全文获取类型
收费全文 | 9772篇 |
免费 | 568篇 |
国内免费 | 627篇 |
专业分类
化学 | 9585篇 |
晶体学 | 14篇 |
力学 | 72篇 |
综合类 | 90篇 |
数学 | 123篇 |
物理学 | 1083篇 |
出版年
2024年 | 7篇 |
2023年 | 126篇 |
2022年 | 448篇 |
2021年 | 312篇 |
2020年 | 270篇 |
2019年 | 290篇 |
2018年 | 287篇 |
2017年 | 420篇 |
2016年 | 492篇 |
2015年 | 445篇 |
2014年 | 420篇 |
2013年 | 635篇 |
2012年 | 717篇 |
2011年 | 651篇 |
2010年 | 524篇 |
2009年 | 625篇 |
2008年 | 472篇 |
2007年 | 597篇 |
2006年 | 440篇 |
2005年 | 438篇 |
2004年 | 372篇 |
2003年 | 235篇 |
2002年 | 205篇 |
2001年 | 175篇 |
2000年 | 133篇 |
1999年 | 138篇 |
1998年 | 107篇 |
1997年 | 113篇 |
1996年 | 119篇 |
1995年 | 110篇 |
1994年 | 89篇 |
1993年 | 84篇 |
1992年 | 74篇 |
1991年 | 72篇 |
1990年 | 72篇 |
1989年 | 48篇 |
1988年 | 51篇 |
1987年 | 46篇 |
1986年 | 34篇 |
1985年 | 17篇 |
1984年 | 19篇 |
1983年 | 7篇 |
1982年 | 9篇 |
1981年 | 2篇 |
1980年 | 4篇 |
1979年 | 4篇 |
1978年 | 8篇 |
1976年 | 1篇 |
1966年 | 1篇 |
1959年 | 2篇 |
排序方式: 共有10000条查询结果,搜索用时 0 毫秒
71.
72.
建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料,经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后,用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积(单次洗脱体积×洗脱次数)对萃取效率的影响。结合高效液相色谱-荧光分析,在0.25~250 μg/L范围内线性关系良好(相关系数r=0.999),3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L,回收率为90.1%~102%,日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效,可用于尿液中羟基多环芳烃的分析。 相似文献
73.
Meng Wang Weiyue Feng Junwen Shi Fang Zhang Bing Wang Motao Zhu BaiLi Yuliang Zhao Zhifang Chai 《Talanta》2007,71(5):2034-2039
A mild, efficient and convenient extraction method of using 2-mercaptoethanol contained extractant solution combined with an incubator shaker for determination of mercury species in biological samples by HPLC–ICP-MS has been developed. The effects of the concentration of 2-mercaptoethanol, the composition of the extractant solution and the shaking time on the efficiency of mercury extraction were evaluated. The optimization experiments indicated that the quantitative extraction of mercury species from biological samples could be achieved by using 0.1% (v/v) HCl, 0.1% (v/v) 2-mercapoethanol and 0.15% (m/v) KCl extractant solution in an incubator shaker for shaking overnight (about 12 h) at room temperature. The established method was validated by analysis of various biological certified reference materials, including NRCC DOLT-3 (dogfish liver), IAEA 436 (tuna fish), IAEA MA-B-3/TM (garfish filet), IAEA MA-M-2/TM (mussel tissue), GBW 08193 (bovine liver) and GBW 08572 (prawn). The analytical results of the reference materials were in good agreement with the certified or reference values of both methyl and total mercury, indicating that no distinguishable transformation between mercury species had occurred during the extraction and determination procedures. The limit of detection (LOD) for methyl (CH3Hg+) and inorganic mercury (Hg2+) by the method are both as 0.2 μg L−1. The relative standard deviation (R.S.D.s) for CH3Hg+ and Hg2+ are 3.0% and 5.8%, respectively. The advantages of the developed extraction method are that (1) it is easy to operate in HPLC–ICP-MS for mercury species determination since the extracted solution can be directly injected into the HPLC column without pH adjustment and (2) the memory effect of mercury in the ICP-MS measurement system can be reduced. 相似文献
74.
