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91.
二氧化碳和氧气的快速电化学方法联合测定 总被引:4,自引:0,他引:4
根据O2和CO2在二甲亚砜(DMSO)介质中Pt电极上的伏安特性,采用微电极并结构计算机控制的电位调制技术,建立了快速联合测定CO2和O2的调制电位脉冲库仑法和调制电位脉冲电流法,取得了满意的结果。一次测量时间快达40ms。CO2检测范围0 ̄10%(体积百分比);O2检测范围不受限制。通过编程设计特定的调制电位-时间波形,可保持连续检测的长期稳定性。 相似文献
92.
Guido Kickelbick Dieter Rutzinger Thomas Gallauner 《Monatshefte für Chemie / Chemical Monthly》2002,133(8):1157-1164
Summary. Hexadentate ligands were formed by the reaction of primary dimethylaminoethyl- or methoxyethylamines with formaldehyde. The
resulting N, N′, N″-functionalized hexahydro-1,3,5-triazines contain pending amino or ether functionalities which are able to coordinate to
metals in addition to the ring nitrogen atoms. Both ligands were reacted with CuBr, and novel tricopper clusters were isolated
and characterized by X-ray structure analysis. In these compounds a ring nitrogen atom, the pending amino or ether functionality,
and two bridging bromine atoms coordinate each of the copper atoms.
Received January 22, 2002; accepted (revised) March 22, 2002 相似文献
93.
This report describes the determination of paraquat (PQ) in human blood plasma samples by a direct-injection reversed-phase ion-pair chromatographic method. Blood plasma filtrate was injected directly into the LiChrospher® RP-18 alkyl-diol silica (ADS) precolumn integrated in a column switching system using a mixture of 3% 2-propanol and 10 mM sodium octane sulfonate (SOS) in a 0.05 M phosphate buffer (pH 2.8). After washing with this phase, the ADS precolumn was back-flushed with the analytical mobile phase consisting of 40% of methanol and 10 mM SOS in a 0.05 M phosphate buffer (pH 2.8) at a flow rate of 1.0 ml min−1, in order to carry the analyte to a conventional reversed-phase analytical column, where the separation of PQ was achieved and finally detected by UV at 258 nm. The recoveries of PQ from human blood plasma samples ranged between 95.0 and 99.5% at nine different concentrations (from 0.05 to 3.00 μg of PQ ml−1) with coefficients of variation <2.5% (n=3). The precision expressed as relative standard deviation was below 3.5% for between-day and below 4.3% for within-day measurements (n=5). The detection limit (signal-to-noise ratio, S/N>3) was 0.005 μg ml−1 with an injection volume of 200 μl. The proposed method is promising for the identification and quantification of PQ at low concentration levels and is suitable for its analysis in human blood plasma samples from intentional or accidental poisonings cases with a sample throughput of 5 samples per hour. 相似文献
94.
95.
A new highly sensitive and selective chromogenic reagent dibromo-p-methyl-carboxysulfonazo (DBMCSA) was synthesized and studied for the spectrophotometric determination of lead in detail. In 0.25 M phosphoric acid medium, which greatly increases the selectivity, lead reacts with DBMCSA to form a 1:2 blue complex, having a sensitive absorption peak at 648 nm. Under the optimal conditions, Beer's law is obeyed over the range from 0 to 0.8 μg ml−1 Pb(II) and the apparent molar absorptivity is 1.04×105 l mol−1 cm−1. The detection limit and the variation coefficient were found to be 2.14 ng ml−1 and 1.0%, respectively. It is found that, except for Ca(II) and Ba(II), all foreign ions studied do not interfere with determination. The interference caused by Ca(II) and Ba(II) can be easily eliminated by prior extraction with potassium iodide-methylisobutylketone. The method has been applied to the determination of lead in vegetables with satisfactory results. 相似文献
96.
