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1.
Criterion for quantifying the reliability of analytical results in method development and evaluation
An important characteristic in judging analytical results for their suitability for a particular use is the reliability of the results. A procedure is developed for quantifying the reliability in a single measure, the maximum total error. This measure comprises both the bias and the precision of the results, and takes account of the statistical uncertainty of these estimates. The applicability of the procedure in method development and method evaluation is illustrated by means of a practical example, the flow-injection determination of orthophosphate. 相似文献
2.
The quantitative validation of the results of a flow-injection determination of penicillin in pharmaceutical formulations is described. The validation procedure is done by using VALID, which is a generally applicable validation program based on an expert system program. The automated penicillin assay is based on the enzymatic hydrolysis of the penicillin to the corresponding penicilloic acid, which reacts with iodine generated on-line; the iodine consumption is detected amperometrically. The method is evaluated for applicability in pharmaceutical quality control. The complete validation procedure is described. During the program run, the system evaluates the calibration procedure, the drift of the analytical systemm and the effect of the sample matrix. The reliability of the flow-injection method is estimated by evaluating the maximum total error (MTE), which includes both random error and systematic error. The latter was assessed by comparing of the results of the flow-injection method with the results obtained by titration with mercury(II) as the reference method. The user requirement for the assay was an MTE of 10%. The validation procedure showed that the analytical method complied with the requirements for the major part of the concentration range (0.066–0.25 mM). 相似文献
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Dr. Laura Orian Lando P. Wolters Prof. Dr. F. Matthias Bickelhaupt 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(40):13337-13347
A mechanistic density functional theory study of acetylene [2+2+2] cyclotrimerization to benzene catalyzed by RhI half metallocenes is presented. The catalyst fragment contains a heteroaromatic ligand, that is, the 1,2‐azaborolyl (Ab) or the 3a,7a‐azaborindenyl (Abi) anions, which are isostructural and isoelectronic to the hydrocarbon cyclopentadienyl (Cp) and indenyl (Ind) anions, respectively, but differ from the last ones on having two adjacent carbon atoms replaced with a boron and a nitrogen atom. The better performance of either the classic hydrocarbon or the heteroaromatic catalysts is found to depend on the different mechanistic paths that can be envisioned for the process. The present analyses uncover and explain general structure–reactivity relationships that may serve as rational design principles. In particular, we provide evidence of a reverse indenyl effect. 相似文献
4.
Inside Cover: New Concepts for Designing d10‐M(L)n Catalysts: d Regime,s Regime and Intrinsic Bite‐Angle Flexibility (Chem. Eur. J. 36/2014) 下载免费PDF全文
5.
New Concepts for Designing d10‐M(L)n Catalysts: d Regime,s Regime and Intrinsic Bite‐Angle Flexibility 下载免费PDF全文
Lando P. Wolters Dr. Willem‐Jan van Zeist Prof. Dr. F. Matthias Bickelhaupt 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(36):11370-11381
Our aim is to understand the electronic and steric factors that determine the activity and selectivity of transition‐metal catalysts for cross‐coupling reactions. To this end, we have used the activation strain model to quantum‐chemically analyze the activity of catalyst complexes d10‐M(L)n toward methane C?H oxidative addition. We studied the effect of varying the metal center M along the nine d10 metal centers of Groups 9, 10, and 11 (M=Co?, Rh?, Ir?, Ni, Pd, Pt, Cu+, Ag+, Au+), and, for completeness, included variation from uncoordinated to mono‐ to bisligated systems (n=0, 1, 2), for the ligands L=NH3, PH3, and CO. Three concepts emerge from our activation strain analyses: 1) bite‐angle flexibility, 2) d‐regime catalysts, and 3) s‐regime catalysts. These concepts reveal new ways of tuning a catalyst’s activity. Interestingly, the flexibility of a catalyst complex, that is, its ability to adopt a bent L‐M‐L geometry, is shown to be decisive for its activity, not the bite angle as such. Furthermore, the effect of ligands on the catalyst’s activity is totally different, sometimes even opposite, depending on the electronic regime (d or s) of the d10‐M(L)n complex. Our findings therefore constitute new tools for a more rational design of catalysts. 相似文献
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G. Wolters L. P. C. Kuijpers A. H. W. M. Schuurs und J. Kaaki 《Fresenius' Journal of Analytical Chemistry》1976,279(2):144
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Enzyme-immunoassay (EIA) of Hepatitis B surface antigen (HBsAg) in microtiter plates相似文献
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For representations of tame quivers the degenerations are controlled by the dimensions of various homomorphism spaces. Furthermore, there is no proper degeneration to an indecomposable. Therefore, up to common direct summands, any minimal degeneration from M to N is induced by a short exact sequence 0→U→M→V→0 with indecomposable ends that add up to N. We study these ‘building blocs’ of degenerations and we prove that the codimensions are bounded by two. Therefore, a quiver is Dynkin resp. Euclidean resp. wild iff the codimension of the building blocs is one resp. bounded by two resp. unbounded. We explain also that for tame quivers the complete classification of all the building blocs is a finite problem that can be solved with the help of a computer. 相似文献