93 resultados para Dimethyl oxalate
Resumo:
The adsorption of triadimenol (1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-ol) on soil samples with varying contents of organic matter was studied. The adsorption was described by means of the Freundlich's isoterm. An increase in the capacity of adsorption was observed as the content of organic carbon in the matrix increased. That effect was observed when removing the organic matter from the soil, when adding a urban waste compost to the soil sample as well as to the soil sample without organic matter, and also after leaving proportions of urban waste compost incubated in these matrices for a period of 120 days. The results show that the adsorption of the triadimenol in the soil is dependent of its content of organic carbon.
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This article describes a novel approach to the separation of fatty acids ranging from 8 to 20 carbons using capillary electrophoresis with contactless conductivity detection. Complete separation of nine linear chain fatty acids (from C8:0 to C20:0) was achieved in 15 min under normal polarity operation. Limits of detection ranged from 35 to 319 µmol L-1 for C20:0 to C8:0, respectively. The optimized running electrolyte composition was 5.0 mmol L-1 phosphate buffer at pH 7, 4.0 mmol L-1 dimethyl-b-cyclodextrin, 2.0 mmol L-1 trimethyl-b-cyclodextrin, acetonitrile 50% (v/v), and methanol 20% (v/v). The applicability of the separation system was demonstrated by the analysis of coconut vegetable oil.
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Internal energy dependence of the competitive unimolecular dissociation channels of dimethyl ether were studied with the statistical RRKM formalism. The C-O and C-H fission reactions and the 1,2-H and 1,3-H shifts, and 1,1-H2 and 1,3-H2 molecular eliminations are discussed as a function of energy dependence of k a(E*), the microcanonical rate constant for production of transition states. C-O fission is the dominant process while reaction channels involving C-H fission, 1,1-H2 and 1,3-H2 elimination and production of MeOH should be competitive at energies around 400 kJ mol-1. The less favorable process is the channel of CH4 formation.
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Ultra-trace amounts of Cu(II) were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone) -2,2-dimethyl-1,3-propanediimine) (SBTD) followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.
Resumo:
The thermal decomposition reaction of trans-3,6-dimethyl-3,6-diphenyl-1,2,4,5-tetraoxacyclohexane (acetophenone cyclic diperoxide, DPAF), in different solvents (methanol, 1,4-dioxane, acetonitrile and 2-propanol/benzene mixtures) in the initial concentration and temperature ranges of (4.2-10.5) x 10-3 M and 140.0 to 185.0 ºC, respectively, follows a pseudo first order kinetic law up to at least 70% DPAF conversion. An important solvent effect on the rate constant values, activation parameters (DH# and DS#) and reaction products obtained in different solvents is detected, showing that the reaction is accelerated in alcohols.
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A simple flow injection procedure was developed for determining dipyrone (1-phenyl-2,3-dimethyl-4-methylaminomethano-5-pyrazolone sodium, metamizol, analgin) in pharmaceutical formulations. The determination is based on the reduction of Ag+ ions to Ag0 by dipyrone. A colloidal suspension of Ag0 produced was transported by carrier solution (0.01 mol L-1 NaOH) and turbidimetrically detected at 425 nm. The analytical curve for dipyrone was linear in the range from 5.0 x 10-4 to 2.5 x 10-3 mol L-1 with a correlation coefficient of 0.9990. The detection limit was 1.3 x 10-4 mol L-1 (3sigmaB/slope). The relative standard deviation for ten successive measurements was 1.8% and an analytical frequency of 45 h-1 was obtained. The recovery values from three samples ranged from 96.0 to 102%.
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Based on a specially created mass spectral database utilizing 23 tetradecenyl and 22 hexadecenyl acetate standards along with Kóvats retention indices obtained on a very polar stationary phase [poly (biscyanopropyl siloxane)] (SP 2340), (Z)-9-hexadecenyl acetate, (Z)-11-hexadecenyl acetate and (E)-8-hexadecenyl acetate were identified in active pheromone extracts of Elasmopalpus lignosellus. This identification was more efficient than our previous study using gas chromatography/mass spectrometry with a dimethyl disulfide derivative where we could only identify the first two acetates. The acetate composition of the pheromone gland differed from region to region in Brazil and from that from the Tifton (GA, USA) population, suggesting polymorphism or a different sub-species.
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Cleaning solutions containing EDTA are widely employed to remove incrustation despite of the costs involved. The free content of EDTA in commercial solutions may be determined by mixing an aliquot to ammonium oxalate and using a standard calcium solution as titrant. The end-point is detected by the formation of insoluble calcium oxalate after all EDTA is complexed. A system for turbidimetric detection of the end-point was envisaged to substitute the visual detection, which impaired the analyses of dark samples. The proposed method was tested with real samples and good accuracy and precision was obtained.
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The investigation of extracts from six species of marine invertebrates yielded one new and several known natural products. Isoptilocaulin from the sponge Monanchora aff. arbuscula displayed antimicrobial activity at 1.3 mg/mL against an oxacillin-resistant strain of Staphylococcus aureus. Five inactive known dibromotyrosine derivatives, 2 6, were isolated from a new species of marine sponge, Aplysina sp. The sponges Petromica ciocalyptoides and Topsentia ophiraphidites yielded the known halistanol sulfate A (7) as an inhibitor of the antileishmanial target adenosine phosphoribosyl transferase. The ascidian Didemnum ligulum yielded asterubin (10) and the new N,N-dimethyl-O-methylethanolamine (11). The octocoral Carijoa riisei yielded the known 18-acetoxypregna-1,4,20-trien-3-one (12), which displayed cytotoxic activity against the cancer cell lines SF295, MDA-MB435, HCT8 and HL60.
