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991.
The quantitative determination of chemical elements in organic or biological samples is an important analytical problem. Normally the elements to be determined in the organic matrix must be transformed into a simple inorganic form. A digestion method by heating on a block digestor has been developed for the determination of Al, As, Ba, Ca, Cd, Co, Cu, Fe, Mg, Mn, V and Zn in Oyster tissue by ICP OES. A simplex centroid statistical mixture design has been used to study the effects of changing HNO3, HCl and H2O2 reagent proportions on the digestion of these samples. Response surface and principal component analyses show that the species Ca, Cd, Cu, Fe, Mg, Mn and Zn have very similar analytical tendencies under this experiment. By means of mixture modeling maximum recoveries for these ions were predicted using 19%, 18% and 63% of the HCl, HNO3 and H2O2 pseudocomponent mixtures, respectively. This corresponds to 21.4%, 30.8% and 47.8% of the HCl, HNO3 and H2O2 commercial solutions. Furthermore the As, Co and V ions present large recoveries for these mixtures as well. The Al and Ba ion recoveries are seen to be independent of the mixture proportions. The analysis of Oyster tissue reference material (SRM 1566b - NIST) under optimized conditions at the selected wavelengths resulted in ion recoveries between 90% and 100%. 相似文献
992.
A simple, sensitive and powerful on-line sequential injection (SI) dispersive liquid-liquid microextraction (DLLME) system was developed as an alternative approach for on-line metal preconcentration and separation, using extraction solvent at microlitre volume. The potentials of this novel schema, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace copper and lead determination in water samples. The stream of methanol (disperser solvent) containing 2.0% (v/v) xylene (extraction solvent) and 0.3% (m/v) ammonium diethyldithiophosphate (chelating agent) was merged on-line with the stream of sample (aqueous phase), resulting a cloudy mixture, which was consisted of fine droplets of the extraction solvent dispersed entirely into the aqueous phase. By this continuous process, metal chelating complexes were formed and extracted into the fine droplets of the extraction solvent. The hydrophobic droplets of organic phase were retained into a microcolumn packed with PTFE-turnings. A portion of 300 μL isobutylmethylketone was used for quantitative elution of the analytes, which transported directly to the nebulizer of FAAS. All the critical parameters of the system such as type of extraction solvent, flow-rate of disperser and sample, extraction time as well as the chemical parameters were studied. Under the optimum conditions the enhancement factor for copper and lead was 560 and 265, respectively. For copper, the detection limit and the precision (R.S.D.) were 0.04 μg L−1 and 2.1% at 2.0 μg L−1 Cu(II), respectively, while for lead were 0.54 μg L−1 and 1.9% at 30.0 μg L−1 Pb(II), respectively. The developed method was evaluated by analyzing certified reference material and applied successfully to the analysis of environmental water samples. 相似文献
993.
ZHAO Zhi-man XIAO Peng CAO Guo-zhong . Faculty of Civil Architectural Engineering Kunming University of Science Technology Kunming P. R. China 《高等学校化学研究》2009,25(5):606-609
Redox response of trace heavy metals ions(THMIs) has better performance on highly ordered vertically oriented titania nanotube arrays(TNA) annealed in nitrogen. Experimental data showed that different THMIs possess different reaction peak shapes and charge and discharge capacities. Therefore, the TNA will become an important tool used for environmental protection and facilitating the rapid determination of THMIs. THMIs of 5×10-4 mol/L concentration were measured at a scan rate of 100 mV/s. The analytical ut... 相似文献
994.
采用荧光光谱、紫外-可见光谱研究了有/无金属Zn2+存在下甲基百里酚蓝(MTB)与牛血清白蛋白(BSA)的相互作用.实验结果表明,无论Zn2+离子存在与否,MTB与BSA之间均为一形成复合物的静态猝灭过程.根据Stern-Volmer方程和Lineweaver-Burk方程求出了其结合常数与热力学参数,发现Zn2+离子存在时,MTB与BSA间的作用力由静电力转为氢键和Van der Waals力作用为主,认为金属Zn2+以"离子架桥"的方式参与MTB与BSA的结合过程,从而ΔH对ΔG的贡献增大. 相似文献
995.
996.
MEIER Herbert 《中国科学B辑(英文版)》2009,52(7):1051-1056
A rapid and efficient synthesis of novel dendrimer homotriptycenes is presented. The dendronized 9,10-dihydroanthracen-9-ols 4, having high electron densities in the benzene rings of the Fréchet-type dendrons, exhibited in the presence of acid a quantitative transannular ring closure to the corresponding dendritic homotriptycenes. The electron-donating Fréchet-type dendrons enabled the intramolecular FC alkylation by a regioselective 1,7-elimination of H2O. 相似文献
997.
