全文获取类型
收费全文 | 1789篇 |
免费 | 154篇 |
国内免费 | 471篇 |
专业分类
化学 | 1913篇 |
晶体学 | 15篇 |
力学 | 35篇 |
综合类 | 33篇 |
数学 | 62篇 |
物理学 | 356篇 |
出版年
2024年 | 3篇 |
2023年 | 27篇 |
2022年 | 23篇 |
2021年 | 113篇 |
2020年 | 118篇 |
2019年 | 79篇 |
2018年 | 60篇 |
2017年 | 71篇 |
2016年 | 77篇 |
2015年 | 75篇 |
2014年 | 75篇 |
2013年 | 200篇 |
2012年 | 130篇 |
2011年 | 142篇 |
2010年 | 88篇 |
2009年 | 120篇 |
2008年 | 113篇 |
2007年 | 113篇 |
2006年 | 124篇 |
2005年 | 125篇 |
2004年 | 68篇 |
2003年 | 95篇 |
2002年 | 61篇 |
2001年 | 39篇 |
2000年 | 48篇 |
1999年 | 36篇 |
1998年 | 24篇 |
1997年 | 19篇 |
1996年 | 18篇 |
1995年 | 20篇 |
1994年 | 17篇 |
1993年 | 8篇 |
1992年 | 11篇 |
1991年 | 8篇 |
1990年 | 10篇 |
1989年 | 5篇 |
1988年 | 14篇 |
1987年 | 6篇 |
1986年 | 6篇 |
1985年 | 4篇 |
1984年 | 10篇 |
1983年 | 1篇 |
1982年 | 4篇 |
1981年 | 2篇 |
1980年 | 1篇 |
1979年 | 3篇 |
排序方式: 共有2414条查询结果,搜索用时 15 毫秒
81.
Li Qiu WANG Xiao Jun PENG* Rong ZHANG Guo Quan XU Jing Nan CUI State Key Laboratory of Fine Chemicals Dalian University of Technology Dalian 《中国化学快报》2003,(1)
Indocyanine dyes as fluorescent labeling reagents have been used in bioanalysis1,2. Arylsulfonate indocyanine dyes 1d and 1e developed by Waggoner A. S. et al.3,4 have excellent fluorescent properties combined with good aqueous solubility, are a new generation of fluorescent label compounds for proteins, oligonucleotides and other compounds containing hydroxyl, mercaptol or primary amine groups5. However, photostability of these dyes has been a problem. Z. G. YAO et al.6 reported that p… 相似文献
82.
自动化样品预处理的一项新技术——吉尔森ASTED系统及其应用(续完)陈小华(华运有限公司香港上环永乐街172—176号永富商业大厦三楼)3应用吉尔森ASTED系统已经被广泛地应用在许多领域,如药理学、药物动力学、药物-蛋白质结合研究、毒理学、临床医学... 相似文献
83.
84.
The title Schiff base compound,C19H19N3O3,a derivative of antipyrine,has been synthesized and characterized by elemental analysis,IR,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group C2/c,with α = 27.935(5),b = 7.553(1),c =16.692(3) (A),β = 105.810(3)°,Z= 8,V= 3388.7(10) (A)3,Dc = 1.323 g/cm3,Mr = 337.37,λ(MoKα) =0.71073 (A),μ = 0.091 mm-1,F(000) = 1424,R = 0.0630 and wR = 0.1273.A total of 3513 unique reflections were collected,of which 2112 with I > 2σ(I) were observed.The molecular structure adopts a trans configuration about the C=N double bond.The pyrazoline and C(1)~C(6) pheny1 ring are approximately coplanar (mean deviation from the combined plane is 0.069(3) (A)),with the dihedral angle of 9.7(2)°.The preliminary biological tests show that the compound has high antibacterial activities. 相似文献
85.
Steroids comprise a large group of natural substances that must frequently be monitored in various biological materials. Due to the metabolic versatility of steroid molecules, extremely complex mixtures are often encountered, necessitating the use of a chromatographic procedure prior to measurement. In this article we present our work, that is, the development of analyses of biological steroids (especially vitamin D compounds and neurosteroids) using gas chromatography/mass spectrometry, high-performance liquid chromatography (including inclusion chromatography using cyclodextrin) and liquid chromatography/mass spectrometry. 相似文献
86.
In order to search for novel agrochemicals with high activity and low toxicity, a series of phosphonate derivatives containing 1,2,3-triazole and thiazole rings were designed and synthesized using 2-chloro-5-(chloromethyl)- thiazole as the starting material. Their structures were confirmed by IR, ^1H NMR, ^31p NMR, EI-MS or ESI-MS and elemental analyses. The crystal structure of 7a was determined by single crystal X-ray diffraction. Preliminary bioassays indicated that most of the target compounds did not display insecticidal activities, but a fraction of them possessed herbicidal and fungicidal activities to some extent. 相似文献
87.
