全文获取类型
收费全文 | 2691篇 |
免费 | 166篇 |
国内免费 | 268篇 |
专业分类
化学 | 2655篇 |
晶体学 | 48篇 |
力学 | 11篇 |
综合类 | 25篇 |
数学 | 53篇 |
物理学 | 333篇 |
出版年
2024年 | 2篇 |
2023年 | 25篇 |
2022年 | 71篇 |
2021年 | 110篇 |
2020年 | 88篇 |
2019年 | 111篇 |
2018年 | 58篇 |
2017年 | 80篇 |
2016年 | 103篇 |
2015年 | 114篇 |
2014年 | 87篇 |
2013年 | 237篇 |
2012年 | 259篇 |
2011年 | 136篇 |
2010年 | 122篇 |
2009年 | 145篇 |
2008年 | 142篇 |
2007年 | 177篇 |
2006年 | 134篇 |
2005年 | 135篇 |
2004年 | 128篇 |
2003年 | 82篇 |
2002年 | 85篇 |
2001年 | 69篇 |
2000年 | 63篇 |
1999年 | 50篇 |
1998年 | 56篇 |
1997年 | 46篇 |
1996年 | 37篇 |
1995年 | 29篇 |
1994年 | 28篇 |
1993年 | 17篇 |
1992年 | 15篇 |
1991年 | 21篇 |
1990年 | 12篇 |
1989年 | 7篇 |
1988年 | 9篇 |
1987年 | 10篇 |
1986年 | 5篇 |
1985年 | 2篇 |
1984年 | 3篇 |
1983年 | 5篇 |
1982年 | 3篇 |
1981年 | 4篇 |
1979年 | 3篇 |
排序方式: 共有3125条查询结果,搜索用时 25 毫秒
81.
镍(Ⅱ)—p—MPAQ络合物极谱吸附波研究 总被引:1,自引:0,他引:1
5-[(对-甲基苯基)偶氮]-8-氨基喹啉(p-MPAQ)的合成及其在光度和荧光分析中的应用已有报道,但对其电化学性质未作研究,本文研究了p-MPAQ的极谱行为,在pH6.8的醋酸铵缓冲溶液中,p-MPAQ在-0.55 V呈现一示波极谱波(P_1),当有Ni~(2+)存在时,在-0.93V处出现一新峰(P_2),加0.0011%Triton X-100后,P_2波高明显增加实验证实该波为络合物 相似文献
82.
微量元素对胎儿发育影响的临床研究 总被引:6,自引:0,他引:6
为了解小于胎龄儿的血锌、铜、铅的变化 ,对 3 8例小于胎龄儿 (其中 1 2例有先天缺陷 )进行了血锌、铜、铅三种微量元素检测 ,并与 3 1例健康足月适于胎龄儿比较。结果表明 ,3 8例小于胎龄儿血锌、铜、铅结果分别为 49 4± 1 9 88μmol/L、 1 0 7± 3 3 μmol/L、 1 5± 0 83 μmol/L ;与正常对照组 (分别为 62 3 9± 1 5 2 9μmol/L、 1 1 0 2± 1 73 μmol/L、 0 82± 0 3 9μmol/L)比较 ,血锌明显低于正常组 ,t=-2 88,P <0 0 1 ;血铅明显高于对照组 ,t =4 6,P <0 0 1 ,有显著性差异。两组血铜无明显差异。小于胎龄儿血锌降低 ,血铅增高 ,而且其先天性缺陷者占3 5 .5 8% ,证明胎儿的低锌高铅状态对其生长发育有重要影响。 相似文献
83.
