Trace elements in a profile of the unsaturated zone of the São Paulo Basin

This study comprises Tertiary sediments (clays, silts, and fine clayey sands) from the unsaturated zone of the Experimental Station in the University of São Paulo, taken from a nine meters depth profile; ten samples were separated in bulk and <53 m fractions. Chemical composition was determined by INAA to ascertain the distribution of trace elements throughout the sediment deposition, and to establish the background parameters, useful for mobilization studies of such elements after industrial waste disposal.     

Natural radionuclide-free phosphoric acid production

High-uranium phosphate rock from Itataia, Brazil, was milled for wet-process phosphoric acid production using the dihydrate method. Uranium contained in the phosphoric acid was recovered by solvent extraction. The distribution of long-lived natural radionuclides of the ²³⁸U and ²³²Th decay series involved in these operations was evaluated. ²²⁶Ra, ²²⁸Ra and ²¹⁰Pb were found to predominate in the phosphogypsum, while ²²⁸Th, ²³⁰Th and ²³²Th in the uranium-free phosphoric acid. Thorium is removed from the phosphoric acid by solvent extraction to produce a NORM-free phosphoric acid.     

Thermogravimetric and differential scanning calorimetric investigations of manganese–glycine interactions

Thermogravimetric (t.g.) and differential scanning calorimetric (d.s.c.) data have been used to study metal–amino acid interactions in adducts of general formula MnCl₂ · ngly (gly = glycine, n = 0.7, 2.0, 4.0 and 5.0). All the prepared adducts exhibit only a one step mass loss associated with the release of glycine molecules, except for the 0.7gly adduct, which exhibits two glycine mass loss steps. From d.s.c. data, the enthalpy values associated with the glycine mass loss can be calculated: MnCl₂ · 0.7gly = 409 and 399 kJ mol^–1, MnCl₂ · 2.0gly = 216 kJ mol^–1, MnCl₂ · 4.0gly = 326 kJ mol^–1 and MnCl₂ · 5.0gly = 423 kJ mol^–1, respectively. The enthalpy associated with the ligand loss, plotted as function of the number of ligands for the n = 2.0, 4.0 and 5.0 adducts, gave a linear correlation, fitting the equation: H (ligand loss)/kJ mol^–1 = 67 × (number of ligands, n) + 76. A similar result was achieved when the enthalpy associated with the ligand loss was plotted as a function of the _a(COO^–) bands associated with the coordination through the carboxylate group, 1571, 1575 and 1577 cm^–1, respectively, for the n = 2.0, 4.0 and 5.0 adducts, giving the equation H (ligand loss) /kJ mol^–1 = 33.5 × _a(COO^–) /cm^–1 – 52418.5. This simple equation provides evidence for the enthalpy associated with the ligand loss being very closely related to the electronic density associated with the metal–amino acid bonds.     

Automatic flow procedure for the determination of ethanol in wine exploiting multicommutation and enzymatic reaction with detection by chemiluminescence

An automatic procedure for the determination of ethanol in wines using a flow system based on multicommutation and enzymatic reaction is described. Alcohol oxidase was immobilized on aminopropyl glass beads and packed in an acrylic column. The peroxide due to enzymatic reaction with ethanol reacted with luminol and generated the chemiluminescence radiation that was monitored by using a laboratory-made detector based on photodiodes. The system manifold comprised a set of 3-way solenoid valves controlled by a microcomputer furnished with electronic interfaces, which ran on software written in Quick BASIC 4.5 to provide facilities to perform on-line sample dilution, reagent addition, and data acquisition. After system parameters optimization, ethanol samples were processed without prior pretreatment. The following suitable features were achieved: linear response ranging from 2.5 to 25% (v/v) ethanol, relative standard deviation of 1.8% (n = 10), detection limit of 0.3% (v/v) ethanol, sampling rate of 23 determinations per hour, and low reagent consumption of 0.23 mg luminol and 7 mg hexacyanoferrate (III) per determination. When the results were compared with those obtained using the AOAC Official Method, no significant difference at the 90% confidence level was observed.     

Synthesis,characterization and a thermogravimetric study of copper,cobalt and tin mono- and bis-adducts with ethyleneurea,ethylenethiourea and propyleneurea

This paper describes the synthesis, characterization and a thermogravimetric (t.g.) study of 11 adducts of general formula MCl₂·nL (M = Cu, Co and Sn; n = 1 and 2 for Sn, and 2 for Cu and Co; L = ethyleneurea eu, ethylenethiourea etu, and propyleneurea pu). The i.r. results shows that the eu and pu adducts are coordinated through oxygen, whereas for etu nitrogen is the coordination site. The (C=O) or (C=S) trend is: Cu > Co > Sn. The t.g. curves show that the adducts release ligand molecules in a single mass loss step. As regards considering adducts with the same stoichiometry, the observed thermal stability trend is: etu > pu > eu.     

