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121.
Highly sensitive catalytic determination of molybdenum 总被引:1,自引:0,他引:1
A novel, highly sensitive, selective, and simple kinetic method was developed for the determination of Mo(VI) based on its catalytic effect on the oxidation of 1-amino-2-naphthol-4-sulfonic acid (ANSA) with H2O2. The reaction was followed spectrophotometrically by tracing the oxidized product at 465 nm after 30 min of mixing the reagents. The optimum reaction conditions were: 10 mmol l−1 ANSA, 50 mmol l−1 H2O2, 100 mmol l−1 acetate buffer of pH 5.0 ± 0.05 and at 40 °C. Addition of 200 μg ml−1 diethylenetriaminepentaacetic acid (DTPA) conferred high selectivity for the proposed method. Following the recommended procedure, Mo(VI) could be determined with a linear calibration graph up to 2.5 ng ml−1 and a detection limit, based on the 3Sb-criterion, of 0.027 ng ml−1. The unique sensitivity and selectivity of the implemented method allowed its direct application to the determination of Mo(VI) in natural and industrial waste water. The method was validated by comparison with the standard ETAAS method. Moreover, published catalytic-spectrophotometric methods for the determination of molybdenum were reviewed. 相似文献
122.
123.
Surface modification of highly dispersed rubber fillers and pigments by titanate proadhesive and hydrophobic compounds 总被引:1,自引:0,他引:1
A method of modifying silicate and carbonate fillers with titanate coupling agents and proadhesive agents was worked out. The modification aimed at hydrophobization of filler surface by introduction to the surface of functional groups with chemical affinity to polymers. Optimum amounts of modifying substances and appropriate conditions for performing the modification process were established. The obtained fillers showed a high degree of hydrophobicity.The modified fillers were applied in rubber mixtures based on butadienestyrene or natural rubber, in polyurethanes, in PVC, and as pigments in oil dyes of high corossive resistance. 相似文献
124.
Sayo Ito Yoshihiro Ishikawa Satoshi Nishino Teruyuki Kobayashi Shigeru Ohba Yuzo Nishida 《Polyhedron》1998,17(25-26)
We have prepared several new iron(III) complexes with ligands which contain a phenol group; these are tetradentate [(X-phpy)H, X and H(phpy) represent the substituents on the phenol ring and N,N-bis(2-pyridylmethyl)-N-(2-hydroxybenzyl)amine, respectively] and pentadentate ligands [(R-enph-X)H; R=ethyl(Et) or methyl(Me) derivative and H(Me-enph) denotes N,N-bis(2-pyridylmethyl)-N″-methyl-N″-(2″-hydroxyl-benzylamine)ethylenediamine] and have determined the crystal structures of Fe(phpy)Cl2, Fe(5-NO2-phpy)Cl2, and Fe(Me-enph)ClPF6, which are of a mononuclear six-coordinate iron(III) complex with coordination of one or two chloride ion(s). These compounds are highly colored (dark violet) due to the coordination of phenol group to an iron(III) atom. When hydrogen peroxide was added to the solution of the iron(III) complex, a color change occurs with bleaching of the violet color, indicating that oxidative degradation of the phenol moiety occurred in the ligand system. The bleaching of the violet color was also observed by the addition of t-butylhydroperoxide. The rate of the disappearance of the violet color is highly dependent on the substituent on the phenol ring; introduction of an electron-withdrawing group in the phenol ring decreases the rate of bleaching, suggesting that disappearance of the violet band should be due to a chemical reaction between the phenol group and a peroxide adduct of the iron(III) species with an η1-coordination mode and that in this reaction the peroxide adduct acts as an electrophile towards phenol ring. The intramolecular interaction between the phenol moiety and an iron(III)-peroxide adduct may induce activation of the peroxide ion, and this was supported by several facts that the solution containing an iron(III) complex and hydrogen peroxide exhibits high activities for degradation of nucleosides and albumin. 相似文献
125.
Ion association in the system Ca(OH)2–H3PO4–KCl–H2O at 37°C has been studied potentiometrically over a range of pH from 3 to 9. The experimental conditions were optimized for the accurate determination of the association constants for the formation of the ion pairs CaH2PO
4
+
, CaHPO4 and CaPO
4
–
which were found to be 27.9±0.1, 591±2, and (1.35±0.02)×106 L-mol–1, respectively. 相似文献
126.
