Synthesis and electrical conductivity of some poly[4‐amino‐2,6‐pyrimidinodi‐thiocarbamate]–metal complexes

Poly[4‐amino‐2,6‐pyrimidinodithiocarbamate] was prepared from the reaction of 2‐mercapto‐4,6‐diaminopyrimidine with carbon disulfide, followed by condensation through the removal of H₂S gas. Five polymer–metal complexes of manganese, ferrous, ferric, zinc and mercury were then prepared. The polymer–metal complexes are investigated by elemental analyses, ultraviolet Fourier transform infrared and magnetic susceptibility. The DC electrical conductivity variation with the temperature in the region 298–498 K of the five polymer–metal complexes was determined. Doping with 5% ZnCl₂ increased the electrical conductivity of the polymer at all temperatures investigated. All the polymer–metal complexes showed an increase in conductivity with an increase in temperature, which is a typical semiconductor behavior. The proposed structure of the complexes is (MLX₂·mH₂O)_n. All the polymer–metal complexes are thermally stable, are insoluble in common organic solvents and have high melting points. Copyright © 1999 John Wiley & Sons, Ltd.     

TOC versus UV spectrophotometry for wastewater quality monitoring

Total organic carbon (TOC) is one of the most important parameter for the knowledge of water and wastewater quality, because it concerns theoretically all organic compounds. Unfortunately, some restrictions with respect to TOC measurement must be considered, explaining that alternative procedures have been envisaged, among which UV spectrophotometry. Starting from a comparison of results between high temperature digestion and UV photo-oxidation techniques for some specific compounds and real wastewater samples, the work shows the complementary interest of using UV spectrophotometry either directly (with multiwavelength procedures) or after UV photo-oxidation.     

Thermal decomposition of basic cobalt and copper carbonates

Basic cobalt and copper carbonates were prepared by precipitation from solutions of their nitrates using KHCO₃ at room temperature in CO₂ atmosphere. The thermal decomposition of the prepared basic carbonates was studied by means of TG and DTA techniques and the phases produced were identified by XRD measurements. The products obtained at 400C were subjected to different doses of gamma-rays (40–160 M rad) and the thermal stabilities of these solids were investigated.The results obtained revealed that basic cobalt carbonate decomposed at 335C to produce Co₃O₄ which remained stable up to 850 and then decomposed above this temperature giving CoO which transformed into Co₃O₄ on cooling to room temperature. Basic copper carbonate dissociated at 290C yielding CuO which yielded Cu₂O and metallic copper at 1060 and 1150C, respectively. However, the produced cuprous oxide and metallic copper solids were converted into CuO and CU₂O, respectively by cooling in air to room temperature.Gamma-irradiation decreased the thermal stability of Co₃O₄ to an extent proportional to the dose employed. On the other hand, this treatment increased the thermal stability of both CuO and Cu₂O.     

Stability-indicating densitometric determination of some antidiabetic drugs in dosage forms, using TLC

The most commonly used antidiabetic sulfonylurea drugs, gliclazide, glipizide and glibenclamide, were determined using stability-indicating densitometric methods. The degradation products were prepared by acid hydrolysis of the intact drugs. Thin layer chromatography was carried out using silica gel 60 F₂₅₄ plates and different mobile phases, followed by scanning of the developed chromatograms. Mixtures of the investigated drugs and their degradation products were prepared and analysed using the proposed methods, with recovery in the range 100.4–101.0% and RSD in the range 0.6–0.7%. Pharmaceutical dosage forms were assayed and found to give results of the same accuracy and reproducibility as official or reference methods.     

