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11.
An unprecedented C,C-linked dimeric norcembranoid (sinulochmodin A, 1), a novel isocembranoid (sinulochmodin B, 2), and a novel yonarane norditerpenoid (sinulochmodin C, 3) were isolated from the soft coral Sinularia lochmodes. The structures of these metabolites were elucidated by extensive spectroscopic analysis and on the basis of the absolute structures of two related norditerpenoids (4 and 5), which were determined for the first time by a modified Mosher method. A plausible pathway for the biosynthesis of 1 and 3-5 from 2 was postulated. [structure: see text] 相似文献
12.
S. C. Sheu M. L. Lee H. L. Hwang H. Y. Lin M. H. Yang 《Fresenius' Journal of Analytical Chemistry》1989,334(2):143-147
Summary CuInS2 is one of the important I–III–VI2 ternary compounds which has in recent years received increasing interest in semiconductor science. In this study an electrochemical method has been developed based on a limited amount of available sample (0.5–10mg) for the precise and accurate determination of CuInS2 composition. After decomposition of the sample in concentrated HNO3 under pressure, copper and indium were sequentially determined by constant potential coulometry, and sulfur (as sulfate) by amperometric titration. Various experimental parameters which ensure high precision and accuracy of the results were carefully evaluated and calibrated. The overall errors for the determination of copper, indium and sulfur in a 10 mg sample were found to be +0.10%, –0.12% and +0.16%, respectively, which fullfills the requirement for accurate stoichiometric assessment.
Presented at the 10th International Symposium on Microchemical Techniques, August 25–29, 1986, Antwerp, Belgium 相似文献
Reproduzierbare und genaue Bestimmung der Stöchiometrie von CuInS2-Halbleitermaterial mit Hilfe elektrochemischer Verfahren
Presented at the 10th International Symposium on Microchemical Techniques, August 25–29, 1986, Antwerp, Belgium 相似文献
13.
14.
A solution of carprofen in methanol at a concentration of 2.74 x 10(-2) mg/mL is subjected to photoirradiation using a Hanovia 200-W high-pressure Hg lamp for 9 h. In total, seven photodegradation products are separated, and their quasimolecular ions are subsequently determined online using a liquid chromatography (LC)-electrospray ionization (ESI)-mass spectrometry (MS) method. The high-performance LC consists of an Inertsil 5 ODS-80A (2.1- x 150-mm) column. The mobile phase is initially CH(3)CN. NH(4)OAc (20mM in de-ionized H(2)O) is 43:57 (v/v), and after 14 min it is CH(3)CN. NH(4)OAc (20mM in de-ionized H2O) is 54: 46 (v/v). The UV detector was set at 260 nm. The parameters of LC-MS for mass determination involves an atmospheric pressure ionization electron spray interface with a negative mode of polarity (ESI(-)). The chemical structures of the degradants are elucidated based on the mass-to-charge ratio of the quasimolecular ions and the molecular weight changes by comparison with the parent drug (carprofen). The degradation proceeds via an initial dechlorination. A dechlorination or esterification reaction is competed with decarboxylation. This finding is in accordance with our previously reported result of first order photodecomposition kinetics for carprofen. 相似文献
15.
A RP-HPLC method for determining fourteen components (gallic acid, chebulic acid, 1,6-di-O-galloyl-D-glucose, punicalagin, 3,4,6-tri-O-galloyl-D-glucose, casuarinin, chebulanin, corilagin, neochebulinic acid, terchebulin, ellagic acid, chebulagic acid, chebulinic acid, and 1,2,3,4,6-penta-O-galloyl-D-glucose) in the fruit of Terminalia chebula Retz. is described. The separation was achieved within 80 min using a binary gradient with mobile phases consisting of a pH 2.7 phosphoric acid solution and an 80% CH3CN solution. Capillary electrophoretic analyses were also attempted, and it was found that CZE (25 mM Na2B4O7, 5 mM NaH2PO4, pH 7.0) was an efficient method for the separation of gallotannins, while an MEKC method (25 mM Na2B4O7, 5 mM NaH2PO4, 20 mM SDS, pH 7.0, and 10% acetonitrile) provided a better separation for most of the tannins examined. The HPLC and CE methods developed were both successfully applied to the assay of tannins in commercial samples of Chebulae Fructus. 相似文献
16.
