全文获取类型
收费全文 | 9411篇 |
免费 | 1063篇 |
国内免费 | 614篇 |
专业分类
化学 | 6470篇 |
晶体学 | 31篇 |
力学 | 250篇 |
综合类 | 105篇 |
数学 | 365篇 |
物理学 | 3867篇 |
出版年
2024年 | 31篇 |
2023年 | 145篇 |
2022年 | 398篇 |
2021年 | 407篇 |
2020年 | 348篇 |
2019年 | 316篇 |
2018年 | 245篇 |
2017年 | 424篇 |
2016年 | 472篇 |
2015年 | 478篇 |
2014年 | 633篇 |
2013年 | 625篇 |
2012年 | 649篇 |
2011年 | 557篇 |
2010年 | 497篇 |
2009年 | 585篇 |
2008年 | 534篇 |
2007年 | 528篇 |
2006年 | 461篇 |
2005年 | 466篇 |
2004年 | 403篇 |
2003年 | 263篇 |
2002年 | 198篇 |
2001年 | 134篇 |
2000年 | 132篇 |
1999年 | 142篇 |
1998年 | 119篇 |
1997年 | 108篇 |
1996年 | 100篇 |
1995年 | 102篇 |
1994年 | 58篇 |
1993年 | 68篇 |
1992年 | 64篇 |
1991年 | 36篇 |
1990年 | 57篇 |
1989年 | 46篇 |
1988年 | 51篇 |
1987年 | 42篇 |
1986年 | 30篇 |
1985年 | 28篇 |
1984年 | 18篇 |
1983年 | 16篇 |
1982年 | 32篇 |
1981年 | 14篇 |
1980年 | 5篇 |
1979年 | 12篇 |
1978年 | 4篇 |
1971年 | 2篇 |
1969年 | 1篇 |
1959年 | 1篇 |
排序方式: 共有10000条查询结果,搜索用时 15 毫秒
101.
毛细管电泳在拮抗药物对氨基苯甲酸、对羟基苯甲酸和磺胺分析测定中的应用 总被引:2,自引:0,他引:2
本文报道了一种用毛细管区带电泳法(CZE)分离与测定对氨基苯甲酸、对羟基苯甲酸及磺胺类药物的新方法.电泳条件为:用 20mmol/L硼砂-20mmol/L H_3PO_4-20 mmol/Lβ-环糊精-4%乙醇(pH 7.0)作电泳液,L-抗坏血酸为内标,280nm为检测波长,样品由电进样方式(10kV/10s)引入毛细管(51.2 cm×50μm i.d.,有效分离长度为 38.5 cm).在24.5°C下,6 min内三者可达基线分离(电泳电压 25kV),且在一定范围内可进行定量分析,保留时间(Tr)及A_(样品)/A_(内标)的RSD值分别小于1.0%和5.0%.本法的建立为研究这三者共存于高等动物及微生物体内时的生理作用提供了一种可共选择的新方法. 相似文献
102.
Nadica Ivošević DeNardis Vera Žutić Vesna Svetličić Ranieri Urbani 《Electroanalysis》2007,19(4):473-478
In situ amperometric characterization of an aggregating system in terms of molecular adsorption and single microparticle interactions at the electrode interface is demonstrated using a model system: alginate/Ca(II) in an aqueous electrolyte solution. Recording of chronoamperometric curves of oxygen reduction at the dropping mercury electrode is designed for detection of dip‐shaped signals of individual gel microparticles. By addition of Ca(II) decrease of alginate adsorption is accompanied by appearance of signals indicating vesicle type association of alginate molecules and microparticles of gel phase. AFM imaging provided evidence of initial stage in calcium alginate gel formation. 相似文献
103.
Summary The highly complex matrix of diesel particulate extracts was analyzed for nitrated polycyclic aromatic hydrocarbons (nitro-PAH)
using fused-silica capillary-column gas chromatography along with a thermionic nitrogen-phosphorus detector (TID) and high-performance
liquid chromatography followed by on-line catalytic reduction of the nitro-PAH to amino-PAH and subsequent fluorescence detection.
Positive isomer identification and quantitation of nitro-PAH are from retention times of authentic standards and their mass
spectra. The ease of nitro-PAH formation by nitration of PAH raises the question regarding the origin of these species, whether
they are produced as “native” products during the engine combustion process and/or in the exhaust, or instead, formed as the
result of chemical conversion to produce artifacts during the sampling procedure. This problem is assessed examing 1-nitropyrene-concentration
in particulates of three light-duty diesel engines for different sampling times. 1-Nitropyrene concentrations show only a
moderate increase with sampling time under average sampling conditions.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
104.
