80 resultados para mass determination
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Avaliou-se o método de determinação gravimétrica da matéria orgânica do solo pela perda de massa por incineração a 300ºC e comparou-se com o carbono determinado pelo método Walkley-Black. Os dois métodos foram correlacionados positivamente com a seguinte equação de regressão linear: y = 3,720x + 0,2914. r = 0,937. O coeficiente. 3,720 foi maior do que os encontrados na literatura. que variaram de 1,68 a 2,13. Esta diferença foi atribuída ao maior grau de oxidação da matéria orgânica dos solos das regiões tropicais. O método de incineração é aplicável para determinação do C do solo em rotina. O método não contamina o meio ambiente com metal tóxico (Cr6+) e não oferece riscos aos analistas com o uso de ácido sulfúrico concentrado.
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A method for the direct determination of Pb in wines by simultaneous multi-element atomic absorption spectrometry (SIMAAS) using a transversely heated graphite atomizer, Zeeman-effect background corrector and internal standardization is proposed. Bismuth was used as an internal standard and Pd(NO3)(2) plus Mg(NO3)(2) as chemical modifier,to stabilize both the analyte and the internal standard. The implementation of two pyrolysis steps avoided any build-up of carbonaceous residues on the graphite platform. All diluted samples (1 + 1 v/v) in 0.2% v/v HNO3 and reference solutions (5.0-50 mug l(-1) Ph in 0.2% v/v HNO3) were spiked with 25 mug l(-1) Bi. For a 20 mul aliquot dispensed into the graphite tube, a good correlation (r = 0.9997) was obtained between the ratio of the analyte signal to the internal standard signal and the analyte concentration of the reference solutions. The electrothermal behaviour of Pb and Bi in red, white and rose wines were compared. In addition, absorbance variations due to changes in experimental conditions, such as atomizer temperature, integration time, injected sample volume, radiation beam intensity, graphite tube surface, dilution and sample composition, were minimized by using Bi as internal standard. Relative standard deviations of measurements based on integrated absorbance varied from 0.1 to 3.4% and from 0.5 to 7.3% (n = 12) with and without internal standard correction, respectively. Good recoveries (91-104%) for Pb spikes were obtained. The characteristic mass was 45 pg Pb and the limit of detection based on integrated absorbance was 0.9 mug l(-1) Pb. Internal standardization increased the lifetime of the tube by 25%. Direct determinations of Pb in wines with and without internal standardization approaches were in agreement at the 95% confidence level. The repeatability and the tube lifetime were improved when using Bi as internal standard. The improvement in accuracy using an internal standard was only observed when the analytical results were affected by errors.
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A method for the direct determination of Ni in soft drinks by graphite furnace atomic absorption spectrometry using a transversely heated graphite atomizer (THGA), Zeeman-effect background corrector, and Co as the internal standard (IS) is proposed. Magnesium nitrate was used to stabilize both Ni and Co. All diluted samples (1+1) in 0.2% (v/v) HNO3 and reference solutions [5.0-50 mu g L-1 Ni in 0.2% (v/v) HNO3] were spiked with 50 mu g L-1 Co. For a 20-mu L sample dispensed into the atomizer, correlations between the ratio of absorbance of Ni to absorbance of Co and the analyte concentration were close to 0.9996. The relative standard deviation of the measurements varied from 0.5 to 3.4% and 1.0 to 7.0% (n=12) with and without IS, respectively. Recoveries within 98-104% for Ni spikes were obtained using IS. The characteristic mass was calculated as 43 pg Ni and the limit of detection was 1.4 mu g L-1. The accuracy of the method was checked for the direct determination of Ni in soft drinks and the results obtained with IS were better than those without IS.
