全文获取类型
收费全文 | 5374篇 |
免费 | 163篇 |
国内免费 | 277篇 |
专业分类
化学 | 4831篇 |
晶体学 | 26篇 |
力学 | 89篇 |
综合类 | 79篇 |
数学 | 138篇 |
物理学 | 651篇 |
出版年
2024年 | 3篇 |
2023年 | 27篇 |
2022年 | 88篇 |
2021年 | 67篇 |
2020年 | 95篇 |
2019年 | 85篇 |
2018年 | 68篇 |
2017年 | 103篇 |
2016年 | 118篇 |
2015年 | 137篇 |
2014年 | 127篇 |
2013年 | 283篇 |
2012年 | 513篇 |
2011年 | 229篇 |
2010年 | 175篇 |
2009年 | 235篇 |
2008年 | 209篇 |
2007年 | 347篇 |
2006年 | 271篇 |
2005年 | 255篇 |
2004年 | 264篇 |
2003年 | 247篇 |
2002年 | 193篇 |
2001年 | 124篇 |
2000年 | 136篇 |
1999年 | 135篇 |
1998年 | 124篇 |
1997年 | 114篇 |
1996年 | 124篇 |
1995年 | 142篇 |
1994年 | 123篇 |
1993年 | 132篇 |
1992年 | 160篇 |
1991年 | 77篇 |
1990年 | 42篇 |
1989年 | 64篇 |
1988年 | 40篇 |
1987年 | 24篇 |
1986年 | 26篇 |
1985年 | 13篇 |
1984年 | 21篇 |
1983年 | 8篇 |
1982年 | 10篇 |
1981年 | 8篇 |
1980年 | 11篇 |
1979年 | 8篇 |
1978年 | 6篇 |
1976年 | 1篇 |
1972年 | 1篇 |
1970年 | 1篇 |
排序方式: 共有5814条查询结果,搜索用时 8 毫秒
51.
M. P. Carril M. Soledad Corbillón J. Manuel Madariaga 《Accreditation and quality assurance》1997,2(6):301-308
The development of an analytical method for the determination of some heavy metals (Fe, Cu, Co, Zn and Ni) in fluoride compounds
[Cu(BF4)2, Sn(BF4)2, Pb(BF4)2 and HBF4] by flame atomic absorption spectroscopy is described. This method is to be used as a routine analytical method in an industrial
quality control laboratory. To this end the "performance characteristics" of an instrumental analytical method such as matrix
effects, sensitivity, linearity, detection and quantitation limits, precision and accuracy were evaluated for every system
under study. The results of these investigations showed that non-spectral interferences (due to the presence of large concentrations
of major metals such as Cu, Sn and Pb) were observed. Nevertheless it was possible to define a matrix concentration interval
where matrix effects were not statistically significant, and therefore a direct calibration approach could be used as the
calibration tool whenever the major metal concentration was not higher than 40×10–3 kg l–1. A guide to the developement of an analytical method for trace metal determination is provided. General tools for quality
control have been used in order to show how an analytical method can be tested daily and evaluated in a convenient manner.
Received: 29 January 1997 Accepted: 11 March 1997 相似文献
52.
The fluorimetric determination of mercury ions with o-vanillin-8-aminoquinoline (OVAQ) in aqueous solutions was investigated. Hg(II) could react with the fluorescent reagent OVAQ
(λex/em = 278/314 nm) to form a nonfluorescent complex in an ethanol-water medium of pH 6.00. The linear range of the proposed method
was from 2.5 to 80 μg/L, and the detection limit was 0.80 μg/L. The interferences of 24 foreign ions were also studied. The
method was successfully applied to the determination of Hg(II) in sludge.
The text was submitted by the authors in English. 相似文献
53.
In this work, a simple and rapid analytical procedure was applied for simultaneous determination of folic acid (vitamin B0), thiamin (vitamin B1), riboflavin (vitamin B2) and pyridoxal (vitamin B6) based on the absorbance data in the pH range 2.0‐12.0 at 25 °C using parallel factor analysis (PARAFAC). The effect of the pH as the most important factor on the sensitivity of the determination was studied. The spectral data were recorded in 400‐650 nm intervals and a 2‐12 pH range for all four vitamins. The calibration set was constructed in the concentration ranges of 4‐22, 1‐20, 6‐26, and 4‐20 μg mL?;1 for B6,B2,B1 and B0, respectively. The root mean squares errors of prediction for the prediction set, (RMSEP), are 0.65, 0.63, 1.13 and 0.34 for B0,B1,B2 and B6, respectively. The recovery percent for the validation set are in the range of 90.6 to 107.0%. The effect of the experimental conditions and diverse species were discussed. The optimum values of these factors were searched according to the relative standard deviation of the prediction set of mixtures solutions. 相似文献
54.
