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51.
以苯胺和乙醇为原料,采用RaneyNi为催化剂,合成了N-乙基苯胺,再在相转移催化剂作用下,经苄基化反应得到标题化合物,第一步合成方法的收率比通常方法的收率提高约30%。 相似文献
52.
A series of titanium complexes [(Ar)NC(CF3)CHC(R)O]2TiCl2 (4b: Ar = -C6H4OMe(p), R = Ph; 4c: Ar = -C6H4Me(p), R = Ph; 4d: Ar = -C6H4Me(o), R = Ph; 4e: Ar = α-Naphthyl, R = Ph; 4f: Ar = -C6H5, R = t-Bu; 4g: Ar = -C6H4OMe(p); R = t-Bu; 4h: Ar = -C6H4Me(p); R = t-Bu; 4i: Ar = -C6H4Me(o); R = t-Bu) has been synthesized and characterized. X-ray crystal structures reveal that complexes 4b, 4c and 4h adopt distorted octahedral geometry around the titanium center. With modified methylaluminoxane (MMAO) as a cocatalyst, complexes 4b-c and 4f-i are active catalysts for ethylene polymerization and ethylene/norbornene copolymerization, and produce high molecular weight polyethylenes and ethylene/norbornene alternating copolymers. In addition, the complex 4c/MMAO catalyst system exhibits the characteristics of a quasi-living copolymerization of ethylene and norbornene with narrow molecular weight distribution. 相似文献
53.
Manju Gupta 《Talanta》2007,71(3):1039-1046
The aim of present work was to optimize the experimental parameters in single drop microextraction under solution immersion (SDME) and headspace (HS-SDME) extraction modes for the determination of periodate using guaifenesine [3-(2′-methoxyphenoxy)-1,2-propane diol] and norephedrine (phenylpropanolamine) as new and alternative reagents for the Malaprade reaction. The reactions were complete within 5 min resulting in the formation of 2-(2′-methoxyphenoxy)-acetaldehyde and benzaldehyde, respectively. SDME/HS-SDME of oxidation products with 2 μl of anisole or 1 μl of toluene, respectively, has permitted the determination of periodate at μg l−1 concentration levels. The results indicated that HS-SDME (range 0.01-10 mg l−1, r2 = 0.9990; limit of detection 1.55 μg l−1) was more sensitive than SDME (range 0.05-50 mg l−1, r2 = 0.9984; limit of detection 3.42 μg l−1), and was inexpensive, rapid and convenient. Tolerance of excess of iodate has permitted the application of this method in the determination of ethylene glycol in motor oil; the average recovery on spiked sample was 98.6% with R.S.D. of 4.2%. 相似文献
54.
《Arabian Journal of Chemistry》2020,13(2):4082-4091
In present study, an investigation was carried out to develop and validate an analytical method for the selective extraction and determination of griseofulvin (GSF) from plasma samples. For this purpose, a rational approach was made to synthesize and characterize the surface molecularly imprinted polymers (SMIPs). The SMIPs were utilized as solid phase extraction (SPE) sorbents. The SMIPs were prepared by using GSF as template molecule on the surface of modified silica particles through a non-covalent technique. The particles demonstrated high adsorption capacity (119.1 µg/mL), fast adsorption equilibrium time (30 min) and good recognition selectivity for the template drug. The scanning electron microscopy and infrared spectroscopy were used to explain the structural and morphological characteristics of the SMIPs and surface non-imprinted polymers. The SPE method was combined with HPLC for plasma analysis. The method validation results demonstrated that the established method possessed good linearity for GSF ranging from 0.1 to 50 µg/mL (R2 = 0.997). The limit of detection for this method was 0.02 µg/mL for rat plasma samples. The recoveries of GSF from spiked plasma samples were (90.7–97.7%) and relative standard deviations were (0.9–4.5%). Moreover, the SMIPs as selective SPE sorbent can be reused more than 8 times which is a clear advantage over commercial SPE sorbents. Finally, the usefulness of the proposed strategy was assessed by extraction and detection of GSF in real rat plasma samples. 相似文献
55.
