Production of metakaolin from industrial cellulose waste

Research focused on the transformation and utilization of industrial wastes into products of commercial interest plays an increasingly important role. Residual pulp can become useful in the manufacture of different materials, providing high value to this waste and reducing its environmental impact when disposed of improperly in the environment. The main constituents of this waste are kaolin and calcium carbonate (CaCO₃). Starting from kaolin, metakaolin can be produced by calcination of the residue at 630?°C for 2?h in a rotary reactor with air flow, followed by solubilization with hydrochloric acid to remove the CaCO₃. The development of technological alternatives aimed at the reuse of certain wastes can result in applications of real economic interest to the chemical industry and ceramics and glass, which is the case in this study. The raw material and metakaolin obtained were analyzed by thermogravimetric analysis and derivative thermogravimetric analysis, X-ray diffraction, and X-ray fluorescence spectroscopy with promising results. This is because metakaolin was obtained free of contamination by other materials.     

Mechanical Behavior of Polymer Gels for RDCs and RCSAs Collection: NMR Imaging Study of Buckling Phenomena

Anisotropic NMR parameters, such as residual dipolar couplings (RDCs), residual chemical shift anisotropies (RCSAs) and residual quadrupolar couplings (RQCs or Δν_Q), appear in solution‐state NMR when the molecules under study are subjected to a degree of order. The tunable alignment by reversible compression/relaxation of gels (PMMA and p‐HEMA) is an easy, user‐friendly, and very affordable method to measure them. When using this method, a fraction of isotropic NMR signals is observed in the NMR spectra, even at a maximum degree of compression. To explain the origin of these isotropic signals we decided to investigate their physical location inside the NMR tube using deuterium 1D imaging and MRI micro‐imaging experiments. It was observed that after a certain degree of compression the gels start to buckle and they generate pockets of isotropic solvent, which are never eliminated. The amount of buckling depends on the amount of cross‐linker and the length of the gel.     

A semi-empirical approach to determine gamma activities in environmental cylindrical samples

A semi-empirical method to determine radionuclide concentrations in large environmental samples without the use of reference material and avoiding the typical complexity of Monte-Carlo codes is proposed. The calculation of full-energy peak efficiencies was carried out from a relative efficiency curve (obtained from the gamma spectra data), and the geometric (simulated by Monte-Carlo), absorption, sample and intrinsic efficiencies for energies between 130 and 3000 keV. The absorption and sample efficiencies were determined from the mass absorption coefficients, whereas the intrinsic efficiency was approximated by an empirical function. The deviations between calculated and experimental efficiencies for a reference material in most cases are less than 10%. Radionuclide activities in marine sediment samples calculated by the proposed method and by the experimental comparative method were not significantly different. This new method can be used for routine environmental monitoring when uncertainties up to 10% are acceptable.     

Spectrophotometric determination of phenylephrine hydrochloride in pharmaceuticals by flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine

This paper presents a method for the determination of phenylephrine hydrochloride in pharmaceuticals by spectrophotometric flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine, which leads to the formation of a condensation product with strong absorptivity at 500 nm. The linear dynamic range was between 0.95 and 9 mg/L, with a limit of detection of 0.2 mg/L and a sampling throughput of 120 samples per hour. The method was applied to eyewashes and nasal decongestant liquid medicines.     

Mössbauer spectroscopy on the double substituted lithium ferrite Li[Fe0.9(AlxGa1−x)0.1]5O8

Room temperature Mössbauer spectra of Ga and Al substituted lithium ferrite Li[Fe_0.9(Al_xGa_1?x)_0.1]₅O₈ with x = 0.00, 0.25, 0.50, 0.75 and 1.00 are reported. It is shown that the varying covalence of bonds caused by gallium and aluminium ions can explain the observed values of hyperfine fields and isomer-shifts.     

