2+
Magnetic Susceptibility:
Diamagnetic substances are repelled quickly by the magnetic field while paramagnetic
compounds are attracted by the magnetic field.
Any atom or ion or molecule that has one or more unpaired electrons is paramagnetic.
Ferromagnetism arises when individual paramagnetic atom or ion are close together and the
interaction of magnetic field is constructive.
Curies Law: for most paramagnetic substances magnetic susceptibility varies inversely with
absolute temperature.
Magnetic susceptibility is the measure of force exerted by magnetic field on unit specimen.
Magnetic moment may be calculated by applying correction to measure susceptibility per mole.
M=[n(n+2)]1/2
1 Mn 4.57 5.47
2 Ni 0 0
3 Co 2.98 3.46
The result of analysis of oxalate, metal ion and ammonium are in good agreement with the
composition 2(NH4)2M(C2O4)]2H2O (where M=Mn /Ni /Co). these compositions are similar to
those of reported metal oxalates of the metal ion under persent study. There is slight variation in
percentage of residue in three complexes than the reported residue because the rate of
decomposition of every complex at a given temperature is different.
The analysis indicate that for Mn, Ni, Co complexes water molecules are not associated with the
metal. Because the temperature at which the complex loses water was lower than 1000C, which
suggests that, the water is not co-ordinated water but lattice water.
From the magnetic susceptibility we get eff less than expected because of the square planar
geometry of the crystal field splitting parameter B larger. In the case of Co(II) it forms a dimer
with another Co atom of complex which results in the anti Ferro magnetic coupling interactions
eff decreases from 3.7 to 2.93.
Acknowledgements:
We express our gratitude to UGC (WRO) Pune and BCUD University of pune, who have
financially supported through research projects for their kind help.
References:
2.Usha, M.G., Subba Rao M. and Kutty N., Indian Journal of Chemistry,20A,319-321(April
1981)
4.Gopal Krishna Murty, H.S., Subba Rao, M, and Narayana Kutty, T.R., J. inorg. Nucl.
Chem.,37,891(1975)
5.Paris, J., Rousset, A. and Chassagneux, F., Prog. Vac. Microbalance Tech., 3,416(1975)
8. B P SINGH and B SINGH Bull. Mater. Sci., Vol. 23, No. 1, February 2000, pp. 1116.
10. A. Coetzee, D. J. Eve and M. E, Brown Journal of Thermal Analysis. Vol. 39 (1993) 947-973