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121.
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
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124.
Vora A. Riga A. Dollimore D Alexander K. 《Journal of Thermal Analysis and Calorimetry》2004,75(3):709-717
This study attempts to identify the degradative process which folic acid undergoes in the solid-state under thermal stress.
In order to facilitate the process, the various pieces of the chemical structure, namely, p-amino benzoic acid, pterin and glutamic acid as both its d- and l-isomers were investigated as separate entities. These structured solid-state pieces were then compared to the composite solid
state folic acid degradative curves in order to identify the peaks seen and provide direction for the interpolation of the
degradative mechanism. It was observed that none of the structural pieces could be superimposed as assumed earlier and hence
an attempt was made to identify the decomposition products using various analytical techniques such as infrared spectroscopy,
mass spectroscopy and X-ray diffraction which suggested that the glutamic acid fragment is lost first as evidenced by acid
loss and amide enhancement in the IR spectra. The vitamin was ultimately degrading to carbon fragments and that further identification
was not necessary.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
125.
河口水体中痕量稀土元素的共沉淀预富集-电感耦合等离子体质谱法测定研究 总被引:3,自引:0,他引:3
建立了氢氧化铟共沉淀预富集 -电感耦合等离子体质谱法测定河口水体中痕量稀土元素的方法。实验结果表明 ,在80mg·L -1的In3 +和pH9.5的实验条件下 ,在1.0L水样中添加5.0~200.0ng的混合稀土标准溶液 ,均能定量回收 ,回收率在82.2 %~106.9 %之间。方法的分析流程空白为0.04(Tb)~10.17(La)ng·L -1,检出限在0.17(Yb)~1.46(La)ng·L-1之间 ,精密度 (RSD ,n=3)小于11.7 % ,可满足河口淡水和海水样品中的痕量稀土元素定量分析的要求 相似文献
126.
127.
毛细管电泳-质谱联用法测定性保健品中的脱水吗啡和西地那非 总被引:10,自引:0,他引:10
脱水吗啡和西地那非是目前治疗男性性功能障碍的常用药物,在临床上已广泛应用。但最近的研究表明,当服用西地那非剂量较大时会引起头痛、消化不良、头晕、皮疹等不良反应。更为严重的是,西地那非能增强硝酸酯类药物的降压能力,与硝酸酯类药物同时使用时,可能会引起致命性低血压 相似文献
128.
LC-MS/MS method for the confirmatory determination of aromatic amines and its application in textile analysis 总被引:1,自引:0,他引:1
Sutthivaiyakit P Achatz S Lintelmann J Aungpradit T Chanwirat R Chumanee S Kettrup A 《Analytical and bioanalytical chemistry》2005,381(1):268-276
A confirmation method for the determination of 18 aromatic amines originating from azo dyes after reductive cleavage was developed. The method is based on the use of high-performance liquid chromatography/tandem mass spectrometry with atmospheric-pressure chemical ionization. For the identification of the analytes one precursor ion and two daughter ions (multi-reaction monitoring, MRM) were selected and the LC-MS/MS parameters optimized to obtain high sensitivity and selectivity. The linear ranges varied from 0.1–1 to 30–50 g mL–1 with correlation coefficients of 0.99 or better. The applicability of the method to determine o-tolidine (3,3-dimethylbenzidine) and 3,3-dimethoxybenzidine in textiles following reductive cleavage of acid red 114, trypan blue, and Chicago sky blue 6B was demonstrated. 相似文献
129.
建立了离子色谱-质谱联用技术测定活性污泥样品中高氯酸盐的分析方法。以高容量、强亲水性的IonPacAS20(2mm)阴离子交换柱为分析柱,EGC在线产生等浓度KOH为淋洗液,淋洗液经抑制成水后将样品带入质谱检测。ESI-MS-MS以多元反应监测模式监控100.8/84.9、98.8/66.9、100.8/68.9和98.8/82.9离子对,以98.8/82.9离子对的峰面积进行定量。该方法对高氯酸盐的检出限(S/N=3)为0.01μg/L,高氯酸盐在0.05~100μg/L浓度范围内具有良好的线性,线性相关系数r=0.9988。0.2μg/L的标准溶液重复进样9次,高氯酸盐峰面积的相对标准偏差(RSD)为2.3%。运用该方法测定采自不同地区的活性污泥样品中的高氯酸盐,并对样品加标回收,得回收率在88.5%~102.2%之间。 相似文献
130.
预富集电感耦合等离子体质谱法测定地下水中超痕量稀土元素及钪、钇 总被引:6,自引:0,他引:6
以P507萃淋树脂为固定相,HCl/EDTA为流动相,建立了地下水中超痕量稀土元素及钪、钇的ICP-MS测定的新方法。详细探讨了稀土元素(REEs)、Sc、Y与基体元素的分离、EDTA小体积洗脱的实验条件及ICP-MS工作参数。在pH2.6时上柱,大部分Ca、Mg,其体可不经淋洗而直接与REEs分离;以100mmol的EDTA洗脱,5mL淋洗体积REEs、Y、Sc回收率为96%-98.5%。详细考察了La、Ce、Pr的氧化物离子及氢氧化物离子的干扰及校正方法。分析方法的检测限为0.7-10.1ng/L,加标回收率为95%-99%。用于实际地下水及人工模拟水样的分析,结果令人满意。 相似文献