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141.
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143.
This work shows the potentiality of As as internal standard to compensate errors from sampling of sparkling drinking water samples in the determination of selenium by graphite furnace atomic absorption spectrometry. The mixture Pd(NO3)2/Mg(NO3)2 was used as chemical modifier. All samples and reference solutions were automatically spiked with 500 μg l−1 As and 0.2% (v/v) HNO3 by the autosampler, eliminating the need for manual dilutions. For 10 μl dispensed sample into the graphite tube, a good correlation (r=0.9996) was obtained between the ratio of analyte absorbance by the internal standard absorbance and the analyte concentrations. The relative standard deviations (R.S.D.) of measurements varied from 0.05 to 2% and from 1.9 to 5% (n=12) with and without internal standardization, respectively. The limit of detection (LD) based on integrated absorbance was 3.0 μg l−1 Se. Recoveries in the 94-109% range for Se spiked samples were obtained. Internal standardization (IS) improved the repeatability of measurements and increased the lifetime of the graphite tube in ca. 15%. 相似文献
144.
Angela Lopedota Adriana Trapani Annalisa Cutrignelli Valentino Laquintana Nunzio Denora Massimo Franco Giuseppe Trapani Gaetano Liso 《Journal of inclusion phenomena and macrocyclic chemistry》2007,57(1-4):425-432
The objective of this work was to develop a novel microparticulate system based on the mucoadhesive polymer Eudragit-RS 100
and cyclodextrins (CDs), potentially useful for the oral administration of Glutathione (γ–glutamylcysteinylglycine, GSH).
For this purpose, an oil-in-oil (O/O) emulsion-solvent evaporation method was used for the preparation of microparticles (MPs)
containing GSH alone or together with one of the following CDs: α-, β-, γ-, methyl-β-(Me-β-), hydroxypropyl-β-(HP-β-) or sulfobutylether-β-cyclodextrin
(SBE7m-β-CD). MPs were obtained by emulsifying a mixture of Eudragit RS 100, GSH, CD and magnesium stearate in acetone or acetonitrile
with a mixture of liquid paraffin and Span 80. Size, encapsulation efficiency, and drug release of the prepared MPs were evaluated.
The results clearly indicated that all the examined properties were dependent on the water-miscible solvents and CD used.
In particular, MPs prepared by using acetone or acetonitrile showed different size distributions with mean diameters in the
ranges 82–350 and 15–22 μm, respectively. Moreover, encapsulation efficiency values were found to be high in all cases (71–99%)
and was significantly affected by the CD type. The GSH release rates were evaluated employing dissolution media with different
pH values (1.2, 6.8 and 7.4) and the following rank order was obtained for MPs prepared using acetone: MPs incorporating Me-β-CD > MPs
without CD > MPs incorporating the remaining CDs. On the other hand, MPs prepared using acetonitrile gave the highest GSH
release rate. Finally, stability of GSH encapsulated in MPs containing HP-β-CD to enzymatic attack by pepsin A, α-chymotrypsin,
and γ-glutamyltranspeptidase was also investigated. 相似文献
145.
Gheorghe A van Nuijs A Pecceu B Bervoets L Jorens PG Blust R Neels H Covaci A 《Analytical and bioanalytical chemistry》2008,391(4):1309-1319
A validated method based on solid-phase extraction (SPE) and liquid chromatography-ion trap tandem mass spectrometry (LC-MS/MS) is described for the determination of cocaine (COC) and its principal metabolites, benzoylecgonine (BE) and ecgonine methyl ester (EME), in waste and surface water. Several SPE adsorbents were investigated and the highest recoveries (95.7 +/- 5.5, 91.8 +/- 2.2 and 72.5 +/- 5.3% for COC, BE and EME, respectively) were obtained for OASIS HLB(R) cartridges (6 mL/500 mg) using 100 mL of waste water or 500 mL of surface water. Extracts were analysed by reversed-phase (RP) or hydrophilic interaction (HILIC) LC-MS/MS in positive ion mode with multiple reactions monitoring (MRM); the latter is the first reported application of the HILIC technique for drugs of abuse in water samples. Corresponding deuterated internal standards were used for quantification. The method limits of quantification (LOQs) for COC and BE were 4 and 2 ng L(-1), respectively, when RPLC was used and 1, 0.5 and 20 ng L(-1) for COC, BE and EME, respectively, with the HILIC setup. For COC and BE, the LOQs were below the concentrations measured in real water samples. Stability tests were conducted to establish the optimal conditions for sample storage (pH, temperature and time). The degradation of COC was minimal at -20 degrees C and pH = 2, but it was substantial at +20 degrees C and pH = 6. The validated method was applied to a set of waste and surface water samples collected in Belgium. 相似文献
146.
