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91.
J Ruiz-Jiménez 《Analytica chimica acta》2003,489(1):1-11
Flow injection (FI) manifolds based on iterative change of the flow direction have been designed to study the influence of auxiliary energy on continuous liquid-liquid extraction without phase separation and compare it with the non-assisted process in a single experiment. In order to demonstrate the utility of ultrasounds as auxiliary energy for the extraction of polyphenols from an organic phase, the approach has been applied to samples of extra virgin olive oil, using an alkaline aqueous phase as extractant and subsequent derivatization with the Folin-Ciocalteu reagent. The proposed method provides results similar to those from the official method-recoveries between 97 and 100%. The sensitivity of the proposed method is 3.5 times higher than that of the non-ultrasound-assisted method. The precision, expressed as relative standard deviation (R.S.D.) for n=5, was within 1-5% and the relative errors for the irradiated and non-irradiated method were within 3 and 5%, respectively. The repeatability and within-laboratory reproducibility, studied at two concentration levels (379 and 813 μg ml−1) ranged between 0.7-4.4% and 0.6-4.8%, respectively. The proposed manifolds can also be applied to either other type of auxiliary energies—microwave, thermal—or two different types of auxiliary energies at the same time. 相似文献
92.
We propose a new approach for high-throughput continuous titration based on a flow ratiometry. The method was applied to potentiometric titrations of acids and bases. A base solution, the flow rate FB of which was varied in response to controller output voltage Vc, was merged with an acid solution under constant total (acid + base) flow rate. Downstream, the pH of the mixed solution was measured with a flow-through glass electrode. Initially, Vc, and thus FB was increased linearly. At the instant the equivalence point (EP) was sensed, the ramp direction of Vc was reversed from upward to downward. The direction was reversed to upward when EP was sensed again. Such the feedback-based operation gives a triangular waveform of Vc, because there is a delay corresponding mainly to the transit time of merged solutions to reach the sensor. The value of Vc that gives EP composition, VE, was estimated by averaging the most recent maximum and minimum values of Vc. Next, fixed triangular waves of Vc was used to control FB. The amplitude and the scan rate of the waves were fixed narrower and faster, respectively, than those in the feedback-based operation in order to improve the throughput rate. The EP can be located as long as the scan range covers VE. These automated processes limited the titration to just the narrow range around EP, and thus realized extremely high throughput rate of maximally 17.6 titrations per minute (=3.4 s per titration) at R.S.D. = 0.35%. 相似文献
93.
An analytical method for the simultaneous determination of some trace elements (Au, Fe, Mg, Li, Sr, Zn) in human serum by inductively coupled plasma atomic emission spectrometry (ICP-AES) with flow injection is described. Physical interference caused by the change of sample viscosity is discussed. When 100 μl of serum was injected, the relevant recoveries of > 99% for Li, > 98% for Cu and Mg, > 95% for Fe were obtained for an NIST SRM with R.S.D. > 1.3% using optimized flow injection parameters. The prepared lyophilized control serum for routine analysis in clinical laboratories was analyzed and verified for the validity of the technique employed in this experiment using NIST SRM 909 as a primary reference material. 相似文献
94.
Two flow injection analyses (FIA) methods for the determination of diffusion coefficients in a straight single tube FIA system were developed. Based on the analytical solution of the convection-diffusion equation, linear relationships of the logarithmic values of the dispersion coefficient (D) and the half-peak width (W1/2) with the diffusion coefficient (Dm) were obtained. Experiments were designed to verify these methods. For example, for potassium hexacyanoferrate (III) a Dm value of 0.72 × 105 cm2 s−1 was found versus a literature value of 0.76 × 105 cm2 s−1 (error, 5%). For potassium hexacyanoferrate (II) a Dm value of 0.67 × 105 cm2 s−1 was obtained versus a literature value of 0.63 × 105 cm2 s−1 (error, 6%). The diffusion coefficients of some important biomedical compounds, such as dopamine, epinephrine, norepinephrine and ascorbic acid, were then determined. The values of 105 Dm/cm2 s−1 are 0.60 ± 0.03, 0.44 ± 0.02, 0.60 ± 0.01 and 0.68 ± 0.06, respectively. 相似文献
95.