Low coordinate germanium and tin compounds (ArO)2ME and (ArO)2MM′Ln M=Ge, Sn; E=S, Se, –NSiMe3 M′=Cr, W, Fe, Pt [Ar=2,4,6-tris((dimethylamino)methyl)phenyl-]

The reactions of the divalent species (ArO)₂M (Ar=2,4,6-[(CH₃)₂NCH₂]₃C₆H₂; M=Ge, Sn) with either Me₃SiN₃, elemental S₈, Se or transition metal complexes M′(CO)_n+1 (M′=Fe, n=4; M′=Cr, W; n=5) (Ph₃P)₂Pt·C₂H₄ have resulted in the isolation of either the new stable formal metallanimines (ArO)₂M=N–SiMe₃, germanethione, -selone (ArO)₂Ge=E (E=S, Se) (the expected formations of the stannanethione and -selone were not observed), or the (ArO)₂M=M′(CO)_n, (ArO)₂M=Pt(PPh₃)₂ complexes, respectively. The direct oxidation of the (ArO)₂M species with various oxidizing agents led to the formation of the corresponding metalloxanes [(ArO)₂M–O–]₂. All of the chalcogenido- and transition metal–metal 14 complexes have been physicochemically and chemically characterized. The reactions of the (ArO)₂Ge=E (E=S, Se) compounds with 3,5-di-tert-butyl-1,2-benzoquinone produced, by extrusion of sulfur or selenium, the dioxametalloles corresponding to the formal addition of the divalent species (ArO)₂M to the benzoquinone. A substitution reaction of chalcogen (S/Se) has been observed permitting to go from germaneselone to germanethione.     

Synthesis of temperature-sensitive micron-sized monodispersed composite polymer particles and its application as a carrier for biomolecules

 Temperature-sensitive micron-sized monodispersed composite polymer particles were prepared by seeded copolymerization of dimethylaminoethyl methacrylate and ethylene glycol dimethacrylate with 1.77 μm-sized monodispersed polystyrene seed particles. The change in surface property at temperature above and below 35 °C was examined by differential scanning calorimetry, trypsin activity and the adsorption/ desorption behaviors of low molecular weight cationic emulsifier as well as biomolecules. Received: 6 August 1997 Accepted: 16 January 1998     

Aromatic polyether, -ketone, -sulfones as laminating resins. XII. Derivatives of 2,2′-diphenylethynyldiphenyl which cure by an intramolecular cyclization

Polymers made from 2,2′-diiododiphenyl-4,4′-dicarbonyl dichloride, diphenyl ether, and isophthaloyl chloride have been made and converted to the 2,2′-diphenylethynyl derivatives. Introduction of units of isophthaloyl chloride reduced the melting point of these polymers to about 200°C, and they could then be cured by heating. A good glass laminate was prepared and cured from one of the polymers.     

Stable gaseous aziridinium ions

Gaseous protonated aziridine ions are produced at the threshold from β-phenoxyethylamine molecular ions. The evidence for this is collisional activation spectra, using various precursors (including labelled analogues) under electron impact and field ionization conditions. Partial conversion to the acyclic \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm CH}_{\rm 3} {\rm CH = }\mathop {\rm N}\limits^ + {\rm H}_{\rm 2} $\end{document} isomer occurs at higher electron energies and is rationalized by means of a potential energy surface constructed from energetic data.     

Determination of rare earths in low grade uranium ores and SRM-rock by instrumental neutron activation analysis

An instrumental neutron activation analysis technique has been developed for simultaneous determination of 10 REE in low grade U/Zr ores and other geological materials. The samples were irradiated with reactor neutrons for 2 min to 8 hrs followed by a cooling of 30 min to 3 weeks. The γ-ray activity was measured with a semi-planar Ge(Li) detector. A precision of 5% has been obtained by the repeated analysis of NBS-SRM. The technique is relatively simple and adaptable on the routine basis.     

Reaction of cholest-4-ene-3,6-dione with perbenzoic acid : Formation of novel oxetalactones

Oxidation of 1 with perbenzoic acid (p-toluene-sulphonic acid monohydrate as catalyst) provided novel oxetalactones 4 and 5 along with compounds 2 and 3. Treatment of 2 with perbenzoic acid yielded 4. A probable pathway for the formation of 4 from 1 involving the intermediacy of 2 has been suggested.