Mixed ugand complexes of iron(III) derived from its dithiocarbamato complexes

Three different types of iron(III) complexes, Fe(A)₃, Fe(A)₂(A') and Fe(A)(A')₂, whereA is either piperidyldithiocarbamate or morpholyl dithiocarbamate andA' is glycine(oxine) acetylacetone have been prepared by reacting Fe(III) salt with sodium salt of piperidinedithiocarbamic acid or morpholine-dithiocarbamic acid and acetylacetone(oxine)-glycine in different ratios. The mixed ligand complexes have been characterised by elemental analysis, magnetic susceptibility measurements, infrared, electronic spectral techniques and by thermal analysis. Electronic spectral studies suggests that all the complexes possess distorted octahedral geometry. The magnetic moment of the high spin iron(III) complexes lies in the range of 5.88–6.00 and for low spin lies in the range of 3.36–4.34 B.M. TG studies show one step decomposition of complexes and formation of Fe₂O₃ at the end of the step.     

Substoichiometric isotope dilution determination of manganese in biological smples using 2-thenoyltrifluoroacetone in isobutyl methyl ketone

A substoichiometric isotope dilution method was developed for the determination of microgram amounts of manganese. The method involves the use of carrier-free ⁵⁴Mn with Mn(II) carrier and its complexation with 2-thenoyltrifluoroacetone (TTA) at pH 8.5, the complex then being extracted into isobutyl methyl ketone. A minimum of 50 ng of manganese can be determined. The method was applied to the determination of manganese in several standard reference materials and biological samples such as tea leaves, spices and condiments. The method is simple and fast and yields results with high accuracy and precision.     

The effect of pressure on the raman spectrum of ice at low temperature

Extensive experimental studies of the Raman spectra of H₂O and D₂O ice in the lattice translational and OH (OD) stretching regions are reported for the first time at 88 K and from 0→6 kbar. An unambiguous transformation from ice I_h to ice IX has been observed, although previous studies suggest that a transition to ice II would have occurred. The ice I_h data are analysed in terms of various coefficients.     

Mössbauer studies in thermally treated iron-samarium mixed oxide system

Mössbauer spectroscopy and X-ray diffractometry have been used to study Sm–Fe mixed oxides (with different SmFe atomic ratios) annealed at 550, 850, 1000 and 1250 °C. The room temperature Mössbauer spectra can be interpreted in terms of one, two or three sextets and in some cases by an additional doublet depending on the composition and the heat treatment. The sextets have been associated with SmFeO₃ perovskite, Sm₃Fe₅O₁₂ garnet and -Fe₂O₃ hematite. These results are in agreement with those of X-ray diffractometric measurements, which give a clear, evidence of the presence of these phases.     

Radiochemical solvent extraction of molybdenum/VI/ using99Mo tracer

A radiochemical solvent extraction method has been developed for the micro determination of Mo/VI/ using⁹⁹Mo tracer. It involves removal of^99mTc by ethyl methyl ketone /EMK/ and extraction of Mo with tri-n-butyl phosphate /TBP/ from 5M HCl. Different parameters affecting the extraction such as pH dependence, nature of solvent and interferences due to other radionuclides have been studied. The method can be used up to 2 g of Mo.     

Microdetermination of silver(I) and iodide ions with a pyridinol azo dye: A spectrophotometric method

A simple, rapid, sensitive, and selective method for the spectrophotometric microdetermination of silver(I) using ammonium(2′,3′-dihydroxy pyridyl-4′-azo)benzene-4-arsonate (DHP-4A), a water soluble pyridinol azo dye is proposed. The red colored 1:1 (metal to ligand) complex formed has molar extinction coefficient (ε) 2.95 × 10⁴ 1 mol⁻¹ cm⁻¹ and absorbs maximum at 535 nm, in highly alkaline medium. Beer's law is obeyed up to 3.36 ppm and Sandell's sensitivity (for an absorbance 0.001) is 0.0037 μg of Ag(I)/cm². The silver(I)-(DHP-4A) complex has also been used in the microdetermination of iodide ions using ligand exchange reaction. The optimum concentration range of iodide ions which can reproducibly be determined is 1.27–37.9 μg/10 ml.