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11.
Tassiane C. M. Matsubara Márcio A. Bacchi Elisabete A. De Nadai Fernandes 《Journal of Radioanalytical and Nuclear Chemistry》2012,291(1):201-205
Phosphorus is an essential element for plants and animals, playing a fundamental role in the production of biochemical energy.
Despite its relevance, phosphorus is not commonly determined by instrumental neutron activation analysis (INAA), because 32P does not emit gamma-rays in its decay. There are alternative methods for the determination of phosphorus by INAA, such as
the use of beta counting or the measurement of bremsstrahlung originated from the high energy beta particle from 32P. Here the determination of phosphorus in plant materials by measuring the bremsstrahlung production was further investigated, to optimize an analytical protocol for minimizing interferences and overcoming the poor
specificity. Eight certified reference materials of plant matrices with phosphorus ranging between 171 and 5,180 mg kg−1 were irradiated at a thermal neutron flux of 9.5 × 1012 cm−2 s−1 and measured with a HPGe detector at decay times varying from 7 to 60 days. Phosphorus solutions added to a certified reference
material at three levels were used for calibration. Counts accumulated in the baseline at four different regions of the gamma-ray
spectra were tested for the determination of phosphorus, with better results for the 100 keV region. The Compton scattering
contribution in the selected range was discounted using an experimental peak-to-Compton factor and the net areas of all peaks
in the spectra with energies higher than 218 keV, i.e. Compton edge above 100 keV. Amongst the interferences investigated,
the production of 32P from sulfur, and the contribution of Compton scattering should be considered for producing good results. 相似文献
12.
Camila Elias Elisabete A. De Nadai Fernandes Márcio Arruda Bacchi 《Journal of Radioanalytical and Nuclear Chemistry》2012,291(1):245-250
Brazil holds the second largest population of domestic dogs in the world, with 33 million dogs, only behind the United States.
The annual consumption of dog food in the country is 1.75 million tons, corresponding to the World’s sixth in trade turnover.
Dog food is supposed to be a complete and balanced diet, formulated with high quality ingredients. All nutrients and minerals
required for an adequate nutrition of dogs are added to the formulation to ensure longevity and welfare. In this context,
the present study aimed at assessing the chemical composition of dry dog foods commercialized in Brazil. Thirty-four samples
were acquired in the local market of Piracicaba and analyzed by instrumental neutron activation analysis (INAA) to determine
the elements As, Br, Ca, Co, Cr, Cs, Fe, K, La, Na, Rb, Sb, Sc, Se, U, and Zn. In general, the concentrations of Ca, Fe, K,
Na, and Zn complied with the values required by the Association of American Feed Control Officials (AAFCO). To evaluate the
safety of dog food commercialized in Brazil, further investigation is necessary to better understand the presence of toxic
elements found in this study, i.e. Sb and U. INAA was useful for the screening analysis of different types and brands of dry
dog foods for the determination of both essential and toxic elements. 相似文献
13.
Arroyo M Miguel D Villafañe F Alegria EC Pombeiro AJ 《Dalton transactions (Cambridge, England : 2003)》2012,41(23):7017-7025
Molybdenum and tungsten complexes containing the pypzH (3-(2-pyridyl)pyrazole) ligand as a chelating bidentate are prepared: [Mo(CO)(4)(pypzH)], cis-[MoBr(η(3)-allyl)(CO)(2)(pypzH)], cis-[MoCl(η(3)-methallyl)(CO)(2)(pypzH)], [MI(2)(CO)(3)(pypzH)] (M = Mo, W) from [Mo(CO)(4)(NBD)] or the adequate bis(acetonitrile) complexes. The deprotonation of the molybdenum allyl or methallyl complexes affords the bimetallic complexes [cis-{Mo(η(3)-allyl)(CO)(2)(μ(2)-pypz)}](2) or [cis-{Mo(η(3)-methallyl)(CO)(2)(μ(2)-pypz)}](2) (μ(2)-pypz = μ(2)-3-(2-pyridyl-κ(1)N)pyrazolate-2κ(1)N). The allyl complex was subjected to an electrochemical study, which shows a marked connection between both metallic centres through the bridging pyridylpyrazolates. 相似文献
14.
