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Wan-Feng Zhang Xiao-Ping Xia Takahashi Eiichi Li Li Qing Yang Yan-Qiang Zhang Ya-Nan Yang Ming-Liang Liu Chunkit Lai 《Surface and interface analysis : SIA》2020,52(5):224-233
Secondary ion mass spectrometry (SIMS) has a wide range of applications in Earth Science research, thanks to its high precision and sensitivity, and its capacity in direct insitu micromeasurement. The technique is operated in ultra-high vacuum (UHV) conditions, especially for the measurement of volatiles such as hydrogen, or the water content in nominally anhydrous minerals (NAMs). To minimize the water background and obtain accurate and precise water contents in NAMs (eg, olivine) critical parameters such as presputtering time, field aperture (FA), dynamic transfer on/off, and primary beam current intensity were investigated for a CAMECA IMS 1280-HR system. When the chamber vacuum reaches approximately 2 × 10−9 mbar, we set the DTOS OFF, raster size to 50 μm and primary beam current to 5 nA, and used 2000 μm FA and 170-second presputtering time. Consequently, an approximately 1.2 ppmw water background and 3.6 ppmw limit of detection (LOD) were yielded, from analyzing the San Carlos olivine. Meanwhile, the water content and homogeneity of a range of olivine minerals were characterized for potential use as reference materials for SIMS water content measurement. Olivine water content calibration curve was also established by comparing the Fourier transform infrared (FTIR) results with the SIMS-measured 16O1H−/16O− ratios. Accuracy and precision of water content measurement were estimated to be better than approximately 10% in this study. 相似文献
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Guo-Qiang Tang Xian-Hua Li Qiu-Li Li Yu Liu Xiao-Xiao Ling 《Surface and interface analysis : SIA》2020,52(5):190-196
Carbonate oxygen (O) and carbon (C) isotopes are widely used as proxies for tracing the processes and physicochemical conditions of many geological events and environmental changes in Earth Science. In particular, O and C isotopic variations at micrometer scales revealed by modern microbeam analytical techniques such as SIMS and NanoSIMS are robust archives for reconstructing palaeoenvironment and paleoclimate changes at annual and seasonal resolution or even higher temporal resolution. Widespread application of carbonate O and C isotopic microanalysis in Earth Sciences, however, has been restricted due to limitation of high-quality carbonate reference materials for O and C isotopic microanalysis. We introduce in this paper a new calcite reference material for calcite O and C isotopic microanalysis. This calcite is collected from a drill-core of the Oka carbonatite complex (Quebec, Canada). We demonstrated that the Oka calcite is fairly homogeneous in O and C isotopic compositions at micrometer scales based on homogeneity test by hundreds of SIMS O and C isotopic analyses. Precise determinations by using conventional gas-source IRMS yield the recommended value of δ18OVPDB = −23.12 ± 0.15‰ (1SD) and δ13CVPDB = −5.23 ± 0.06‰ (1SD) for the Oka calcite, which has been certified as the first class of Chinese national certified reference material (GBW04481) for O and C isotopic microanalysis. 相似文献
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G-protein-coupled receptors (GPCRs) are the largest family of human membrane proteins and serve as primary targets of approximately one-third of currently marketed drugs. In particular, adenosine A1 receptor (A1AR) is an important therapeutic target for treating cardiac ischemia–reperfusion injuries, neuropathic pain, and renal diseases. As a prototypical GPCR, the A1AR is located within a phospholipid membrane bilayer and transmits cellular signals by changing between different conformational states. It is important to elucidate the lipid–protein interactions in order to understand the functional mechanism of GPCRs. Here, all-atom simulations using a robust Gaussian accelerated molecular dynamics (GaMD) method were performed on both the inactive (antagonist bound) and active (agonist and G-protein bound) A1AR, which was embedded in a 1-palmitoyl-2-oleoyl-glycero-3-phosphocholine (POPC) lipid bilayer. In the GaMD simulations, the membrane lipids played a key role in stabilizing different conformational states of the A1AR. Our simulations further identified important regions of the receptor that interacted distinctly with the lipids in highly correlated manner. Activation of the A1AR led to differential dynamics in the upper and lower leaflets of the lipid bilayer. In summary, GaMD enhanced simulations have revealed strongly coupled dynamics of the GPCR and lipids that depend on the receptor activation state. © 2019 Wiley Periodicals, Inc. 相似文献
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研究了快速溶剂萃取-液相色谱/质谱联用技术测定血液中PFAAs的方法。血液样品经过冷冻干燥,利用加速溶剂萃取的方法,最后使用液相色谱-质谱仪分析检测PFAAs成分。方法的回收率为74.6%~128.8%,检出限为1.10~25.1 ng/L。通过对珠江三角洲地区人群血液样本的分析,发现∑9PFAAs的浓度为26.8~557 ng/g,平均值为176±90.1 ng/g。血液中PFAAs的主要成分以PFHxA和PFOS为主,分别占血液中PFAAs浓度的20.97%和66.98%。人群血液中最常见和浓度最高的PFAAs是PFOS,而PFOA浓度相对较低。 相似文献
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养殖过程中的不合理使用和滥用使得水产品中氟喹诺酮抗生素残留累积量呈递增趋势,对人类的健康造成潜在的风险。建立高效、灵敏和可靠的水产品中氟喹诺酮类药物的同时分析方法十分重要。该研究建立了加速溶剂萃取-磁固相萃取-高效液相色谱-串联质谱法(ASE-MSPE-HPLC-MS/MS)测定水产品中沙拉沙星、氧氟沙星、恩诺沙星、丹氟沙星、洛美沙星、培氟沙星、环丙沙星、依诺沙星、诺氟沙星和双氟沙星残留的检测方法。采用室温自组装法,即在室温(25 ℃)下,将氧化石墨烯和零价纳米铁储备液快速涡旋混合,磁性分离收集沉淀物,得到GO@nZVI磁性复合材料。以扫描电镜、傅里叶变换红外光谱和X-射线衍射对磁性复合材料进行表征,结果显示GO@nZVI成功制备。该材料应用于MSPE净化中,ASE萃取温度为70 ℃,萃取溶剂为甲醇,萃取压力为10.34 MPa,静态萃取时间为5 min,循环萃取3次。萃取液浓缩后经MSPE有效净化后,采用Agilent ZORBAX Eclipse Plus C18色谱柱(100 mm×3.0 mm, 1.8 μm)梯度洗脱分离,MS/MS电喷雾正离子(ESI+)扫描、多反应监测(MRM)模式进行定量分析。氟喹诺酮的线性范围为1~100 μg/kg,线性相关系数(r2)均大于0.9995;目标物的检出限(S/N=3)为0.02~0.29 μg/kg,定量限(S/N=10)为0.07~0.98 μg/kg。所建方法成功用于黄鱼、草鱼、黑鱼、明虾和沼虾中氟喹诺酮的测定,在1倍、2倍、10倍定量限加标水平下得到的加标回收率为81.6%~105.8%,相对标准偏差(RSD)为4.2%~13.6%。研究表明,将ASE与MSPE有机结合,利用外部磁场实现萃取液的净化,无需离心和过滤操作,溶剂用量少,并且该方法所使用磁性萃取材料制备方法简单,具有自动化程度高、简便快速、方法灵敏度高、准确度高、重复性好等特点,可满足对水产品中FQs残留限量检测要求,具有实际应用前景。 相似文献
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对食品室内实物标样的定义、特点和应用进行了介绍,提出了食品室内实物标样的具体制作步骤和测试方法,并提供了室内实物标样制作和应用的实例。 相似文献
90.