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951.
H. A. Khan 《Chromatographia》2006,64(7-8):423-427
Biogenic polyamines are sensitive markers for various diseases including cancer. Polyamines are difficult to analyze by chromatography due to their high polarity and water-solubility so that derivatization is an essential step for their chromatographic analysis. Earlier studies have shown the efficacy of calcium sulfate (CaSO4) as a TLC coating material for the separation of polar compounds. The aim of this study was to explore the potential of CaSO4 for the analysis of aliphatic polyamines without derivatization. The TLC of six polyamines (ornithine, citrulline, putrescine, cadaverine, spermidine and spermine) was carried out on CaSO4 and silica gel plates using 11 different mobile phases. The results showed that CaSO4 is superior to silica for the separation of underivatized polyamines. The development time of the CaSO4 plates was also about one-third shorter as compared to silica. Methanol was the only solvent to produce differential R
F
values for the polyamines studied. Ornithine (R
F
, 0–2) and citrulline (R
F
, 1–3) were separated from cadaverine (R
F
, 0.93), spermine (R
F
, 0.85) and spermidine (R
F
, 0.85). For quantitative analysis, the polyamines were eluted from the coating material scratched from the plate and the absorbance of the supernatant was measured at 550 nm. The limits of detection (LOD) and quantification (LOQ) were found to be 0.75 and 1.88 μg, respectively. The procedure was applied to the quantitative separation of polyamines in spiked human urine samples (12.5–50 μg). This is probably the first study reporting a TLC method for the separation of underivatized polyamines. 相似文献
952.
We report a novel separation method that is applicable to both DNA and protein samples, based on electrophoresis in a three-dimensional (3-D) geometry. In contrast to conventional electrophoresis, samples are applied in a two-dimensional, planar array to one of the surfaces of a 3-D geometry separation medium. Loading onto a plane results in a very high sample capacity. Sample migration and separation occur along the third spatial dimension, which is perpendicular to the loading plane. The key problem of electrophoresis in a 3-D geometry separation setup is that temperature gradients are caused by Joule's heat, affecting the electrical conductivity and viscosity of the separation medium. A means of achieving straight sample migration under these circumstances is to force heat flow through the separation medium parallel to the axis of sample migration. This can be done by dissipating the heat via the electrode sides of the gel and blocking any other heat transfer. The separation of DNA and proteins by this method has been tested using agarose gel electrophoresis, polyacrylamide gel electrophoresis, and sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Data were acquired off-line by conventional staining methods as well as on-line by detection of laser-induced fluorescence. We describe how to excise samples from the separation medium for preparative purposes. Possible unique applications of this 3-D geometry electrophoresis separation method are also discussed. 相似文献
953.
等色染料离子对—溴酚蓝.亚甲蓝体系萃取光度法测定镍 总被引:1,自引:0,他引:1
研究了利用溴酚蓝与亚甲蓝所形成的等色染料离子对萃取测定镍的方法。用酸将l,2-二氯乙烷中的Ni(phen)_3·BPB解析后,并加入与溴酚蓝颜色相近的亚甲蓝。利用1,2-二氯乙烷中溴酚蓝·亚甲蓝的染料离子对协同增敏效应提高了测定镍的灵敏度,其摩尔吸光系数ε=1.58×10~5。镍量在4×10~(-7)~2×10~(-5)mol·L~(-1)的范围服从比耳定律。方法用于测定标样ZDL—109中镍的含量,相对标准偏差为3.5%。 相似文献
954.
结晶水对硫酸铜与丁腈橡胶之间配位交联反应的影响 总被引:2,自引:0,他引:2
利用动态力学分析(DMA)、差示扫描量热分析(DSC)、扫描电子显微镜(SEM)、平衡溶胀法、力学性能测试等分析手段, 通过研究五水硫酸铜(CuSO4·5H2O)填充的NBR考察了结晶水对CuSO4与NBR之间配位交联反应的影响. 结果表明, 结晶水的存在可以促进该配位交联反应. 相似文献
955.
本文利用溶液的稀释度与其吸光度的关系,导出一个适用于不稳定络合物稳定常数的测定方法。当络合物的摩尔吸光系数(ε)不能直接测定时,本法可直接求算它的稳定常数及摩尔吸光系数。本文还讨论了方法误差与络合物离解度以及溶液稀释度的关系。 相似文献
956.
Martin Bröring Prof. Dr. Stephan Link Meike Cordes Carsten D. Brandt 《无机化学与普通化学杂志》2007,633(2):211-218
A new hydrogen terminated 2,2′‐bidipyrrin ligand was prepared from a bipyrrole dialdehyde and 3,4‐diethylpyrrole by a POCl3 induced condensation and isolated as the nickel(II) chelate. Unexpectedly a side reaction occured when base‐deficient and aerobic conditions were chosen in the metalation step. This side reaction led to a novel pentapyrrolic nickel(II) complex with one externally bound pyrrole ring. Further studies showed that the reactions of 2,2′‐bidipyrrins with 3,4‐diethyl‐ or 2,3,4‐trimethylpyrrole and an oxidant resulted in a stepwise exchange of the terminal pyrrole moieties and, in the former case, the introduction of one additional pyrrole ring into one of the two meso positions of the open‐chain tetrapyrrole. 相似文献
957.
