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61.
M. P. Carril M. Soledad Corbillón J. Manuel Madariaga 《Accreditation and quality assurance》1997,2(6):301-308
The development of an analytical method for the determination of some heavy metals (Fe, Cu, Co, Zn and Ni) in fluoride compounds
[Cu(BF4)2, Sn(BF4)2, Pb(BF4)2 and HBF4] by flame atomic absorption spectroscopy is described. This method is to be used as a routine analytical method in an industrial
quality control laboratory. To this end the "performance characteristics" of an instrumental analytical method such as matrix
effects, sensitivity, linearity, detection and quantitation limits, precision and accuracy were evaluated for every system
under study. The results of these investigations showed that non-spectral interferences (due to the presence of large concentrations
of major metals such as Cu, Sn and Pb) were observed. Nevertheless it was possible to define a matrix concentration interval
where matrix effects were not statistically significant, and therefore a direct calibration approach could be used as the
calibration tool whenever the major metal concentration was not higher than 40×10–3 kg l–1. A guide to the developement of an analytical method for trace metal determination is provided. General tools for quality
control have been used in order to show how an analytical method can be tested daily and evaluated in a convenient manner.
Received: 29 January 1997 Accepted: 11 March 1997 相似文献
62.
Piotr Kutrowski Dominika Sukowska Renata Pytlowany Roman Dziembaj 《Reaction Kinetics and Catalysis Letters》2004,81(1):3-11
Catalytic performance of Ba(OH)2 and Sr(OH)2 in self-condensation of acetone was examined in the temperature range from 273 to 303 K. A kinetic model of second order with respect to acetone was used for interpretation of the results obtained for the diacetone alcohol formation.This revised version was published online in December 2005 with corrections to the Cover Date. 相似文献
63.
Summary The ion exchange selectivity of trivalent metal ions has been determined on titanium antimonate cation exchanger prepared by coprecipitation of antimony to titanium at different mole ratios. The selectivity sequence Al3+<Cr3+<Ga3+<In3+<Fe3+ was found for trivalent metal ions at an initial concentration of 10–4 mol dm–3 in nitric acid media. A high separation factor Ga/Al = KdGa/KdAl, 4.8×103, was observed for the Ga3+–Al3+ pair on titanium antimonate with an antimony to titanium ratio of 0.34. The effective separation of Ga3+ and In3+ from Al3+ was achieved using a 3 cm×0.5 cm i.d. column containing titanium antimonate with an antimony to titanium ratio of 0.34. 相似文献
64.
Methane reforming by carbon dioxide has been studied over ultra-stable Ni catalysts. The catalyst was characterized by XRD, IR and TEM and temperature programmed hydrogenation. The nickel–magnesia solid solution catalyst containing low nickel has shown excellent stability (>3000 h) and no carbon deposition in the methane reforming by carbon dioxide. It was also found that the small nickel metal particle interaction with support surface is effective for the inhibition of carbon formation. 相似文献
65.
A. A. El-Asmy 《中国化学会会志》1988,35(1):29-34
The preparation and characterization of a series of new coordination compounds of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) containing o-methyl- or o-chlorobenzoyl-4-phenyl-3-thiosemicarbazide (HMBPT, HCBPT=HL) are reported. The reaction products were investigated by analyses, electrolytic conductance, magnetic susceptibility, reflectance and IR spectral studies. The IR spectra show that HMBPT and HCBPT coordinate with the metal ions via different coordination sites (NS and/or NO). The spectral data support the suggestion that the ligands form his-chelates with Ni(II) and Cu(II) of square planar stereochemistry and of general formulae ML2·H2O, where L is the uninegatively charged bidentate ligand. The Co(II) ion forms octahedral and tetrahedral structures with HMBPT and HCBPT, respectively. The ligand field parameters (D4, B and β) for the Co(II) chelates were calculated using the averaged-ligand-field approximation. The influence of the benzene ring substituents (o-chloro or o-methyl) on the stereochemistry are discussed. Also, the formation of the complexes in solution was tested by the pH-metric method. 相似文献
66.
Presenting a condensation of the opening lecture of the 12th ICFIA conference, this communication presents a view of the impact that flow injection analysis (FIA) has had on modern analytical chemistry, evaluated both within the academic community and outside it, i.e. in “industry”. The ensuing developments of FIA, encompassing sequential injection analysis (SIA) and bead injection lab-on-valve (BI-LOV), are described and their individual features discussed. Finally, some recent results of the activities from the author’s own research group are briefly mentioned. 相似文献
67.
