Development of a fast capillary electrophoresis method to determine inorganic cations in biodiesel samples

The aim of this study was to develop a fast capillary electrophoresis method for the determination of inorganic cations (Na(+), K(+), Ca(2+), Mg(2+)) in biodiesel samples, using barium (Ba(2+)) as the internal standard. The running electrolyte was optimized through effective mobility curves in order to select the co-ion and Peakmaster software was used to determine electromigration dispersion and buffer capacity. The optimum background electrolyte was composed of 10 mmol L(-1) imidazole and 40 mmol L(-1) of acetic acid. Separation was conducted in a fused-silica capillary (32 cm total length and 23.5 cm effective length, 50 mu m I.D.), with indirect UV detection at 214 nm. The migration time was only 36 s. In order to obtain the optimized conditions for extraction, a fractional factorial experimental design was used. The variables investigated were biodiesel mass, pH, extractant volume, agitation and sonication time. The optimum conditions were: biodiesel mass of 200 mg, extractant volume of 200 mu L. and agitation of 20 min. The method is characterized by good linearity in the concentration range of 0.5-20 mg kg(-1) (r > 0.999), limit of detection was equal to 0.3 mg kg(-1), inter-day precision was equal to 1.88% and recovery in the range of 88.0-120%. The developed method was successfully applied to the determination of cations in biodiesel samples. (c) 2010 Elsevier B.V. All rights reserved.

Mild and efficient one-pot synthesis of chiral beta-chalcogen amides via 2-oxazoline ring-opening reaction mediated by indium metal

A simple and efficient procedure for the synthesis of beta-seleno and beta-thio amides via the ring-opening reaction of chiral 2-oxazolines in the presence of indium metal has been developed. Features of this method include the following: (i) easily and accessible starting materials; (ii) indium metal is more stable and less expensive then its respective salts; (iii) useful to excellent yields of beta-chalcogen amides derivatives. (C) 2008 Elsevier B. V. All rights reserved.

Chemoselective cross-coupling Suzuki-Miyaura reaction of (Z)-(2-chlorovinyl)tellurides and potassium aryltrifluoroborate salts

An ultrasound-assisted synthesis of functionalized vinylic chlorides is described by palladium-catalyzed cross-coupling reaction of potassium aryltrifluoroborate salts and (Z)-2-chloro vinylic tellurides. This procedure offers easy access to vinylic chlorides architecture that contains sterically demanding groups in good yields. (C) 2008 Elsevier Ltd. All rights reserved.

Crown ethers : applications in inorganic synthesis

The ability of macroheterocyclic compounds to complex with ionic species has led to the synthesis and investigation of many multidentate macroheterocyclic species. The most stable complexes are formed between macrocyclic polyetheral ligands (crown ethers) with alkali or alkaline earth metal iona. There is an excellent correlation of the stability of these complexes with the size of the cation and the site of the cavity in the macrocyclic ligand. Additional factors, such as the basicity of the ligand and the solvating ability of the solvent, also play important roles in the stabilization of the complex. The stability of such complexes has been advantageously used to increase anionic reactivity and has been successfully applied to several organic fluorinations, oxidations, and similar reactions. The use of macrocyclic ligands in inorganic syntheses of otherwise difficult to obtain fluoro compounds has not been reported. O-carborane and m-carborane, C2BlOHl2, are icosahedral cage systems derived from Bl2H122- by replacement of BH with the isoelectronic CH group. These stable molecules exhibit electron-deficient bonding which can best be explained by delocalization of electrons. This delocalization gives rise to stability similar to that found in aromatic hydrocarbons. Crown ether activated potassium fluoride has been successfully employed in the conversion of alkyl, acyl and aryl halides to their respective fluorides. Analogously halide substituted carboranes were prepared, but their fluoro-derivatives were not obtained. The application of crown ethers in the synthesis of transition metal complexes is relatively unexplored. The usual synthesis of fluoro-derivative transition metal complexes involves highly reactive and toxic fluorinating agents such as antimony trifluoride, antimony penta fluoride. bromine trifluoride and hydrogen fluoride, An attempted preparation of the hexafluoroosmate (IV) ion via a crown activated, or naked fluoride~was unsuccessful. Potassium hexafluoroosmate (IV), K208F6. was eventually prepared using bromine trifluoride as a fluorinating and oxidizing agent .

