收费全文 | 9596篇 |
免费 | 503篇 |
国内免费 | 176篇 |
化学 | 7279篇 |
晶体学 | 51篇 |
力学 | 510篇 |
数学 | 1037篇 |
物理学 | 1398篇 |
2024年 | 15篇 |
2023年 | 62篇 |
2022年 | 306篇 |
2021年 | 405篇 |
2020年 | 445篇 |
2019年 | 461篇 |
2018年 | 509篇 |
2017年 | 451篇 |
2016年 | 661篇 |
2015年 | 452篇 |
2014年 | 616篇 |
2013年 | 1134篇 |
2012年 | 833篇 |
2011年 | 731篇 |
2010年 | 501篇 |
2009年 | 458篇 |
2008年 | 473篇 |
2007年 | 387篇 |
2006年 | 256篇 |
2005年 | 224篇 |
2004年 | 173篇 |
2003年 | 146篇 |
2002年 | 128篇 |
2001年 | 44篇 |
2000年 | 35篇 |
1999年 | 39篇 |
1998年 | 26篇 |
1997年 | 23篇 |
1996年 | 28篇 |
1995年 | 17篇 |
1994年 | 15篇 |
1993年 | 14篇 |
1992年 | 20篇 |
1991年 | 13篇 |
1990年 | 12篇 |
1989年 | 11篇 |
1988年 | 7篇 |
1987年 | 15篇 |
1986年 | 6篇 |
1985年 | 17篇 |
1984年 | 16篇 |
1983年 | 7篇 |
1982年 | 16篇 |
1981年 | 8篇 |
1980年 | 14篇 |
1979年 | 7篇 |
1978年 | 8篇 |
1977年 | 7篇 |
1976年 | 5篇 |
1975年 | 5篇 |
We describe a simple and efficient method for solid phase extraction and speciation of trace quantities of arsenic. It is based on the use of functionalized aluminum oxide nanoparticles and does not require any oxidation or reduction steps. The experimental parameters affecting extraction and quantitation were optimized using fractional factorial design methods. Adsorbed arsenic was eluted from the sorbent with 1 M hydrochloric acid and determined by graphite furnace atomic absorption spectrometry. Preconcentration factors up to 750 were achieved depending on the sample volume. Studies on potential interferences by various anions and cations showed the method to be highly selective. Under optimum conditions, the calibration plots are linear in the 5.0 to 280 ng L−1 and 8.0 to 260 ng L−1 concentration ranges for As(III) and total arsenic, respectively. The detection limits (calculated for S/N ratios of 3) are 1.81 and 1.97 ng L−1 for As(III) and total arsenic, respectively. The method was successfully applied to the determination and speciation of arsenic in (spiked) environmental, food and biological samples and gave good recoveries. The method was validated using a certified geological reference material.
相似文献A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L−1 with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L−1) is ±3.8 %, the detection limit is 31 pg L−1 (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g−1. The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %.
相似文献