全文获取类型
收费全文 | 1653篇 |
免费 | 227篇 |
国内免费 | 105篇 |
专业分类
化学 | 786篇 |
力学 | 143篇 |
综合类 | 17篇 |
数学 | 52篇 |
物理学 | 987篇 |
出版年
2024年 | 2篇 |
2023年 | 6篇 |
2022年 | 35篇 |
2021年 | 27篇 |
2020年 | 34篇 |
2019年 | 25篇 |
2018年 | 21篇 |
2017年 | 71篇 |
2016年 | 96篇 |
2015年 | 72篇 |
2014年 | 108篇 |
2013年 | 141篇 |
2012年 | 167篇 |
2011年 | 122篇 |
2010年 | 104篇 |
2009年 | 101篇 |
2008年 | 93篇 |
2007年 | 114篇 |
2006年 | 85篇 |
2005年 | 77篇 |
2004年 | 86篇 |
2003年 | 58篇 |
2002年 | 41篇 |
2001年 | 39篇 |
2000年 | 41篇 |
1999年 | 22篇 |
1998年 | 19篇 |
1997年 | 31篇 |
1996年 | 26篇 |
1995年 | 13篇 |
1994年 | 19篇 |
1993年 | 22篇 |
1992年 | 15篇 |
1991年 | 9篇 |
1990年 | 9篇 |
1989年 | 3篇 |
1988年 | 2篇 |
1987年 | 2篇 |
1986年 | 4篇 |
1985年 | 3篇 |
1984年 | 5篇 |
1983年 | 1篇 |
1982年 | 6篇 |
1981年 | 2篇 |
1980年 | 1篇 |
1979年 | 2篇 |
1978年 | 1篇 |
1973年 | 1篇 |
1957年 | 1篇 |
排序方式: 共有1985条查询结果,搜索用时 15 毫秒
1.
Quantitative determination of omega-6 and omega-3 polyunsaturated fatty acids in human plasma and urine with high accuracy and precision provides significant information to monitor the underlying etiology of several diseases. In this regard, liquid chromatography-mass spectrometry is a good choice owing to its great selectivity and sensitivity. Additionally, the hybrid quadrupole–time of flight–mass spectrometer systems provides easy identification of target compounds with superior mass measurements. In this study, an analytical method has been developed for simple, accurate and simultaneous determination of linoleic acid, arachidonic acid, docosahexaenoic acid and eicosapentaenoic acid in a short chromatographic analysis period. The developed method is suitable for the quantitative detection of these four compounds with detection limits ranging between 1.1–3.0 ng ml−1 and its applicability was assessed in human urine and plasma samples. As a result, acceptable accuracy (between 83 and 111%) and good precision (<6%) were obtained for target compounds using matrix matching calibration strategy. 相似文献
2.
CongZhan Liu YiFei Zhang XuFang Li XueFeng Lu Zhi Chang ZhengWei Li AiMei Zhang YongJie Jin HuiMing Yu Zhao Zhang MinXue Fu YiBao Chen JianFeng Ji YuPeng Xu JingKang Deng RenCheng Shang GuoQing Liu FangJun Lu ShuangNan Zhang YongWei Dong TiPei Li Mei Wu YanGuo Li HuanYu Wang BoBing Wu YongJie Zhang Zhi Zhang ShaoLin Xiong Yuan Liu Shu Zhang HongWei Liu YiJung Yang Fan Zhang 《中国科学:物理学 力学 天文学(英文版)》2020,(4):20-34
The Insight-Hard X-ray Modulation Telescope(Insight-HXMT) is a broadband X-ray and γ-ray(1-3000 ke V) astronomy satellite. One of its three main telescopes is the High Energy X-ray telescope(HE). The main detector plane of HE comprises 18 Na I(Tl)/Cs I(Na) phoswich detectors, where Na I(Tl) is used as the primary detector to measure ~ 20-250 ke V photons incident from the field of view(FOV) defined by collimators, and Cs I(Na) is used as the active shielding detector to Na I(Tl) by pulse shape discrimination. Additionally, Cs I(Na) is used as an omnidirectional γ-ray monitor. The HE collimators have a diverse FOV,i.e. 1.1°×5.7°(15 units), 5.7°×5.7°(2 units), and blocked(1 unit). Therefore, the combined FOV of HE is approximately5.7°×5.7°. Each HE detector has a diameter of 190 mm resulting in a total geometrical area of approximately 5100 cm2, and the energy resolution is ~15% at 60 ke V. For each recorded X-ray event by HE, the timing accuracy is less than 10 μs and the deadtime is less than 10 μs. HE is used for observing spectra and temporal variability of X-ray sources in the 20-250 ke V band either by pointing observations for known sources or scanning observations to unveil new sources. Additionally, HE is used for monitoring the γ-ray burst in 0.2-3 Me V band. This paper not only presents the design and performance of HE instruments but also reports results of the on-ground calibration experiments. 相似文献
3.
The amount of data collected during synchrotron X-ray diffraction (XRD) experiments is constantly increasing. Most of the time, the data are collected with image detectors, which necessitates the use of image reduction/integration routines to extract structural information from measured XRD patterns. This step turns out to be a bottleneck in the data processing procedure due to a lack of suitable software packages. In particular, fast-running synchrotron experiments require online data reduction and analysis in real time so that experimental parameters can be adjusted interactively. Dioptas is a Python-based program for on-the-fly data processing and exploration of two-dimensional X-ray diffraction area detector data, specifically designed for the large amount of data collected at XRD beamlines at synchrotrons. Its fast data reduction algorithm and graphical data exploration capabilities make it ideal for online data processing during XRD experiments and batch post-processing of large numbers of images. 相似文献
4.
