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《Journal of separation science》2018,41(17):3415-3423
A rapid analytical method was developed for the determination of 4‐methylimidazole from red ginseng products containing caramel colors by using dispersive liquid–liquid microextraction with in situ derivatization followed by gas chromatography with mass spectrometry. Chloroform and acetonitrile were selected as the extraction and dispersive solvents, and based on the extraction efficiency, their optimum volumes were 200 and 100 μL, respectively. The optimum volumes of the derivatizing agent (isobutyl chloroformate) and catalyst (pyridine), pH, and concentration of NaCl in the sample solution were determined to be 25 and 100 μL, pH 7.6, and 0% w/v, respectively. Validation of the optimized method showed good linearity (R2 > 0.999), accuracy (≥89.86%), intra‐ (≤6.70%) and interday (≤4.17%) repeatability, limit of detection (0.96 μg/L), and limit of quantification (5.79 μg/L). The validated method was applied to quantify 4‐methylimidazole in red ginseng juices and concentrates, 4‐methylimidazole was only found in red ginseng juices containing caramel colorant (42.91–2863.4 μg/L) and detected in red ginseng concentrates containing >1% caramel colorant. 相似文献
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AbstractA multiple columns and detections liquid chromatography system, including size exclusion chromatography (SEC) and reversed phase liquid chromatography (RPLC), for the analysis of macromolecules and micromolecules in ginseng root and leaf was developed. The columns were connected by two switching valves. Macromolecules were separated on a SEC column (TSK gel SuperMultipore PW-H column, 6?mm× 150?mm, 8?μm) by isocratic elution of 50?mM ammonium acetate aqueous solution, 0.3?mL/min of flow rate and detected by evaporative light scattering detection (ELSD). Micromolecules were analyzed on a Poroshell RP column (Agilent Poroshell 120?SB-Aq column, 4.6?mm × 50?mm, 2.7 µm) with gradient elution of water and acetonitrile, 0.6?mL/min of flow rate and detected by ultraviolet detection (UV). As a result, in the macromolecules chromatogram of ginseng root sample showed two main peaks while only one major peak for ginseng leaf. For micromolecules analysis, 17 compounds (3 nucleosides + 14 saponins) and 17 compounds (3 nucleosides + 1 flavonoid + 13 saponins) were found in ginseng root and leaf, respectively. The developed method is helpful for the quality evaluation of ginseng root and leaf. 相似文献
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Mechanical stress exerted upon impact-modified polycarbonate (PC) and poly(ethylene terephthalate) (PET) blends has been reported to generate microscopic voids via rubber-toughener (RT) particle cavitation which can macroscopically manifest to visibly whiten the material. Previous work has revealed a whitening phenomenon in collegiate American football helmet outer shells after a single season and in helmet-grade plaques following linear impact testing. The purpose of this research was to quantify the effects of repetitive linear drop exposures on the (i) impact performance; (ii) physical and thermal properties; and (iii) surface and tensile mechanical properties of a stress-whitened American football helmet outer shell material. Statistically significant changes in plaque impact performance corresponded to substantial stress-whitening that penetrated up to 40–45% into the plaque thickness and elicited shifts in surface and tensile mechanical properties. Nanoscale microscopy revealed elongation of the PC/PET matrix and delamination at the RT-matrix interface. Thermal property analysis suggested the concomitant occurrence of RT cavitation and strain-induced PET crystallization. Overall, the research identified a battery of diagnostic tools to characterize material property changes of stress-whitening in rubber-toughened helmet outer shell materials. 相似文献
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随着金融市场的不断发展, 期权作为一种能够规避风险的金融衍生产品越来越引起投资者的青睐, 成交量呈逐年上升的趋势, 期权定价问题已经成为金融数学领域中一个重要的研究课题. 本文主要研究Black-Scholes模型下美式回望期权定价问题的数值解法. 美式回望期权定价问题是一个二维非线性抛物问题, 难以直接应用数值方法进行求解. 通过分析该问题的求解难点, 本文给出解决该困难的有效方法. 首先利用计价单位变换将定价问题转换为一维自由边值问题, 并采用Landau's变换将求解区域规范化; 而后针对问题的非线性特点,利用有限体积法和Newton法交替迭代求解期权价格和最佳实施边界, 并对数值解的非负性进行了分析. 最后, 通过与二叉树方法进行比较, 验证了本文方法的正确性和有效性, 为实际应用提供了理论基础. 相似文献
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建立了固相萃取-超高效液相色谱测定人参中5种原人参二醇型人参皂苷的方法。人参药材经粉碎后通过水饱和正丁醇溶液进行超声提取,经过亲水作用固相萃取柱净化后,在ACQUITY UPLC BEH Shield RP18色谱柱(100 mm×2.1 mm,1.7 μm)上分离,利用乙腈/水作为流动相进行梯度洗脱,采用光电二极管阵列检测器检测。结果表明,5种原人参二醇型人参皂苷在5~500 μg/mL范围内具有很好的线性关系,相关系数均大于0.999。方法精密度的RSD值在0.95%~2.62%(n=6)之间,22 h内样品稳定性的RSD值在0.90%~2.15%(n=8)之间,日内和日间重复性的RSD值分别为5.35%~6.47%(n=6)和5.56%~6.34%(n=8)。方法的加标回收率在87.16%~101.92%之间,相对标准偏差在1.54%~4.01%(n=6)之间。所建立的方法采用亲水作用色谱模式的固相萃取材料,药材的提取液可直接作为固相萃取的上样溶液进行人参皂苷的富集和净化,并且超高效液相色谱大大缩短了分析时间。该方法简单快速、通量高、重现性好,适用于人参中5种原人参二醇型人参皂苷的定量分析。 相似文献
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因课程设置、学情等不同, PBL教学模式在中美高校化学实验课的实施过程中各具特色。本文从教材、课程考核、师资培训、研究机构和基金等4个角度客观分析PBL教学模式在中美2国高校化学实验课应用中的差异,并在此基础之上提出,应该客观公正地看待这种差异,树立文化自信。 相似文献
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假设股票变化过程服从跳一分形布朗运动,根据风险中性定价原理对股票发生跳跃次数的收益求条件期望现值推导出M次离散支付红利的美式看涨期权解析定价方程,并使用外推加速法求出当M趋于无穷时方程的二重、三重正态积分多项式表达,依此计算连续支付红利美式看涨期权价值.数值模拟表明通常仅需二重正态积分多项式能产生精确价值,而在极实值状态下则需三重正态积分多项式才能满足,结合两种多项式可以编出有效数字程序评价支付红利的美式看涨期权. 相似文献