全文获取类型
收费全文 | 14344篇 |
免费 | 1583篇 |
国内免费 | 952篇 |
专业分类
化学 | 12249篇 |
晶体学 | 42篇 |
力学 | 699篇 |
综合类 | 55篇 |
数学 | 349篇 |
物理学 | 3485篇 |
出版年
2024年 | 6篇 |
2023年 | 211篇 |
2022年 | 351篇 |
2021年 | 352篇 |
2020年 | 550篇 |
2019年 | 535篇 |
2018年 | 491篇 |
2017年 | 634篇 |
2016年 | 708篇 |
2015年 | 724篇 |
2014年 | 715篇 |
2013年 | 993篇 |
2012年 | 1023篇 |
2011年 | 980篇 |
2010年 | 766篇 |
2009年 | 863篇 |
2008年 | 832篇 |
2007年 | 881篇 |
2006年 | 777篇 |
2005年 | 723篇 |
2004年 | 644篇 |
2003年 | 562篇 |
2002年 | 419篇 |
2001年 | 321篇 |
2000年 | 259篇 |
1999年 | 207篇 |
1998年 | 176篇 |
1997年 | 152篇 |
1996年 | 139篇 |
1995年 | 145篇 |
1994年 | 136篇 |
1993年 | 96篇 |
1992年 | 83篇 |
1991年 | 70篇 |
1990年 | 65篇 |
1989年 | 53篇 |
1988年 | 43篇 |
1987年 | 35篇 |
1986年 | 28篇 |
1985年 | 29篇 |
1984年 | 22篇 |
1983年 | 14篇 |
1982年 | 22篇 |
1981年 | 15篇 |
1980年 | 5篇 |
1979年 | 8篇 |
1978年 | 4篇 |
1976年 | 3篇 |
1973年 | 3篇 |
1959年 | 3篇 |
排序方式: 共有10000条查询结果,搜索用时 375 毫秒
81.
《印度化学会志》2023,100(1):100825
The improved thermal association of heat transfer is considerably observed due to interaction of nanoparticles in recent days. The lubrication phenomenon with heat and mass transfer effects plays a key role in the hydraulic systems. In current research, the thermal impact of nanofluid over a lubricated stretching surfaces near a stagnation point analytical has been studied. A thin layer of lubricating fluid with a variable thickness provides lubrication. The inspection of thermophoresis and Brownian motion phenomenon is illustrated via Boungrino model. The analytical finding of refurbished boundary layer ordinary differential equations is obtained by a reliable and proficient technique namely variational iteration method (VIM). The Lagrange Multiplier is a potent tool in proposed technique to reduce the computational work. In addition, a numerical comparison is presented to show the effectiveness of this study. The range of flow parameters is based on theoretical flow assumptions. Physical inspection of involved parameters on velocities, temperatures, concentrations, and other quantities of interest when lubrication is presented. The current results present applications in polymer process, manufacturing systems, heat transfer and hydraulic systems. 相似文献
82.
Thankan Jayasekharan 《Chemphyschem》2023,24(13):e202300036
Mercury fluoride ions formed during the laser ablation of HgF2( s ) show the formation of six different cluster ion series viz., HgFn±, HgnFn–2±, HgnFn–1±, (HgF)n±, HgnFn+1±, and HgnFn+2±. Among the different ion series, the observation of high valent HgFn±(n±=3,4; n−=6–8) indicates the existence of corresponding molecules which signify the remarkable participation of 5d Hg electrons in the chemical bonding with F atoms and thus make Hg a truly transition metal. Further, molecular orbital calculations show a large HOMO-LUMO energy gap (≥3 eV) and high electron affinity (≥5 eV) that indicates highly stable HgFn=3,4,6,8 with super halogen properties. 相似文献
83.
Deniss Fedorenko Antons Podjava Arvis Prikulis Vadims Bartkevics 《Journal of separation science》2023,46(11):2201002
A new method for quantitative analysis of several biomarkers and pharmaceutical compounds in wastewater has been developed employing nanoflow liquid chromatography with Orbitrap mass spectrometry. An easy dilute-and-shoot approach has been used for sample preparation with a dilution factor of 5. Improved retention of ionic and highly polar compounds has been achieved by the addition of tetrabutylammonium bromide as an ion pair reagent into the final diluted sample. The new nanoflow liquid chromatography method has demonstrated low matrix effects (70%–111%), high sensitivity in terms of limits of quantification (0.005 to 0.3 μg/L), low injection volume (70 nl) and solvent consumption, and the ability to analyze diverse polar and ionic analytes within one run using a single reversed-phase nanoflow liquid chromatography column. Wastewater samples (n = 116) from the wastewater treatment plants of different cities in Latvia were analyzed using the developed method. The observed concentrations of biomarkers were in line with the literature data. 相似文献
84.