A spot test was implemented in a flow-injection system for the spectrophotometric determination of zinc in digests of plant materials. It is based on the influence of Zn2+ on the oxidation rate of 1-naphthylethylenediamine (NED) by hexacyanoferrate(III) under acidic conditions. In order to control the precipitate formation and to maintain the resulting suspension, a micellar medium was established by adding Triton X-100. The proposed system handles about 65 samples per hour, meaning 72 μg NED and 9.0 mg K3[Fe(CN)6] per determination. Baseline drift is usually <0.01 absorbance per hour and the analytical signals for 0.5-2.5 mg l−1 Zn range within ca. 0.07-0.45 absorbance. Linearity of the analytical curve is fair (r>0.999, n=6) and detection limit was estimated as 0.2 mg l−1 Zn. Results are precise (R.S.D.<1%, n=10) and in agreement with flame atomic absorption spectrometry and with certified values of standard reference materials. 相似文献
96.
Surowiec I Baena JR Frank J Laurell T Nilsson J Trojanowicz M Lendl B 《Journal of chromatography. A》2005,1080(2):132-139
A flow-through microdispenser has been coupled to a micro HPLC separation system and used as a solvent elimination interface for Fourier transform infrared (FTIR) and Raman spectroscopic detection of the separated compounds. Using the microdispenser picoliter sized droplets can be generated and deposited on an appropriate target placed on a computerized x, y-stage. Evaporation of volatile solvent and buffer is rapid and allows analysis of the obtained dry deposits by various techniques. Due to the destruction free character of Raman and FTIR spectroscopy they can be applied sequentially to interrogate the same deposit. In the reported application five phenolic acids typically present in wine have been separated on a C-18 column technique using a mixture of water, methanol and acetic acid as mobile phase. For spectrum acquisition infrared and Raman microscopes have been used. The spectra recorded from the dried deposits of the separated compounds agreed well with the reference spectra of corresponding components. 相似文献
97.
Kim WS Park M Lee DW Moon MH Lim H Lee S 《Analytical and bioanalytical chemistry》2004,378(3):746-752
Fly ash has been regarded as hazardous because of its high adsorption of toxic organic and/or inorganic pollutants. Fly ash is also known to have broad distributions of different chemical and physical properties, such as size and density. In this study, fly ash emitted from a solid waste incinerator was pre-fractionated into six sub-populations by use of gravitational SPLITT fractionation (GSF). The GSF fractions were then analyzed by sedimentation field-flow fractionation (SdFFF) and ICP–AES. SdFFF analysis showed the fly ash has a broad size distribution ranging from a few nanometers up to about 50 µm. SdFFF results were confirmed by electron microscopy. Inductively coupled plasma–atomic emission spectroscopy (ICP–AES) analysis of the GSF fractions showed the fly-ash particles contain a variety of inorganic elements including Ca, Si, Mg, Fe, and Pb. The most abundant in fly ash was Ca, followed by Si then Mg. No correlations were found between trace element concentration and particle size. 相似文献
98.
99.
A flow-injection system is described for the determination of d-mannitol. Mannitol dehydrogenase is immobilized on poly(vinyl alcohol) beads and packed in a column (5 cm × 4 mm i.d.). The NADH formed is detected fluorimetrically. The response is linear between 5 × 10?7 and 1 × 10?4 M mannitol and the detection limit is 1 × 10?7 M. The throughput is 30 samples per hour. The reactor is stable for at least 8 weeks. 相似文献
100.
流动注射分光光度法测定微量硫氰酸根 总被引:2,自引:0,他引:2
基于3,5-Br2-PADAP硫氰酸根分别与重铬酸根,铈(IV)在硫酸介质中反应成不稳定的蓝色产物,建立了两种测定微量硫氰酸根的流动注射分光光度新方法,在前一方法中,硫氰酸根含量在0.80~7.20mg/L范围内可定量测定,检出限为0.27mg/L在后一方法中,硫氰酸根含量在0.80~6.40mg/L范围内呈线性,检出限为0.30mg/L。当进样体积为100μL时,进样频率为60次/h,所建立的两 相似文献