提出了同时测定铜基合金中铝和铁的流动注射分析法。以0.04mol/LHCl作载液,铬天青S为显色剂,通过测定628nm处铝、铁两配合物的吸光度之和及铝配合物的吸光度,实现了两组分的同时测定。在优化的实验条件下,检测限:Al和Fe分别为1.69×10-3和1.73×10-3mg/L,Al浓度在0~0.8mg/L;Fe浓度在0~1.0mg/L时服从比耳定律。进样频率为60样/h,所拟方法用于实际样品分析,获得满意结果。 相似文献
55.
An extraction‐spectrophotometric method for the determination of trace amounts of copper and cobalt based on their extraction into n‐pentanol with 0. carboxyphenylhydrazoethylacetoacetate (O.CPHEAA) was per formed. Copper was extracted from pH 6.0 – 8.0 and ionic strength 0.5 M – KCl. The maximum absorption of the extracted Cu(II) ‐ O.CPHEAA complex (1:1 & 1:2 species) occurs at 415 nm. The proposed method succeeded in as saying a concentration of 3–63 μg per 10 mL of n‐pentanol (? = 1.25 × 104L mol?1 cm?1). The method failed to ex tract cobalt ion into various organic sol vents over a pH range of 2–11. The suggested method is highly selective and sensitive according to a wide scheme of interference studied. Copper in some plant samples was accurately estimated using the suggested method. The obtained results and the results of the AAS method were consistent. The reproducibility test shows a relative standard deviation of 1%. Sandell sensitivity for A = 0.001 is 5 × 10?3 μg cm?2. 相似文献
56.
Summary A method is described for the determination of small quantities of hydrochloric acid in two chlorinated organic solvents (CHCl3 and CCl4). An excess of gaseous ethylene oxide is added to a liquid sample; the 2-chloroethanol formed is then analyzed by gas chromatography. The procedure is simpler and more sensitive in comparison with other conventional methods. It can be modified for other organic solvents.D.G.R.C.S.T. grant. 相似文献
57.
S. Korhammer Rolf Herzig Peter Schramel Jorma Kumpulainen Bernd Markert Herbert Muntau Philippe Quevauviller 《Accreditation and quality assurance》2000,5(6):238-242
Cabbage is frequently used in environmental monitoring and food control, and, hence, cabbage reference materials (RMs) are
required for ensuring quality assurance. A cabbage RM was prepared in view of certification of specific elements from the
"black list" of high toxicological interest and nutritive importance. All tasks of the RM production (production of the plant
material, cutting and freeze-drying, determination of the residual water content, preparation of the RM, homogeneity testing,
stability testing, certification measurements) are described in detail.
Received: 12 November 1999 / Accepted: 29 January 2000 相似文献
58.
A simple, sensitive and rapid derivative spectrophotometric method using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) has been developed for simultaneous determination of Co(II), Ni(II) and Fe(II) which have very similar chemical behavior and appear together in many real samples. The complexes of all these metal ions with 5-Br-PADAP were formed immediately at pH 7.0 ammonium acetate buffered solution and were stable for at least 24 h. Second derivative spectra were selected for evaluation, because working wavelength determination was more precise and spectral overlap was less than in the ordinary and first derivative spectra. Three wavelengths at which the complexes exhibit extremum 2D values for Co(II), Ni(II) and Fe(II) were selected as analytical wavelengths, i.e., 640, 600 and 740 nm, respectively. Calibration curves drawn with zero-to-peak values at mentioned wavelengths were linear between 80 and 2000 ng ml−1 for each metal ion. Concentrations of Co(II) and Ni(II) were calculated from the total 2D values and the sum of the linear equations for these three cations at 640 and 600 nm, after Fe(II) assay by making use of the 2D value at 740 nm. Limits of detection (LOD) for Co(II), Ni(II) and Fe(II) were 2.7, 13.9 and 3.0 ng ml−1, respectively. The method has been applied to tool steel and heater resistance wire samples successfully. 相似文献
59.
60.
本文研究了Cu(Ⅱ)-PEG(聚乙二醇-2000)-Zincon(锌试剂)-(NH4)2SO4体系的析相光度法并应用于测定Cu(Ⅱ)。最宜酸度为pH5.5~8.5(KH2PO4-K2HPO4)缓冲溶液)其络合物的最大吸收位于610nm,表观摩尔吸光系数为4.0×10^4L.mol^-1.cm^-1,Cu(Ⅱ)浓度在0~1.5mg/L范围内服从比尔定律,铜与Zincon形式组成为1:2的稳定的蓝色络 相似文献