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1.
Determination of trace elements in biological materials using tetramethylammonium hydroxide for sample preparation 总被引:1,自引:0,他引:1
Patrícia Martins Dirce Pozebon Valderi L. Dressler Gisele A. Kemieciki 《Analytica chimica acta》2002,470(2):62-204
A method to prepare milk powder, bovine liver and bovine muscle samples for analysis by electrothermal atomic absorption spectrometry (ETAAS) is proposed. Samples are mixed with a small amount of tetramethylammonium hydroxide (TMAH) and a stable and homogeneous slurry is produced in ca. 2 h with heating at 60–70 °C. After such sample preparation and dilution with water, trace elements are determined in certified reference materials. Pyrolysis and atomisation temperatures are optimised for each element, and several modifiers are investigated. External calibration is used for every analyte. Limits of detection (LODs), precision and accuracy are reported for Cd, Pb, Ni, Cr, Cu and Ag and compared with those obtained after conventional acid digestion. The main advantages of the proposed method are the simplicity of sample preparation and the longer lifetime of the graphite tube. 相似文献
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Chung MK Orlova G Goddard JD Schlaf M Harris R Beveridge TJ White G Hallett FR 《Journal of the American Chemical Society》2002,124(35):10508-10518
Palladium(0)-catalyzed silane alcoholysis was applied to sugars for the first time using tert-butyldimethylsilane (TBDMS-H) and Ph(3)SiH as the silanes. The catalyst is a colloidal solution of Pd(0) generated in situ from PdX(2) (X = Cl(-), OAc(-)) and TBDMS-H in N,N-dimethylacetamide. The colloid has been characterized by dynamic light scattering and transmission electron microscopy and consists of catalytically highly active nanoparticles of approximately 2 nm diameter. The silane alcoholysis reaction is an effective method for the regioselective silylation of methyl and phenyl glycosides and generates hydrogen gas as the only side product. For many of the sugar substrates investigated, the distribution of regioisomers obtained is complementary to that of the traditional R(3)SiCl/base (base = pyridine, imidazole) methodology and gives convenient access to the 3,6- rather than the 2,6-silylated pyranosides, obtained as the main product by the silyl chloride method. The method also allows a selective axial silylation of levoglucosan and 1,3,5-O-methylidene-myo-inositol. In an attempt to rationalize the observed regioselectivities, ab initio predictions (HF/3-21G) have been made on the relative energies of some of the silylated products. They suggest that the observed regioselectivities do not reflect a kinetic vs thermodynamic product distribution but are induced by the silylation agent employed. Models for the possible origin of the observed regioselectivity in both silylation methods (silane- and silyl chloride-based) are discussed. 相似文献
4.
Antonio Da Costa Christian Mathieu Yolande Barbaux Hilde Poelman Gisele Dalmai-Vennik Lucien Fiermans 《Surface science》1997,370(2-3):339-344
Constant force images of the V2O5(001) surface were recorded in ambient conditions with atomic force microscopy. All images exhibit the 11.5 Å × 3.5 Å. periodicity expected for a bulk terminated surface. However, images reveal differences from the ideal structure. The experimental results are interpreted in terms of preferential adsorption sites for water molecules. Because these sites are thought to influence the catalytic properties of the surface, their characterization is an important step towards understanding how the atomic-scale structure of a surface influences its properties. 相似文献
5.
Facile Synthesis and Structural Characterization by NMR,ESI–MS/MS and DFT Calculations of New (E)‐6‐[2‐Ferrocenylalkylidenehydrazino]nicotinic Hydrazides and Their (E)‐Ferrocenyl‐pyrazolyl‐pyridine Heterocyclic System 下载免费PDF全文
Liliane M. F. Porte Gisele R. Paim Thiago G. Schwanz Alexandre R. Meyer Helio G. Bonacorso Marcos A. P. Martins Nilo Zanatta 《Journal of heterocyclic chemistry》2014,51(5):1333-1339
This paper reports a facile and convenient access by a conventional thermal procedure in ethanol as solvent to a new examples of (E)‐6‐[2‐ferrocenylalkylidenehydrazino]nicotinic hydrazides ( 3 ) (53–72%) from the quimioselective reactions of 6‐hydrazinonicotinc hydrazide ( 1 ) with acylferrocenes ( 2 ), where acyl = formyl and acetyl. Subsequently, cyclocondensation reactions of ferrocenylalkylidene hydrazones ( 3 ) with 4‐R1‐4‐alkoxy‐1,1,1‐trifluoroalk‐3‐en‐2‐ones ( 4 ), where R1 = Me, Ph, 2‐Furyl, to obtain new six heterocyclic derivatives as (E)‐pyrazolyl‐pyridinohydrazones ( 5 ) (58–63%), are also presented. The structures of these new heterocyclic compounds 5 containing an organometallic unit were characterized and studied by NMR, ESI–MS/MS techniques. DFT calculations were also employed to assign the E configuration for compounds 3 and 5 . 相似文献
6.