Determination of trace elements in tree rings ofPinus by neutron activation analysis

The elemental composition of pine trees as a function of age was achieved by the tree-ring method. By using instrumental neutron activation analysis, trace elements were determined in individual rings ofPinus elliottii var.elliottii of 32, 14 and 9 years, from an implanted forest ofPinus sp., Buri, São Paulo, far away from industrial pollution. Different components of the system such as needles, pith, bark, soil and litter were also analyzed for 18 elements (As, Br, Ce, Co, Cs, Eu, Fe, Hf, K, La, Mn, Na, Rb, Sc, Sm, Yb, Zn, and Zr). Al, B, Ba, Ca, Fe, K, Mg, and P concentrations were determined by atomic absorption and/or emission spectrometry (AAS; ICP-AES). Some elements have showed similar radial distribution of the concentration for the three ages. Abrupt concentration changes in the pith and ring-bark boundary corresponding to the first and last growth rings were observed.     

2,4,6‐Trimethylphenyl isocyanide

The title compound, C₁₀H₁₁N, displays a crystallographic mirror plane that incorporates all the non‐H atoms, as well as the H atoms attached to the aromatic ring. The iso­cyano group is almost linear and shows an N[triple‐bond]C bond distance of 1.158 (3) Å.     

Development of Neuropeptide Y and Cell-Penetrating Peptide MAP Adsorbed onto Lipid Nanoparticle Surface

Functionalization of nanoparticles surfaces have been widely used to improve diagnostic and therapeutic biological outcome. Several methods can be applied to modify nanoparticle surface; however, in this article we focus toward a simple and less time-consuming method. We applied an adsorption method on already formulated nanostructured lipid carriers (NLC) to functionalize these nanoparticles with three distinct peptides sequences. We selected a cell-penetrating peptide (CPP), a lysine modified model amphipathic peptide (Lys(N₃)-MAP), CPP/drug complex, and the neuropeptide Y. The aim of this work is to evaluate the effect of several parameters such as peptide concentration, different types of NLC, different types of peptides, and incubation medium on the physicochemical proprieties of NLC and determine if adsorption occurs. The preliminary results from zeta potential analysis indicate some evidence that this method was successful in adsorbing three types of peptides onto NLC. Several non-covalent interactions appear to be involved in peptide adsorption with the possibility of three adsorption peptide hypothesis that may occur with NLC in solution. Moreover, and for the first time, in silico docking analysis demonstrated strong interaction between CPP MAP and NPY Y1 receptor with high score values when compared to standard antagonist and NPY.     

Vibrational analysis of d-PCL(530)/siloxane-based hybrid electrolytes doped with two lithium salts

The present study has been focused on environmentally friendly sol–gel-derived electrolytes based on a di-urethane cross-linked d-PCL(530)/siloxane network [where d represents di, PCL identifies the poly(ε-caprolactone) biopolymer, and 530 is the average molecular weight in grams per mole] doped with a wide range of concentration of lithium perchlorate and lithium bis(trifluoromethanesulfonyl)imide. Fourier Transform Infrared and Raman spectroscopies have been applied to evaluate the extent of ionic association. Characteristic bands of the PCL(530) segments, of the urethane cross-links, and of the anions have been examined to gain insight into the cation/biopolymer, cation/anion, and cation/cross-link interactions. In both electrolyte systems, “free” ions and contact ions have been identified. The addition of salt modifies the hydrogen-bonded array of the host matrix, causing the destruction/formation of the urethane/urethane aggregates.     

Synthesis of pentabromopseudilin and other arylpyrrole derivatives via Heck arylations

Pentrabromopseudilin and other 2 and 3-arylpyrrole derivatives were synthesized through the Heck–Matsuda reaction involving endocyclic enecarbamates and N-protected 3-pyrrolines, respectively. The overall processes permitted an easy and efficient access to these structural motifs present in several bioactive compounds. Attempts to synthesize the compound isopentabromopseudilin led to a tribromo aryl maleimide. We hypothesize that this latter compound is the putative product arising from the unusual thermal instability of isopentabromopseudilin.