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861.
A new class of monocrystalline diamond paste-based electrodes is proposed for the determination of chromium(III) at trace levels in vitamins. Three types of monocrystalline diamond—natural diamond 1 (natural diamond), synthetic diamond 50 (synthetic-1), and synthetic diamond 1 (synthetic-2)—were used for electrode construction. The linear concentration ranges are between 10–10 and 10–8; 10–9 and 10–7, and 10–10 to 10–8 mol L–1, with limits of detection of 10–12, 10–12, and 10–11 mol L–1, when natural diamond, synthetic-1, and synthetic-2, respectively, are used as electrode materials. For electrodes based on natural diamond and synthetic-1 it was found that Cr(III) yields a peak at about +0.275±0.015 V (vs. Ag/AgCl) within a predetermined positive potential range situated between +0.4 and +0.2 V, while for the electrode based on synthetic-2 the peaks are found at +0.300±0.015 V (vs. Ag/AgCl). The proposed method is reliable for the determination of chromium(III) at trace levels in two vitamin tablets (RSD<0.2%). 相似文献
862.
Poly(acrylp-aminobenzenesulfonamideamidine-p-aminobenzenesulfonylamide) chelating fiber containing "S", "N", and "O" elements was synthesized from polyacrylonitrile fiber and p-aminobenzene sulfonamide and used to enrich and separate trace Bi(III), Hg(III), Au(III), and Pd(IV) ions from wastewater and ore sample solution. The enrichment acidity, flow rate, elution conditions, reuse, interference ions, saturated adsorption capacity, constant of adsorption rate, analytical accuracy, and actual samples on chelating fiber were investigated by means of inductively coupled plasma optical emission spectrometry (ICP-OES) with satisfactory results. Solutions of 100 ng mL–1 of Bi(III), Hg(III), Au(III), and Pd(IV) ions can be enriched quantitatively by this chelating fiber at a rate of 1.0 mL min–1 at pH 4 and desorbed quantitatively with 20 mL of 0.25 M HCl and 2% CS(NH2)2 solution at 50 °C (with recovery 97%). When the chelating fiber was reused for 20 times, the recoveries of the analyzed ions enriched by the fiber were still over 95% (except for Hg(III)). One thousand-fold excesses of Mn2+, Ca2+, Zn2+, Mg2+, Fe3+, Cu2+, Ni2+, Al3+, and Ba2+ ions and thousands-fold excesses of Na+ and K+ cause little interference in the pre-concentration and determination of the analyzed ions. The saturated adsorption capacity of Bi(III), Hg(III), Au(III), and Pd(IV) was 4.850×10–4, 3.235×10–4, 2.807×10–4, and 3.386×10–4 mol g–1, respectively. The constants of adsorption rate were 0.409 min–1 for Bi, 0.122 min–1 for Hg, 0.039 min–1 for Au, and 0.080 min–1 for Pd. The relative standard deviations (RSDs) for the enrichment and determination of 10 ng mL–1 Bi(III), Hg(III), Au(III), and Pd(IV) were lower than 2.3%. The results obtained for these ions in actual samples by this method were basically in agreement with the given values with average errors of less than 1.0%. FT-IR spectra shows that the existence of –SO2–Ar, –H2N–Ar, O=C–NH–, HN=C–NH–, and –HN–SO2 functional groups are verified in the chelating fiber. From the FT-IR spectroscopy, we can see that Hg(III), Au(III), and Pd(IV) are mainly combined with nitrogen and sulfur (or oxygen), and Bi(III) is mainly combined with nitrogen (or oxygen) of the groups to form a chelating complex. 相似文献
863.
Masaaki?HanedaEmail author Isao?Nakamura Tadahiro?Fujitani Hideaki?Hamada 《Catalysis Surveys from Asia》2005,9(4):207-215
Comprehensive studies combining surface science and real catalyst were performed to get further insight into catalytic active
site and reaction mechanism for NO decomposition over supported palladium and cobalt oxide-based catalysts. On palladium single-crystal
model catalysts, adsorption, dissociation and desorption behavior of NO was found to be closely related to the surface structures,
the stepped surface palladium being active for dissociation of NO. In accordance with this result, the activity of powder
Pd/Al2O3 catalysts for NO decomposition was directly related to the number of step sites exposed on the surface, suggesting that the
step sites act as the catalytic active site for NO decomposition on Pd/Al2O3. NO decomposition over cobalt oxide was found to be significantly promoted by addition of alkali metals. Surface science
study and catalyst characterization led to the same conclusion that the interface between the alkali metal and Co3O4 serves as the catalytic active site. From the results of in situ Fourier transform infrared (FT-IR) spectroscopy and isotopic transient kinetic analysis, a reaction mechanism was proposed
in which the reaction is initiated by NO adsorption onto alkali metals to form NO2− species and then NO2− species react with the adsorbed NO species to form N2 over the interface between the alkali metal and Co3O4. 相似文献
864.