用2-(5-硝基-2-吡啶偶氮)-5-二乙氨基苯酚反相高效液相色谱测定痕量铁、钴、镍 总被引:1,自引:0,他引:1
本文采用新试剂2-(5-硝基-2-吡啶偶氮)-5-二乙氨基苯酚(5-NO_2-PADAP)为柱前衍生试剂,不需对离子试剂,用含40mmol/L 的 pH6.0的乙酸-乙酸钠缓冲溶液和10~(-4)mol/LEDTANa_2的甲醇-水溶液(67.5:32.5)为流动相,在 ODS 柱上,20min 内 HPLC 测定了 Fe(Ⅲ)、CO(Ⅱ)和 Ni(Ⅱ)的5-NO_2-PADAP 的络合物,这是同类衍生试剂中最简单流动相体系。当信噪比 SNR=2时,检出限分别为0.17、0.17和0.09ng/ml。是同类体系中灵敏度最高的。方法用于同时测定硝酸试剂和茶叶中的铁、钴和镍,结果良好。 相似文献
958.
Donald F. Cook Neil F. Curtis Clifton E.F. Rickard Joyce M. Waters 《Polyhedron》2005,24(18):3022-3031
The imine functions of [Ni(mL1)](ClO4)2 (mL1 = meso-7RS,14SR-5,12-dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene) are reduced by using NaBH4 in acetonitrile/methanol to form the meso–meso and rac–meso isomeric cyclic tetramine complex cations [Ni(mmL2)]2+ and [Ni(rmL2)]2+ (mml2 = 5RS,7RS,12SR,14SR- and rmL2 = 5SR,7RS,12SR,14SR-5,12-dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradecane) in ca. 8:1 proportions. [Ni(rmL2)]2+ is also prepared from rmL2, formed in <1% yield by the reduction of mL1 by NaBH4 in ethanol. Square planar singlet ground state (S = 1) salts [Ni(rmL2)](ClO4)2 and [Ni(rmL2)][ZnCl4] and triplet ground state (S = 3) trans-di-ligand octahedral compounds trans-[Ni(rmL2)X2] ,μ-Y-trans-[Ni(rmL2)Y] and folded macrocycle compounds cis-[Ni(rmL2)(acac)]CIO4 (acac− = pentane-2,4-dionato), cis-[{Ni(rmL2)}2(C2O4)](ClO4)2, cis-[Ni(rmL2)(H2O)2](ClO4)2 and cis-[Ni(rmL2)X2], X− = Cl−, Br−, are described. The S = 1 salt 1SR,4SR,5SR,7RS,8RS,11RS,12SR,14SR-[Ni(rmL2)](ClO4)2 · 0.5H2O has a disordered structure with Ni(II) in square planar coordination by the nitrogen atoms of the macrocycle, in N-configuration III, with Ni–Nmean = 1.96(2) Å. The six-membered chelate rings both have chair conformations, with the phenyl substituents equatorially oriented and with the methyl substituents disordered over axial and equatorial orientations. The S = 3 compound cis-1SR,4SR,5SR,7RS,8SR,11SR,12SR,14SR-[Ni(rmL2)(acac)]ClO4 has N-configuration V. The macrocycle is folded along N1–Ni–N8, adjacent to the phenyl substituents {N1–Ni–N8 = 176.45(6), N4–Ni–N11 = 98.16(6)°}, with mean Ni–N = 2.09(2) Å and mean Ni–O = 2.121(5) Å. Both six-membered chelate rings have chair conformations with the methyl substituents equatorially oriented, while one has the phenyl substituent equatorially and the other has it axially oriented. The structures of the isomeric [M(rmL2)(acac)]ClO4, [M(rrL2)(acac)]CIO4 and [M(mmL2)(acac)]ClO4 compounds are compared. 相似文献
959.
960.
聚乙二醇-硫酸铵-亚硝基R盐体系中钴(Ⅱ)的分离及其存在形态 总被引:2,自引:0,他引:2
在 pH 4.0~6.0的 HAc-NaAc缓冲溶液中,Co(Ⅱ)、Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)等金属离子与亚硝基R盐可形成稳定络合物。加入HCI适当提高溶液酸度(HCI浓度在0.3~0.6mol/L),用聚乙二醇2000(PEG)-硫酸铵-亚硝基R盐体系萃取,Co(Ⅱ)可被PEG相几乎完全萃取,而Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)基本上不被萃取。实现了Co(Ⅱ)、Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)混合离子合成样品和硅酸盐岩矿实际样品中Co(Ⅱ)的分离与测定。同时吸收光谱、摩尔比、连续浓度变换、加入表面活性剂等实验表明,在萃取相Co(Ⅱ)与亚硝基R盐是1:3络阴离子形式存在的。 相似文献