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Bioguided fractionation of the extracts from leaves of Piper mollicomum and Piper lhotzkyanum against the fungi Cladosporium cladosporioides and C. sphaerospermum afforded seven bioactive compounds, four being chromenes: methyl 2,2-dimethyl-2H-chromene-6-carboxylate, methyl 8-hydroxy-2,2-dimethyl-2H-chromene-6-carboxylate, 2-methyl-2-[4'-methyl-3'-pentenyl]-2H-1-benzopyran-6-carboxylic acid, 2,2-dimethyl-2H-chromene-6-carboxylic acid, one a dihydrochalcone: 2',6'-dihydroxy-4'-methoxydihydrochalcone, and two flavanones: 7-methoxy-5,4'-dihydroxy-flavanone and 7,4'-dimethoxy-5-hydroxy-flavanone. The structures of the bioactive isolated derivatives were elucidated by interpretation of their NMR data [¹H and 13C (BBD, DEPT 135º)], and mass spectral data as well as by comparison with data described in the literature.
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This work describes a hydrometallurgical route for processing spent commercial catalysts (CoMo and NiMo/Al2O3). Samples were preoxidized (500 ºC, 5 h) in order to eliminate coke and other volatile species present. The calcined solid was dissolved in concentrated H2SO4 and water (1:1 vol/vol) at 90 ºC; the insoluble matter was separated from the solution. Molybdenum was recovered by solvent extraction using tertiary amines at pH around 1.8. Cobalt (or nickel) was separated by addition of aqueous ammonium oxalate at the above pH. Phosphorus was removed by passing the liquid through a strong anion exchange column. Aluminum was recovered by neutralizing the solution with NaOH. The route presented in this work generates less final aqueous wastes because it is not necessary to use alkaline medium during the metal recovery steps.
Caracterização das O-acetil-(4-O-metilglicurono)xilanas isoladas da madeira de Eucalyptus urograndis
Resumo:
The O-acetyl-4-O-methyl-(glucurono)xylans were isolated from E. urograndis by extraction with dimethyl sulfoxide, analysed for monosaccharide composition and structurally characterized by NMR spectroscopy. These xylans contained one 4-O-methyl-glucuronic acid substituent and 5.5 acetyl groups for approximately 10 xylose residues. About 10% of 4-O-methyl-glucuronic acid (MeGlcA) units were branched at O-2. The O-acetyl-4-O-methyl-(glucurono)-xylans were composed of the following (1 → 4)-linked β-D-xylopyranosyl structural elements: unsubstituted (51 mol%), 2-O-acetylated (12 mol%), 3-O-acetylated (20 mol%), 2,3-di-O-acetylated (6 mol%) and [MeGlcA α-(1 → 2)] [3-O-acetylated] (11 mol%). The weight-average molar mass and polydispersity of this xylan were 34.9 kDa and 1.16, respectively, as measured by size-exclusion chromatography.
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The chemical investigation of the hexane and ethanol extracts from aerial parts of Vernonia chalybaea conducted to the isolation and characterization of a new aliphatic tetrahydroxyl ether, along with a series of known compounds such as 4 α,10 α-epoxyaromadendrane, friedelin, taraxasteryl acetate, pseudotaraxasteryl acetate, lupeyl acetate, lupeol, α-amiryn, β-amiryn, β-sitosterol, stigmasterol, 2,3-dimethyl-1,2,3-tri-hydroxybuthanol, angophorol, angophorol-7-O-glucoside, angophorol-7-O-rutinoside, 3,7-dimethoxy-5,3',4'-trihydroxyflavone and acacetin. The structures of all compounds were determined by spectroscopic analysis and comparison with published spectral data.
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This work aimed to assess the photocatalytic degradation of a model odor compound (dimethyl disulfide, DMDS), found in liquid and gaseous wastes of plants for processing poultry byproducts. The effect of pH and temperature on adsorption and photocatalytic degradation was evaluated through factorial experimental designs. The results suggest the presence of an optimum region for adsorption, at 45.0 ºC and pH 4.0. In the photocatalytic runs an optimum for temperature and pH was also observed. At 45 ºC and pH 4.0 the removal of DMDS was 99% after 60 min of irradiation.
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The anti-Mycobacterium tuberculosis activity of Campomanesia adamantium fruits extracts were evaluated. Six compounds, identified as flavanones and chalcones were quantified by HPLC-DAD-UV. Promising antitubercular activity was observed with ethyl acetate extract (MIC 62.5 µg/mL) and their fractions (MIC values ranging from 39 to above 250 µg/mL). The better MIC result of 39 µg/mL was associated with two fractions that contain bigger amounts of 5,7-dihydroxy-6, 8-di-C-methylflavanone and 2',4'-dihydroxy-3',5'-dimethyl-6'-methoxychalcone. These compounds exhibited MICs >250 and 62.5 µg/mL, respectively, while their mixtures showed values ranging from 62.5 to 7.8 µg/mL, demonstrating a synergism between them.