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41.
Electrochemical oxidation of thio/carbohydrazide and their hydrazone derivatives Benzaldehyde thiocarbohydrazone [BTCH] diacetylene
thiocarbohydrazone [DATCH] have been studied in Brit-ton Robinson buffer in aqueous and nonaqueous media at a glassy carbon
electrode. The effects of pH, sweep rate, concentration, temperature and surfactants have been studied. The complex bis (carbo/thiocabohydrazide) Zn(II) chloride was also subjected to voltammetric analysis in order to understand the reactivity
both in free and metal bound states. The reaction conditions were optimized for the determination of above compounds in micrograms
quantities by differential pulse voltammetry, analytical utility of this investigation is also highlighted. 相似文献
42.
Arjan J. H. Louter Philo A. Jones J. David Jorritsma Jolan J. Vreuls Udo A. Th. Brinkman 《Journal of separation science》1997,20(7):363-368
An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1–12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1–0.3 μg/1 range. 相似文献
43.
A simple and rapid method is developed to determine the high acidity and the basicity of solutions by chronopotentiometry with a platinum working electrode. The acidity range from 5.0 mol/l H+ to 1.0 mol/l OH− can be measured by the adjustment of deposition potential and time. The response mechanism to acidity and basicity has been explored. The transition potential plateau in chronopotentiograms is caused from the oxidation of hydrogen adsorbed on electrode surface. 相似文献
44.
Influence of boric acid on the electrochemical deposition of Ni 总被引:1,自引:0,他引:1
M. Šupicová R. Rozik L. Trnková R. Oriňáková M. Gálová 《Journal of Solid State Electrochemistry》2006,10(2):61-68
The electrolytic deposition of Ni onto a paraffin-impregnated graphite electrode from supporting chloride electrolyte (0.5 mol dm−3 NaCl) adjusted to the required pH using dilute HCl is investigated. The effect of electrolyte composition on the Ni electrodeposition
is studied using linear sweep voltammetry in the cathodic region. An elimination voltammetry procedure was applied to evaluate
the polarization curves. The aim of this work was to deduce the mechanism of Ni reduction in the chloride bath as well as
the influence of boric acid on this. Positively-charged NiCl+ ions were found to be the electroactive particles in the Ni reduction mechanism. The strong competition between the NiCl+, Cl− and H+ ions for active sites at the electrode is discussed. Kinetically-controlled adsorption/desorption processes of various species
were also confirmed using elimination voltammetry with a linear scan. The evolution of gaseous hydrogen, catalyzed by the
freshly-deposited Ni, accompanies the electrodeposition process. The presence of boric acid at a sufficiently high concentration
inhibits the deposition of Ni and, at the same time, improves the morphology and brightness, as well as the adhesion of the
deposited Ni.
Elimination voltammetry with a linear scan is an efficient way to evaluate current–potential curves that reflect the electrodeposition
of one-component Ni coatings. By eliminating selected currents, additional interesting and useful information can be obtained
from voltammetric data. 相似文献
45.
《Electroanalysis》2006,18(22):2218-2224
This article deals with the development of a method for the determination of osmium at a carbon paste electrode (CPE) modified with cationic surfactants of the quaternary ammonium salt type; namely, cetyltrimethylammonium bromide (CTAB) and 1‐(ethoxycarbonyl)‐pentadecyltrimethyl‐ammonium bromide (Septonex); both being added in situ and serving for preconcentration of osmium via its hexachloroosmate(IV) anion. The proper electrochemical detection was performed by cathodic scanning in the differential pulse voltammetric mode. Optimization studies concerning important experimental parameters also included a specially performed potentiometric titration, helping to define the actual stoichiometry for the ion‐pairing process, the main principle and driving force of the accumulation step. In a chloride/acetate buffer based supporting medium and with Septonex as the modifier of choice, the reduction signal for osmium was found to be proportional to the Os(IV) concentration in a range from 5×10?9 to 5×10?7 mol L?1 with a limit of detection close to 5×10?9 mol L?1 (with preconcentration for 60 s). The method capable to determine Os(IV) in the presence of both Pt(IV) and Ir(III) was tested on model solutions as well as with real sample of industrial waste water (spiked with the analyte); both yielding the recovery rates within 88–99%. 相似文献
46.
We have carried out some photon interaction measurements using 59.54 keV γ-rays from a 241Am source. These include γ attenuation studies as well as photoelectric absorption studies in various samples. The attenuation
studies have been made using leaf and wood samples, samples like sand, sugar etc., which contain particles of varying sizes
as well as pellets and aqueous solutions of rare earth compounds. In the case of the leaf and wood samples, we have used the
γ-ray attenuation technique for the determination of the water content in fresh and dried samples. The variation of the attenuation
coefficient with particle size has been investigated for sand and sugar samples. The attenuation studies as well as the photoelectric
studies in the case of rare earth elements have been carried out on samples containing such elements whose K-absorption edge
energies lie below and close to the γ-energy used. Suitable compounds of the rare earth elements have been chosen as mixture
absorbers in these investigations. A narrow beam good geometry set-up was used for the attenuation measurements. A well-shielded
scattering geometry was used for the photoelectric measurements. The mixture rule was invoked to extract the values of the
mass attenuation coefficients for the elements from those of the corresponding compounds. The results are consistent with
theoretical values derived from the XCOM package. 相似文献
47.
《Analytica chimica acta》1998,360(1-3):53-59
A procedure is described for the preparation of a tubular electrode by chemical deposition of platinum at the end of a fused-silica capillary. The properties of the electrode were tested under liquid chromatographic conditions, demonstrating that both the static and the dynamic behaviour of the detection system satisfy the requirements of capillary chromatographic separations and compare well with a wall-jet amperometric system and with UV photometric detection. The detection system described is easy to prepare and does not require any time-consuming positioning of the electrode system as it is integrated into the separation part of the apparatus. 相似文献
48.
在原子吸收光谱分析中,固体样品直接进样是目前的研究课题之一。本文主要报道作者在分析汞中所进行的固体直接进样技术工作和讨论。在我们研制成功的KT—81型塞曼效应测汞仪中,针对元素汞蒸气压高的特点,用饱和汞蒸气作为汞量标准,实现了固体样品,如土壤、污泥、毛发、煤、食品等汞含量的直接进样测定。汞蒸气一次制备后可长期使用。分析汞时,只要用标准气体任意校验一次就可测量。1~2分钟能分析一个样品,S<0.3ng。r<5%。此法用NBS标准物质验证过。 相似文献
49.
50.
用结晶紫选择性电极(自制)以催化电位法对测定微量锰进行了研究。该方法测定标的线性范围为7~74μg/L,对标准钢样中的锰含量测定结果满意,且操作方便。 相似文献