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A multi-analyte method without any pre-treatment steps using reversed-phase liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was developed and applied for the determination of 20 primary aromatic amines (PAA) associated with polyurethane (PUR) products or azo-colours. The method was validated in-house for water and 3% acetic acid food simulants using spiked migrates from plastic laminates. Detection limits ranged from 0.27 to 3 microg amine/L food simulants, and RSD values of within-laboratory reproducibility at the 2 microg PAA/L level ranged from 3.9 to 19%. PAA migration from plastic laminates and black nylon cooking utensils were determined with the method, and high levels of 4,4'-methylenedianiline and aniline were found in migrates from about half of the tested cooking utensils. The method fulfils present legislative demands in the EU for screening and verification of PAA migration from food contact materials. 相似文献
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Synthesis of fused imidazo-pyridine and -azepine derivatives by sequential van Leusen/Heck reactions
Fused imidazo-pyridine and -azepine derivatives were synthesized using a sequential van Leusen/intramolecular Heck protocol. The combination of a multicomponent reaction followed by an intramolecular carbon-carbon bond forming reaction generates heterocycles of significant molecular complexity from readily available starting materials in just two steps. 相似文献
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Amashukeli X Gruhn NE Lichtenberger DL Winkler JR Gray HB 《Journal of the American Chemical Society》2004,126(47):15566-15571
Inner-sphere electron-transfer reorganization energies of Zn(protoporphyrin IX) and Zn(octaethylporphyrin) are determined from band-shape analyses of the first ionization obtained by gas-phase valence photoelectron spectroscopy. The experimentally determined total inner-sphere reorganization energies for self-exchange (120-140 meV) indicate that structural changes upon oxidation are largely confined to the porphyrin ring, and substituents on the ring or solvent and other environmental factors make smaller contributions. Computational estimates by different models vary over a wide range and are sensitive to numerical precision factors for these low reorganization energies. Of current computational models that are widely available and practical for molecules of this size, functionals that contain a mixture of Hartree-Fock exchange and DFT exchange-correlation appear to be the most applicable. 相似文献
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Filip X Tripon C Filip C 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2005,176(2):239-243
A new heteronuclear decoupling mechanism under fast magic-angle spinning MAS is introduced. It is based on refocusing the coherences responsible for the dephase of low-gamma nuclei ((13)C, (15)N) transverse spin-polarization in the presence of strongly dipolar-coupled protons, and has the advantage that can be implemented by pulsed techniques, with all the benefits resulting from a reduced duty cycle compared with conventional decoupling by continuous rf irradiation. The decoupling efficiency of a simple rotor-synchronized Hahn-echo pulse train is analyzed both theoretically and experimentally. It was found that a substantial improvement in sensitivity and resolution can be achieved in compounds with small (1)H chemical shielding parameters even at moderate sample spinning, and some interesting applications are shown. It is also shown that much faster spinning frequencies, or alternative refocusing sequences, are needed for applications on rigid organic solids, i.e., in systems with larger (1)H chemical shifts. 相似文献
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H. E. Cox N. Evers J. Hetzer American Chemical Society F. W. Smither R. E. Divine C. P. Long M. L. Sheely H. P. Trevithick P. H. Walker G. Knigge C. Bergell A. Korennowa M. T. Bolschakowa E. Randa American Oil Chemist Society N. Spasskij S. Pleschkowa und A. Chernitschkina 《Fresenius' Journal of Analytical Chemistry》1939,117(5-6):225-234
Ohne Zusammenfassung 相似文献
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A. D. Bauer C. S. Ford A. K. Church J. H. Wilson P. A. Popow J. Davidsohn G. Knigge E. Walter F. Wittka E. J. Better K. Scheringa Per Ekwall H. Janistyn P. Wulff W. Poethke W. Bleyberg H. Lettner J. W. Mc Bain H. E. Martin und E. L. Lederer 《Fresenius' Journal of Analytical Chemistry》1936,104(7-8):306-316
Ohne Zusammenfassung 相似文献
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A construction of grand unified models of the strong, weak and electromagnetic interactions is described based on the transformation properties of the group generators under a maximal subgroup decomposition without recourse to large representation matrices or to the specific algebraic structures of some classical Lie-groups, such as the Clifford algebra associated with the orthogonal groups or the octonionic structure of the exceptional groups. To illustrate the procedure an explicit construction is given of the SU(5) model useful in the discussion of higher rank groups, of SO(10) under the maximal subalgebras SU(2)L × SU(2)R × SU(4)c and SU(5) × U(1)r and of the exceptional group E6 under SU(3)L × SU(3)R × SU(3)c and SO(10) × U(1)t. The construction procedure can be used as well with any classical Lie-group. 相似文献
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In two experiments we explored the instructional value of a cross‐domain mapping between “number” and “line” in secondary school students' understanding of density. The first experiment investigated the hypothesis that density would be more accessible to students in a geometrical context (infinitely many points on a straight line segment) compared to a numerical context (infinitely many numbers in an interval). The participants were 229 seventh to eleventh graders. The results supported this hypothesis but also showed that students' conceptions of the line segment were far from that of a dense array of points. We then designed a text-based intervention that attempted to build the notion of density in a geometrical context, making explicit reference to the number-to-points correspondence and using the “rubber line” bridging analogy (the line as an imaginary unbreakable rubber band) to convey the no-successor principle. The participants were 149 eighth and tenth graders. The text intervention improved student performance in tasks regarding the infinity of numbers in an interval; the “rubber line” bridging analogy further improved performance successfully conveying the idea that these numbers can never be found one immediately next to the other. 相似文献
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Xenia Engelmann Deesha D. Malik Teresa Corona Katrin Warm Erik R. Farquhar Marcel Swart Wonwoo Nam Kallol Ray 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2019,131(12):4052-4056
The generation of a nonheme oxoiron(IV) intermediate, [(cyclam)FeIV(O)(CH3CN)]2+ ( 2 ; cyclam=1,4,8,11‐tetraazacyclotetradecane), is reported in the reactions of [(cyclam)FeII]2+ with aqueous hydrogen peroxide (H2O2) or a soluble iodosylbenzene (sPhIO) as a rare example of an oxoiron(IV) species that shows a preference for epoxidation over allylic oxidation in the oxidation of cyclohexene. Complex 2 is kinetically and catalytically competent to perform the epoxidation of olefins with high stereo‐ and regioselectivity. More importantly, 2 is likely to be the reactive intermediate involved in the catalytic epoxidation of olefins by [(cyclam)FeII]2+ and H2O2. In spite of the predominance of the oxoiron(IV) cores in biology, the present study is a rare example of high‐yield isolation and spectroscopic characterization of a catalytically relevant oxoiron(IV) intermediate in chemical oxidation reactions. 相似文献