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991.
O. M. Radul M. Z. Krimer O. N. Rebrova V. N. Biyushkin I. V. Feofanova A. A. Panasenko 《Russian Chemical Bulletin》1993,42(3):522-527
The rearrangement of enol acylates of aryl 1H-1, 2, 4-triazol-1-ylmethyl ketones at 140–150°C in acetic anhydride is studied. The migration of the acyl group to the C(5) atom of the heterocycle is found to be intramolecular. The characteristics of the original and final products are presented. X-ray structural studies of the enol acetates of 2, 4-dichlorophenyl 1H-1, 2, 4-triazol-1-ylmethyl ketone and 2, 4-dichlorophenyl 5-acetyl-1H-1, 2, 4-triazol-1-ylmethyl ketone are carried out.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 560–564, March, 1993. 相似文献
992.
Jenn-Lin Lin 《中国化学会会志》1984,31(4):395-399
The reaction of 3-(4-phenyl-2-pyridyl)-5,6-diphenyl-1,2,4-triazine (PPDT) and tetraphenylborate (TPB) with cobalt (II) has been studied to determine the optimum conditions for the extraction and quantitative spectrophotometry determination of this metal. The ternary complex is extracted into molten naphthalene at pH 3.6–7.4. The solid naphthalene containing the cobalt associated complex is separated by filtration and dissolved in acetonitrile. Beer's law is obeyed in the concentration range 8–140 μg cobalt in 10 ml of acetonitrile solution. The molar absorptivity and sensitivity are 4.2×103 l·mol?1·cm?1 and 0.01408 μg/cm2, respectively. The other factors such as pH, amounts of reagents and naphthalene, shaking and standing times, and the effect of diverse ions are studied. The method has been applied to the determination of cobalt in iron steel alloys. 相似文献
993.
R. WinterP.G. Nixon R.J. TerjesonJ. Mohtasham N.R. HolcombD.W. Grainger D. GrahamD.G. Castner G.L. Gard 《Journal of fluorine chemistry》2002,115(2):107-113
A new perfluorinated acrylate monomer containing the SF5(CF2)6-perfluorinated side chain was synthesized and polymerized into films. Bulk monomer characterization is consistent with the molecular structure based on FTIR, mass spectrometry and NMR analyses. The surface properties of polymer coatings were studied with aqueous wetting (contact angle) and X-ray photoelectron spectroscopy (XPS) methods. The surface composition is shown to be highly enriched in the terminal side chain SF5-chemistry and exhibits properties consistent with a highly apolar, non-wetting perfluorinated polymer surface. Depth-dependent XPS studies using angular-resolved methods (ADXPS) confirmed a non-stoichiometric enrichment of sulfur and fluorine at the film ambient interface, consistent with a surface presence of the terminal SF5-group and possibly film structural anisotropy in the surface zone. Time-of-flight (TOF) secondary ion mass spectrometry (SIMS) analysis supplements the XPS data by showing the presence of all expected SF5-acrylate chemistry components in the outer 15 Å of the film surface. 相似文献
994.
M.G.?CarvalhoEmail author J.M.R.C.A.?Santos A.A.?Martins M.M.?Figueiredo 《Cellulose (London, England)》2005,12(4):371-383
In this work attention has been focused on the effects of papermaking beating, web forming and sizing operations on the physical/chemical
surface properties of bleached Eucalyptus globulus kraft fibres. Inverse gas chromatography (IGC) was used to determine the dispersive component of surface tension (γsd) as well as the acidic/basic character (according to the Lewis concept) of the solid surfaces (pulp fibres and pulp handsheets).
The results have shown that the main effect of beating is to increase the fibre's Lewis acidic character. Web forming caused
a strong decrease in γsd and significant increments in the adhesion works of both acidic and basic probes, lowering the ratio between the two. Nevertheless,
the surface of handsheets still exhibited a dominant acidic character. The sizing operation did not change the dispersive
component of the surface tension significantly but decreased the difference between the adhesion works of the acidic and basic
probes, rendering the handsheet surface less Lewis acidic and more Lewis basic. Thus, although internal sizing is expected
to strongly influence liquid spreading at the paper surface and liquid penetration of the fibre's network, it is concluded
that beating and web forming lead to important changes in the surface energetic properties of the Eucalyptus globulus kraft fibres. 相似文献
995.
辉光放电原子发射光谱法快速分析生铸铁 总被引:3,自引:0,他引:3
通过对辉光光源参数-放电电流、放电电压、预溅射时间和分析时间对生铸铁标样放电强度和稳定性影响的研究,优化光源参数,建立了辉光放电原子发射光谱法同时测定生铸铁中碳、硅、锰、磷、硫等12个元素的快速分析方法。分析生铸铁试样时发现了不同灰口铸铁在碳分析结果方面存在偏差,对碳的偏差进行了讨论并通过制样条件和光源参数的调整可以有效地减小偏差。通过对不同生铸铁样品进行准确度和精密度试验,结果表明:分析结果与标准值或化学法结果一致。分析一件试样的时间仅需2~5 min。 相似文献
996.
