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961.
Summary A method for the gas chromatographic trace analysis of underivatized nitrophenols in ground-water is presented. Using a highly
de-activated separation system a satisfactory precision for their quantitative GC analysis could be achieved by avoiding condensation
of the solvent and by fast injection of the sample. The reproducibility of the peak areas of eleven nitrophenols in ethylacetate
was <5 % RSD. Using a nitrogen-phosphorus detector detection limits were in a range from 10 to 30 pg. Within the concentration
range from 0.1 to 10 ng μl−1 the calibrations were linear with correlation coefficients >0.992.
The approach described was applied to the analysis of nitrophenols in ground-water near a former ammunition plant, after preconcentration
by continuous liquid/liquid extraction with ethylacetate. Using a GC-MS technique and retention times various nitrophenols
were identified and then quantified in the μg/L-range by applying NPD. 相似文献
962.
高效液相色谱法测定细胞分裂素的方法研究 总被引:4,自引:0,他引:4
利用高效液相色谱法测定水稻愈伤组织和微生物发酵产品中的玉米素,二氢玉米素,核糖基玉米素和核糖基二氢玉米素。样品用抽提液抽提,经Bio-Rex70弱阳离子交换柱和XAD-7/Sep-pakC18复合柱净化和富集后,直接用HPLC分析,方法回收率达94%~84%,相对标准偏差小于3.3%。最低检测限达2.0ng。 相似文献
963.
SynthesisandCharacterizationofChiralLiquidCrystalCMPPCDPTIANYan-qing,ZHAOYing-ying,SUFeng-yuandTANGXin-yi(DepartmentofChemist... 相似文献
964.
Simultaneous isolation and determination of esculin and rutin in natural materials using SPE and HPLC 总被引:1,自引:0,他引:1
Summary Esculin (ESC) and rutin (RUT) have been simultaneously isolated from pharmaceutical natural materials by solid phase extraction (SPE). Determination of both substances was performed by reversed phase high performance liquid chromatography (RPHPLC) with UV detection. Optimization of the separation conditions showed that simultaneous isolation and determination of rutin and esculin from pharmaceutical material was possible. The recovery obtained was not lower than 95±2%. 相似文献
965.
We describe the topology, structure, and stability of giant fullerenes exhibiting various symmetries (I, I
h
, D
2h
, T). Our results demonstrate that it is possible to create two new families of nested chiral icosahedral (I) fullerenes namely C260@C560@C980@C1520@, ...,and C140@C380@C740@C1220@ ..., which exhibit interlayer separations of ca. 3.4 Å. These chiral fullerenes are thought to possess metalliclike conduction properties. We discuss in detail the transformation of polyhedral graphitic particles into quasispherical nested giant fullerenes by reorganization of carbon atoms, which result in the formation of additional pentagonal and heptagonal carbon rings. These spherical structures are metastable and we believe they could be formed under extreme conditions, such as those produced by high-energy electron irradiation. There is circumstantial experimental evidence for the presence of heptagonal rings within these spherical fullerenes. 相似文献
966.
The monodisperse, porous poly(chloromethylstyrene-co-divinylbenzene) beads of 7.9 microm were prepared by a single-step swelling and polymerization method. The seed particles prepared by dispersion polymerization exhibited good absorption of the monomer phase. Based on this media, a weak cation-exchange (WCX) stationary phase for HPLC was synthesized by a new chemically modified method. The prepared resin has advantages of biopolymer separation, high column efficiency, low column backpressure, high protein mass recovery, and good resolution for proteins. The dynamic protein-loading capacity of the synthesized WCX packings was 18.2 mg/g. Five proteins were separated in 3.0 min using the synthesized WCX stationary phase. The experimental results show that the obtained WCX resin has very weak hydrophobicity. The WCX resin was also used for the rapid separation and purification of lysozyme from egg white in 5.0 min with only one step. The purity and specific bioactivity of the purified lysozyme were found to be more than 93% and 70 245 U/mg, respectively. 相似文献
967.
用角分布X射线光电子能谱(XPS)测试和样品原位加热相结合的方法研究了阴离子是对甲苯磺酸根的电生导电聚吡咯的化学和聚集态结构.其结果表明聚吡咯表面约几个原子层内原子的相对浓度依下述次序递减:C>O>S>N;导电聚吡咯中的氮原子至少有吡咯氮和氧化态氮两种;在200℃加热以后聚合物链不受影响,但阴离子向表面迁移,同时氧化态氮大大减少. 相似文献
968.
以大孔微硅胶作基体,经γ-氨丙基三乙氧基硅烷活化与间隔臂氯代环内烷反应后,再与预先合成的四(对羟基苯基)卟啉配体键合,构成电荷转移型亲和色谱固定相。以PH=7.0的磷酸盐缓冲溶液作流动相,成功实现对一些核苷酸的高效液相亲和色谱分离。 相似文献
969.
The precision of isotopic measurements of Pb by thermal ionization mass spectrometry (TIMS) is limited by the fact that this element does not possess an invariant isotope ratio that can be used for the correction of mass fractionation by internal normalization. Multiple-collector inductively coupled plasma mass spectrometry (MC-ICPMS) can overcome this limitation, because with plasma ionization, elements with overlapping mass ranges are thought to display identical mass discrimination. With respect to Pb, this can be exploited by the addition of Tl to the sample solutions; the mass discrimination factor obtained for Tl can then be used for the correction of the measured Pb isotope ratios. In this article we present the results of a detailed study that investigates the accuracy and precision of such an external correction technique for mass discrimination based upon the results of multiple analyses of a mixed standard solution of NIST SRM-981 Pb and SRM-997 Tl. Our data indicate that normalization of the Pb isotope ratios to the certified isotopic composition of SRM-997 Tl produces Pb isotopic results that are significantly lower than recently published reference values by TIMS. This systematic offset can be eliminated by renormalization of the Pb data to a different Tl isotopic composition to obtain an empirically determined mass discrimination factor for Pb that generates accurate results. It is furthermore shown that a linear law is least suited for the correction of mass discrimination, whereas a power or exponential law function provide significantly more accurate and precise results. In detail, it appears that a power law may provide the most appropriate correction procedure, because the corrected Pb isotope ratios display less residual correlations with mass discrimination compared to the exponentially corrected data. Using an exponential or power law correction our results, obtained over a period of over seven months, display a precision (2σ) of better than 60 parts per million (ppm) for 208Pb/206Pb and 207Pb/206Pb and of better than 350 ppm for 206Pb/204Pb, 207Pb/204Pb/204Pb, and 208Pb/204Pb. This represents a significant improvement compared to conventional TIMS techniques and demonstrates the potential of MC-ICPMS for routine, high-precision measurements of Pb isotopic compositions. 相似文献
970.