Derivatographic studies on dehydration of salt hydrates and their deuterium oxide analogues. V

Non-isothermal thermal studies of the dehydration of the double salt hydrates of the type M(I)₂SO₄·M(II)SO₄·6H₂O and their D₂O analogues were carried out where M(I) = TI(I) and M(II) = Mg(II), Co(II), Ni(II), Cu(II) or Zn(II). Thermal parameters like activation energy, order of reaction, enthalpy change, etc. were evaluated from the analysis of TG, DTA and DTG curves. These thermal parameters were compared with those of other series, like NH₄(I), K(I), Rb(I) and Cs(I) studied earlier. On deuteration the nature of dehydration altered in the case of Tl₂Zn(SO₄)₂·6H₂O only. The thermal stability of the salt hyd discussed in relation to the salt hydrates of other series. The role of divalent cation on the thermal properties of dehydration of salt hydrates is also discussed. The order of reaction was always found unity. The values of ΔH were within ≈12–≈16 kcal mol^?1.     

Derivatographic studies on dehydration of salt hydrates and their deuterium oxide analogues. III

Dehydration of double salt hydrates of the type M(I)₂SO₄·M(II)SO₄·6H₂O where M(I)Rb(I) and M(II)Mg(II), Mn(II), Co(II), Ni(II), Zn(II) and Cu(II) has been studied by derivatograph. Thermal parameters like activation energy, order of reaction, enthalpy change etc. for each step of dehydration have been evaluated from the analyses of TG, DTA and DTG curves and these parameters are compared with corresponding salt hydrates of the NH₄ and K(I) series. These double salt hydrates are deuterated and studied similarly. Activation energies for the first step of dehydration of these salt hydrates increase with the increase of second ionisation potential of the central metal except for Mg. The nature of dehydration changes in the cases of double salt hydrates of Mg(II) and Ni(II) on deuteration. The order of reaction for each case of dehydration has been found to be unity. The enthalpy change per mole of water varies from 11.4 to 17 kcal.     

Capillary Electrophoretic Determination of Gatifloxacin from Pharmaceutical Preparation

Capillary zone electrophoresis has been used for the determination of gatifloxacin from its pharmaceutical preparation (tablets), using fused silica capillary. Separation was performed after hydrodynamic injection; the separation was achieved by applying 21 Kv voltage. Phosphate buffer solution (pH 9.5) was used as separation electrolyte. Detection was at 280 nm using a UV- detector. Under these experimental conditions the analysis takes 8 min. A linearity range for gatifloxacin was between 20.0 g mL^–1 to 60.0 g mL^–1. The method was validated and was found to be specific, precise, accurate, reproducible and robust and can be applied for the routine analysis of gatifloxacin from formulation and bulk drug.     

Dicyclohexano 18 crown 6 in butanol-octanol mixture: A promising extractant of Sr(II) from nitric acid medium

The extraction of strontium from nitric acid medium was investigated employing DCH18C6 in aliphatic alcohols as the diluents. 80% Butanol-20% octanol mixture was found to give higher D(Sr) values as compared to other alcohols investigated. A linear correlation between the organic phase water content and D(Sr) was observed, based on which the extraction mechanism was postulated. Effect of anion, cation, extractant concentration, nitric acid concentration and temperature on D(Sr) was also studied. Conditions for recovery (>90%) were arrived at and selectivity with respect to other interfering fission products was observed with most of the metal ions studied.     

Sorption studies of europium(III) on hydrous silica

Summary Sorption behavior of europium, Eu³⁺, on SiO₂ ^. xH₂O (silica gel) has been investigated as a function of time, the amount of silica gel, Eu³⁺ concentration, the ionic strength, and pH (in absence and in presence of carbonate). The sorption data were fitted to Freundlich, Langmuir and Dubinin-Radushkevich (D-R) isotherms. The sorption capacity of silica gel was determined to be in the range of (2.62-8.00) ^. 10^-7 mol/g at pH 5.30±0.05 and 0.20M NaClO₄. The mean energy of sorption was calculated to be 13.50±0.05 kJ/mol from the D-R isotherm, suggesting the involvement of ion-exchange reactions in the sorption process. Sorption of Eu³⁺ decreased with increased ionic strength. A gradual decrease in pH with increased ionic strength supports the involvement of an ion-exchange mechanism in the sorption process. The diffusion coefficient of Eu³⁺ ion on silica gel was calculated as (3.98±0.12) ^. 10^-13 m^{2 .} s^-1 under the particle diffusion-controlled conditions.     

Preparation and analytical properties of a chelating resin functionalized with 1-hydrazinophthalazine ligand

A poly[styrene-co-(divinylbenzene)] resin (XAD-4) functionalized with 1-hydrazinophthalazine ligand has been prepared and its analytical properties investigated. The pH dependence of sorption of metal ion on the resin has been determined for Cu(II), Ni(II), Co(II), Zn(II), Cd(II), Pb(II), Fe(III) and Cr(III). Trace amounts of these metal ions were quantitatively retained on the resin and recovered by eluting with 1 mol l(-1) hydrochloric acid. The resin was found to be selective for Fe(III) and its separation from other metal ions was carried out effectively. Metal ions concentrations were determined using AAS.     

Extraction chromatographic separation of thorium (IV) with tri-n-octylphosphine oxide (TOPO)

Thorium was extracted from a mixture of nitric acid and NaNO₃ of 0.01M each at pH 2.2 on a column of silica gel coated with TOPO. Thorium was separated from alkalis, alkaline earths, chromium, iron, cobalt, nickel, zinc, cadmium, mercury, lead, trivalent rare earths, platinum group metals, chloride, phosphate and acetate in binary mixtures by selective extraction of thorium. Thorium was separated from cerium (IV), zirconium, uranium and molybdenum by selective elution of thorium with 0.01M H₂SO₄. The method was extended for the analysis of thorium in monozite ore.     

Jacobi temperature

The Poisson-Jacobi transform of a function ? defined by $$v(n,t) = \sum\limits_{m = 0}^\infty {h(n,m;t)\phi (m)h_{\alpha ,\beta } } (m)$$ is considered. A theorem for the Jacobi temperaturev (n, t) is established which is analogous to that due to Tychnoff¹ for ordinary temperatures. Its Huygens property and growth pattern are also discussed. A representation theory for Poisson-Jacobi transforms is developed.     

Emission properties of manganese-doped ZnS nanocrystals

We have performed steady-state and time-resolved fluorescence studies on undoped and Mn-doped ZnS nanocrystals with approximately 16 A diameter. While there is no band-edge emission, the intensity of the steady-state blue fluorescence from ZnS surface states decreases upon Mn incorporation, which gives rise to an orange emission. These results show that Mn incorporation competes very effectively with the donor-acceptor surface states for the energy transfer from the electron-hole pair excited across the band gap. In both undoped and doped samples, the time-resolved fluorescence studies establish the presence of a distribution of decay lifetimes possibly due to a number of emission centers in the nanocrystals. A faster short-time decay of the blue emission in the Mn-doped samples compared to that in the undoped sample suggests an additional decay channel for the surface states via an energy transfer from these states to the dopant levels.