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11.
气相法分析3-氯-2-羟丙基三甲基氯化铵中的微量有机杂质 总被引:9,自引:0,他引:9
以氯仿为萃取剂 ,对 3 氯 2 羟丙基三甲基氯化铵 (CHPTMA)水溶液进行萃取 ,用气相法分析了CHPT MA溶液中的微量有机杂质环氧氯丙烷和 1 3 二氯丙醇。柱为 2m× 3mmi d 的不锈钢填充柱 ,固定相为10 %的PEG 2 0M ,载体为ChromosorbW/AW。环氧氯丙烷和 1,3 二氯丙醇的回收率分别为 97 5 %~ 10 5 0 %和93 3%~ 98 8% ,相对标准偏差分别为 11 5 %和 13 1% ,最低检测限分别为 5 0 μg/g和 10 0 μg/ g。 相似文献
12.
Alexandra Lieb Juliane A. Kechele Robert Kraut Wolfgang Schnick Prof. Dr. 《无机化学与普通化学杂志》2007,633(1):166-171
The oxonitridoalumosilicates (so‐called sialons) MLn[Si4?xAlxOxN7?x] with M = Eu, Sr, Ba and Ln =Ho, Er, Tm, Yb were obtained by the reaction of the respective lanthanoid metal, the alkaline earth carbonates or europium carbonate, resp., AlN, “Si(NH)2” and MCl2 as a flux in a radiofrequency furnace at temperatures around 2100 °C. The compounds MLn[Si4?xAlxOxN7?x] are relevant for the investigation of substitutional effects on the materials properties due to their ability of tolerating a comparatively large phase width up to x ≈ 2.0(5). The crystal structures of the twelve compounds were refined from X‐ray single crystal data and X‐ray powder data and are found to be isotypic to the MYb[Si4N7] structure type. The compounds crystallize in space group P63mc (no. 186, hexagonal) and are made up of chains of so‐called starlike units [N[4](SiN3)4] or [N[4]((Si,Al)(O,N)3)4], respectively. These units are formed by four (Si,Al)(N/O)4 tetrahedra sharing a common central nitrogen atom. The structure refinement was performed utilizing an O/N‐distribution model according to Paulings rules, i.e. nitrogen was positioned on the four‐fold bridging site and nitrogen and oxygen were distributed equally on both of the two‐fold bridging sites, resulting in charge neutrality of the compound. The Si and Al atoms were distributed equally on their two crystallographic sites, referring to their elemental proportion in the compound, due to being poorly distinguishable by X‐ray methods. The chemical compositions of the compounds were derived from electron probe micro analyses (EPMA). 相似文献
13.
The micro construction of poly(epsilon-caprolactone) (PCL) and poly(L-lactic acid) (PLLA) blend films fabricated by solution casting under microwave irradiation was investigated by selective enzymatic degradation and scanning electron microscopy (SEM). The results were totally different from the blends obtained by conventional methods. The blend was more homogeneous and the PCL continuous phase more compact as no spherulites and tiny zone separation were observed from the film surface and no PCL network was observed inside the film, and the degradation of a PCL plank by Pseudomonas lipase was significantly retarded. The distributed PLLA micro spheres were enlarged and amorphous. The thermal behavior of the blend by microwave heating revealed that PCL and PLLA underwent a melting process, which induced the variations of the PCL phase and PLLA spheres. The weight loss caused by degradation of the PCL/PLLA blend obtained by conventional methods (B50c) is greater than that of the blend obtained by microwave methods (B50m), which reflects the change in morphology from a loose PCL network (B50c) to a dense PCL plank (B50m). 相似文献
14.
A. D. Davydov V. M. Volgin V. V. Lyubimov 《Russian Journal of Electrochemistry》2004,40(12):1230-1265
Basic problems of metal electrochemical shaping theory are considered. Exact and approxi1mate (quasi-steady-state, locally one-dimensional) methods for solving direct and inverse problems are analyzed. Experimental methods for improving the electrochemical shaping accuracy are considered.Translated from Elektrokhimiya, Vol. 40, No. 12, 2004, pp. 1438–1480.Original Russian Text Copyright © 2004 by Davydov, Volgin, Lyubimov. 相似文献
15.