Protasiewyck GM Nunes FS 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2006,65(3-4):549-552
Herein we describe the synthesis and spectroscopic (infrared and UV-vis) analysis of [Cu(II)(dohpn)(L)](n+) (dohpn=imineoximic tetraazamacrocyclic ligand 2,3,9,10-tetramethyl-1,4,8,11-tetraazaundecane-1,3,8,10-tetraen-11-ol-1-olate) and L=SCN(-), I(-), Cl(-) (n=0) and 4-aminopyridine (ampy), 4,4'-bipyridine (bipy), imidazole (im), 2-aminopyrazine (ampz) and water (n=1+). The following order of the Jahn-Teller stabilization energy (cm(-1)) was observed: I(-)(6452)相似文献
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Carbon Dots (C‐dots) from Cow Manure with Impressive Subcellular Selectivity Tuned by Simple Chemical Modification 下载免费PDF全文
Cintya D'Angelis do E. S. Barbosa Dr. José R. Corrêa Gisele A. Medeiros Gabrielle Barreto Dr. Kelly G. Magalhães Dr. Aline L. de Oliveira Prof. Dr. John Spencer Prof. Dr. Marcelo O. Rodrigues Prof. Dr. Brenno A. D. Neto 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(13):5055-5060
Improved cellular selectivity for nucleoli staining was achieved by simple chemical modification of carbon dots (C‐dots) synthesized from waste carbon sources such as cow manure (or from glucose). The C‐dots were characterized and functionalized (amine‐passivated) with ethylenediamine, affording amide bonds that resulted in bright green fluorescence. The new modified C‐dots were successfully applied as selective live‐cell fluorescence imaging probes with impressive subcellular selectivity and the ability to selectively stain nucleoli in breast cancer cell lineages (MCF‐7). The C‐dots were also tested in four other cellular models and showed the same cellular selection in live‐cell imaging experiments. 相似文献
8.
Lopes WA da Rocha GO Pereira PA Oliveira FS Carvalho LS Bahia Nde C Conceição Ldos S de Andrade JB 《Journal of separation science》2008,31(10):1787-1796
This paper describes the development and optimization, by using multivariate analysis, of a GC-MS-SIM method for evaluation of the 16 polyaromatic hydrocarbons considered as priority pollutants in atmospheric particulate material by the US EPA. In order to assure an adequate separation in the shortest analysis time, a multivariate design was used to set the conditions of the oven temperature program. The optimization process was carried out using factorial fractional design and Box-Behnken design. The following factors were evaluated: initial temperature, temperature rate #1, intermediary temperature, temperature rate #2, and final temperature. The optimized conditions were set at: 70 degrees C (2 min) --> 200 degrees C (30 degrees C/min, 5 min) --> 300 degrees C (5 degrees C/min, 1.67 min). Moreover, we have also optimized the injector temperature as 310 degrees C and sampling time as 0.8 min. The total analysis time was 33 min. Validation of GC-MS-SIM yielded satisfactory results for repetitivity of the detector response and retention times, and linearity of calibration curves. LOD were established as 0.13-0.34 ng/mL (peak area) and 0.18-0.72 ng/mL (peak height). The method has been shown to be appropriate for the analysis of samples of atmospheric particulate material and/or other environmental matrices. 相似文献
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Agricultural residues as sugarcane straw and bagasse are burned in boilers for generation of energy in sugar and alcohol industries.
However, excess of those by-products could be used to obtain products with higher value. Pulping process generates cellulosic
pulps and lignin. The lignin could be oxidized and applied in effluent treatments for heavy metal removal. Oxidized lignin
presents very strong chelating properties. Lignins from sugarcane straw and bagasse were obtained by ethanol–water pulping.
Oxidation of lignins was carried out using acetic acid and Co/Mn/Br catalytical system at 50, 80, and 115 °C for 5 h. Kinetics
of the reaction was accomplished by measuring the UV-visible region. Activation energy was calculated for lignins from sugarcane
straw and bagasse (34.2 and 23.4 kJ mol−1, respectively). The first value indicates higher cross-linked formation. Fourier-transformed infrared spectroscopy data of
samples collected during oxidation are very similar. Principal component analysis applied to spectra shows only slight structure
modifications in lignins after oxidation reaction. 相似文献
10.
Adam Tracz Jeremiasz Jeszka Iwona Kuciska Jean‐Paul Chapel Gisele Boiteux 《Macromolecular Symposia》2001,169(1):129-135
High density polyethylene (PE) was crystallised from the melt on freshly cleaved surface of highly oriented pyrolitic graphite (HOPG) or mica. Atomic force microscopy (AFM) studies of structure of the polymer surface adjacent to the graphite or mica were performed after peeling of from the substrate. Significant differences of crystalline structure on the interface were found between PE crystallised on graphite and mica. The surface of polyethylene crystallised on graphite shows large areas with regularly arranged rectangular structures. These objects (ca 20‐80 nm big) probably represent the nucleation centres of the lamellar growth. The surface of polyethylene crystallised at mica surface shows some dot‐like structures showing no particular arrangement. 相似文献