Leslie D. Field Adrian V. George Trevor W. Hambley Peter Turner Brian J. Wallace 《Journal of organometallic chemistry》1997,540(1-2):95-99
Reaction of cis-[FeH2(dmpe)2](1) with diphenylbutadiyne results in an insertion into both of the iron-hydride bonds to form an iron metallocycle. Spectroscopic and crystallographic data of [Fe(PhHCC2CHPh)(dmpe)2] (3) show 1,4-diphenylbutatriene is symmetrically bound to the metal via the central double bond. The reaction to form the metallocyclic complex is greatly accelerated by application of external pressure. A 41% yield of (3) is isolated after two days at atmospheric pressure or after approximately 75 min at 800MPa. 相似文献
68.
对梅州农村饮用水中的重金属元素进行了监测和分析,选择Fe,Mn,Zn,Cu,Ag,Pb,Cd七种元素为检测指标。从实验结果来看,Cu,Ag,Cd含量低,未超标;Fe,Mn,Zn,Pb有超标现象:按其危害程度,Pb,Mn的超标是急需解决的问题。 相似文献
69.
CoSm(SeO3)2Cl, CuGd(SeO3)2Cl, MnSm(SeO3)2Cl, CuGd2(SeO3)4 and CuSm2(SeO3)4: Transition Metal containing Selenites of Samarium and Gadolinum The reaction of CoCl2, Sm2O3, and SeO2 in evacuated silica ampoules lead to blue single crystals of CoSm(SeO3)2Cl (triclinic, , Z = 4, a = 712.3(1), b = 889.5(2), c = 1216.2(2) pm, α = 72.25(1)°, β = 71.27(1)°, γ = 72.08(1)°, Rall = 0.0586). If MnCl2 is used in the reaction light pink single crystals of MnSm(SeO3)2Cl (triclinic, , Z = 2, a = 700.8(2), b = 724.1(2), c = 803.4(2) pm, α = 86.90(3)°, β = 71.57(3)°, γ = 64.33(3)°, Rall = 0.0875) are obtained. Green single crystals of CuGd2(SeO3)2Cl (triclinic, , Z = 4, a = 704.3(4), b = 909.6(4), c = 1201.0(7) pm, α = 70.84(4)°, β = 73.01(4)°, γ = 70.69(4)°, Rall = 0.0450) form analogously in the reaction of CuCl2 and Gd2O3 with SeO2. CoSm(SeO3)2Cl contains [CoO4Cl2] octahedra, which are connected via one edge and one vertex to infinite chains. The Mn2+ ions in MnSm(SeO3)2Cl are also octahedrally coordinated by four oxygen and two chlorine ligands. The linkage of the polyhedra to chains occurs exclusively via edges. Both, the cobalt and the manganese compound show the Sm3+ ions in eight and ninefold coordination of oxygen atoms and chloride ions. In CuGd(SeO3)2Cl the Cu2+ ions are coordinated by three oxygen atoms and one Cl— ion in a distorted square planar manner. One further Cl— and one further oxygen ligand complete the [CuO3Cl] units yielding significantly elongated octahedra. The latter are again connected to chains via two common edges. For the Gd3+ ions coordination numbers of ?8 + 1”? and nine were found. Single crystals of the deep blue selenites CuM2(SeO3)4 (M = Sm/Gd, monoclinic, P21/c, a = 1050.4(3)/1051.0(2), b = 696.6(2)/693.5(1), c = 822.5(2)/818.5(2) pm, β = 110.48(2)°/110.53(2)°, Rall = 0.0341/0.0531) can be obtained from reactions of the oxides Sm2O3 and Gd2O3, respectively, with CuO and SeO2. The crystal structure contains square planar [CuO4] groups and irregular [MO9] polyhedra. 相似文献
70.
Spectrafluorimetric method for the rapid screening of toxic heavy metals in water samples 总被引:1,自引:0,他引:1
B. San Vicente de la RivaJ.M. Costa-Fernández R. PereiroA. Sanz-Medel 《Analytica chimica acta》2002,451(2):203-210
A fast and inexpensive sensitive screening test for recognising potential wastewater contamination by the presence of highly toxic heavy metals is described. The test is based on the reaction of the toxic heavy metals Hg(II), Cd(II), Pb(II) and Ag(I) with 6-mercaptopurine (6-MP) to produce highly fluorescent complexes.Optimum experimental conditions include a buffer of pH 7.2 (0.1 M citric acid/0.2 M Na2HPO4), a chelating reagent concentration of 6×10−4 M and the addition of 10−4 M of o-phenanthroline. The fluorescence emitted by the complexes was measured at 380 and 540 nm for excitation and emission wavelengths, respectively.Detection limits of 4, 3, 6 and 3 μg l−1 were achieved for Hg, Cd, Pb and Ag. Relative standard deviation (R.S.D.) were between ±2 and ±6% of the fluorescence signals for five identical samples. Potential interference effects from other heavy metals (Zn, Mn, Co, Fe, Ni and Cu), which could affect the response of the proposed screening test was investigated. Results showed that none of these metals give rise to noticeable fluorescence signals under the above described experimental conditions.Finally, the capability of the proposed heavy metal screening test for the analysis of contaminated water samples is discussed. 相似文献