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991.
采用电感耦合等离子体原子发射光谱法(ICP-AES)法测定钛合金中W,Nb,Ta元素的含量。样品采用盐酸、氢氟酸和硝酸溶解,并对仪器工作参数和试验条件进行了优化试验,确定了仪器最佳工作条件,考察了钛合金基体和共存元素对待测元素的影响,确定了各待测元素谱线为W207.911nm,Nb309.418nm,Ta240.063nm。选定的待测元素分析线不受合金基体和共存元素的干扰,通过基体匹配消除基体的影响。加标回收率在98%104%之间,测定结果的相对标准偏差为0.3%~2.4%(n=8),方法的检出限为0.003-0.013μg/mL。进行了标准物质对照试验,试验结果与标准值相符。 相似文献
992.
993.
994.
Ik Hyun Kwon Hye Ryoung Park Young Youp Song 《Russian Journal of Electrochemistry》2013,49(3):221-227
LiNi1 ? y Ti y O2 (0.000 ≤ y ≤ 0.100) and LiNi0.990M0.010O2 (M = Zn, Al, and Ti) were synthesized by the combustion method. The effects of Zn, Al and Ti substitution for Ni of LiNiO2 on the electrochemical properties of LiNiO2 were investigated. LiNi0.995Ti0.005O2 has the largest first discharge capacity (188.1 mA h/g) among the Ti-substituted samples. LiNi0.990Ti0.010O2 has a relatively large first discharge capacity (185.5 mA h/g) and a relatively good cycling performance. Among LiNi0.990M0.010O2 (M = Ni, Zn, Al, and Ti), LiNiO2 has the largest discharge capacities at a rate of 0.1 C from n = 1(189.3 mA h/g) to n = 10. LiNi0.990Al0.010O2 has the lowest discharge capacities from n = 1 to n = 10, but it has the best cycling performance. LiNi0.990Zn0.010O2 showed poor crystallinity, LiNi0.990Ti0.010O2 showed high cation mixing, and LiNi0.990Al0.010O2 had good crystallinity and showed low cation mixing. Fewer occurrence of phase transitions and the least change of the ?dx/|dV| vs. voltage curve at the second cycle from the curve at the first cycle of LiNi0.990Al0.010O2 suggest that Al substitution stabilizes the structure and leads to a good cycling performance. 相似文献
995.
离子排斥色谱中色谱柱温度对有机酸保留的影响 总被引:1,自引:0,他引:1
研究了离子排斥色谱中色谱柱温度对有机酸(脂肪酸、芳香酸)保留的影响。采用Shim-pack SCR-102H离子排斥柱,分别以0.2 mmol/L p-甲苯磺酸为淋洗液分离6种脂肪族有机酸(甲酸、乙酸、丙酸、丁酸、戊酸和己酸)以及0.08 mmol/L H2SO4为淋洗液分离6种芳香酸(邻苯二甲酸、水杨酸、苯乙酸、对羟基苯甲酸、苯甲酸、邻甲苯甲酸),流速为1.2 mL/min,柱温控制为25~50℃,直接电导检测。结果表明,有机酸的保留值随温度升高而减小。但每种有机酸的保留受温度的影响程度不同,即当温度改变时,每种有机酸保留值的变化程度不同。一般规律为:有机酸的保留越强,其保留值随温度的变化程度越大。依据范特霍夫曲线的线性回归数据,可知有机酸的范特霍夫曲线具有良好的线性关系,其保留为放热过程。通过改变柱温,可以实现有机酸,特别是强保留有机酸保留值的改变,改善有机酸的色谱峰形和分离状况。 相似文献
996.
Arbia Khemiri Bertrand Naudin Xavier Franck Philippe Chan Tchi Song Thierry Jouenne Pascal Cosette 《Analytical and bioanalytical chemistry》2013,405(30):9835-9842
In prokaryote organisms, N-glycosylation of proteins is often correlated to cell–cell recognition and extracellular events. Those glycoproteins are potential targets for infection control. To date, many surface-glycosylated proteins from bacterial pathogens have been described. However, N-linked Pseudomonas surface-associated glycoproteins remain underexplored. We report a combined enrichment and labeling strategy to identify major glycoproteins on the outside of microorganisms. More precisely, bacteria were exposed to a mix of biotinylated lectins able to bind with glycoproteins. The latter were then recovered by avidin beads, digested with trypsin, and submitted to mass spectrometry. The targeted mixture of glycoproteins was additionally deglycosylated in the presence of H2 18O to incorporate 18O during PNGase F treatment and were also analyzed using mass spectrometry. This approach allowed us to identify a few tens of potential N-glycoproteins, among which flagellin FliC was the most abundant. To detect the possible sites of FliC modifications, a de novo sequencing step was also performed to discriminate between spontaneous deamidation and N-glycan loss. This approach led to the proposal of three potential N-glycosylated sites on the primary sequence of FliC: N26, N69, and N439, with two of these three asparagines belonging to an N-X-(S/T) consensus sequence. These observations suggest that flagellin FliC is a heterogeneous protein mixture containing both O- and N-glycoforms. Figure
Analytical scenario developed for bacterial glycoprotein enrichment. This strategy includes three main steps: (1) exposure of Pseudomonas aeruginosa cells to a mixture of biotinylated lectins [wheat germ agglutinin (WGA) and concanavalin A (ConA)]; (2) enrichment of N-glycoproteins by elution with avidin beads; and (3) mass spectrometry (MS) identification and characterization of intact and deglycosylated peptides before and after H2 18O PNGase F enzymatic treatment, respectively 相似文献
997.