本采用压缩X因子导数光谱技术实现了宽峰体系灵敏度的大幅度提高,提出了测定痕量锗的方法。在0.72mol/LH2SO4和3.0mol/LH3PO4的混酸介质中,锗-水杨基荧光酮-OP三元显色体系的压缩X因子四阶导数光谱摩尔响应系数达1.89×10^6L.mol^-1.cm^-1,灵敏度比常规光度法高12.4倍;最低检测出限为0.00033mg/L,比常规光谱法低4倍;选择性也进一步提高,绝大多数离 相似文献
16.
Single phase of ammonium tetramolybdate in the micro power form was prepared from polyphase ammonium paramolybdate. Its heat capacity from 14.25℃ to 120.12 ℃ was measured by drop method and the result is
Cp=0.3936+7.4047×10-4T+6.3543×10-3T-2(J•K-1•g-1) 相似文献
Cp=0.3936+7.4047×10-4T+6.3543×10-3T-2(J•K-1•g-1) 相似文献
17.
Detection of ethanol in human body fluids by headspace solid-phase micro extraction (SPME)/capillary gas chromatography 总被引:1,自引:0,他引:1
Summary Ethanol has been found extractable from human whole blood and urine samples by headspace solid-phase micro extraction (SPME) with a Carbowax/divinylbenzene-coated fiber. After heating a vial containing the body fluid sample with ethanol, and isobutanol as internal standard (IS) at 70°C in the presence of (NH4)2SO4, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial to allow adsorption of the compounds. The fiber needle was then injected into a middle-bore capillary gas chromatography (GC) port. The headspace SPME-GC gave intense peaks for both compounds; a small amount of background noises appeared, but did not interfere with the detection of the compounds. Recoveries of ethanol and IS were 0.049 and 0.026% for whole blood, respectively, and 0.054 and 0.085% for urine, respectively. The calibration curves for ethanol showed excellent linearity in the range of 80–5000 mg L–1 for whole blood and 40–5000 mg L–1 for urine; the detection limits for both samples were 20 and 10 mg L–1, respectively. The data on actual determination of ethanol after the drinking of beer are also presented for two subjects. 相似文献
18.
19.
以高校基础化学实验"从海带中提取碘""三草酸合铁(Ⅲ)酸钾的制备"为例,分别探讨了微视频技术在化学基本操作实验和综合设计型实验中的具体应用;此外,举例说明利用Flash软件制作的虚拟微视频可以在仪器分析实验中清晰地再现仪器真实操作中的每一个步骤,弥补了学生在实验前无法实际操作仪器的不足。实践证明,微视频技术的应用,丰富了基础化学实验教学模式,增强了学生自主学习的能力和动手能力,提高了实验成功率和实验教学效果。 相似文献
20.
Massoud SS Corfù NA Griesser R Sigel H 《Chemistry (Weinheim an der Bergstrasse, Germany)》2004,10(20):5129-5137
The first acidity constant of fully protonated xanthosine 5'-monophosphate, that is, of H3(XMP)+, was estimated by means of a micro acidity constant scheme and the following three deprotonations of the H2(XMP)+/- (pKa=0.97), H(XMP)- (5.30), and XMP2- (6.45) species were determined by potentiometric pH titrations; further deprotonation of (XMP-H)3- is possible only with pKa>12. The most important results are that the xanthine residue is deprotonated before the P(O)2(OH)- group loses its final proton; that is, twofold negatively charged XMP carries one negative charge in the pyrimidine ring and one at the phosphate group. Micro acidity constant evaluations reveal that this latter mentioned species occurs with a formation degree of 88 %, whereas its tautomer with a neutral xanthine moiety and a PO3(2-) group is formed only to 12 %; this distinguishes XMP from its related nucleoside 5'-monophosphates, like guanosine 5'-monophosphate. At the physiological pH of about 7.5 mainly (XMP-H)3- exists. The question, which of the purine sites, (N1)H or (N3)H, is deprotonated in this species cannot be answered unequivocally, though it appears that the (N3)H site is more acidic. By application of several methylated xanthine species intrinsic micro acidity constants are calculated and it is shown that, for example, for 7-methylxanthine the N1-deprotonated tautomer occurs with a formation degree of about 5 %; a small but significant amount that, as is discussed, may possibly be enhanced by metal ion coordination to N7, which is known to occur preferably to this site. 相似文献