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Five samples of stannic antimony silicate inorganic ion exchanger have been synthesized under different conditions of preparation. The sample possessing the maximum ion exchange capacity (0.90 meq g−1 of dry exchanger) was selected for detailed studies and its chemical composition was determined. The exchanger was found to be thermally stable, possessing good ion exchange capacity and exhibiting regeneration phenomenon after heating at elevated temperatures when compared to the corresponding ion exchanger stannic antimonate. The ion exchange capacity is almost completely regained when determined on regenerated exchanger samples. The gain/loss of ion exchange capacity has been studied in the temperature range 40–800 °C. The reproducibility in the properties of the exchanger has been checked by duplicate preparations. The X-ray, pH titrations, TG and FTIR spectral studies have been performed. TG curve of the exchanger shows a higher percent mass loss in H+ form than that in K+ form and also gives an idea of the internal and the external water molecules present in the exchanger. On the basis of the above studies, the empirical formula of stannic antimony silicate has been proposed. Quantitative separations of Zn2+ from Mn2+, Cu2+ and Ni2+ have been carried out on the exchanger columns.
Hydrazinated nickel cobalt zinc ferrous fumarate precursor has been synthesized and decomposed autocatalytically to Ni0.4Co0.2Zn0.4Fe2O4. The thermal decomposition behavior of the precursor has been investigated by thermogravimetric (TG) and differential thermal analysis (DTA). The chemical composition was assigned to precursor based on chemical analysis, TG–DTA, infrared (IR), isothermal mass loss, and total mass loss studies. The X-ray powder diffraction of the decomposed precursor confirms the formation of monophasic nickel cobalt zinc ferrite, and IR spectrum exhibits two peaks in the region of 340–420 and 550–660 cm−1 characteristic of spinel ferrites. The average grain size evaluated by TEM is found to be 15–20 nm. The electrical DC resistivity measurement was carried out with respect to temperature using two-probe method and dielectric properties as a function of frequency. The high dielectric constant values found at lower frequencies were due to nanosize nature of the “as prepared” ferrite. The Curie temperature of the “as-prepared” Ni0.4Co0.2Zn0.4Fe2O4 determined by alternating current susceptibility measurements was found to be 380 °C.
The induction period of various proportions of urea–thiourea mixed crystal (UTMC) in methanol and absolute alcohol has been measured experimentally by the visual observation method. It decreased from 0.1 to 0.5 UTMC and then slightly increased from 0.66 to 0.9 UTMC. The solubility of various proportions of UTMC was determined. It decreases with increase in proportions of thiourea. The induction period, which is inversely proportional to the nucleation rate, has been used to estimate the interfacial tension between the UTMC and methanol, absolute alcohol, hence the nucleation parameters like critical radius (r*), number of molecules in the radius (r*) and Gibbs free energy change for the formation of a critical nucleus (∆G*) have been calculated. The ∆G* of UTMC in methanol was lower than absolute alcohol. The morphologies in all proportions of UTMC are completely changed.
Single crystals of di-μ-thioureabis(thiocyanato)cobalt(II), Co(NCS)2(tu)2 (tu—thiourea) are grown by slow evaporation of a mixed solvent system water–methanol (1:1, v/v) containing thiourea, potassium thiocyanate, and cobalt chloride (1:1:0.5) at room temperature. The dark brown plate-like crystals belong to triclinic system with space group \(P\overline{1}, \) and the cell parameters are a = 3.8469(7) Å, b = 7.5749(13) Å, c = 10.1184(17) Å, α = 92.599(8)°, β = 98.036(8)°, γ = 104.132(7)°, V = 282.15(9) Å3, and Z = 1. The cobalt atom lies at the center of symmetry with four bridging thiourea molecules. The powder X-ray diffraction study reveals the crystallinity of the material. The complex formation is evidenced by the vibrational patterns in Fourier transform infrared spectrum. The scanning electron microscopy study reveals the surface morphology of the metal–thiourea complex. Thermogravimetric and differential thermal analysis shows that the complex is stable up to the melting point. The crystal is further characterized by UV–Vis and mechanical studies.
Nowadays, there is the widespread use of clay minerals as fillers in polymeric materials. One of the most widely used mineral is montmorillonite belonging to the smectite. We have prepared organically modified clays using two different types of accelerators TP and ZDT for sulfur vulcanization. Intercalation of these accelerators into the interlayer of clays was performed using a gas reaction at room temperature. They were examined (characterized) by thermal analysis (DTA, TG), X-ray analysis, and infrared spectroscopy (FTIR).