Da-Hee Park Hee-Jung Cho Se-Hyeong Kang Hong-Hee Lee Jae-Yong Shin A. M. Abd El-Aty Ho-Chul Shin 《Journal of separation science》2023,46(20):2300377
A sensitive and accurate analytical method was developed and validated to detect bambermycin, a commonly used antibiotic in animal feed and livestock. The presence of bambermycin residues in food products can pose health risks to consumers, emphasizing the need for a sensitive and accurate analytical method. A reversed-phase analytical column was utilized with a mobile phase comprising 0.005 mol/L ammonium acetate in 5% acetonitrile (A) and 0.005 mol/L ammonium acetate in 95% acetonitrile (B) to achieve effective chromatographic separation. Quantitative determination of bambermycin in various samples, including beef, pork, chicken, milk, eggs, flatfish, eel, and shrimp, was performed using ultra-high-performance liquid chromatography-tandem mass spectrometry. Sample extraction involved a mixture of methanol and a 25% ammonium hydroxide solution, followed by low-temperature purification and phospholipid removal utilizing a Phree cartridge. The method exhibited a satisfactory recovery rate ranging from 69% to 100%. Validation results demonstrated the reliability, robustness, and accuracy of the method, exhibiting good linearity, precision, and recovery. This validated method can be applied for routine analysis of bambermycin residues, assisting in the development of effective monitoring and control measures to ensure the safety of livestock and aquatic products. 相似文献
85.
摘 要 为研究甘肃地区松针中无机元素的含量,探究不同品种松针中无机元素的差异,采用HNO3(65%)对松针样品进行微波消解,电感耦合等离子体质谱(ICP-MS)法测定甘肃两地区6种松针中28种无机元素的含量,结合主成分分析以及偏最小二乘判别分析对松针地区差异进行判别;结果显示松针中无机元素含量丰富,其中Na、Mg、Al、K、Ca、Fe、Zn、Mn、Sr等元素在不同品种松针中均有较高含量,主成分分析结果显示共有7个主成分,累积贡献率达到92.58%,偏最小二乘判别分析显示两地区6种松针在地区上可被明显分开,其中Mg、Fe、Zn、Mn、Sr、K 6种元素为造成地区差异的主要元素。实验结果表明松针中元素种类丰富,人体必需微量元素含量较高,且不同地区松针在地区上具有一定的一致性和特异性。 相似文献
86.
为了准确测定黄精中稀土元素的含量,采用电感耦合等离子体质谱(ICP-MS)法同时测定黄精中15种稀土元素(La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu)的含量,进而绘制稀土元素指纹图谱,以稀土元素含量的平均值构建黄精稀土元素标准指纹图谱,作为鉴定黄精中药材的参考依据。黄精样品采用微波消解法处理后,通过在线引入内标溶液,采用ICP-MS法测定15种稀土元素的含量,采用OriginPro 2021绘制稀土元素指纹图谱和进行主成分分析,采用SPSS 26.0进行聚类分析。15种稀土元素的线性关系、重复性、精密度良好,平均加标回收率在97.0%~103.3%,相对标准偏差小于等于1.74%。黄精中Ce、La、Nd含量相对较高,Ce含量为53.02~2004.58 μg/kg,位居第一。聚类分析和主成分分析结果表明,样品聚为2类,同一产地的样品能够较好地聚在一起。黄精药材中15种稀土元素的指纹图谱具有相似的分布形态,具有较强的特征性和一致性,相似度均大于0.950。该方法操作简单,准确可靠,能满足实验分析要求,可为黄精的质量控制和药理研究提供参考;建立的指纹图谱可用于黄精的鉴别。 相似文献
87.
通过电感耦合等离子体质谱法(ICP-MS)测定土壤中的碘。样品预处理采用艾斯卡试剂熔融、热水提取和阳离子树脂静态交换,试验加入了不同剂量的阳离子交换树脂在不同程度上降低了溶液中Na+ 和Zn2+等阳离子的盐效应干扰。研究了乙醇在ICP-MS中对碘元素的增强效应,用3%的氨水溶液清洗进样系统,有效减少的碘的记忆效应和清洗时间。该方法线性范围宽,方法灵敏度高,检出限低,试剂用量少,环境友好。对苏州及周边区域若干非污染土壤点位进行采样、制备和测试,碘平均含量为2.7μg.g-1;同步测试国家有证标准物质,精密度和准确度良好。 相似文献
88.