Luminescence of Fe3+ in single crystals of LiAl5O8

We have measured the luminescent properties of single crystals of LiAl₅O₈:Fe³⁺. In addition to a zero-phonon line due to Fe³⁺ in A-sites, we have observed another sharp fluorescent line at 699.2 nm which we assign to Fe³⁺ occupying B-sites. The excitation spectrum of the B-site Fe³⁺ shows characteristics similar to those of the A-site Fe³⁺ but are also shifted towards longer wavelengths. The spectra of the single crystals are compared with those of ordered and disordered powder samples.     

Synthesis of In<Subscript>2</Subscript>O<Subscript>3</Subscript>nanoparticles by thermal decomposition of a citrate gel precursor

This paper describes the synthesis of indium oxide by a modified sol–gel method, and the study of thermal decomposition of the metal complex in air. The characterization of the intermediate as well as the final compounds was carried out by thermogravimetry, differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and small angle X-ray scattering. The results show that the indium complex decomposes to In₂O₃ with the formation of an intermediate compound. Nanoparticles of cubic In₂O₃ with crystallite sizes in the nanosize range were formed after calcination at temperatures up to 900°C. Calcined materials are characterized by a polydisperse distribution of spherical particles with sharp and smooth surfaces.This revised version was published online in August 2005 with a corrected issue number.     

From labdanes to drimanes. Degradation of the side chain of dihydrozamoranic acid

A new route for the degradation of the saturated side chain of dihydrozamoranic acid has been devised, giving an advanced intermediate, compound 14, useful for the synthesis of insect antifeedants such as warburganal and polygodial.     

Immobilization of oxomolybdenum species in a layered double hydroxide pillared by 2,2'-bipyridine-5,5'-dicarboxylate anions

A Zn,Al layered double hydroxide (LDH) with Zn/Al = 1.45 and containing nitrate anions was prepared by coprecipitation and characterized by powder X-ray diffraction, Zn K-edge extended X-ray absorption fine structure spectroscopy (EXAFS), thermogravimetric analysis, FTIR and FT Raman spectroscopy, and (27)Al MAS NMR spectroscopy. Three Zn...O and four Zn...M (M = Zn, Al) shells could be fitted to the low-temperature (40 K) EXAFS spectrum, in accordance with a model for an ordered cationic sheet. The nitrate anions were easily exchanged by 2,2'-bipyridine-5,5'-dicarboxylate anions, resulting in an increase in the basal spacing from 9 to 18 A. The basal spacing of the pillared derivative indicates that the anions are arranged with their longest dimension nearly perpendicular to the host layers. This material exhibits a high encapsulating ability, as evidenced by its interaction with a dichloromethane solution of the dioxomolybdenum(VI) complex MoO(2)Cl(2)(THF)(2). A material with a metal loading of 11.2 wt % was obtained. Molybdenum K-edge EXAFS analysis could not substantiate the formation of a supported complex of the type MoO(2)Cl(2)(N-N) but instead indicated the formation of unidentate-bridged entities of the type [O(2)Mo-O-MoO(2)] with a metal-metal separation of 3.29 A. The molybdenum-containing LDH was active as a catalyst for the liquid-phase epoxidation of cis-cyclooctene, 1-octene, and trans-2-octene using tert-butyl hydroperoxide as the oxygen source, yielding the corresponding epoxides as the only products. For reactions carried out with no additional solvent (other than n-decane) or in the presence of 1,2-dichloroethane, the solid catalyst could be recycled with no major loss of activity. Other tests confirmed that the systems functioned as true heterogeneous catalysts.     

Mass spectrometric study of aliphatic alpha-carbonyl azides

A series of derivatives of 2-azidoacetic acid and 2-azidoacetone were synthesized and their behaviour under electron ionization conditions was investigated. This paper reports the electron ionization fragmentation mechanisms for five aliphatic alpha-carbonyl azides, which were clarified by accurate mass measurements and B/E linked scans. The substituent influences the abundance and the nature of the ions resulting from the molecular ion fragmentation.