Good quality single crystals of 4-hydroxy tetramethylpiperazinium picrate (TMPP) were grown by slow evaporation solution growth method at room temperature. The average dimensions of the grown crystals were 0.6 × 0.2 × 0.2 cm 3. The solubility of the compound was estimated using methanol and acetone. The elemental analysis confirms the formation of the compound in the stoichiometric proportion. The UV-visible transmittance study indicates that the crystal possesses minimum transmittance at 370 nm and no absorption at 470-900 nm. The Bragg peaks obtained in the powder X-ray diffraction pattern confirm its crystallinity. The thermal behaviour of the crystal was investigated using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The structure of the compound was determined by using single crystal X-ray diffraction method. The compound was found to be crystallize in the monoclinic space group P2 (1) /c (a = 6.9513(8)Å, b = 11.8016(14)Å, c = 22.018(2)Å, α = 90.00 • , β = 92.575(2) • , γ = 90.00 •). The thermal anomalies observed in the differential scanning calorimetry (DSC) heating and cooling cycles indicate the occurrence of first order phase transition. Fourier transform infrared (FTIR) and polarized Raman spectral analyses were used to confirm the presence of various functional groups in the compound. The nonlinear optical property (NLO) of the crystal was analysed by Kurtz-Perry powder technique and found that the compound has SHG efficiency 1.5 times greater that of potassium dihydrogen phosphate (KDP).
Single crystals of a new compound, (NH 4 ) 2 CuBr 2 Cl 2 .2H 2 O, were grown from saturated aqueous solution at room temperature by slow evaporation method. The grown crystals were characterized through elemental, powder XRD, thermal and DSC analyses and FTIR and far IR spectra. The elemental analysis and the decomposition pattern formulated using the TG-DTG studies confirm the stoichiometry of the compound. The crystallinity of the compound is confirmed from the powder XRD pattern. A preliminary single crystal X-ray diffraction structural analysis reveals that the title compound belongs to the orthorhombic system with a = 7.7466Å, b = 7.783Å and c = 8.1211Å. The low temperature DSC shows thermal anomalies at -161.1, -156.5, -152.4, -145.2, -134, -18.5, and 1.4°C during the heating run and at -4.3, -54.8, -66.1, -90.6, -109.7 and -147.2°C during the cooling run. The thermal hysterses indicate first order phase transitions in the title compound at these temperatures. The FTIR spectra were used to assign the characteristic vibrational frequencies due to NH 4 + , CuX 4 2-ions and other chemical bonds. The effect of substitution of two bromine atoms on the phase transitions of a closely related crystal, diammonium tetrachloro cuprate dihydrate is also discussed.
Conducting polymers of polyaniline (PANi) and poly(o-phenylenediamine) (PoPD) were electropolymerized by cyclic voltammetric technique on low nickel stainless steel (LN SS) in H 2 SO 4 solution containing aniline and o-phenylenediamine monomers. The coatings were characterized by Fourier transform infrared spectroscopy, UV-visible and scanning electron microscopic techniques and the results are discussed. The corrosion protective properties of PANi and PoPD coatings on LN SS in 0·5 M NaCl were evaluated using potentiodynamic polarization and electrochemical impedance spectroscopic (EIS) techniques. The potentiodynamic polarization and electrochemical impedance spectroscopic results indicate that the PoPD coating inhibits the corrosion of LN SS in 0·5 M NaCl solution more effectively than PANi.
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