Faster and simpler determination of chlorophenols in water by fiber introduction mass spectrometry

Solid phase microextraction (SPME) of chlorophenols [2-chlorophenol (2CP), 2,4-dichlorophenol (24CP), 4-chloro-3-methylphenol (43CP), 2,4,6-tri-chlorophenol (246CP) and pentachlorophenol (PCP)] followed by direct mass spectrometric analysis has been performed by fiber introduction mass spectrometry (FIMS). Two SPME fibers (65 μm PDMS/DVB and 85 μm PA fibers) were tested, and FIMS was performed via selective ion monitoring (SIM). The extractions were evaluated at 10% ionic strength and pH 1. Best extraction times were determined for both fibers. Limits of detection (LOD) and limits of quantification (LOQ) for both fibers were in the low μg L⁻¹ range. Coefficients of correlation for the analytical curves showed linear responses and mineral water and river water samples spiked with 50 μg L⁻¹ presented high recoveries. FIMS, as compared to current EPA methods, is demonstrated to allow faster and simpler (elimination of pre-separation or derivatization steps) analysis of chlorophenols in water with the required sensitivity.     

Hydrogen adsorption on carbon-doped boron nitride nanotube

The adsorption of atomic and molecular hydrogen on carbon-doped boron nitride nanotubes is investigated within the ab initio density functional theory. The binding energy of adsorbed hydrogen on carbon-doped boron nitride nanotube is substantially increased when compared with hydrogen on nondoped nanotube. These results are in agreement with experimental results for boron nitride nanotubes (BNNT) where dangling bonds are present. The atomic hydrogen makes a chemical covalent bond with carbon substitution, while a physisorption occurs for the molecular hydrogen. For the H(2) molecule adsorbed on the top of a carbon atom in a boron site (BNNT + C(B)-H(2)), a donor defect level is present, while for the H(2) molecule adsorbed on the top of a carbon atom in a nitrogen site (BNNT + C(N)-H(2)), an acceptor defect level is present. The binding energies of H(2) molecules absorbed on carbon-doped boron nitride nanotubes are in the optimal range to work as a hydrogen storage medium.     

Isolation and Screening of Microorganisms for R-(+)-Limonene and (−)-β-Pinene Biotransformation

This work is focused on the biotransformation of R-(+)-limonene and (?)-β-pinene to bioflavor production. To carry out the present study, 405 microorganisms were tested for their ability to bioconvert the substrates. From the isolated microorganisms, 193 were selected in the prescreening using mineral medium for limonene degradation. At the screening step, eight strains were able to convert R-(+)-limonene and 15 to transform (?)-β-pinene, both in α-terpineol. The highest concentration in α-terpineol from R-(+)-limonene was about 3,450 mg/L for Penicillium sp. isolated from eucalyptus steam. From (?)-β-pinene, the highest product concentration of 675.5 mg/L was achieved using an Aspergillus sp. strain isolated from orange tree stem.     

High-pressure phase diagram of the drug mitotane in compressed and/or supercritical CO2

This work provides experimental phase diagram of mitotane, a drug used in the chemotherapy treatment of adrenocortical carcinoma, in compressed and/or supercritical CO₂. The synthetic-static method in a high-pressure variable-volume view cell coupled with a transmitted-light intensity probe was used to measure the solid-fluid (SF) equilibrium data. The phase equilibrium experiments were determined in temperature ranging from (298.2 to 333.1) K and pressure up to 22 MPa. Peng–Robinson equation of state (PR-EoS) with classical mixing rule was used to correlate the experimental data. Excellent agreement was found between experimental and calculated values.     

Electrophoresis microchip fabricated by a direct-printing process with end-channel amperometric detection

We describe the development of an electrophoresis microchip fabricated by a direct-printing process, based on lamination of printed polyester films with end-channel amperometric detection. The channel structures are defined by polyester (base and cover) and by a toner layer (walls). The polyester-toner devices presented an electroosmotic flow (EOF) magnitude of approximately 10(-5) cm2 V(-1) s(-1), which is generated by a polymeric mixture of the toner and polyester composition. The microelectrodes used for detection were produced combining this laser-printer technology to compact discs. The performance of this device was evaluated by amperometric detection of iodide and ascorbate. The detection limits found were 500 nmol.L(-1) (135 amol) and 1.8 micromol.L(-1) (486 amol) for iodide and ascorbate, respectively.     

Facile and efficient aerobic one-pot synthesis of benzimidazoles using Ce(NO3)3·6H2O as promoter

A series of 2-substituted benzimidazoles was synthesized under aerobic conditions, by simply heating 1,2-diaminobenzene and aldehydes in DMF at 80 °C, employing Ce(NO₃)₃·6H₂O as promoter and atmospheric air as an efficient oxidant. The procedure afforded the products from good to excellent yields. Furthermore, this new economic and eco-friendly protocol avoids the use of toxic metal catalysts, as well as additional bases and oxidants.     

Biomimetic Mineralization of the Alginate/Gelatin/Calcium Oxalate Matrix for Immobilization of Pectinase: Influence of Matrix on the Pectinolytic Activity

Pectinases catalyze the degradation of pectic substances and are used in several processes, mainly in food and textile industries. In this study, a biomimetic matrix of alginate/gelatin/calcium oxalate (AGOCa) was synthesized for the in situ immobilization via encapsulation of crude pectinase from Aspergillus niger ATCC 9642, obtaining an immobilization efficiency of about 61.7 %. To determine the performance of AGOCa matrix, this was compared to control matrices of alginate/calcium oxalate (AOxal) and alginate/water (ACa). By the evaluation of pH and temperature effects on the enzyme activity, it was observed an increase on pectinolytic activity for both three tested matrices with an increase on pH and temperature. The kinetic parameters for pectinase immobilized in the three matrices were determined using citric pectin as substrate. Values of K _m of 0.003, 0.0013, and 0.0022 g mL^?1 and V _max of 3.85, 4.32, and 3.17 μmol min^?1 g^?1 for AGOCa, AOxal, and ACa matrices were obtained, respectively. After 33 days of storage, the pectinase immobilized in the three different matrices kept its initial activity, but that immobilized in AGOCa presented high stability to the storage with a relative activity of about 160 %. The enzyme immobilized in AGOCa, AOxal, and ACa could be used in 10, 8, and 7 cycles, respectively, keeping 40 % of its initial activity.     

Ultrasound-promoted synthesis of 3-trichloromethyl-5-alkyl(aryl)-1,2,4-oxadiazoles

The alternative synthesis of 12 1,2,4-oxadiazoles using ultrasound irradiation from trichloroacetoamidoxime and acyl chlorides is reported. Seven of them are novel compounds. The 3-trichloromethyl-5alkyl(aryl)-1,2,4-oxadiazoles have been synthesised in better yields and shorter reaction times compared to the conventional method. This protocol can be applicable for preparation of 1,2,4-oxadiazoles containing aryl or alkyl groups attached at their C-5 side-chain.