George O. Buica Christophe Bucher Jean‐Claude Moutet Guy Royal Eric Saint‐Aman Eleonora M. Ungureanu 《Electroanalysis》2009,21(1):77-86
Complexing polymer‐coated electrodes have been synthesized by oxidative electropolymerization of ethylenediamine tetra‐N‐(3‐pyrrole‐1‐yl)propylacetamide (monomer L ). The presence of four polymerizable pyrrole fragments on the same EDTA skeleton was thought to confer enhanced rigidity and controlled dimensionality to the resulting complexing materials, which were used for the electrochemical detection of Hg(II), Cu(II), Pb(II) and Cd(II) ions by means of the chemical preconcentration‐anodic stripping technique. The polyamide electrode material showed particularly a significant selectivity towards mercury ions, even in the presence of a large excess of other metal cations. Moreover, the use of imprinted polymer‐coated electrodes prepared by electropolymerization of L in the presence of metal cations turned out to significantly improve the detection limits, down to 5×10?10 mol L?1 for Hg(II) and Cu(II) species. 相似文献
998.
Stéphanie Goubert‐Renaudin Mathieu Moreau Christelle Despas Michel Meyer Franck Denat Bénédicte Lebeau Alain Walcarius 《Electroanalysis》2009,21(15):1731-1742
2‐(4,8,11‐Triscarbamoylmethyl‐1,4,8,11‐tetraazacyclotetradec‐1‐yl)acetamide (TETAM) derivatives bearing 1, 2, or 4 silylated arms have been synthesized and grafted to the surface of silica gel and ordered mesoporous silica samples. The resulting organic‐inorganic hybrids have been incorporated into carbon paste electrodes and applied to the preconcentration electroanalysis of Pb(II). The attractive recognition properties of these cyclam derivatives functionalized with amide pendent groups toward Pb(II) species and the highly porous structure of the adsorbents can be exploited for the selective and sensitive detection of the target analyte. Various parameters affecting the preconcentration and detection steps have been discussed with respect to the composition and pH of both accumulation and detection media, the nature of the adsorbent (number of silylated groups linking the macrocycle to silica, texture of materials), the accumulation time, and the presence of interfering cations. Under optimal conditions and for 2 min accumulation at open‐circuit, the voltammetric response increased linearly with the Pb(II) concentration in a range extending from 2×10?7 to 10?5 M, while a longer accumulation time of 15 min afforded a linear calibration curve between 10?8 and 10?7 M with a detection limit of 2.7×10?9 M which is well below the European regulatory limit of lead in consumption water. 相似文献
999.
Kathryn E. Toghill Lei Xiao Gregory G. Wildgoose Richard G. Compton 《Electroanalysis》2009,21(10):1113-1118
We report the simultaneous electroanalytical determination of Pb2+ and Cd2+ by linear sweep anodic stripping voltammetry (LSASV) using an antimony nanoparticle modified boron doped diamond (Sb‐BDD) electrode. Sb deposition was performed in situ with the analytes, from a solution of 1 mg L?1 SbCl3 in 0.1 M HCl (pH 1). Pb2+ inhibited the detection of Cd2+ during simultaneous additions at the bare BDD electrode, whereas in the presence of antimony, both peaks were readily discernable and quantifiable over the linear range 50–500 μg L?1. 相似文献
1000.
Anthony Midey Itzhak Dotan J.V. Seeley A.A. Viggiano 《International journal of mass spectrometry》2009,280(1-3):6
The rate constants and product ion branching ratios were measured for the reactions of various small negative ions with O2(X 3Σg−) and O2(a 1Δg) in a selected ion flow tube (SIFT). Only NH2− and CH3O− were found to react with O2(X) and both reactions were slow. CH3O− reacted by hydride transfer, both with and without electron detachment. NH2− formed both OH−, as observed previously, and O2−, the latter via endothermic charge transfer. A temperature study revealed a negative temperature dependence for the former channel and Arrhenius behavior for the endothermic channel, resulting in an overall rate constant with a minimum at 500 K. SF6−, SF4−, SO3− and CO3− were found to react with O2(a 1Δg) with rate constants less than 10−11 cm3 s−1. NH2− reacted rapidly with O2(a 1Δg) by charge transfer. The reactions of HO2− and SO2− proceeded moderately with competition between Penning detachment and charge transfer. SO2− produced a SO4− cluster product in 2% of reactions and HO2− produced O3− in 13% of the reactions. CH3O− proceeded essentially at the collision rate by hydride transfer, again both with and without electron detachment. These results show that charge transfer to O2(a 1Δg) occurs readily if the there are no restrictions on the ion beyond the reaction thermodynamics. The SO2− and HO2− reactions with O2(a) are the only known reactions involving Penning detachment besides the reaction with O2− studied previously [R.S. Berry, Phys. Chem. Chem. Phys., 7 (2005) 289–290]. 相似文献