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31.
A method based on solid-phase extraction (SPE) coupled to high-performance liquid chromatography (HPLC) with positive ion electrospray ionization tandem mass spectrometry (ESI-MS/MS) detection was developed for the simultaneous determination of lamivudine (3TC) and zidovudine (AZT) in human serum, using didanosine (ddI) as internal standard. The acquisition was performed in multiple reaction monitoring (MRM) mode, monitoring the transitions m/z 230.0 --> 111.8 for 3TC, m/z 268.1 --> 126.8 for AZT, and m/z 237.2 --> 136.8 for ddI. The limits of detection and quantitation were 3 and 10 ng/mL for 3TC, and 5 and 15 ng/mL for AZT. The method was linear in the studied ranges (10-1500 ng/mL for 3TC and 15-3000 ng/mL for AZT), with r(2) > 0.99 for each drug, and the run time was 4 min. The intra-assay precisions (%) were in the ranges 1.9-8.7 (3TC) and 2.2-8.9 (AZT), the inter-assay precisions were in the ranges 2.6-9.0 (3TC) and 4.2-8.1 (AZT), and the intra- and inter-assay accuracies were >97% for both drugs. The absolute recoveries were 95-99% for 3TC (45, 600 and 1200 ng/mL) and 104-112% for AZT (45, 1000 and 2400 ng/mL). The analytical method was applied to a bioequivalence study in which 24 healthy adult volunteers received single oral doses of the reference formulation and two test combined AZT/3TC tablets, in an open, three-period, balanced, randomized, crossover protocol. Based on the 90% confidence interval of the individual ratios (test formulation/reference formulation) for C(max) (peak serum concentration) and AUC(0-inf) (extrapolated area under the serum concentration vs. time curve from time zero to infinity), it was concluded that the two test formulations are bioequivalent to the reference formulation with respect to the rate and extent of absorption of both 3TC and AZT.  相似文献   
32.
Loss of vinyl alcohol from 1-amino-3-aryloxy-2-propanols under electron impact Under electron impact compounds of type 1 (see Scheme 1) split off 44 mass units from the molecular ion. This unusual reaction was studied using derivatives and deuterium labelled compounds. It could be demonstrated that for this fragmentation reaction 16 is the important structural feature from which H2(C3)?C(2)HOH (44 mass units) is lost. The preferred reaction mechanism involves a transition state in which four members of the side chain are involved (Scheme 2, mechanism 2).  相似文献   
33.
A simple, sensitive and inexpensive method for the speciation of Cr(VI) and Cr(III) in river and industrial wastewater was developed, optimized and validated. Samples were collected, filtered and then chromium species were determined in the filtrate. In the filtrate, total Cr was determined directly by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). A portion of the filtered sample was buffered to pH 6.4, extracted with Amberlite LA-2/MIBK and finally Cr(VI) was determined in the organic extract and Cr(III) in the aqueous phase using GFAAS. The method was evaluated by analysis of the certified reference material, CRM 544, and good accuracy was obtained. The limit of detection for Cr(VI) and Cr(tot)/Cr(III) was found to be 0.30 and 0.08 µg L−1, respectively, and a precision expressed as relative standard deviation of better than 11% was achieved for nine replicates. A number of water samples from the Tinishu Akaki River, Ethiopia, and wastewater samples from a chemical plant in Germany, were analysed. In addition to the GFAAS method, Cr(tot) was also determined using ICP-MS (in CRM 544, lyophilized water, and Tinishu Akaki River water samples) and Cr(tot) and Cr(VI) using UV-VIS spectrophotometry (in CRM 544 and industrial wastewater samples). Good agreement between the different methods was found.  相似文献   
34.
A new series of DNA binding 5,10,15-tri(N-methyl-4-pyridiniumyl)porphyrin (TrisMPyP)-platinum(II) conjugates was synthesized, in which different spacer ligands were used for appropriate coordination to platinum(II) complexes. Compound 9b exhibited in vivo antitumor activity (T/C%, 294) superior to cisplatin (T/C%, 184) against the leukemia L1210 cell line.  相似文献   
35.