Pirólise de borras oleosas de petroleo utilizando nanomateriais

The oily sludge is a complex mix of hydrocarbons, organic impurities, inorganic and water. One of the major problems currently found in petroleum industry is management (packaging, storage, transport and fate) of waste. The nanomaterials (catalysts) mesoporous and microporous are considered promising for refining and adsorbents process for environment protection. The aim of this work was to study the oily sludge from primary processing (raw and treated) and vacuum residue, with application of thermal analyses technique (pyrolysis), thermal and catalytic pyrolysis with nanomaterials, aiming at production petroleum derived. The sludge and vacuum residue were analyzed using a soxhlet extraction system, elemental analysis, thin layer chromatography, thermogravimetry and pyrolysis coupled in gas chromatography/mass spectrometry (Py GC MS). The catalysts AlMCM-41, AlSBA-15.1 e AlSBA-15.2 were synthesized with molar ratio silicon aluminum of 50 (Si/Al = 50), using tetraethylorthosilicante as source of silicon and pseudobuhemita (AlOOH) as source of aluminum. The analyzes of the catalysts indicate that materials showed hexagonal structure and surface area (783,6 m2/g for AlMCM-41, 600 m2/g for AlSBA-15.1, 377 m2/g for AlSBA-15.2). The extracted oily sludge showed a range 65 to 95% for organic components (oil), 5 to 35% for inorganic components (salts and oxides) and compositions different of derivatives. The AlSBA-15 catalysts showed better performance in analyzes for production petroleum derived, 20% increase in production of kerosene and light gas oil. The energy potential of sludge was high and it can be used as fuel in other cargo processed in refinery

Organic and inorganic sources of zinc, copper and selenium in diets for dairy cows: intake, blood metabolic profile, milk yield and composition

The present study was carried out with the objective of evaluating the effects of feeding dairy cows with organic or inorganic sources of zinc (Zn), copper (Cu) and selenium (Se) on blood concentrations of these minerals, blood metabolic profiles, nutrient intake and milk yield and composition. Nineteen Holstein cows were selected and randomly assigned to two groups for receiving organic (n = 9) or inorganic (n = 10) sources of Zn, Cu and Se from 60 days before the expected date of calving to 80 days of lactation. Samples of feed, orts and milk were collected for analysis. Body condition score (BCS) was determined and blood samples were collected for analysis of Zn, Cu and Se concentrations, as well as for metabolic profile. Supplying organic or inorganic sources of Zn, Cu, and Se did not affect dry matter and nutrient intake, blood metabolic profile, milk yield and composition, plasma concentration of these minerals, and BCS or change the BCS in cows from 60 days before the expected date of calving to 80 days of lactation. An effect of time was observed on all feed intake variables, plasma concentrations of Zn and Se, milk yield, milk protein content, BCS and change in BCS.

Inorganic pyrophosphate-phosphohydrolytic activity associated with rat osseous plate alkaline phosphatase

Purified membrane-bound alkaline phosphatase from rat osseous plate hydrolyzed pyrophosphate in the presence of magnesium ions, with a specific activity of 92.7 U/mg. Optimal apparent pH for pyrophosphatase activity was 8.0 and it remained unchanged on increasing the pyrophosphate concentration. In the absence of magnesium ions the enzyme had a K-m = 88 mu M and V = 36.7 U/mg for pyrophosphate and no inhibition by excess substrate was observed. Pyrophosphatase activity was rapidly destroyed at temperatures above 40 degrees C, but magnesium ions apparently protected the enzyme against danaturation. Sodium metavanadate (Ki = 1.0 mM) was a competitive inhibitor of pyrophosphatase activity, while levamisole (Ki = 8.2 mM) and theophylline (Ki = 7.4 mM) were uncompetitive inhibitors. Magnesium ions (K-0.5 = 1.7 mu M) stimulated pyrophosphatase activity, while cobalt (Ki = 48.5 mu M) and zinc (Ki = 22.0 mu M) ions were non-competitive inhibitors. Manganese and calcium ions had no effect on pyrophosphatase activity. The M-w of the pyrophosphatase: protein was 130 kDa by gel filtration, but a value of 65 kDa was obtained by dissociative gel electrophoresis, suggesting that it was a dimer of apparently identical subunits. These results suggested that pyrophosphatase activity stems from the membrane-bound osseous plate alkaline phosphatase and not from a different protein.