Tiago Augusto Donegatti Alnilan Lobato Luís Moreira Gonalves Elisabete Alves Pereira 《Electrophoresis》2019,40(22):2929-2935
Aldehydes are important compounds in a large number of samples, especially food and beverages. In this work, for the first time, cyclohexane‐1,3‐dione (CHD) was used as a derivatizing reagent aiming aldehyde (formaldehyde, acetaldehyde, propionaldehyde, and valeraldehyde) analysis by MEKC‐DAD. The optimized separation of the derivates was performed using a voltage program (+20 kV, 0–15 min.; +23 kV, 15–17 min.) at a temperature of 26°C, and using as the running buffer a mixture containing 100 mmol/L of sodium dodecyl sulfate and 29 mmol/L of sodium tetraborate at pH 9.2, with maximum absorbance at 260 nm. CHD was compared with two other derivatizing agents: 3‐methyl‐2‐benzothiazolinone hydrazone and phenylhydrazine‐4‐sulfonic acid. The CHD‐aldehyde derivatives were also characterized by LC‐MS. The calibration curves for all aldehydes had r2 above 0.999 and LODs ranged from 0.01 to 0.7 mg/L. The optimized methodology was applied in sugar cane brandy (cachaça) samples successfully. CHD showed to be an alternative derivatization reagent due to its stability, aqueous solubility, high selectivity and sensitivity, reduced impurities, and simple preparation steps. 相似文献
15.
Bruno M. Soares Ederson R. Pereira Juliana V. Maciel Augusto A. Vieira Fabio A. Duarte 《Journal of separation science》2013,36(20):3411-3418
This work reports the development of a dispersive liquid – liquid microextraction method for the simultaneous extraction, preconcentration, and derivatization of Hg2+ and CH3Hg+ species from water samples for further determination by GC – MS. Some parameters of the proposed method, such as volume and type of disperser and extraction solvent, and Na[B(C6H5)4] concentration were investigated using response surface methodology. Suitable recoveries were obtained using 80 μL C2Cl4 (as extraction solvent), 1000 μL ethanol (as disperser solvent), and 300 μL 2.1 mmol/L Na[B(C6H5)4] (as derivatizing agent). Accuracy was evaluated in terms of recovery and ranged from 87 to 99% with RSD values <7%. In addition, a certified reference material of water (NIST 1641d) was analyzed and agreed with the certified value about 107% (for Hg2+), with RSD values <8.5%. LODs were 0.3 and 0.2 μg/L, with enrichment factors of 112 and 115 for Hg2+ and CH3Hg+, respectively. The optimized method was applied for the determination of Hg2+ and CH3Hg+ in tap, well, and lake water samples. 相似文献
16.
Federico Palazzetti Glauciete S. Maciel Andrea Lombardi Gaia Grossi Vincenzo Aquilanti 《中国化学会会志》2012,59(9):1045-1052
Astrochemistry is a discipline consolidated recently, although its roots extend back to the dawn of early civilization with the observation and mapping of the sky. The way to the understanding of the common natural laws on earth and in space paved by Galilei's observations by the telescope, has been extended in the last decades, by new technologies such as radioastronomy and space missions. Plenty of new chemistry was surprisingly discovered. Extreme rich information on the chemical “composition” of the universe is being obtained, either from the other planets and satellites in the Solar System, from meteorites and comets, or from the interstellar space. In this article we will present selected topics regarding the chemical structures and reactions being discovered. Particular attention will be devoted to aspects considered as relevant for the prebiotic processes on earth, such as those involving chirality and its role played in the origin and evolution of life. 相似文献
17.
Evaluation of tocopherol recovery through simulation of molecular distillation process 总被引:7,自引:0,他引:7
E. B. Moraes C. B. Batistella M. E. Torres Alvarez Rubens Maciel Filho M. R. Wolf Maciel 《Applied biochemistry and biotechnology》2004,114(1-3):689-711
DISMOL simulator was used to determine the best possible operating conditions to guide, in future studies, experimental works.