A. E. Goncharov A. A. Politov N. A. Pankrushina O. I. Lomovskii 《Chemistry of Natural Compounds》2006,42(3):336-339
Extracts of Aconitum septentrionale Koelle roots obtained using chloroform, isopropanol, and ethanol were purified using chloroform and basic γ-Al2O3. Ballast materials were selectively adsorbed by γ-Al2O3, increasing the mass fraction of lappaconitine in the extract. The ethanol extract was purified most. The degree of lappaconitine
extraction by chloroform was unaffected by the presence of γ-Al2O3. However, the mass fraction in the extract and lappaconitine extraction from Aconitum septentrionale were increased more than twice.
__________
Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 274–276, May–June, 2006. 相似文献
75.
Hiroshi Iwase 《Analytica chimica acta》2002,463(1):21-29
Determination of small amounts of the fat-soluble species Vitamin A (VA) (2.5 μg/g) and β-carotene (9 μg/g) from emulsified nutritional supplements containing 50 kinds of co-existing compounds and a fat content between 2000 and 8000 times higher was performed by solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) with fluorescence detection set at ex. 350 nm and em. 480 nm, and visible detection at 450 nm using an Inertsil ODS 80A (5 μm) analytical column. Mobile phases of methanol-ethanol (50:50) and acetonitrile-ethanol (70:30) were used for the both vitamins. A Bond Elut C18 cartridge was chosen for SPE after comparison with eight other types of SPE cartridge. Retention time of VA and β-carotene was 7 and 8 min, respectively, giving a limit of detection of ca. 0.1 ng per injection at a signal-to-noise ratio 3:1. Recoveries of VA and β-carotene were over 90% by the standard addition method. Relative standard deviation of VA and β-carotene were ca. 2.9 (n=5) and 2.3% (n=5), respectively. 相似文献
76.
77.
A procedure of analysis for small-angle X-ray scattering (SAXS) data has been established to obtain density fluctuation of supercritical fluids near the critical point. It is indispensable for the certain analysis to utilize both of high-quality SAXS data measured under stable thermodynamic condition and accurate P–ρ–T data in supercritical region. As a standard example, SAXS measurements have been performed for supercritical CO2, which is a suitable sample satisfying the condition for both experiment and analysis. The measurements were carried out along four isothermal conditions at reduced temperature of Tr = T/Tc = 1.020, 1.022, 1.043 and 1.064. Comparing the experimental density fluctuation with calculated one from the most reliable equation of state, the differences are within 8% at most. 相似文献
78.
流动注射在线液—液萃取原子吸收光谱法测定生物样品中的铅 总被引:8,自引:2,他引:8
本文利用所设计的一种新型流动注射液-液萃取重力分相器,建立了流动注射液溶剂萃取原子吸收光谱法测定铅的新方法,详细地研究了流动注射在线萃取的实验条件及流路系统,方法的精密度和检出限分别为2.5%(n=11)和2.8μg/L(k=3)。用拟定的方法测定了峰蛹,粮食等生物样品中的铅,结果与参考值相吻合。 相似文献
79.
用硅胶-氧化铝柱色谱预分离和色谱-质谱分析研究了两种褐煤超临界流体抽提物中脂肪烃馏分组成结构特征。结果表明,除主要成份正构烷烃(C_(13)~C_(33))外,尚有少量的类异戊二烯烃(姥鲛烷、植烷等)和萜烷。其中萜烷以五环三萜为主(C_(27)、C_(29)~C_(32)藿烷类化合物),并有一定量的C_(27)、C_(29)和C_(30)藿烯,倍半萜和三环二萜烷含量很少。未检出甾烷。此外,还检出一完整系列的烯烃。试验结果表明,超临界流体抽提条件对褐煤抽出物各组分、含量及其分布有一定的影响。 相似文献
80.