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A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer (THGA((R))) used together with Pd(NO3)(2) + Mg(NO3)(2) as modifier is proposed for the direct determination of lead in vinegar by graphite furnace atomic absorption spectrometry. The optimized heating program (temperature, ramp time, hold time) of atomizer involved drying stage (110 degrees C, 5 s, 30 s; 130 degrees C, 5 s, 30 s), pyrolysis stage (1000 degrees C, 15 s, 30 s), atomization stage (1800 degrees C, 0 s, 5 s) and clean-out stage (2450 degrees C, I s, 3 s). For 10 mu L of vinegar delivered into the atomizer and calibration using working standard solutions (2.5-20.0 mu g L-1 Pb) in 0.2% (v/v) HNO3, analytical curve with good linear correlation (r = 0.9992) was established. The characteristic mass was 40 pg Pb and the lifetime of the tube was around 730 firings. The limit of detection (LOD) was 0.4 mu g L-1 and the relative standard deviations (n = 12) were typically <8% for a sample containing 25 pg L-1 Pb. Accuracy of the proposed method was checked after direct analysis of 23 vinegar samples. A paired t-test showed that results were in agreement at 95% confidence level with those obtained for acid-digested vinegar samples. The Pb levels varied from 2.8 to 32.4 pg L-1. Accuracy was also checked by means of addition/recovery tests and recovered values varied from 90% to 110%. Additionally, two certified reference materials were analyzed and results were in agreement with certified values at a 95% confidence level. (C) 2006 Elsevier Ltd. All rights reserved.
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Parkia platycephala lectin 2 was purified from Parkia platycephala (Leguminosae, Mimosoideae) seeds by affinity chromatography and RP-HPLC. Equilibrium sedimentation and MS showed that Parkia platycephala lectin 2 is a nonglycosylated monomeric protein of molecular mass 29 407 +/- 15 Da, which contains six cysteine residues engaged in the formation of three intramolecular disulfide bonds. Parkia platycephala lectin 2 agglutinated rabbit erythrocytes, and this activity was specifically inhibited by N-acetylglucosamine. In addition, Parkia platycephala lectin 2 hydrolyzed beta(1-4) glycosidic bonds linking 2-acetoamido-2-deoxy-beta-D-glucopyranose units in chitin. The full-lengthamino acid sequence of Parkia platycephala lectin 2, determined by N-terminal sequencing and cDNA cloning, and its three-dimensional structure, established by X-ray crystallography at 1.75 angstrom resolution, showed that Parkia platycephala lectin 2 is homologous to endochitinases of the glycosyl hydrolase family 18, which share the (beta alpha)(8) barrel topology harboring the catalytic residues Asp125, Glu127, and Tyr182.
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This paper reports the separation and identification of indole alkaloids, steroids and triterpenoids from the ethanolic extracts of Tabernaemontana hilariana (Apocynaceae). The alkaloidal fractions from the ethanolic extracts obtained (root barks, green fruits, ripe fruits and seeds) were fractionated and analysed by thin-layer chromatography, capillary gas chromatography-flame ionization detection (cGC-FID) as well as by high-resolution gas chromatography-mass spectrometry (HRGC-MS). 3-Hydroxycoronaridine, ibogamine, coronaridine pseudoindoxyl, coronaridine, catharanthine, voacangine hydroxyindolenine, voacangine pseudoindoxyl, tabernanthine, tetraphyllicine, 3-hydroxyvoacangine, voacangine, isovoacangine and 3-oxocoronaridine were identified. The insoluble fraction of ethanolic extracts obtained from the root barks and green fruits were analysed and ten aliphatic constituents were also identified by cGC-FID and HRGC-MS. (C) 1998 Elsevier B.V. B.V. All rights reserved.
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A method has been developed for the direct determination of As in sugar by graphite furnace atomic absorption spectrometry with a transversely heated graphite atomizer (end-capped THGA) and longitudinal Zeeman-effect background correction. The thermal behavior of As during the pyrolysis and atomization steps was investigated in sugar solutions containing 0.2% (v/v) HNO3 using Pd, Ni, and a mixture of Pd + Mg as the chemical modifiers. For a 60-muL sugar solution, an aliquot of 8% (m/v) in 0.2% (v/v)HNO3 was dispensed into a pre-heated graphite tube at 70 degreesC. Linear analytical curves were obtained in the 0.25 - 1.50-mug L-1 As range. Using 5 mug Pd and a first pyrolysis step at 600 degreesC assisted by air during 40 s, the formation of a large amount of carbonaceous residue inside the atomizer was avoided. The characteristic mass was calculated as 24 pg As and the lifetime of the graphite tube was around 280 firings. The limit of detection (L.O.D.) based on integrated absorbance was 0.08 mug L-1 (4.8 pg As) and the typical relative standard deviation (n = 12) was 7% for a sugar solution containing 0.5 mug L-1. Recoveries of As added to sugar samples varied from 86 to 98%. The accuracy was checked in the direct analysis of eight sugar samples. A paired t-test showed that the results were in agreement at the 95% confidence level with those obtained for acid-digested sugar samples by GFAAS.