Exposure risk assessment of uranium intake of the milk products from the region of Pernambuco,Brazil

Journal of Radioanalytical and Nuclear Chemistry - Haloperidol (HP) is a dopamine blocking agent. HP was radiolabeled with 125I using direct electrophilic substitution. Different HP formulations...     

Powdered activated carbons as effective phases for bar adsorptive micro-extraction (BAμE) to monitor levels of triazinic herbicides in environmental water matrices

Bar adsorptive micro-extraction using three powdered activated carbons (ACs) as adsorbent phases followed by liquid desorption and high performance liquid chromatography with diode array detection (BAμE(ACs)-LD/HPLC-DAD), was developed to monitor triazinic herbicides (atrazine, simazine and terbutylazine) in environmental water matrices. ACs used present apparent surface areas around 1000 m² g⁻¹ with an important mesoporous volume and distinct surface chemistry characteristics (pH_PZC ranging from 6.5 to 10.4). The textural and surface chemistry properties of the ACs adsorbent phases were correlated with the analytical data for a better understanding of the overall enrichment process. Assays performed on 10 mL water samples spiked at the 10.0 μg L⁻¹ levels under optimized experimental conditions yielded recoveries around 100% for the three herbicides under study. The analytical performance showed good precision (RSD < 15.0%), convenient detection limits (≈0.1 μg L⁻¹) and suitable linearity (1.0-12.0 μg L⁻¹) with good correlation coefficients (r² > 0.9914). By using the standard addition method, the application of the present method on real water matrices, such as surface water and wastewater, allowed very good performances at the trace level. The proposed methodology proved to be a suitable sorptive extraction alternative for the analysis of priority pollutants with polar characteristics, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor triazinic compounds in water matrices.     

Dynamic mechanical analysis

Using dynamic mechanical analysis (DMA) we have studied thermal degradation for a system containing a diglycidyl ether of bisphenol A (DGEBA) and 1,3-bisaminomethylcylohexane (1,3-BAC). The changes of dynamic mechanical properties during thermal degradation indicated a shift of the glass transition temperature (T _g) to higher temperatures and a decrease in the peak value of the dynamic loss factor (tan δ) with an increasing of aging time. The value of dynamic storage modulus (E′) at the rubbery state showed an increase with aging time, whiteE′ at the glassy state only underwent a moderate change with increased thermal degradation. From these results it can be argued that thermal degradation during the stage prior to the onset of the severe degradation involves structural changes in the epoxy system, as further crosslinking and loss of dangling chains in the crosslinked network.     

Theoretical spectroscopic study of europium tris(bipyridine) cryptates

A series of europium cryptates are studied, using semiempirical methods to predict electronic and spectroscopic properties. The results are compared with theoretical (DFT) and experimental results published by Guillaumont and co-workers (ChemPhysChem2007, 8, 480). Triplet energies calculated by semiempirical methods have errors similar to those obtained by TD-DFT methodology but hundreds of times faster. Moreover, the semiempirical results not only reproduce well the experimental values but also help explain the low values of quantum efficiency observed for these complexes.     

A new procedure for bovine milk digestion in a focused microwave oven: gradual sample addition to pre-heated acid

Milk samples can be efficiently digested using a focused microwave oven, however the conventional procedure of addition of concentrated acids to the liquid sample leads to digestates with elevated acidity and residual carbon concentrations. In this work a focused microwave oven was applied for acid digestion of bovine milk samples using a conventional and an alternative procedure based on gradual sample addition to hot and concentrated acids. A two-level 2³ full factorial design experiment with eight runs was carried out to evaluate the optimum experimental conditions for reducing both the residual carbon and the final acidity of digestates. The three studied parameters were: temperature of the digestion medium for sample addition, addition of sulfuric acid before the sample or during the first step, and number of aliquots of the sample gradually added. The best conditions were attained by adding small aliquots of milk (ten-fold a volume of 0.5 ml added during 5.0 min) to a digestion mixture containing 3.0 ml nitric acid plus 1.0 ml sulfuric acid heated at 105 °C. It was demonstrated that the digestion efficiency of the alternative procedure was better than the conventional procedure, i.e. 98 and 80%, respectively. The alternative procedure was applied for determination of Ba, Ca, Cu, K, Mg, Na, P, and Zn in whole and non-fat bovine milk. The accuracy was proved using two certified reference materials (whole and non-fat milk powder).     