Fatores determinantes das estratégias de gestão ambiental na indústria millennium inorganic chemicals: cristal global

The general aim of this research was to analyze the factors that determine the environmental management strategies in the industry Millennium Inorganic Chemicals: Crystal Global, but also analyze which environmental management strategies are used by industry. For the achievement of the proposed objective, we conducted a case study organization based in twenty-eight environmental management strategies raised in the literature. Following this survey, it was possible to ascertain which of these strategies are used in the industry studied, as well as which factors are decisive for the implementation of these. The research is characterized as qualitative and applied, as the goals is exploratory and descriptive, with regard to the data, these were obtained through interviews with the directors of the organization and also documents made available by the industry. As a main result, it was realized that the industry practices twenty-eight twenty of environmental management strategies proposed in this study, the scale Waste Management that encompasses more strategies. Regarding the determinants realized that the endogenous factors that are most pressing for the organization creating environmental strategies, and these determinants, since the exogenous, with the exception of environmental legislation, not put pressure on the organization

Ruthenium(II) phosphine/diimine/picolinate complexes: Inorganic compounds as agents against tuberculosis

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Bacterial cellulose-silica organic-inorganic hybrids

Bacterial cellulose (BC) hydrated membranes present nanometric reticulated structure that can be used as a template in the preparation of new organic-inorganic hybrids. BC-silica hybrids were prepared from BC membranes and tetraethoxysilane, (TEOS) at neutral pH conditions at room temperature. Macroscopically homogeneous membranes were obtained containing up to 66 wt.% of silica spheres, 20-30 nm diameter. Scanning electron micrographs clearly show the silica spheres attached to cellulose microfibrils. By removing the cellulose, the silica spheres can be easily recovered. The new hybrids are stable up to 300 degrees C and display a broad emission band under UV excitation assigned to oxygen-related defects at the silica particles surface. Emission color can be tuned by changing the excitation wavelength.

Strategic supplementation of calcium salts of polyunsaturated fatty acids to enhance reproductive performance of Bos indicus beef cows

Five experiments evaluated the effects of supplemental Ca salts of PUFA on reproductive function of Bos indicus beef cows. In Exp. 1, nonlactating and multiparous grazing cows (n = 51) were assigned to receive (as-fed basis) 0.1 kg of a protein-mineral mix + 0.1 kg of ground corn per cow/d, in addition to 0.1 kg per cow/d of 1) Ca salts of PUFA (PF), 2) Ca salts of SFA (SF), or 3) kaolin (control). Treatments were offered from d 0 to 20 of the estrous cycle. No treatment effects were detected on serum progesterone concentrations (P = 0.83), day of luteolysis (P = 0.86), or incidence of short cycles (P = 0.84). In Exp. 2, nonlactating and multiparous grazing cows (n = 43) were assigned to receive PF, SF, or control from d 0 to 8 of the estrous cycle. on d 6, all cows received (intramuscularly) 25 mg of PGF(2 alpha). No treatment effects were detected on serum progesterone concentrations on d 6 (P = 0.37), and incidence (P = 0.67) or estimated time of luteolysis (P = 0.44). In Exp. 3, twenty-seven lactating and multiparous grazing cows, approximately 30 to 40 d postpartum, were assigned to receive PF or control for 10 d beginning at the first postpartum ovulation. No treatment effects were detected (P = 0.85) on incidence of short cycles. In Exp. 4, lactating and multiparous grazing cows (n = 1,454), approximately 40 to 60 d postpartum, were assigned to receive 1 of the 7 treatments for 28 d after timed AI (TAI; d 0): 1) control from d 0 to 28, 2) SF from d 0 to 14 and then control, 3) PF from d 0 to 14 and then control, 4) SF from d 0 to 21 and then control, 5) PF from d 0 to 21 and then control, 6) SF from d 0 to 28, and 7) PF from d 0 to 28. Cows receiving PF for more than 21 d after TAI had greater (P < 0.01) pregnancy to TAI compared with all other treatments combined (50.4 vs. 42.4%, respectively). In Exp. 5, lactating and multiparous grazing cows (n = 501), approximately 40 to 60 d postpartum, were assigned to receive 1 of the 4 treatments for 21 d after TAI (d 0): 1) PF from d 0 to 14 and then control, 2) control from d 0 to 6 and then PF, 3) control from d 0 to 13 and then PF, and 4) PF from d 0 to 21. Cows receiving PF after d 14 of the experiment had greater (P = 0.02) pregnancy to TAI compared with cows not receiving PF during the same period (46.8 vs. 33.1%, respectively). In summary, supplemental Ca salts of PUFA during the expected time of luteolysis increased pregnancy to TAI in beef cows.