Single nucleotide polymorphisms (SNPs) are currently being mapped and databased at a remarkable pace, providing a viable means for understanding disease susceptibility, differential drug response and human evolution. Consequently, there is an increasing demand for SNP genotyping technologies that are simple, rapid, cost effective and readily amenable to automation for high-throughput analyses. In this study, we improved the Survivor Assay, a SNP detection method based on electrospray ionization mass spectrometry (ESI-MS), with several developments. One improvement is the development of a one-well assay, requiring no off-line purification of the polymerase chain reaction product, achieved by simple addition of reagent solution into a single well. Another is the on-line separation of magnesium and dideoxynucleotides using an in-house made monolithic metal chelating column, eliminating any off-line sample preparation prior to mass spectrometric analysis. Here the Survivor Assay is extended from a proof-of-principle concept to a validated method by genotyping six SNPs from five different regions of human genomic DNA in 55 individual samples with 100% accuracy. This improved Survivor Assay eliminates the tedious and time-consuming steps of sample preparation, minimizes sample handing and offers a high-throughput analysis of SNPs by ESI-MS. The current combined preparation and analysis time is 2 min per sample. The simplicity of this method has potential for full automation and parallel chromatography and, thus, reduced analysis time. In addition, we have adapted the Survivor Assay for quantitative SNP analysis in pooled DNA samples. The capabilities and sensitivity of this approach were evaluated. We demonstrate that an allele occurring at a frequency of 2% can consistently be quantitated. 相似文献
84.
头发铅含量测定的应用价值评价 总被引:1,自引:4,他引:1
调查了125例2-5岁儿童铅中毒状况,测定其全血铅含量和头发铅含量,以全血铅含量为标准,应用诊断试验评价方法评价头发铅测定的应用价值。结果表明,该试验的灵敏度可达88.3%,应用串联试验,即同时测定头发中锌、铁、钙含量,可将该试验的特异度提高至81.8%,阳性预测值达69.6%,阴性预测值达78.8%。 相似文献
85.
Synthesis and Structure of the First Ternary Lead(II) Copper(I) Oxide: PbCu2O2 PbCu2O2 can be prepared by solid state reaction or by precipitation from a basic aqueous solution. Single crystals of the new compound were prepared by recrystallisation from a molten mixture (PbO? Cu2O) and investigated by X-ray diffractometer technique. PbCu2O2 crystallizes isotypically with the homologue silver compound PbAg2O2 (monoclinic with a = 8.223 Å, b = 8.289 Å, c = 6.015 Å, β = 132.62°, Z = 4, space group C? C 1 2/c 1). The crystallographic data from the X-ray investigation are reported. The structure is built by endless [PbO4/4]- and [CuO2/4]-chains. Pb2+ has a one-sided asymmetric coordination with four next oxygen neighbours and Cu+ forms a stretched dumbbell with two oxygen atoms. 相似文献
86.
Wen HW Borejsza-Wysocki W DeCory TR Durst RA 《Analytical and bioanalytical chemistry》2005,382(5):1217-1226
A competitive lateral flow assay for detecting the major peanut allergen, Ara h1, has been developed. The detector reagents are Ara h1-tagged liposomes, and the capture reagents are anti-Ara h1 polyclonal antibodies. Two types of rabbit polyclonal antibodies were raised either against the entire Ara h1 molecules (anti-Ara h1 Ab) or against an immunodominant epitope on Ara h1 (anti-peptide Ab). All of them reacted specifically with Ara h1 in Western Blot against crude peanut proteins. Moreover, the anti-Ara h1 Ab was chosen for this assay development because of its highest immunoactivity to Ara h1-tagged liposomes in the lateral flow assay. The calculated limit of detection (LOD) of this assay is 0.45 g mL–1 of Ara h1 with a dynamic range between 0.1 and 10 g mL–1 of Ara h1 in buffer. Additionally, the visually determined detection range is from 1 to 10 g mL–1 of Ara h1 in buffer. Results using this assay can be obtained within 30 min without the need of sophisticated equipment or techniques; therefore, this lateral flow assay has the potential to be a cost-effective, fast, simple, and sensitive method for on-site screening of peanut allergens. 相似文献
87.
Rodová M. Brožek J. Knížek K. Nitsch K. 《Journal of Thermal Analysis and Calorimetry》2003,71(2):667-673
Phase transitions in ternary caesium lead bromide (CsPbBr3) were studied by means of DSC, TMA and high temperature X-ray diffraction. The samples were prepared from the solution by
water evaporation and from the melt. on the DSC curves as well as on the temperature dependence of the lattice constants of
CsPbBr3 only two effects were found belonging to the earlier published phase transitions at 88 and 130°C and no further effects.