Thermal study of l-alanine, l-threonine, and taurine crystals related to hydrogen bonding

In this study l-alanine, l-threonine, and taurine crystals were characterized through dilatometric technique and thermogravimetric and differential thermal analysis. The dilatometric analysis shows that the thermal expansion of the crystals is correlated with the strengths of local hydrogen bonding in the amino acid structures at room temperature. Thermogravimetric analysis and differential thermal analysis of the l-alanine, taurine, and l-threonine crystals have been performed at high temperatures. No clear correlation between the hydrogen bonding strengths and endothermic peak positions was observed.     

Lipase production by solid-state fermentation

The production of lipase by Penicillium simplicissimum in solid-state fermentation was studied using babassu cake as the basal medium. Tray-type and packed-bed bioreactors were employed. In the former, the influence of temperature; content of the medium, and medium supplementation with olive oil, sugarcane molasses, corn steep liquor, and yeast hydrolysate was studied. For all combinations of supplements, a temperature of 30°C, a moisture content of 70%, and a concentration of carbon source of 6.25% (m/m, dry basis) provided optimum conditions for lipase production. When used as single supplements olive oil and molasses also were able to provide high lipase activities (20 U/g). Using packed-bed bioreactors and molasses-supplemented medium, optimum conditions for enzyme production were air superficial velocities above 55 cm/min and temperatures below 28°C. The lower temperature optimum found for these reactors is probably related to radial heat gradient formation inside the packed bed. Maximum lipase activities obtained in these bioreactors (26.4 U/g) were 30% higher than in tray-type reactors.     

Adsorption of silanes bearing nitrogenated Lewis bases on SiO2/Si (100) model surfaces

The present paper describes the one-pot procedure for the formation of self-assembled thin films of two silanes on the model oxidized silicon wafer, SiO2/Si. SiO2/Si is a model system for other surfaces, such as glass, quartz, aerosol, and silica gel. MALDI-TOF MS with and without a matrix, XPS, and AFM have confirmed the formation of self-assembled thin films of both 3-imidazolylpropyltrimethoxysilane (3-IPTS) and 4-(N-propyltriethoxysilane-imino)pyridine (4-PTSIP) on the SiO2/Si surface after 30 min. Longer adsorption times lead to the deposition of nonreacted 3-IPTS precursors and the formation of agglomerates on the 3-IPTS monolayer. The formation of 4-PTSIP self-assembled layers on SiO2/Si is also demonstrated. The present results for the flat SiO2/Si surface can lead to a better understanding of the formation of a stationary phase for affinity chromatography as well as transition-metal-supported catalysts on silica and their relationship with surface roughness and ordering. The 3-IPTS and 4-PTSIP modified SiO2/Si wafers can also be envisaged as possible built-on-silicon thin-layer chromatography (TLC) extraction devices for metal determination or N-heterocycle analytes, such as histidine and histamine, with "on-spot" MALDI-TOF MS detection.     

Cellulose/iron oxide hybrids as multifunctional pigments in thermoplastic starch based materials

Cellulose/iron oxide hybrids were prepared by the controlled hydrolysis of FeC₂O₄ in the presence of vegetable and bacterial cellulose fibres as substrates. By varying the relative amount of FeC₂O₄ and NaOH, either hematite or magnetic iron oxides were grown at the cellulose fibres surfaces. This chemical strategy was used for the production of a number of materials, whose coloristic properties associated to their reinforcement role allowed their use as new hybrid pigments for thermoplastic starch (TPS) based products. The TPS reinforced materials were characterized by several techniques in order to evaluate: the morphology and the compatibility between the matrix and the fillers; the mechanical reinforcement effect of the cellulose/iron oxide pigments on TPS and the coloristic properties of the composites. All materials showed good dispersion and strong adhesion for the cellulose/iron oxide nanocomposites in the TPS matrix thus resulting in improved mechanical properties.