Junia O. Alves Bruno G. Botelho Marcelo M. Sena Rodinei Augusti 《Journal of mass spectrometry : JMS》2013,48(10):1109-1115
Direct infusion electrospray ionization mass spectrometry in the positive ion mode [ESI(+)‐MS] is used to obtain fingerprints of aqueous–methanolic extracts of two types of olive oils, extra virgin (EV) and ordinary (OR), as well as of samples of EV olive oil adulterated by the addition of OR olive oil and other edible oils: corn (CO), sunflower (SF), soybean (SO) and canola (CA). The MS data is treated by the partial least squares discriminant analysis (PLS‐DA) protocol aiming at discriminating the above‐mentioned classes formed by the genuine olive oils, EV (1) and OR (2), as well as the EV adulterated samples, i.e. EV/SO (3), EV/CO (4), EV/SF (5), EV/CA (6) and EV/OR (7). The PLS‐DA model employed is built with 190 and 70 samples for the training and test sets, respectively. For all classes (1–7), EV and OR olive oils as well as the adulterated samples (in a proportion varying from 0.5 to 20.0% w/w) are properly classified. The developed methodology required no ions identification and demonstrated to be fast, as each measurement lasted about 3 min including the extraction step and MS analysis, and reliable, because high sensitivities (rate of true positives) and specificities (rate of true negatives) were achieved. Finally, it can be envisaged that this approach has potential to be applied in quality control of EV olive oils. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
147.
Electrochemical Behaviour and Rapid Determination of L‐Dopa at Electrochemically Pretreated Screen Printed Carbon Electrode
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Andreea Alexandra Rabinca Mihaela Buleandra Adriana Balan Ioan Stamatin Anton Alexandru Ciucu 《Electroanalysis》2015,27(10):2275-2279
A simple and rapid voltammetric method based on a disposable electrochemically pretreated screen‐printed carbon electrode is proposed for the determination of L ‐dopa. Under optimum differential pulse voltammetry conditions a limit of detection of 3.6×10?7 M for L ‐dopa was obtained. The method was successfully applied to the determination of L ‐dopa in a commercial pharmaceutical formulation. 相似文献
148.
Carolina M. Rodrigues Odair P. Ferreira Oswaldo L. Alves 《Journal of nanoparticle research》2010,12(7):2355-2361
In this work is reported the synthesis of nanotubes and nanoribbons from mixed oxides (Ti1−x
Zr
x
O2·nH2O), employing hydrothermal treatment in a highly alkaline medium. The morphology and crystal structure of the products obtained
via hydrothermal treatment depend on the value of x. For example, for x equal to 0 and 0.50 were observed the presence of nanotubes (diameter around 9 nm) and nanoribbons (diameter around 200 nm),
respectively. However, for x values above 0.50, there was no morphological change. Regarding the crystalline structure of these samples, for x equal to 0 was observed the sodium titanate phase; already for x values up to 0.50, we observed the presence of two crystalline phases: sodium titanate and tetragonal ZrO2. For x values above 0.50, only tetragonal ZrO2 was observed. Furthermore, only the product obtained from x equal to 0.15 was observed the presence of three-dimensional flower-like arrangements. The results obtained by the characterization
techniques showed the segregation of zirconium after hydrothermal treatment of precursors with x less or equal to 0.50. Thus, we describe the important role that Ti/Zr molar ratio of the precursor plays on the morphology
and crystalline phase of the products formed by hydrothermal treatment. 相似文献
149.
Vivian?Regina?Trist?o Fernando?Felippe?de?Carvalho Cinthia?Zanini?Gomes Adriana?Regina?Miranda Cíntia?C.?Vequi-Suplicy Maria?Teresa?Lamy Nestor?Schor Maria?Helena?Bellini 《Journal of fluorescence》2010,20(3):665-669
The progression to end-stage renal failure is independent of the initial pathogenic mechanism. Metabolic acidosis is a common
consequence of chronic renal failure that results from inadequate ammonium excretion and decreased tubular bicarbonate reabsorption.
Protoporphyrin IX (PpIX) is the immediate metabolic precursor of the heme molecule. The purpose of this study was to evaluate
the levels of erythrocytes protoporphyrin IX at an animal model during progressive renal disease. A total of 36 eight-week-old
male Wistar rats were divided into six groups: Normal, 4 and 8 weeks after 5/6 nephrectomy (NX). Renal function was evaluated
by creatinine clearance and plasma creatinine levels. The autofluorescence of erythrocytes porphyrin of healthy and NX rats
was analyzed using fluorescence spectroscopy. Emission spectra were obtained by exciting the samples at 405 nm. Significant
differences between normal and NX rats autofluorescence shape occurred in the 600–700 nm spectral region. A correlation was
observed between emission band intensity at 635 nm and progression of renal disease. 相似文献
150.
Dayanne Cristiane Mozaner Bordin Marcela Nogueira Rabelo Alves Eduardo Geraldo de Campos Bruno Spinosa De Martinis 《Journal of separation science》2016,39(6):1168-1172
Disposable pipette tips extraction consists of a solid‐phase extraction in which the sorbent is poorly dispersed in a pipette tip, which allows a quick and dynamic contact between the aspirated analyte from the sample and the solid phase. It is a technique used particularly in food and forensic analysis, since it requires a small amount of sample and solvent. This article highlights the principles, advantages and disadvantages of the disposable pipette tips extraction method and reviews recent applications. 相似文献