Parameters are developed for a practical application of the empirical van der Waals (vdW) correction infrastructure available in the CPMD density functional theory (DFT) code. The binding energy, geometry, and potential energy surface (PES) are examined for methane, ethane, ethylene, formaldehyde, ammonia, three benzene dimer geometries, and three benzene–water geometries. The vdW corrected results compare favorably with MP2 and CCSD(T) calculations near the complete basis set limits, and with experimental results where they are available. 相似文献
56.
以去离子水与乙二醇的混合液(体积分数分别为36.5%,48.7%,59.0%及71.2%,以下简称混合液)作为同轴传输线的绝缘介质,进行了μs级高电压负充电条件下的正电极击穿实验,研究了混合液的击穿电压、击穿时间、相对介电常数及电阻率与体积分数的关系。实验结果表明:在充电电压为20kV时,71.2%的混合液比36.5%的混合液的平均击穿电压提高25.1%,平均击穿时间延长10.49%,而相对介电常数减小868%。同时,随着充电时间的缩短,混合液的击穿电压提高。 相似文献
57.
Hydrogen peroxide activated by boric acid in the presence of sulfuric acid has been shown to be an efficient oxidizing system for direct conversion of aromatic aldehydes and ketones to phenols. 相似文献
58.
《高分子科学杂志,A辑:纯化学与应用化学》2013,50(9):1171-1180
Polymerization of ethylene and propylene with VCl4-BuLi (Bu = n-Bu, sec-Bu, tert-Bu) catalysts was investigated. The VCl4-BuLi catalysts were found to initiate the polymerization of ethylene and propylene. The VCl4-BuLi catalysts gave an ultra high molecular polyethylene. The effect of the Li /V mole ratio on the polymerization of ethylene with the VCl4-BuLi catalysts was observed, an the catalyst gave an optimum rate at the Li/V ratio of about 3.0. The polyethylene obtained with the VCl4-BuLi catalyst was found to be a linear structure. In the polymerization of propylene with the VCl4-BuLi catalyst, the polymers contain mm contents of 56–66% were produced. 相似文献
59.
Salvatore Sotgia Angelo Zinellu Gianfranco Pintus Gerard Aime Pinna Luca Deiana Ciriaco Carru 《Journal of separation science》2013,36(6):1002-1006
A new hydrophilic interaction ultra‐performance LC method was established for the whole blood measurement of L‐ergothioneine. Chromatographic separation was achieved in a fairly short time, less than 4 min, on a 100 × 2.1 mm Acquity UPLC BEH HILIC 1.7 μm column with a mobile phase consisting of a mixture of 100 mmol/L ammonium acetate/ACN/water (5:85:10, v/v/v) that flowed isocratically at 0.250 mL/min. The LOD and the limit of quantification were 3.85 and 11.67 μmol/L, respectively. The method exhibited linearity in a concentration range of 15.63–1000 μmol/L (R2 > 0.999). Mean recovery was 96.34% whereas intraassay and interassay precision were 1.52 and 1.82% RSD, respectively. On the whole, the developed method is simple, fast, precise, accurate, and sensitive and may be useful for routine analyses. 相似文献
60.
A simple porogen containing only DMF and aqueous buffer was used for synthesis of monolithic stationary media for CEC). Butyl methacrylate (BMA)‐based capillary monoliths were obtained using proposed porogen together with acrylic/methacrylic cross‐linking agents with different alkyl chain lengths. For this purpose, ethylene glycol dimethacrylate, butanediol dimethacrylate and hexanediol diacrylate (HDDA) were used. The monoliths with better electrochromatographic separation performance were obtained when the acrylic cross‐linking agent with the longest alkyl chain length (i.e. HDDA) was used with the proposed porogen. The electrochromatographic separation of alkylbenzenes, phenols and benzoic acids were sucessfully performed in CEC particularly using poly(BMA‐co‐HDDA) monolithic stationary phase with the column efficiency up to 270 000 plates/m. 相似文献