Linear thermal expansion coefficient α of individual CsPbBr3 modifications were calculated from both TMA and high temperature X-ray diffraction. The structural parameters of the room
temperature orthorhombic phase were refined and the results are presented. CsPbBr3 prepared from the solution contained about 10% of CsPb2Br5 and so the DSC curve of pure CsPb2Br5 was also measured and an effect at a temperature of 68.5°C was found.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
88.
B. G. Bazarov R. F. Klevtsova A. E. Sarapulova K. N. Fedorov L. A. Glinskaya Zh. G. Bazarova 《Journal of Structural Chemistry》2005,46(4):756-760
Single crystals of triple molybdate of composition 5:1:3 K5Pb0.5Hf1.5(MoO4)6 have been grown and their crystal structure has been solved from X-ray diffraction data (an automated diffractometer X8 APEX, MoK α -radiation, 2173 F(hkl), R = 0.0321). Trigonal unit cell parameters are: a = b = 10.739(2) Å, c = 37.933(9) Å; V = 3789(1) Å3, Z = 6, ρcalc = 4.014 g/cm3, space group \(R\bar 3\). Three-dimensional mixed framework of the structure is formed by two types of MoO4 tetrahedra and Pb and Hf octahedra linking via common O-vertices. Potassium atoms of three types occupy large vacancies in the framework. 相似文献
89.
Drochioiu G 《Talanta》2002,56(6):1163-1165
A very simple, accurate, fast, selective and sensitive assay of cyanide based on its reaction with 2,2-dihydroxy-l,3-indanedione at basic pH is proposed. As little as 0.01 μg ml−1 of cyanide can be determined. The molar absorptivity may reach 5.1–8.0×104 l mol−1 cm−1 depending on the reaction conditions. Thus, 1 ml of sample solution is mixed with 500 μl of 5 mg ml−1 solution of 2,2-dihydroxy-1,3-indanedione monohydrate in 2% sodium carbonate. The absorbance of the purple color is measured at 510 nm in 1-cm glass cuvettes, 10–15 min after mixing the reagents. The procedure could also be used to identify free CN− in natural waters and hydrocyanic acid in the environment. 相似文献
90.
Gino Morisi Marina Patriarca Ferdinando Chiodo Anna Minoprio Antonio Menditto 《Mikrochimica acta》1996,123(1-4):281-290
Between 1992 and 1994, a new screening campaign for blood Pb monitoring in the Italian general population was carried out. Since the first campaign (started in 1978, in accomplishment of the European Community Directive 77/312/EEC) a working group of the Laboratory of Clinical Biochemistry at the Italian National Institute of Health (Istituto Superiore di Sanità), as the Reference Centre (RC), has coordinated the activity of various laboratories spread over the national territory. Appropriate quality assurance procedures, including an external quality assessment scheme (EQAS), were elaborated. Within the EQAS, three or four trials were carried out every year. Each laboratory participating in the trial analyzed eight control samples prepared from cow blood at different Pb concentrations. The results obtained by each peripheral laboratory and the RC between 1992 and 1994 have been compared by regression analysis. The same statistical method was adopted to compare the results obtained by each peripheral laboratory and the RC in the duplicate analysis of about 10 per cent of the human samples collected during the 1992–1994 monitoring campaign. There was no evidence of systematic differences between the regression lines obtained on control and human samples. In spite of the lower Pb concentration in the control samples analyzed during the 1992–1994 campaign, the analytical performance of the laboratories was better than that obtained in the previous screening campaign (1985–1986). Blood Pb levels observed in human samples collected between 1992 and 1994, confirm the downward time trend observed in the campaigns carried out in 1978–1979, 1980–1981 and 1985–1986. This study confirms that the results obtained in an EQAS are representative of the actual performance in the analysis of real (human) samples. 相似文献