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71.
Dehouck P Jaggavarapu PK Desmedt A Van Schepdael A Hoogmartens J 《Electrophoresis》2004,25(18-19):3313-3321
We describe an intermediate precision study on a capillary electrophoretic (CE) method for chlortetracycline. It is shown how in one setup the influence of the factors time, analyst, and equipment on the precision can be investigated. As different types of CE equipments were included, the transferability of the method could be examined. Both the qualitative and quantitative aspect of the method were investigated. It was shown that small adaptations in method conditions can have a large influence on the method transferability. Although the method could be transferred to different types of CE equipments, the precision of the method was found poor when the between-equipment variability was taken into account. Despite the use of an internal standard, the between injection variability was found rather high. 相似文献
72.
J.L. Endrino J.F. Marco P. Poolcharuansin A.R. Phani A. Anders 《Applied Surface Science》2008,254(17):5323-5328
A dielectric barrier discharge (DBD) technique has been employed to produce uniform atmospheric plasmas of He and N2 gas mixtures in open air in order to functionalize the surface of filtered-arc deposited hydrogen-free diamond-like carbon (DLC) films. XPS measurements were carried out on both untreated and He/N2 DBD plasma-treated DLC surfaces. Chemical states of the C 1s and N 1s peaks were collected and used to characterize the surface bonds. Contact angle measurements were also used to record the short- and long-term variations in wettability of treated and untreated DLC. In addition, cell viability tests were performed to determine the influence of various He/N2 atmospheric plasma treatments on the attachment of osteoblast MC3T3 cells. Current evidence shows the feasibility of atmospheric plasmas in producing long-lasting variations in the surface bonding and surface energy of hydrogen-free DLC and consequently the potential for this technique in the functionalization of DLC-coated devices. 相似文献
73.
A domino reaction that is pericyclic in nature is thought to be triggered upon treatment of alkenynol 10 with arylsulfenyl chlorides. The process comprises an ordered sequence of sigmatropic rearrangements: a reversible [2,3]-allyl sulfenate to allyl sulfoxide shift, followed by a [2,3]-propargyl sulfenate to allenyl sulfoxide rearrangement, and last a stereodifferentiating [1,5]-sigmatropic hydrogen migration leading to polyene 13. The occurrence of the C7 to C11 hydrogen migration has been demonstrated by labeling experiments. The double diastereoselection of the [1,5]-sigmatropic hydrogen shift to afford a single isomer of the final polyene 13 is thought to arise from a combination of the electronic effect of the sulfoxide at one terminus, and the steric effect imparted by the bulky trimethylcyclohexenyl substituent at the other terminus. The overall process thus constitutes a stereoselective synthesis of an E,Z,Z-triene fragment from an alkenynol and, in particular, a retinoid with the 7E,9Z,11Z,13E configuration on the conjugated polyenic side chain. Application of this method to the synthesis of retinoids, including labeled analogues, is straightforward. 相似文献
74.
Kabir MS Namjoshi OA Verma R Lorenz M Tiruveedhula VV Monte A Bertz SH Schwabacher AW Cook JM 《The Journal of organic chemistry》2012,77(1):300-310
The stereospecific synthesis of aryloxy and amino substituted E- and Z-ethyl-3-acrylates is of interest because of their potential in the polymer industry and in medicinal chemistry. During work on a copper-catalyzed cross-coupling reaction of ethyl (E)- and (Z)-3-iodoacrylates with phenols and N-heterocycles, we discovered a very simple (nonmetallic) method for the stereospecific synthesis of aryloxy and amino substituted acrylates. To study this long-standing problem on the stereoselectivity of aryloxy and amino substituted acrylates, a series of O- and N-substituted nucleophiles was allowed to react with ethyl (E)- and (Z)-3-iodoacrylates. Screening of different bases indicated that DABCO (1,4-diazabicyclo[2.2.2]octane) afforded successful conversion of ethyl (E)- and (Z)-3-iodoacrylates into aryloxy and amino substituted ethyl acrylates in a stereospecific manner. Herein are the details of this DABCO-mediated stereospecific synthesis of aryloxy and amino substituted E- or Z-acrylates. 相似文献
75.
Kumar BV Priyadharsini SU Prameela GK Mandal AB 《Journal of colloid and interface science》2011,360(1):154-162
The present work was undertaken with a view to understand the influence of a model non-ionic tri-block copolymer PEO-PPO-PEO (poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide)) with molecular weight 5800 i.e., P123 [(EO)(20)-(PO)(70)-(EO)(20)] on the self-aggregation characteristics of the anionic surfactant sodium dodecylsulfate (SDS) in aqueous solution (D(2)O) using NMR chemical shift, self-diffusion and nuclear spin-relaxation as suitable experimental probes. In addition, polymer diffusion has been monitored as a function of SDS concentration. The concentration-dependent chemical shift, diffusion data and relaxation data indicated the significant interaction of polymeric micelles with SDS monomers and micelles at lower and intermediate concentrations of SDS, whereas the weak interaction of the polymer with SDS micelles at higher concentrations of SDS. It has been observed that SDS starts aggregating on the polymer at a lower concentration i.e., critical aggregation concentration (cac=1.94 mM) compared to polymer-free situation, and the onset of secondary micelle concentration (C(2)=27.16 mM) points out the saturation of the 0.2 wt% polymer or free SDS monomers/micelles at higher concentrations of SDS. It has also been observed that the parameter cac is almost independent in the polymer concentrations of study. The TMS (tetramethylsilane) has been used as a solubilizate to measure the bound diffusion coefficient of SDS-polymer mixed system. The self-diffusion data were analyzed using two-site exchange model and the obtained information on aggregation dynamics was commensurate with that inferred from chemical shift and relaxation data. The information on slow motions of polymer-SDS system was also extracted using spin-spin and spin-lattice relaxation rate measurements. The relaxation data points out the disintegration of polymer network at higher concentrations of SDS. The present NMR investigations have been well corroborated by surface tension and conductivity measurements. 相似文献
76.