High-performance liquid chromatographic analysis for the characterization of triterpenoids from Ganoderma 总被引:1,自引:0,他引:1
A high-performance liquid chromatographic (HPLC) analysis of triterpenoids from Ganoderma is developed and validated in an attempt to explore a way to differentiate a number of species of the genus Ganoderma. Results show that 64 samples examined in this study could be divided into 18 groups based on characteristics of the HPLC pattern of triterpenoids. This result also conforms with those of the morphological examination and the interfertility test by di-monokaryotic mating. The HPLC analysis of triterpenoids further reveals that differentiation among samples from three different regions each of the two species G. lucidum and G. tsugae is workable. Even then, an incorrect designation is found for two of the groups of samples that were originally classified as G. resinaceum but showed different morphological characteristics and mating incompatibility. In conclusion, an HPLC analysis of triterpenoids is a simple and easy way to differentiate among different species of the genus Ganoderma. 相似文献
17.
Two stacking methods of capillary electrophoresis (CE) were developed for the separation of very dilute solutions of ephedra-alkaloids, namely ephedrine, pseudoephedrine, methylephedrine, methylpseudoephedrine, norephedrine, and norpseudoephedrine. A sweeping method which uses a carrier comprised of phosphoric acid, sodium dodecyl sulfate (SDS), diethylamine and acetonitrile permits the detection of the alkaloids down to the 10(-1) microg/mL level, and the cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography (CSEI-Sweep-MEKC) method using phosphoric acid, SDS, and acetronitrile as electrolytes can detect down to the 10(-3) microg/mL level. The former requires the conductance of the sample solution to be adjusted beforehand, and only five peaks were observed, two of which were overlapped. The latter is capable of separating the six alkaloids but has a somewhat poorer reproducibility. Using an optimized injection time, it was found that the more diluted a solution is, the greater the sweeping effect will be. The CSEI-Sweep-MEKC method with a 600 s injection time and a 10(-1) microg/mL solution concentration provides an amplification effect of approximately 10(4). The method is suitable for analyses of dilute herb drug extracts and mouse sera. The effect of buffers on the separation and validation of the methods in this study are also discussed. 相似文献
18.
Shey-Huei Sheu 《The Journal of the Operational Research Society》1991,42(4):331-341
A generalization of the block replacement policy (BRP) is proposed and analysed for a multi-unit system which has the specific multivariate distribution. Under such a policy an operating system is preventively replaced at times kT (k = 1, 2, 3,...), as in the ordinary BRP, and the replacement of the failed system at failure is not mandatory; instead, a minimal repair to the component of the system can be made. The choice of these two possible actions is based on some random mechanism which is age-dependent. The cost of the ith minimal repair of the component at age y depends on the random part C(y) and the deterministic part Ci(y). The aim of the paper is to find the optimal block interval T which minimizes the long-run expected cost per unit time of the policy. 相似文献
19.
We study asymptotic properties of discrete and continuous time generalized simulated annealing processesX(·) by considering a class of singular perturbed Markov chains which are closely related to the large deviation of perturbed diffusion processes. Convergence ofX(t) in probability to a setS
0 of desired states, e.g., the set of global minima, and in distribution to a probability concentrated onS
0 are studied. The corresponding two critical constants denoted byd and withd are given explicitly. When the cooling schedule is of the formc/logt, X(t) converges weakly forc>0. Whether the weak limit depends onX(0) or concentrates onS
0 is determined by the relation betweenc, d, and . Whenc>, the expression for the rate of convergence for each state is also derived. 相似文献
20.
C. Allen Chang Tamar E. Woodhouse Qihui Wu Ceshing Sheu Katherine McManus 《中国化学会会志》1988,35(4):253-260
Substitution-inert metal complexes, [Co(edda)(H2O)2]+, (Co(edda)(en)]+, [Co(edda)(dmen)]+, [Co(en)2-(gly)]2+, [Co(en)2(acac)]2+, and [Co(trien)(gly)]2+ in their nitrate salt solutions are used as eluents in nonsuppressed cation chromatography (where edda = ethylenediamine-N,N′-diacetic acid, en = ethylenediamine, dmen = N,N′-dime-thylethylenediamine, gly = glycine, acac = acetylacetone, and trien = triethylenetetraamine). It is found that all the mono- and di-valent charged complexes can be used to separate alkali and alkaline earth metal cations, respectively. The separations for monovalent cations are sometimes comparable to those using ultrapure HNO3 solutions. However, the divalent Ca2+ and Sr2+ ions cannot be resolved using the metal complex eluents. On the other hand, a selected, direct non-suppressed IC separation of zinc(II) and cadmium(II) ions is demonstrated for the first time using a substitution-inert metal complex eluent and a conductivity detector. Comparisons of these eluents with those reported previously, i. e. HNO3 and ethylenediammonium salt solution are made and explanations are proposed to account for the different selectivities observed where possible. The future development of this technique is also briefly discussed. 相似文献