An automated analysis system is described for the measurement of hydrogen peroxide based on a chemiluminescence reaction with phenyl 10-methylacridinium-9-carboxylate (PMAC). A reversed FIA experimental arrangement is used to establish the operating conditions for the measurement of submicromolar levels of hydrogen peroxide. The carrier stream consists of hydrogen peroxide standards prepared in a pH 9.0, boric acid buffer and the flow rate for this carrier/sample stream is 4 ml/min. Twenty microliters of a 10 mM PMAC solution, prepared in a pH 3 phosphate buffer, are injected into the carrier/sample stream. Hydrogen peroxide mixes with the PMAC reagent in an incubation coil that is constructed by wrapping 107 cm of polyethylene tubing around a 1 cm o.d. plastic rod. The chemiluminescence reaction is then initiated by adding base just before the sample passes in front of a photomultiplier tube (PMT) detector. The calculated limit of detection (S/N = 3) for hydrogen peroxide is 0.25 M. In addition, the pH dependent hydrolysis of the PMAC reagent is characterized by an HPLC method which has been specifically developed for the separation and detection of the hydrolysis products of PMAC. Results indicate that a pH of 3.0 is required for long term stability of the PMAC reagent. Finally, this system has been successfully extended to the measurement of glutamate by coupling a bioreactor column of glutamate oxidase with the hydrogen peroxide detection scheme. A detection limit (S/N = 3) of 0.5 M has been established for glutamate with a throughput of 200 samples per hour. 相似文献
127.
The Raman spectra of molten mixtures of Ca(NO3)2\4H2O–KNO3 have been examined, covering the concentration range of 0–70 mole% KNO3. The frequencies in the spectra of the mixtures have been found to change slightly with concentration. Striking variations in the band shapes have been observed in the regions corresponding to the O–H stretching mode (2850–3850 cm–1) and the v4-NO
3
–
mode (700–750 cm–). The results are discussed in terms of perturbed quasi-lattice structure for the melt, in which there could be a displacement of water molecules in the first coordination sphere around Ca2+ by the NO
3
–
ion. 相似文献
128.
O. A. Kholdeeva R. I. Maksimovskaya G. M. Maksimov K. I. Zamaraev 《Reaction Kinetics and Catalysis Letters》1998,63(1):95-102
Alkylammonium salts of Ti(IV)-substituted heteropolytungstate, PW11TiO
10
5−
, catalyze the oxidation of methyl phenyl sulfide with hydrogen peroxide. The yield of the corresponding sulfoxide and sulfone
is practically quantitative. A31P NMR study confirms the formation and reactivity of the PW11O39TiO
2
5−
peroxo complex in organic media. 相似文献
129.
刘晓庚 《理化检验(化学分册)》2006,42(10):809-812
联合应用BPO与KIO3(在KI存在下)的倍增反应和光度滴定数据的二阶导数法处理,使面粉中微量BPO测定的灵敏度较常规碘量法提高了200倍,方法的检出限可达0.1 mg.L-1。在面粉实样分析中,测定结果的RSD值在1.3%~2.8%之间,加标回收率在98.6%~102.2%之间。提出的方法所得测定结果与国标法(GB/T 18415-2001)所得结果一致。 相似文献
130.
Guangdong Zhou Zhanlin Xu Xiaohong Guo Hong Zhuang Yanan Li Xueju Lü Tiexin Cheng Wenxing Li Kaiji Zhen 《Reaction Kinetics and Catalysis Letters》2005,85(1):57-64
Summary The oxidation of hexanol in the presence of the Keggin-type heteropoly compounds (HPCs) H3PMonW12-nO40 (denoted as PMonW12-n, n=0,1) and Na5PW11ZO39 (denoted as PW11Z, Z = Mn, Fe, Co, Ni, Cu and Zn) was carried out to produce hexanal and hexanoic acid. The reaction was conducted in tert-butanol (t-BuOH), using cetylpyridinium bromide (CPB) salts of HPA and 15% aqueous H2O2 as oxidant under mild condition. The PMoW11 catalyst showed higher hexanol conversion of 25%, the lowest selectivity to hexanal of 64.4% and an efficient utilization of H2O2 of 34%. Over the transition metal substituted PW11Z catalysts decomposition of H2O2 was rapid. For these PW11Z catalysts, the efficient utilization of H2O2 decreased to 9% or even lower. By means of IR, UV-visible and GC-MS techniques the catalysts were characterized. 相似文献