This simulator needs several physical-chemical properties and often it is very difficult to determine them because of the
complexity of the involved components. Their determinations must be made through correlations and/or predictions, in order
to characterize the system and calculate it. The first try is to have simulation results of a system that later can be validated
with experimental data. To implement, in the simulator, the necessary parameters of complex systems is a difficult task. In
this work, we aimed to determe these properties in order to evaluate the tocopherol (vitamin E) recovery using a DISMOL simulator.
The raw material used was the crude deodorizer distillate of soya oil. With this procedure, it is possible to determine the
best operating conditions for experimental works and to evaluated the process in the separation of new systems, analyzing
the profiles obtained from these simulations for the falling film molecular distillator. 相似文献
18.
In this work, a capillary electrophoresis (CE) method using indirect UV detection (214nm) for the simultaneous determination of monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), diethylethanolamine (DEEA), monocyclohexylamine (MCHA) and dicyclohexylamine (DCHA) in water/ethanol extracts of wrapping materials containing volatile corrosion inhibitors (VCIs) was described. A running buffer consisting of 0.010 molL(-1) imidazole, 0.010 molL(-1) 2-hydroxyisobutyric acid (HIBA) and 0.010 molL(-1) 18-crown-6 ether enabled separation of the analytes in less than 7 min. A few method validation parameters were determined revealing good migration time repeatability (<0.7% RSD) and area repeatability (< 1.8% RSD). Limits of detection were in the range of 0.52-1.54 mg L(-1). Recovery values were in the range of 94.8-100.9%. The methodology was successfully applied to the analysis of three commercial products (VCI treated paper, foam and plastic). The concentration of amines in these materials varied from 0.050 to 22.3% (w/w). 相似文献
19.
Three new compounds bearing furyl, aryl, or thienyl moieties linked to an imidazo-crown ether system (1, 2, and 3) were synthesized and fully characterized by elemental analysis, infrared, UV-vis absorption, and emission spectroscopy, X-ray crystal diffraction, and MALDI-TOF-MS spectrometry. The interaction toward metal ions (Ca(2+), Cu(2+), Ni(2+), and Hg(2+)) and F(-) has been explored in solution by absorption and fluorescence spectroscopy. Mononuclear and binuclear metal complexes using Cu(2+) or Hg(2+) as metal centers have been synthesized and characterized. Compounds 2 and 3 show a noticeable enhancement of the fluorescence intensity in the presence of Ca(2+) and Cu(2+) ions. Moreover compound 3 presents a dual sensory detection way by modification of the fluorimetric and colorimetric properties in the presence of Cu(2+) or Hg(2+). EPR studies in frozen solution and in microcrystalline state of the dinuclear Cu(II)3 complex revealed the presence of an unique Cu(2+) type. 相似文献
20.
Anthony J. Burke Elisabete da Palma Carreiro Nuno M.M. Moura Ana Isabel Rodrigues 《Journal of organometallic chemistry》2007,692(22):4863-4874
In our quest to find new ligands for highly stereoselective reactions, we tested a variety of chiral non-racemic pseudo-C2 symmetric bis-oxazolines derived from malonic acid containing an arylidene bridge unit (and appropriately termed Arylid-Box) in the catalytic asymmetric cyclopropanation (CAP) reaction of styrene and ethyl diazoacetate using between only 1-2 mol% of a Cu(I) pre-catalyst. Some very good e.e.s (up to 86%), were obtained. It was possible to isolate 10a′-[Cu(CH3CN)4]PF6 which existed as a bench stable solid that proved to be more efficient than the catalyst prepared in situ. Cu(I) pre-catalysts were used for the first time in the CAP reaction with the Isbut-Box ligands 13a and 13b and, although, the e.e.s were better for ligand 13a using these pre-catalysts, in the case of ligand 11b this was not the case. Spectroscopic studies (UV-Vis and 1H NMR) were carried out to gain an insight into the nature of the catalytic species at work so that the conditions could be optimised giving better results. Some theoretical studies were conducted to try to explain the better enantioselectivities obtained using Evans’ tert-Box-Cu(I) complex over our complex. 相似文献