Mingqiang Li Shixian Lv Zhaohui Tang Wantong Song Haiyang Yu Hai Sun Huaiyu Liu Xuesi Chen 《Macromolecular bioscience》2013,13(9):1150-1162
Rapid and efficient side‐chain functionalization of polypeptide with neighboring carboxylgroups is achieved via the combination of ring‐opening polymerization and subsequent thiol‐yne click chemistry. The spontaneous formation of polymersomes with uniform size is found to occur in aqueous medium via electrostatic interaction between the anionic polypeptide and cationic doxorubicin hydrochloride (DOX·HCl). The polymersomes are taken up by A549 cells via endocytosis, with a slightly lower cytotoxicity compared with free DOX ·HCl. Moreover, the drug‐loaded polymersomes exhibit the enhanced therapeutic efficacy, increase apoptosis in tumor tissues, and reduce systemic toxicity in nude mice bearing A549 lung cancer xenograft, in comparison with free DOX ·HCl. 相似文献
998.
Hongbin Zhu Shu Liu Xue Li Fengrui Song Zhiqiang Liu Shuying Liu 《Analytical and bioanalytical chemistry》2013,405(23):7437-7445
A novel fingerprinting method, bioactivity fingerprint analysis, based on an ultrafiltration–ultraperformance liquid chromatography–multistage tandem mass spectrometry (UPLC–MS n ) method is proposed for the quality control of herbal medicines from the bioactivity viewpoint concerning the efficacy of herbal medicines. The bioactivity fingerprints reflecting the anti-inflammatory activities of radix Aconiti and radix Aconiti preparata were established. With use of ultrafiltration UPLC–MS n , 11 cyclooxygenase-2 ligands from radix Aconiti preparata and 14 cyclooxygenase-2 ligands from radix Aconiti were found after incubation with cyclooxygenase-2. Twelve of the cyclooxygenase-2 ligands were identified by the ultraperformance UPLC–MS n method. The enrichment factor of each peak in the bioactivity fingerprint was calculated and was demonstrated to be characteristic, which makes bioactivity fingerprint analysis for the quality control of herbal medicines possible from the viewpoint of their bioactivities. Figure
Bioactivity fingerprint analysis is defined as the chromatograms and spectra of the complex system of effective constituents containing information on their pharmacodynamic activities 相似文献
999.
Tangbin Zou Hongfu Wu Huawen Li Qing Jia Gang Song 《Journal of separation science》2013,36(20):3457-3462
Mangiferin is the main bioactive component in mango leaves, which possesses anti‐inflammatory, antioxidative, antidiabetic, immunomodulatory, and antitumor activities. In the present study, a microwave‐assisted extraction method was developed for the extraction of mangiferin from mango leaves. Some parameters such as ethanol concentration, liquid‐to‐solid ratio, microwave power, and extraction time were optimized by single‐factor experiments and response surface methodology. The optimal extraction conditions were 45% ethanol, liquid‐to‐solid ratio of 30:1 (mL/g), and extraction time of 123 s under microwave irradiation of 474 W. Under optimal conditions, the yield of mangiferin was 36.10 ± 0.72 mg/g, significantly higher than that of conventional extraction. The results obtained are beneficial for the full utilization of mango leaves and also indicate that microwave‐assisted extraction is a very useful method for extracting mangiferin from plant materials. 相似文献
1000.
Xi‐Kai Shu Jia Li Feng Liu Xiao‐Jing Lin Xiao Wang Chun‐Xia Song 《Journal of separation science》2013,36(16):2680-2685
This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom. by accelerated solvent extraction combined with pH‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L9 (3)4. Then a separation and purification method was established using pH‐zone‐refining counter‐current chromatography with a two‐phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (5:5:2:8, v/v) with 10 mM triethylamine in the upper phase and 10 mM HCl in the lower phase. From 2 g crude extract, 224 mg of 8‐deacetylyunaconitine (I) and 841 mg of yunaconitine (II) were obtained with a purity of over 98.0%. The chemical structures were identified by ESI‐MS and 1H and 13C NMR spectroscopy. 相似文献