Marengo E Liparota MC Robotti E Bobba M Gennaro MC 《Analytical and bioanalytical chemistry》2005,381(4):884-895
A new method has been developed for monitoring the degradation of paintings. Two inorganic pigments (ultramarine blue and red ochre) were blended with linseed oil and spread on canvas. Each canvas was subjected to simulated accelerated ageing in the presence of typical degradation agents (UV radiation and acidic solution). Periodically the painted surfaces were analysed by FT-Raman, to investigate the status of the surface. The data obtained were analysed by principal component analysis (PCA). Finally the Shewhart and cumulative sum control charts based on the relevant principal components (PC) and the so called scores monitoring and residuals tracking (SMART) charts were built. The method based on the use of PC to describe the process was found to enable identification of the presence of relevant modification occurring on the surface of the samples studied.Electronic supplementary material Supplementary material is available for this article at 相似文献
865.
Functional characterization of two-dimensional gel-separated proteins using sequential staining 总被引:4,自引:0,他引:4
Proteins separated by two-dimensional (2-D) gel electrophoresis can be visualized using various protein staining methods. This is followed by downstream procedures, such as image analysis, gel spot cutting, protein digestion, and mass spectrometry (MS), to characterize protein expression profiles within cells, tissues, organisms, or body fluids. Characterizing specific post-translational modifications on proteins using MS of peptide fragments is difficult and labor-intensive. Recently, specific staining methods have been developed and merged into the 2-D gel platform so that not only general protein patterns but also patterns of phosphorylated and glycosylated proteins can be obtained. We used the new Pro-Q Diamond phosphoprotein dye technology for the fluorescent detection of phosphoproteins directly in 2-D gels of mouse leukocyte proteins, and Pro-Q Emerald 488 glycoprotein dye to detect glycoproteins. These two fluorescent stains are compatible with general protein stains, such as SYPRO Ruby stain. We devised a sequential procedure using Pro-Q Diamond (phosphoprotein), followed by Pro-Q Emerald 488 (glycoprotein), followed by SYPRO Ruby stain (general protein stain), and finally silver stain for total protein profile. This multiple staining of the proteins in a single gel provided parallel determination of protein expression and preliminary characterization of post-translational modifications of proteins in individual spots on 2-D gels. Although this method does not provide the same degree of certainty as traditional MS methods of characterizing post-translational modifications, it is much simpler, faster, and does not require sophisticated equipment and expertise in MS. 相似文献
866.
867.
A bifunctional amido-thiophene namely hexamethylene (bis-3-thiophene acetamide) (HMTA) was synthesized by the reaction of 3-thiophene acetic acid with hexamethylene diamine. Copolymerization in the presence of thiophene was achieved electrochemically in tetrabutylammonium tetrafluoroborate/acetonitrile (TBAFB/AN). Spectroelectrochemical analysis of the resulting copolymer [P(HMTA-co-Th)] reflected electronic transitions at 505 nm, 740 nm and ∼1000 nm, revealing π to π* transition, polaron and bipolaron band formation respectively. Switching ability was evaluated by a kinetic study via measuring the transmittance (%T) at the maximum contrast. Dual type polymer electrochromic devices (ECDs) based on P(HMTA-co-Th) and poly(ethylene dioxythiophene) (PEDOT) have been constructed. Spectroelectrochemistry, switching ability and stability of the devices were investigated by UV-vis spectroscopy and cyclic voltammetry. These devices exhibit low switching voltages (between 0.0 V and +1.6 V), short switching times with reasonable switching stability under atmospheric conditions. 相似文献
868.
Carper WR Wahlbeck PG Antony JH Mertens D Dölle A Wasserscheid P 《Analytical and bioanalytical chemistry》2004,378(6):1548-1554
The molecular structure and rotational motion of the ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF6]) were studied over a wide temperature range using the Bloembergen–Purcell–Pound 13C NMR spin–lattice relaxation method and NOE factors. Examination of the spin–lattice relaxation times (T
1) and the rates (R
1=1/T
1) of the 1-butyl-3-methylimidazolium cation reveals the relative motions of each carbon in the imidazolium cation. The rotational characteristics of the [BMIM] cation are supported by ab-initio molecular structures of [BMIM][PF6] using density functional theory (DFT) and Hartree–Fock (HF) methods. The ab-initio gas phase structures of [BMIM][PF6] indicate that the 1-butyl-3-methylimidazolium C2 hydrogen, the ring methyl group, and the butyl side-chain hydrogen atoms form hydrogen bonds with the hexafluorophosphate anion. 相似文献
869.
New complexes {M(CO)4[Ph2P(S)P(S)Ph2]} (M = Cr, Mo and W), (1a)–(3a), [(1a), M = Cr; (2a), M = Mo; (3a), M = W] and {M2(CO)10[-Ph2P(S)P(S)Ph2]} (M = Cr, Mo, W), [(1b)–(3b) [(1b), M = Cr; (2b), M = Mo; (3b), M = W]] have been prepared by the photochemical reaction of M(CO)6 with Ph2P(S)P(S)Ph2 and characterized by elemental analyses, f.t.-i.r. and 31P-(1H)-n.m.r. spectroscopy and by FAB-mass spectrometry. The spectra suggest cis-chelate bidentate coordination of the ligand in {M(CO)4[Ph2P(S)P(S)Ph2]} and cis-bridging bidentate coordination of the ligand between two metals in (M = Cr, Mo and W). 相似文献
870.
A simple modification of a previously published ellipticine synthesis is reported, which decreases the reaction time and increases the yield and purity of the product. Benzylic oxidations of 1,4-dimethylcarbazole and ellipticine derivatives were studied and 13-hydroxyellipticine was prepared. 相似文献