Wen Li Xu Xu Zhuoshi Tang Yina Guo Dongqing Fei Na Yan Fangdi Hu 《Journal of separation science》2023,46(8):2200835
Recently, we confirmed that the 95% ethanol-extracted fraction of Codonopsis Radix, which contains several triterpenoids and sterols, possesses pharmacological activities. However, due to the low content and diverse types of triterpenoids and sterols, their similar structures, lack of ultraviolet absorption, and difficulty in obtaining controls, few studies have so far assessed their contents in Codonopsis Radix. We accordingly constructed an ultra-high-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry technique for the simultaneous quantitative determination of 14 terpenoids and sterols. Separation was performed on the Waters Acquity UPLC HSS T3 C18 column (100 × 2.1 mm, 1.8 μm) with 0.1% formic acid (A) and 0.1% formic acid in methanol (B) as mobile phase under gradient elution. The determination coefficients for each of the matrix calibration curves were ≥0.9925. The average recovery ranged from 81.25% to 118.05%, with relative standard deviations of <4%. The contents of 14 components in 23 batches were quantified and further analyzed through chemometrics. Linear discriminant analysis can distinguish sample varieties. The quantitative analysis method can accurately determine the contents of 14 components and thereby provide the chemical basis for the quality control of Codonopsis Radix. It also could be a valuable approach for the classification of different Codonopsis Radix varieties. 相似文献
89.
Lei Lv Hang Su Shanbin Chen Jinxing He Yuhong Yang Yuan Liu Hanzhu Xing 《Journal of separation science》2023,46(11):2200910
3-Chloro-1,2-propanediol is a common food contaminant, but reports on its determination in biological tissues are lacking. In the present study, a method was developed to detect 3-chloro-1,2-propanediol contents in rat tissues by quick-easy-cheap-effective-rugged-and-safe extraction and gas chromatography-mass spectrometry analysis. Biological samples were extracted with ethyl acetate and purified with adsorbents. The optimized adsorbent for each sample was selected from 4–5 combinations of N-propylethylenediamine, octadecylsilane, graphitized carbon black, strong anion exchange, and florisil. Extracted 3-chloro-1,2-propanediol was derivatized with heptafluorobutyric anhydride and subjected to gas chromatography-mass spectrometry. This method had good linearity (correlation coefficients >0.99) in the range of 2–2000 ng/g for blood, kidney, liver, testis, and brain samples. The limits of detection were under 0.8 ng/g; the limits of quantification were 2 ng/g; the recovery rates were 85%–102%; and the matrix effects were 1.98%–7.67%. This method also had good precision. The dynamic changes in 3-chloro-1,2-propanediol in rats gavaged with 20 mg/kg b.w. for 24 h were detected using this method. The 3-chloro-1,2-propanediol content in each tissue sharply increased to a peak, rapidly decreased within 2 h, and stabilized at 12 h. 3-Chloro-1,2-propanediol persisted in the kidney, testis, and liver 24 h after gavage. 相似文献
90.
Ali Akbar Fathi Mohammad Reza Afshar Mogaddam Saeed Mohammad Sorouraddin Mir Ali Farajzadeh Ali Mohebbi 《Journal of separation science》2023,46(17):2201055
This research aims to synthesize a specific and efficient sorbent to use in the extraction of apixaban from human plasma samples and its determination by high-performance liquid chromatography-tandem mass spectrometry. High specific surface area of metal-organic framework, magnetic property of iron oxide nanoparticles, selectively of molecular imprinted polymer toward the analyte, and the combination of dispersive solid-phase extraction method with a sensitive analysis system provided an efficient analytical method. In this study, first, a molecularly imprinted polymer combined with magnetic metal organic framework nanocomposite was prepared and then characterized using different techniques. Then the sorbent particles were used for selective extraction of the analyte from plasma samples. The efficiency of the method was improved by optimizing effective parameters. According to the validation results, wide linear range (1.02–200 ng mL−1), acceptable coefficient of determination (0.9938), low limit of detection (0.32 ng mL−1) and limit of quantification (1.02 ng mL−1), high extraction recovery (78%), and good precision (relative standard deviations ≤ 2.9% for intra- (n = 6) and interday (n = 6) precisions) were obtainable using the proposed method. These outcomes showed the high potential of the proposed method for screening apixaban in the human plasma samples. 相似文献