A flow injection system was proposed to evaluate the transient product of a colorimetric reaction between hydrolysable tannin and potassium iodate (KIO3) solution. The system optimization was accomplished by using statistical methods based on experimental design. Flow rate of KIO3 solution, sample volume, carrier flow rate, and reaction coil were the selected factors for evaluation. On screening step, complete factorial 24 was used and two levels for each selected factor were studied. For the optimization phase, a centered face composite design 22 + star was employed to evaluate sample volume and flow rate of KIO3 solution, which were the factors identified in the screening phase as having more influence on the absorbance signal. After optimization, the proposed system was compared with batch determination. Some characteristics, such as analytical frequency, reagent consumption and chemical residues generation presented better results by the use of the proposed system if compared with batch method. The system presented good repeatability with standard deviation lower than 3%, for n = 10, linearity (R2 = 0.9974) for tannic acid standard, analytical frequency of 15 injections h− 1 and limit of quantification of 24 mg L− 1 of tannic acid. Good results were obtained when the proposed system was applied to hydrolysable tannin determination in Stryphnodendron barbatimão, Eucalyptus citriodora and Phyllanthus niruri, samples of plants commonly used in popular medicine.  相似文献   
36.
Magnetic anisotropy and susceptibility of a so-called one-dimensional crystal, dimethylammonium trichlorocuprate(II), DMACuCl3, measured between 300 and 77 K can be explained on the basis of a Cu2+ ion in a large tetragonal crystal field, although the shortest Cu-Cu distance is 3.443 Å. Measurements of anisotropic susceptibilities below 77 K are needed to ascertain the real magnetic behaviour in this system.  相似文献   
37.
38.
Summary The reaction of ()-(tetren)CoOH2+ with S2O 3 2- in the 7.25–8.28 pH range at 20–40 °C yielded S- (yellow) and O- (purple) bonded thiosulfato(tetren)cobalt(III) complexes, the former in larger quantities. The rate determining step is preceded by diffusion-controlled ion-pair [(tetren)CoOH2+,S2O 3 2- ] formation. Replacement of coordinated OH- by S2O 3 2- is interpreted in terms of an internal conjugate base mechanism: (tetren)CoOH2+ (tetren-H)CoOH 2 2+ , the reactive amido conjugate base being generated by intramolecular proton transfer from the coordinated NH site.In acid medium the S-bonded (tetren)Co(S2O3)+ is highly stable to redox decomposition, in contrast to its pentaammine analogue. The complex however, undergoes base hydrolysis yielding the corresponding hydroxo complex. The rate and activation parameters for the base hydrolysis have been reported. Photolysis of O- and S-bonded isomers of [(tetren)CoS2O3]+ in acidic medium at 254 and 313 nm, respectively, yielded aquation products accompanied by some decomposition of S2O 3 2- .  相似文献   
39.
We show for the first time that a classical Hookean viscoelastic constitutive law for rubbery materials can predict the impact forces and deflections measured with a commercial drop tester when a mass, or tup with a flat impacting surface is dropped onto a flat pad of commercial impact-absorbing rubber. The viscoelastic properties of the rubber, namely the relaxation times and strengths, are obtained by a standard rheological linear-oscillatory test, and the equation of momentum transfer is then solved, using these measured parameters, assuming a uniaxial deflection of the pad during the impact. Good agreement between measured and predicted forces and deflections is obtained for a series of various drop heights, tup masses, impact areas, and pad thicknesses, as long as the deflection of the pad relative to its thickness is small or modest (<50% or so), and as long as the area of the pad is less than or equal to that of the tup. When the pad area is greater than the tup, forces are higher than predicted, unless an empirical factor is introduced to account for the nonuniaxial stretching of the ring of material that extends outside of the impact area. These results imply that the impact-absorbing properties of a rubbery polymeric material can be assessed by simply examining the material's linear viscoelastic spectrum.  相似文献   
40.
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