A novel method is developed for the direct determination of naphazoline hydrochloride(NAP) and pyridoxine hydrochloride(VB6) in commercial eye drops. By using excitation–emission matrix(EEM)fluorescence coupled with second-order calibration method based on the alternating trilinear decomposition(ATLD) algorithm, the proposed approach can achieve quantitative analysis successfully even in the presence of unknown and uncalibrated interferences. The method shows good linearity for NAP and VB6 with correlation coefficients greater than 0.99. The results were in good agreement with the labeled contents. To further confirm the feasibility and reliability of the proposed method, the same batch samples were analyzed by multiple reaction monitoring(MRM) based on LC–MS/MS method.T-test demonstrated that there are no significant differences between the prediction results of the two methods. The satisfactory results obtained in this work indicate that the use of the second-order calibration method coupled with the EEM is a promising tool for industrial quality control and pharmaceutical analysis due to its advantages of high sensitivity, low-cost and simple implementation. 相似文献
5.
Roberto Kawakami Harrop Galvão Sófacles Figueredo Carreiro Soares Marcelo Nascimento Martins Maria Fernanda Pimentel Mário César Ugulino Araújo 《Analytica chimica acta》2015
This paper proposes a new method for calibration transfer, which was specifically designed to work with isolated variables, rather than the full spectrum or spectral windows. For this purpose, a univariate procedure is initially employed to correct the spectral measurements of the secondary instrument, given a set of transfer samples. A robust regression technique is then used to obtain a model with low sensitivity with respect to the univariate correction residuals. The proposed method is employed in two case studies involving near infrared spectrometric determination of specific mass, research octane number and naphthenes in gasoline, and moisture and oil in corn. In both cases, better calibration transfer results were obtained in comparison with piecewise direct standardization (PDS). The proposed method should be of a particular value for use with application-targeted instruments that monitor only a small set of spectral variables. 相似文献
6.
Anneli Kruve Riin Rebane Karin Kipper Maarja-Liisa Oldekop Hanno Evard Koit Herodes Pekka Ravio Ivo Leito 《Analytica chimica acta》2015
This is the part I of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry (LC–MS) and discuss specific issues that arise with MS (and MS/MS) detection in LC (as opposed to the “conventional” detectors). The Part I briefly introduces the principles of operation of LC–MS (emphasizing the aspects important from the validation point of view, in particular the ionization process and ionization suppression/enhancement); reviews the main validation guideline documents and discusses in detail the following performance parameters: selectivity/specificity/identity, ruggedness/robustness, limit of detection, limit of quantification, decision limit and detection capability. With every method performance characteristic its essence and terminology are addressed, the current status of treating it is reviewed and recommendations are given, how to determine it, specifically in the case of LC–MS methods. 相似文献
7.
The extrapolation scheme of correlation energy is revisited to evaluate the complete basis set limit from double‐zeta (DZ) and triple‐zeta levels of calculations. The DZ level results are adjusted to the standard asymptotic behavior with respect to the cardinal number, observed at the higher levels of basis sets. Two types of adjusting schemes with effective scaling factors, which recover errors in extrapolations with the DZ level basis set, are examined. The first scheme scales the cardinal number for the DZ level energy, while the second scheme scales the prefactor of the extrapolation function. Systematic assessments on the Gaussian‐3X and Gaussian‐2 test sets reveal that these calibration schemes successfully and drastically reduce errors without additional computational efforts. © 2015 Wiley Periodicals, Inc. 相似文献
8.
该文提出了一种基于麻雀搜索算法结合深度前馈神经网络(SSA-DFN)的近红外光谱模型转移方法。使用深度前馈神经网络拟合不同仪器采集到的光谱之间的非线性函数映射,并将麻雀搜索算法用于网络各层连接权值和阈值的初始化,通过种群中个体位置的迭代更新,求得连接权值和阈值的最优初始值;通过多次调整深度前馈神经网络模型的超参数,使网络拟合效果趋于最优,最终确定转移函数。为验证方法的有效性,分别从烟叶近红外光谱谱图、主成分投影和预测结果的角度,将SSA-DFN方法与分段直接校正算法(PDS)、典型相关性分析算法(CCA)转移前后的效果进行了对比。结果表明SSA-DFN方法转移后的从机光谱与原主机光谱重合度最高,转移后主、从机总糖、烟碱含量的预测结果差异不显著,预测平均误差从8.32%、9.15%分别降至4.65%、4.82%,预测均方根误差(RMSEP)和决定系数(R2)等指标均优于PDS和CCA,取得了最佳的转移效果,可满足企业需求。结果表明该方法是一种有效的模型转移方法。 相似文献
9.
10.
Anna Maria Orani Petko Mandjukov 《International journal of environmental analytical chemistry》2017,97(8):710-729
Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine biota samples using solid sampling high-resolution continuum source atomic absorption spectrometry (HR CS AAS) and accelerated fast temperature programmes has been developed. Calibration technique based on the use of solid certified reference materials similar to the nature of the analysed sample and statistics of regression analysis were applied. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability and reproducibility, limits of detection and quantification and expanded uncertainty for all investigated elements were assessed. The major contributors to the combined uncertainty of the analyte mass fractions were found to be the homogeneity of the samples and the microbalance precision. Traceability to the SI system of units of the obtained with the proposed analytical procedure results was also demonstrated. The potential of the proposed analytical procedure based on solid sampling HR CS AAS technique was demonstrated by direct analysis of marine reference biota samples. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of selected trace elements in marine biota samples, such as straightforward calibration, a high sample throughput, sufficient precision, a suitable limit of detection and reduced risk of analyte loss and contamination. 相似文献