Effects of calcium salts of polyunsaturated fatty acids on productive and reproductive parameters of lactating Holstein cows

Two experiments evaluated milk production, serum progesterone and insulin, and reproductive performance of lactating Holstein cows receiving or not receiving Ca salts of polyunsaturated fatty acids (PUFA), or receiving Ca salts of PUFA at different daily frequencies. In experiment 1, 1,125 cows randomly distributed in 10 freestall barns were enrolled. Barns were assigned randomly to receive a high-concentrate diet containing (PI?) or not containing (control, CON) 1.1% (dry matter basis) Ca salts of PUPA. Diets were offered 6 times daily, whereas the Ca salts of PUFA were included in the PF treatment in the first feeding of the day. In experiment 2, 1,572 cows were randomly distributed in 10 freestall barns, which were assigned randomly to receive a diet similar to PF, but with Ca salts of PUFA included only in the first feeding of the day (PF1X), or equally distributed across all 6 feedings (PF6X). During both experiments, cows were artificially inseminated 12 h after the onset of estrus. Once per month, cows that did not conceive to artificial insemination were assigned to a fixed-time embryo transfer protocol. Pregnancy was determined via transrectal ultrasonography 28 and 60 d after expected ovulation. Pregnancy loss was considered in cows that were pregnant on d 28 but nonpregnant on d 60. During both experiments, feed intake, milk yield, and milk protein and fat content were recorded weekly. Blood samples were collected concurrently with embryo transfer. During experiment 1, feed intake was similar between treatments. Compared with CON, PF cows had greater milk yield (37.8 vs. 35.3 kg/d), and reduced milk fat content (3.41 vs. 3.55%). However, PF cows had reduced pregnancy losses per service compared with CON (12.6 vs. 18.3%). Serum progesterone was greater and serum insulin tended to be greater in primiparous cows receiving PF compared with CON cohorts (4.50 vs. 3.67 ng of progesterone/mL, and 10.4 vs. 7.5 mu UI of insulin/mL). During experiment 2, no treatment effects were detected for feed intake, milk yield, or milk fat, whereas PF1X cows tended to have reduced pregnancy losses per service compared with PF6X (14.4 vs. 18.4%). In summary, feeding Ca salts of PUFA to dairy cows increased milk production, did not alter feed intake, and reduced pregnancy losses per service. Further, the total daily amount of Ca salts of RITA should be fed during the first feeding of the day to optimize its benefits on pregnancy maintenance of dairy cows.

The volumetric fraction of inorganic particles and the flexural strength of composites for posterior teeth

Objective. To evaluate the content of inorganic particles and the flexural strength of new condensable composites for posterior teeth in comparison to hybrid conventional composites.Method. The determination of the content of inorganic particles was performed by mass weighing of a polymerized composite before and after the elimination of the organic phase. The volumetric particle content was determined by a practical method based on Archimedes' principle, which calculates the volume of the composite and their particles by differential mass measured in the air and in water. The flexural. strength of three points was evaluated according to the norm ISO 4049:1988.Results. The results showed the following filter content: Alert, 67.26%; Z-100, 65.27%; Filtek P 60, 62.34%; Ariston pHc, 64.07%; Tetric Ceram, 57.22%; Definite, 54.42%; Solitaire, 47.76%. In the flexural strength test, the materials presented the following decreasing order of resistance: Filtek P 60 (170.02 MPa) > Z-100 (151.34 MPa) > Tetric Ceram (126.14 MPa) = Alert (124.89 MPa) > Ariston pHc (102.00 MPa) = Definite (93.63 MPa) > Solitaire (56.71 MPa).Conclusion. New condensable composites for posterior teeth present a concentration of inorganic particles similar to those of hybrid composites but do not necessarily present higher flexural strength. (C) 2003 Elsevier B.V. Ltd. Alt rights reserved.

A systematic study of transfection efficiency and cytotoxicity in HeLa cells using iron oxide nanoparticles prepared with organic and inorganic bases

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Phase Diagrams of the Aqueous Two-Phase Systems of Poly(ethylene glycol)/Sodium Polyacrylate/Salts

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)