Sixteen samples of a new phase of stannic phosphor–silicate inorganic ion exchanger have been synthesized under different conditions of preparation. The sample possessing the maximum ion-exchange capacity (1.50 meq g−1 of dry exchanger) was chosen for the detailed study and its chemical composition was determined. The new phase is found to be thermally stable, possessing a high ion-exchange capacity, and showing an interesting regeneration phenomenon after heating at elevated temperatures when compared to the corresponding ion exchanger stannic phosphate. The ion-exchange capacity is found to be almost completely regained when determined on regenerated samples. The gain/loss of ion-exchange capacity has been studied as a function of temperature, in the range of 40–800 °C. Thermo gravimetric (TG) analysis, X-ray, pH titrations and IR spectral studies have been performed. TG of the exchanger shows a higher percent mass loss in H+ form than that in the K+ form. Thermal studies give an idea of the internal and the external water molecules present in the exchanger. On this basis, the empirical formula of the new phase of the stannic phosphor–silicate prepared in these studies has been proposed. Quantitative separation of UO 2 2+ from VO2+ and Zn2+, and that of Cu2+ from Al3+ and Ni2+ have been achieved on the basis of its adsorption behaviour. The reproducibility in the properties of the exchanger has been checked by duplicate preparations.
Comfort is seen as a comprehensive concept involving the transport of heat, moisture and air in the fabric of interactions and the human body on the basis of used material, design clothing and other parameters. These transports are slowed down or accelerated. One of the impulses for the detection of comfort is to know the impact of heat transfer, moisture through clothing that is intended to be precisely the objective of activity. Textiles intended for clothing would be reported in some places about the local compression behaviour, resistance to failure and increased transport sweat and moisture. Such clothing should allow ventilation to the outside and dry as quickly as possible, so after some activity remained, thermal resistance prevents the body hypothermia. Textiles are now designed not only to achieve certain properties, but also with respect to such security—sensors, the monitor’s vital functions of the body of the wearer.
Single crystals of (2E, 6E)-2-(4-bromobenzylidine)-6-(4-methoxybenzylidine)cyclohexanone are grown by slow evaporation solution growth technique from ethanol at room temperature. The single crystal-X-ray diffraction study reveals that as-grown crystal belongs to triclinic system and the cell parameters are, a = 9.3720(3) Å, b = 11.0500(7) Å, c = 18.1790(3) Å, and V = 1,734.90(13) Å3. The structure and the crystallinity of the material were further confirmed by nuclear magnetic resonance spectroscopy and powder X-ray diffraction analysis. Simulated XRD pattern closely resembles the powder XRD profile with lowered intensities. FT-IR and FT-Raman spectral analyses reveal the various modes of vibrations. The crystal is transparent in the visible region having a lower optical cut-off at ~503 nm with band gap energy of 2.55 eV, estimated by the application of Kubelka–Munk algorithm. Theoretical calculations were performed using the Hartree–Fock method at level with 6-31G(d,p) as the basis set for to derive the optimized geometry and first-order molecular hyperpolarizability (β) values. The as-grown specimens were further characterized by dielectric and mechanical studies.
Thermogravimetry (TG) and derivative thermogravimetry (DTG) have been applied to the investigation of the thermal behavior of the compounds Cu(2-Clbz)2(denia)2(H2O)2 (I), Cu(2-Brbz)2(denia)2(H2O)2 (II), and Cu(3-Brbz)2(denia)2(H2O)1 (III), where 2-Clbz and 2-Brbz and 3-Brbz = 2-chloro-, 2-bromo- and 3-bromobenzoate anions, denia = N,N-diethylnicotinamide, H2O = water molecules. Thermal decomposition of all studied compounds proceeds in three steps. Heating of the compounds first results in the release of water molecules. The final product of thermal decomposition of studied complexes was CuO. The thermal stability of the complexes can be ordered in the sequence: (II) < (I) < (III). IR data suggest unidentate coordination of benzoate anions to Cu(II) in complexes (I)–(III).
Many papers have been published concerning the influence of different steric properties of metylamine, dimethylamine and trimethylamine on the type of interactions with different exchanged montmorillonite and their properties. The most effective active sites in montmorillonite are placed between two silicate layers, where the naturally occurring cations can easily be replaced by heavy metals and organic groups. Mercury is one of the most serious contaminants in environment. All forms of mercury are poisonous; however, organic mercury species are the most dangerous. It is harmful even in very small amount and presents a significant environmental threat. The results of thermogravimetry, differential thermogravimetry, X-ray powder diffraction and IR spectroscopy analysis show that methyl, dimethyl and trimethylamines are intercalated into the interlayer space of Hg-MMT. The effect of different steric properties of studied alkylamines is evident.