《Analytica chimica acta》2002,459(2):229-234
The ligand 1,4,8-tri(n-octyl)-1,4,8,11-tetraazacyclotetradecane (L1) containing pendant octyl groups has been synthesised. L1 is a tetraazamacrocycle derived from the well-known cyclam unit, and the Ni2+ and Co2+ complexes, [Ni(L1)]2+ and [Co(L1)]2+, have been isolated and characterised. The ability of the nickel(II) and cobalt(II) complexes to act as anion receptors has been studied by using them as ionophores in membrane-based ion-selective electrodes (ISEs). The PVC membrane containing the complex [Ni(L1)]2+ and 2-nitrophenyloctylether as plasticizer shows a Nernstian response against iodide in a concentration range from 1×10−1 to 4×10−5 M I− with a detection limit of 1.6×10−5 M I− and a slope of 58.6 mV/pI− at pH 7 (25 °C). In comparison, the electrode containing [Co(L1)]2+ as ionophore gave a sub-Nernstian slope and a low lifetime. A comparison between the iodide-selective electrode containing [Ni(L1)]2+ and other reported iodide-selective electrodes is also reported. 相似文献
97.
98.
In the photovoltaic industry the etching of silicon in HF/HNO3 solutions is a decisive process for cleaning wafer surfaces or to produce certain surface morphologies like polishing or texturization. With regard to cost efficiency, a maximal utilisation of etch baths in combination with highest quality and accuracy is strived. To provide an etch bath control realised by a replenishment with concentrated acids the main constituents of these HF/HNO3 etch solutions including the reaction product H2SiF6 have to be analysed. Two new methods for the determination of the total fluoride content in an acidic etch solution based on the precipitation titration with La(NO3)3 are presented within this paper. The first method bases on the proper choice of the reaction conditions, since free fluoride ions have to be liberated from HF and H2SiF6 at the same time to be detected by a fluoride ion-selective electrode (F-ISE). Therefore, the sample is adjusted to a pH of 8 for total cleavage of the SiF62− anion and titrated in absence of buffers. In a second method, the titration with La(NO3)3 is followed by a change of the pH-value using a HF resistant glass-electrode. Both methods provide consistent values, whereas the analysis is fast and accurate, and thus, applicable for industrial process control. 相似文献
99.
Jadranka Vuković Shiro Matsuoka Kazuhisa Yoshimura Vladimir Grdinić Renata Jurišić Grubešić 《Mikrochimica acta》2007,159(3-4):277-285
A simple, sensitive and rapid solid-phase spectrophotometric procedure was developed for the determination of traces of phenol
with 4-aminoantipyrine as a reagent (AAP-SPS), and the optimal experimental conditions were established. This method was performed by sorption and direct absorbance measurements
of the product phenol-AAP sorbed on the anion-exchanger Dowex 1-X4 (0.2 g) at 495 nm (absorption maximum) and 700 nm (non-absorption wavelength). The
sensitivity offered by the AAP-SPS procedure was higher by a factor of 40 compared with the respective conventional spectrophotometric method. Metrological
characteristics were established using a prevalidation strategy. The AAP-SPS procedure is characterized by a linear calibration function in the working range of 0.05–0.50 μmol, low standard deviation
of procedure (±0.012), low limit of determination (0.021 μmol), and favorable random (±0.85 to ±11.27%) and systematic deviations
(−4.55 to +11.50%). Moreover, the accuracy of the system investigated by the recovery test is acceptable (99–102%). Favorable
working and performance characteristics make the new SPS method ideal for phenol monitoring in pharmaceutical preparations
as well as other matrices. 相似文献
100.
催化极谱法连续测定岩石中钨和钼 总被引:2,自引:0,他引:2
本文提出了在二苯基乙醇酸-二苯胍-氯酸钠催化极谱体系测钨后,加入少许钛铁试剂,使钼产生一个极灵敏的导数波。谊波形尖锐、对称,便于测量钼。建立的连测体系简便灵敏,用于岩石样品中钨和钼的测定,取得了满意的效果。 相似文献