化学气相淀积法合成氮化铝薄膜及其工艺设计 总被引:1,自引:0,他引:1
对AlBr3-NH3-N2体系化学气相淀积法合成A1N膜进行了热力学分析和工艺设计,研究了在不同淀积温度和体系总压时,体系中主要气态物种的平衡分压和A1N膜的理论淀积速率与源温和载气流量的关系,并与微波等离子体化学气相淀积A1N膜的实验结果进行了比较。 相似文献
997.
With frontal analysis(FA),the dependence of adsorption isotherms of insulin on the composition of mobile phase in reversed phase liquid chromatography (RPLC) has been investigated,This is also a good example to employ the stoichiometric displacement theory (SDT) for ivestigating solute adsorption in physical chemistry.Six kinds of mobile phase in RPLC were employed to study the effects on the elution curves and adsorption isotherms of insulin.the key points of this paper are:(1) the stability of insulin due to delay time after preparing,the organic solvent concentration,the kind and the concentration of ion-pairing agent in mobile phase were found to affect both elution curve and adsorption isotherm very seriously.(2)To obtain a valid and comparable result,the composition of the mobile phase employed in FA must be as same as possible to that in usual RPLC of either analytical scale or preparative purpose.(3)Langmuir Equation and the SDT were employed to imitate these obtained adsorption isotherms.The expression for solute adsorption from solution of the SDT was found to have a better elucidation to the insulin adsorption from mobile phase in RPLC. 相似文献
998.
蛋白质水解液中氨基酸组成的定量分析 总被引:12,自引:0,他引:12
以氯甲酸-9-芴基甲酯(FMOC-Cl)为柱前衍生化试剂在液相色谱上分离17种常见氨基酸的衍生物并测定其摩尔吸光系数。用绝对分析法和标准曲线法对标准氨基酸溶液进行了定量分析,除组氨酸外两种方法测定结果的相对偏差为5.00%以内。对氨基酸的稳定性进行了模拟水解实验,发现在110℃/24h的水解条件下,丝氨酸等不稳定氨基酸的降解较在150℃/1.5h条件下小。用绝对分析法测定测定了牛胰岛素不同水解条件下水解液中氨基酸的含量,大部分氨基酸的相对收率都接近100%。 相似文献
999.
Principal component analysis (PCA) is applied to 32 disubstituted unsaturated compounds (Y–CH2–X): cyanides, oximes and propenes; bearing 12 -substituents: F, Cl, Br, I, OMe, OEt, SMe, SEt, NMe2, NEt2, Me, and Et. The experimental 13C chemical shifts for the -carbon and functional carbon atoms are correlated with theoretically derived molecular properties, i.e. partial charges, electronegativity, hardness, dipole moments and the nuclear repulsion energies. In the first PCA, the clustering of these three classes of organic compounds occurred mostly because of the chemical shifts and partial charges, and also of the dipole moments, hardness and electronegativity parameters as confirmed by loading graph. A strong grouping is observed in the second PCA, showing the chemical shift dependence on the type of heteroatom substituents. Therefore, sulfur, nitrogen, oxygen and neutral groups exhibit four types of C-13 SCS influences, indicating that the heteroatom (Y) properties play a significant role on the effects on chemical shifts. The -halogenated compounds represent a very heterogeneous group due to possible orbital interactions between the functional group and the substituent. The third PCA shows the grouping of F, Cl, Br and I derivatives, confirming the second PCA results that same halogen presents the same or very similar effects on the chemical shifts. 相似文献
1000.
Molecular dynamics simulations of double-helical DNA oligomers have been performed to investigate differences in the structure, dynamics, and hydration of F-F and T-T mispairs. Hexamers containing F-F pairs were found to be more dynamic, especially in the region of the mispair itself. This dynamic variability derives from greater flexibility of F-F pairs. The T-T mispairs, on the other hand, were found to be comparatively tightly bound as wobble pairs. The major and minor groove edges of the T-T pairs were observed to be solvated at exposed carbonyl positions by at least one water molecule, while F-F pairs lacked solvating waters. Stacking interactions were nearly identical for T-T and F-F pairs, leading to similar average structures, even though F stacking was more dynamically variable. Solvation differences between F-F and T-T therefore support the steric exclusion model for nucleotide incorporation in DNA replication. Large differences in the orientation of minor groove functional groups, in addition to differences in solvation, further rationalize why F bases present during DNA extension events induce stalls. Two novel nucleotides are proposed to further elucidate minor groove interactions of DNA with polymerase molecules.Electronic Supplementary Material This Material consists of equilibration protocol, plots of center-of-mass stacking, water radial distribution functions, helical parameter dynamics, and dynamics data for a control AT sequence. Supplementary material is available in the online version of this article at Contribution to the Jacopo Tomasi Honorary Issue 相似文献