Sublimation print applied onto layered sports textiles can significantly change their functionality and properties, which were so significantly emphasised at production. One of the issues, we focused on in this article is measurement of thermal conductivity of membrane textiles before and after sublimation print application. To find out the effect of colouring on properties of the material, the sublimation process was applied by two methods—using colouring (printed transfer paper) and without colouring. Sublimation print onto examined textiles was applied in the temperatures ranging from 180 to 220/°C. Thermal conductivity was measured using the (C-THERM Cti) device. Results of the measurements imply that the value of thermal conductivity increases proportionally with rising temperature of the sublimation process.
A new semi organic nonlinear optical (NLO) crystal, l -valine thiourea has been synthesized and good optical quality single crystals were grown by slow evaporation technique. The growth conditions of the crystals are studied and the grown crystals are confirmed by powder X-ray diffraction studies. The grown crystal was characterized using powdered XRD, FT-IR, UV–Vis–NIR, EDX, and TG–DTA. The crystalline nature and its various planes of reflections were observed by the powder XRD. The presence of various functional groups was confirmed by FT-IR spectra. The UV–Vis–NIR spectra indicate that the crystal has very good absorption in the entire visible and near IR region spectrum suggesting the suitability of the material for NLO applications. The decomposition temperatures and mass loss have been estimated from the thermogravimetric analysis.
Acetaldehyde Thiosemicarbazone (ATSC) is an interesting example of organic crystal. It has been grown by slow evaporation solution growth technique for the first time using methanol as solvent. The grown crystal has been characterized by Fourier transform Infrared spectral analysis, UV–Visible spectral analysis, Proton nuclear magnetic resonance, 13 C nuclear magnetic resonance studies, and X-ray diffraction studies, ATSC crystal was also subjected to thermal studies to determine its optical transparency and thermal stability suitable for application oriented properties.
The influence of picric acid on second harmonic generation (SHG) of tris (thiourea) zinc(II) sulphate (ZTS) crystal is investigated. ZTS, a potential semi-organic nonlinear optical material, is doped with picric acid (1:1). Good quality crystals in the presence and absence of picric acid are grown by slow evaporation solution technique. XRD and FT-IR spectral analyses confirm that there is slight distortion in crystal structure due to doping. The surface morphology of the as-grown specimen which is changed with the nature and concentration of dopant is studied by scanning electron microscopy. TG–DTA study reveals that the sample is pure and there is no decomposition up to the melting point. Single crystal XRD indicates that the inclusion of picric acid is not to an appreciable extent. The SHG efficiency of the crystal is decreased substantially by the dopant.
The catalytic decomposition of KClO3 is studied in the presence of MnO2, activated carbons and sodium sulphide. This investigation describes the use of thermogravimetry as a convenient technique to investigate catalytic activity of a simple chemical reaction. It is observed that the MnO2 catalyst decreases the decomposition temperature from 480 to 350 °C while the activated carbons cause its decomposition at 320–325 °C. At the same time the carbons undergo facile gasification. Presence of Na2S was the most effective as it induced the carbon-catalysed decomposition of KClO3 at a temperature as low as 220 °C, a temperature at which the carbons were stable and no gasification was observed.
Mixed crystal, potassium zinc vanadium sulphate was grown from an aqueous solution containing equimolar proportions of K2Zn(SO4)2·6H2O (Tutton’s salt) and VOSO4 by slow evaporation at room temperature. Single crystal XRD analysis reveals that it belongs to monoclinic system with P21/c space group, and cell parameters are a = 9.006, b = 12.163, c = 1.36, and V = 649.6 Å3. The co-existence of VO(II)- and Zn in the Tutton’s salt crystalline matrix was confirmed by atomic absorption spectroscopy and energy dispersive X-ray spectroscopy. Scanning electron microscopy exhibits defect centres and crystal voids. The XRD and FT-IR analyses indicate the stress that the mixed crystal undergoes as a result of incorporation of vanadium. Thermal patterns of Tutton’s salt and the mixed crystal are compared. DTA curve exhibited a sharp endothermic peak at 420 °C for the pure K2Zn(SO)4·6H2O and at 410 °C for the mixed crystal.