Barnes JH Schilling GD Stone SF Sperline RP Denton MB Young ET Barinaga CJ Koppenaal DW Hieftje GM 《Analytical and bioanalytical chemistry》2004,380(2):227-234
The use of a separation step, such as liquid chromatography, prior to inductively coupled plasma mass spectrometry (ICP–MS) has become a common tool for highly selective and sensitive analyses. This type of coupling has several benefits including the ability to perform speciation analysis or to remove isobaric interferences. Several limitations of conventional instruments result from the necessity to scan or pulse the mass spectrometer to obtain a complete mass spectrum. When the instrument is operated in such a non-continuous manner, duty cycle is reduced, resulting in poorer absolute limits of detection. Additionally, with scanning instruments, spectral skew can be introduced into the measurement, limiting quantitation accuracy. To address these shortcomings, a high-performance liquid chromatograph has been coupled to an ICP–MS capable of continuous sample introduction and simultaneous multimass detection. These features have been realized with a novel detector array, the focal plane camera. Instrument performance has been tested for both speciation analysis and for the elimination of isobaric interferences. Absolute limits of detection in the sub picogram to tens of picograms regime are obtainable, while the added mass dimension introduced by simultaneous detection dramatically increases chromatographic peak capacity. 相似文献
105.
Bernard Herbreteau Michel Lafosse Luc Morin-Allory Michel Dreux 《Journal of separation science》1990,13(4):239-243
An evaluation of the most commonly used HPLC system (reversed phase octadecyl sillica gel) was undertaken in order to determine the level of certain carbohydrates in molasses produced in the refining of sugar beet. Chromatographic parameters and purification operations prior to analysis are discussed in order to develop an analytical method permitting automation of sugar determination. A Zorbax ODS column (250 × 9.4 mm), water elution, and light scattering detection allow easy determination of glucose + fructose, sucrose, and raffinose in molasses using an internal standard (maltose). 相似文献
106.
Summary A packed flow cell was used for fluorometric detection in micro high-performance liquid chromatography. The flow cell consisted of fused-silica tubing packed with the same material as the separation column. A focusing effect of the stationary phase on the signal intensity was observed, leading to an improvement of the mass detection limit, as achieved by on-column detection. 相似文献
107.
Summary Four most frequently used presentation forms of the ECD response are described. Equations describing the dependence of the
sensitivity, linearity and minimum detectable concentration of the ECD working under constant frequency mode of operation
on the pulse period are derived from Wenthworth’s kinetic model for all four forms mentioned above. The forms presented are
compared on the basis of equations derived. Results of the calculations are given and some predictions are experimentally
tested for sulphur hexafluoride. Good agreement was found between the predicted and observed relationships.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
108.
This paper describes the screening for metabolites of butoprozine, a new anti-anginal drug, in dog bile by means of reverse-phase HPLC. Although it does involve a simple clean-up step to remove a substantial amount of endogenous bile compounds, this screening method nevertheless avoids extraction of metabolites and thus allows all metabolites to be introduced into the chromatographic system. A single run of 100 minutes from 100% water to 100% methanol in a linear gradient effects adequate separation of the great majority of metabolites without interference from remaining endogenous compounds. Two methods of differentiating between metabolite peaks and endogenous peaks have been worked out. The first one makes use of 14C-labeled butoprozine by measuring the amount of radioactivity in the column effluent while simultaneously recording the UV absorbance. The second method compares continuous gradient chromatograms of bile recorded before and after butoprozine administration under very similar conditions. The latter method can be applied to both radioactive and non-radioactive materials. 相似文献
109.
Kizek R Masarik M Kramer KJ Potesil D Bailey M Howard JA Klejdus B Mikelova R Adam V Trnkova L Jelen F 《Analytical and bioanalytical chemistry》2005,381(6):1167-1178
The electroanalytical determination of avidin in solution, in a carbon paste, and in a transgenic maize extract was performed in acidic medium at a carbon paste electrode (CPE). The oxidative voltammetric signal resulting from the presence of tyrosine and tryptophan in avidin was observed using square-wave voltammetry. The process could be used to determine avidin concentrations up to 3 fM (100 amol in 3 l drop) in solution, 700 fM (174 fmol in 250 l solution) in an avidin-modified electrode, and 174 nM in a maize seed extract. In the case of the avidin-modified CPE, several parameters were studied in order to optimize the measurements, such as electrode accumulation time, composition of the avidin-modified CPE, and the elution time of avidin. In addition, the avidin-modified electrode was used to detect biotin in solution (the detection limit was 7.6 pmol in a 6 l drop) and to detect biotin in a pharmaceutical drug after various solvent extraction procedures. Comparable studies for the detection of biotin were developed using HPLC with diode array detection (HPLC-DAD) and flow injection analysis with electrochemical detection, which allowed biotin to be detected at levels as low as 614 pM and 6.6 nM, respectively. The effects of applied potential, acetonitrile content, and flow rate of the mobile phase on the FIA-ED signal were also studied. 相似文献
110.