Orhan Acar 《Mikrochimica acta》2005,151(1-2):53-58
Lead, Cr, Mn and Zn in slurries of botanic and biological samples were determined by electrothermal atomic absorption spectrometry (ETAAS) using W, Ir, NH4H2PO4, W and NH4H2PO4, Ir and NH4H2PO4, W and Ir, and W + Ir + NH4H2PO4 chemical modifiers in an 0.2% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture. Zeeman effect background correction was performed and platforms inserted into graphite tubes were used. Comprehensive comparative studies were carried out with respect to pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, detection limits and accuracy of the determinations in the presence and absence of modifiers. The mixture of W + Ir + NH4H2PO4 was found to be preferable for the determination of Pb, Cr, Mn and Zn in slurry samples. The pyrolysis temperatures of the analytes were increased up to 1250 °C for Pb, 1000 °C for Zn, 1400 °C for Cr and Mn by using W + Ir + NH4H2PO4 with an 0.2% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture used as diluent solution. The optimum masses of the mixed modifier components were found to be 20 µg W + 4 µg Ir + 50 µg NH4H2PO4. The characteristic masses of Pb, Cr, Mn and Zn obtained are 16.3, 5.6, 0.1 and 1.1 pg, respectively. The detection limits of Pb, Cr, Mn and Zn based on integrated absorbance for 0.5% (m v−1) slurries were found to be 0.14, 0.06, 0.02 and 0.01 µg g−1, respectively. The slurries of botanic and biological certified and standard reference materials were analyzed with and without the modifiers. Depending on the sample type, the percent recoveries increased from 63 up to 104% for analytes when using the proposed modifier mixture. 相似文献
88.
Nitrogen doped nano porous graphene as a sorbent for separation and preconcentration trace amounts of Pb,Cd and Cr by Ultrasonic assisted in‐syringe dispersive micro solid phase extraction 下载免费PDF全文
Nitrogen doped nano porous graphene was used as an efficient sorbent in solid‐phase extraction process for simultaneous separation and pre‐concentration of metal ions lead (II), cadmium(II), and chromium(III)) in biological samples. Ultrasonic assisted in‐syringe dispersive micro solid phase extraction coupled with micro sampling atomic absorption spectrometry was utilized for the determination of metal ions. Nitrogen doped nano porous graphene was synthesized as a nano sorbent by chemical vapour deposition method. Methane and aniline were used as carbon and nitrogen sources. The characterization of sorbent was performed by field emission scanning electron microscope, transmission electron microscopy, atomic force microscope, fourier transform infrared, chemical element analysis and raman analysis. Effective parameters on the extraction efficiency such as pH, sorbent dosage, eluent volume and eluent concentration were optimized by central composite design and desirability function. Experimental results indicate that the optimal conditions for this extraction were pH = 6.4, 1.42 mg of sorbent, 100 μL of eluent, and 0.84 mol L‐1 of eluent concentration. The detection limits are as low as 1.5, 0.3 and 0.9 μg L‐1 for lead, cadmium, and chromium, respectively. The intra‐day precisions were 3.6, 4.38 and 2.94 and Inter‐day precision were 4.83, 5.26 and 4.52 for lead, cadmium, and chromium, respectively. Method performance was investigated by determination of mentioned heavy metals in complicated biological matrixes such as human plasma, urine and saliva samples with good recoveries. 相似文献
89.
Determination of hydroxysafflor yellow A in biological fluids of patients with traumatic brain injury by UPLC‐ESI‐MS/MS after injection of Xuebijing 下载免费PDF全文
Yong Guo Yang Wang Xi. Huang Huiying Lv Rong Fan Wei Huang Pingping Gan Wei Liu Kuipo Yan Zian Xia Jinfang Liu 《Biomedical chromatography : BMC》2014,28(8):1090-1095
A simple, novel, specific, rapid and reproducible ultra‐performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for the determination of hydroxysafflor yellow A (HSYA) in biological fluids (plasma, urine and cerebrospinal fluid) of patients with traumatic brain injury after intravenous injection of Xuebijing (XBJ). Liquid–liquid extraction was performed, and separation was carried out on an Acquity UPLC? BEH C18 column, with gradient elution using a mobile phase composed of methanol and 0.1% formic acid at a flow rate of 0.3 mL/min. A triple quadrupole tandem mass spectrometer with electrospray ionization was used for the detection of HSYA. The mass transition followed was m/z 611.0 → 491. The retention time was less than 3.0 min. The calibration curve was linear in the concentration range from 2 to 6125 ng/mL for cerebrospinal fluid, plasma and urine. The intra‐ and inter‐day precisions were <10%, and the relative standard deviation of recovery was <15% for HSYA in biological matrices. The method was successfully applied for the first time to quantify HSYA in the biological fluids (especially in cerebrospinal fluid) of patients with traumatic brain injury following intravenous administration of XBJ. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
90.
P. Garrigues C. Raoux P. Lemaire A. Mathieu D. Ribera J. F. Narbonne 《International journal of environmental analytical chemistry》2013,93(3):379-387
Abstract Biochemical indices based on enzymatic activities have been determined in fish and mussels sampled in various different coastal locations in the Mediterranean Sea. Preliminary results show a good agreement between biochemical measurements in marine organisms and chemical analyses of polycyclic aromatic hydrocarbons present in sediments. The results obtained suggest the use of biochemical indices for application in chemical contaminant biomonitoring. 相似文献