Phani Motamarri Mrinal Iyer Jaroslaw Knap Vikram Gavini 《Journal of computational physics》2012,231(20):6596-6621
In the present work, we study various numerical aspects of higher-order finite-element discretizations of the non-linear saddle-point formulation of orbital-free density-functional theory. We first investigate the robustness of viable solution schemes by analyzing the solvability conditions of the discrete problem. We find that a staggered solution procedure where the potential fields are computed consistently for every trial electron-density is a robust solution procedure for higher-order finite-element discretizations. We next study the convergence properties of higher-order finite-element discretizations of orbital-free density functional theory by considering benchmark problems that include calculations involving both pseudopotential as well as Coulomb singular potential fields. Our numerical studies suggest close to optimal rates of convergence on all benchmark problems for various orders of finite-element approximations considered in the present study. We finally investigate the computational efficiency afforded by various higher-order finite-element discretizations, which constitutes the main aspect of the present work, by measuring the CPU time for the solution of discrete equations on benchmark problems that include large Aluminum clusters. In these studies, we use mesh coarse-graining rates that are derived from error estimates and an a priori knowledge of the asymptotic solution of the far-field electronic fields. Our studies reveal a significant 100–1000 fold computational savings afforded by the use of higher-order finite-element discretization, alongside providing the desired chemical accuracy. We consider this study as a step towards developing a robust and computationally efficient discretization of electronic structure calculations using the finite-element basis. 相似文献
77.
Shehanaz Bano A. K. Nayak U. B. Misra Y. Balaji Rao C. Phani Babu G. Kalyanakrishnan 《Journal of Radioanalytical and Nuclear Chemistry》2017,312(1):151-160
To accurately determine 241Am by mass spectrometry, interfering elements (IEs) including Bi, Hf, Hg, Pb, Pt, Pu and Tl need to be decontaminated. In this study, the extraction behaviors of IEs in HNO3 and HCl mediums were systematically studied for the employed extraction resins (TRU, DGA-N and DGA-B). Based on the results, chemical separation procedures were proposed. After cooperation with proper co-precipitation methods, the proposed procedures can be used to determine 241Am in environmental samples. The results of evaluation showed that IEs in soil samples were completely removed and 241Am was accurately determined for all proposed procedures. 相似文献
78.
Disorder and long-range interactions are two of the key components that make material failure an interesting playfield for the application of statistical mechanics. The cornerstone in this respect has been lattice models of the fracture in which a network of elastic beams, bonds, or electrical fuses with random failure thresholds are subject to an increasing external load. These models describe on a qualitative level the failure processes of real, brittle, or quasi-brittle materials. This has been particularly important in solving the classical engineering problems of material strength: the size dependence of maximum stress and its sample-to-sample statistical fluctuations. At the same time, lattice models pose many new fundamental questions in statistical physics, such as the relation between fracture and phase transitions. Experimental results point out to the existence of an intriguing crackling noise in the acoustic emission and of self-affine fractals in the crack surface morphology. Recent advances in computer power have enabled considerable progress in the understanding of such models. Among these partly still controversial issues, are the scaling and size-effects in material strength and accumulated damage, the statistics of avalanches or bursts of microfailures, and the morphology of the crack surface. Here we present an overview of the results obtained with lattice models for fracture, highlighting the relations with statistical physics theories and more conventional fracture mechanics approaches.
Statistical models of fracture
Published online:
28 November 2010Table 相似文献
79.
The semileptonic decay width of heavy baryons such as (Λ
b
→ Λcev) has been estimated in the framework of a nonrelativistic field theoretic quark model where four component quark field
operators along with a harmonic oscillator wave function are used to describe translationally invariant hadronic states. The
present estimation does not make an explicit use of heavy quark symmetry and has a reasonable agreement with the experimentally
measured decay width, polarisation ratio and form factors with the harmonic oscillator radii and quark momentum distribution
inside the hadron as free parameters. 相似文献
80.
A chiron approach for the total synthesis of (+)-centrolobine has been described from the commercially available aldehyde 3 employing an acid-catalyzed stereoselective formation of tetrahydropyran ring as the key step. The desired molecule was accomplished in eight steps with 62% overall yield. 相似文献