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71.
含胆酸酯侧基梳状均聚物和共聚物的制备和特性研究 总被引:1,自引:0,他引:1
以盐酸为催化剂合成了胆酸酯(2a~2d);用甲基丙烯酸酐(MAA)做酰化剂,4-二甲氨基吡啶(DMAP)做催化剂,三乙胺(Et3N)做缚酸剂,对2a~2d分子中伯羟基选择酰化,合成了分子中含有一个乙烯基的胆酸衍生物(3a~3d);应用溶液聚合方法制备了3a~3d均聚物及3a~3d与N-异丙基丙烯酰胺(NIPAA)的共聚物,并研究了聚合物的性能.结果显示: pH值为3~4时,反应得到2a~2d的产率最高;MAA做酰化剂,2a~2d分子中的伯羟基优先发生酰化反应;以胆酸为侧基的线性高分子化合物的性质随着二醇碳原子数增加而呈规律性变化. 相似文献
72.
Radical addition of 2-benzoxypentafluoropropene [CF2C(CF3)OCOC6H5] (BPFP) with alcohols such as ethanol and 2-propanol was investigated to afford fluorinated alcohols. Radical addition of BPFP with cyclic ethers such as tetrahydrofuran, 1,3-dioxolane and tetrahydropyran was also achieved to afford addition products followed by hydrolysis to yield fluorinated alcohols possessing cyclic structures. Novel fluoroalkyl acrylates and methacrylates were synthesized from the fluorinated alcohols with (meth)acryloyl chlorides. Radical polymerization of the fluoroalkyl (meth)acrylates yielded polymers of 1.2 × 105 as the highest molecular weight. 相似文献
73.
The present study describes the application of capillary electromigration techniques; CEC and micellar EKC (MEKC), and the application of spectroscopic methods; 1H NMR and 1H NOESY spectroscopy to investigate interactions between CDs (alpha-CD, statistically methylated beta-CD, hydroxypropyl-beta-CD, and 2-hydroxypropyl-gamma-CD) and different methacrylates (adamantyl, isobornyl, cyclohexyl, and phenyl methacrylate). It is shown that these methods complement each other. While CD-mediated MEKC is a rapid screening technique for comparing complex stabilities in aqueous media, 1H NMR chemical shift analysis provides quantitative data for very strong methacrylate-CD complexes and CD-mediated CEC provides quantitative data for complexes with lower complex forming constants. CD-mediated MEKC did not prove to be suitable for the calculation of complex forming constants. Reasons are discussed. 1H NOESY spectra were used to study spatial relationships between host and guest atoms. 相似文献
74.
Konieczka P Sejerøe-Olsen B Linsinger TP Schimmel H 《Analytical and bioanalytical chemistry》2007,388(4):975-978
Extraction conditions for the determination of tributyltin (TBT) in sediment samples have been developed further. The analytical
procedure is based on spiking with isotopically labelled analyte, pressurised liquid extraction (PLE) with a hexane/tropolone
mixture, Grignard derivatization and quantification by GC–MS. It was applied to two unknown sediment samples as part of an
intercomparison exercise of the Comité Consultatif pour la Quantité de Matière (CCQM). The detection limit was approximately
1.5 ng/g TBT as Sn, while the repeatability and intermediate precision (as the coefficient of variation) were 1.9% and 3.2%,
respectively. The expanded uncertainty was 6.2% (coverage factor k = 2), and the accuracy was confirmed by measurement of a certified reference material. 相似文献
75.
76.
《Journal of separation science》2003,26(18):1623-1628
Four methacrylate ester‐based monolithic columns for capillary liquid chromatography (CLC) were prepared by radical polymerization with ammonium peroxodisulfate (3 columns) and by thermal initiation (1 column). The polymerization mixture consisted of butyl methacrylate (BMA) and ethylene glycol dimethacrylate (EDMA), propan‐1‐ol, butane‐1,4‐diol, water, and ammonium peroxodisulfate as initiator. It was necessary to add N,N,N′,N ′‐tetramethylethylenediamine (TEMED) to the polymerization mixture to activate the reaction. The amount of initiator and activator was optimized to attain quantitative polymerization. The reproducibility of three columns prepared at ambient temperature was studied. The most efficient column with HETP of 29 μm for uracil was compared to the monolithic column prepared by thermal initiation with α,α′‐azobisisobutyronitrile (AIBN). The efficiencies of all the test columns were characterized by van Deemter curves. Their total porosities were calculated from the retention time of uracil. Walters indices of hydrophobicity (HI) were calculated from the retention factors of anthracene and benzene. The columns prepared by both methods are comparable in their selectivities and efficiencies. They show the same characteristics because their total porosities and Walters indices of hydrophobicity are consistent. However, the preparation of monoliths using ammonium peroxodisulfate was less demanding, because polymerization was possible at ambient temperature. 相似文献
77.
光聚合法快速制备甲基丙烯酸酯类毛细管整体柱 总被引:1,自引:0,他引:1
采用甲基丙烯酸正丁酯(BMA)为功能单体, 乙二醇二甲基丙烯酸酯(EDMA)为交联剂, 正丙醇、1,4-丁二醇和水为致孔剂, Irgacure 1800为引发剂, 在毛细管内采用光引发原位聚合150 s快速制备了有机聚合物整体柱. 分别采用电色谱(CEC)、加压电色谱(p-CEC)和低压色谱(LPLC)模式对所制备的整体柱进行了性能评价, 基线分离了硫脲、甲苯、萘和联苯, 在加压电色谱(p-CEC)模式下硫脲的最低理论塔板高度达到了8.0 μm. 扫描电镜结果表明, 整体材料在毛细管柱中形成并与毛细管内壁结合紧密. 相似文献
78.
Zeki Altun Christina Skoglund Mohamed Abdel-Rehim 《Journal of chromatography. A》2010,1217(16):2581-2588
In the pharmaceutical industry the growing number of samples to be analyzed requires high throughput and fully automated analytical techniques. Commonly used sample-preparation methods are solid-phase extraction (SPE), liquid–liquid extraction (LLE) and protein precipitation. In this paper we will discus a new sample-preparation technique based on SPE for high throughput drug extraction developed and used by our group. This new sample-preparation method is based on monolithic methacrylate polymer as packing sorbent for 96-tip robotic device. Using this device a 96-well plate could be handled in 2–4 min. The key aspect of the monolithic phase is that monolithic material can offer both good binding capacity and low back-pressure properties compared to e.g. silica phases. The present paper presents the successful application of monolithic 96-tips and LC–MS/MS by the sample preparation of busulphan, rescovitine, metoprolol, pindolol and local anaesthetics from human plasma samples and cyklophosphamid from mice blood samples. 相似文献
79.
Visualizing tributyltin (TBT) in bacterial aggregates by specific rhodamine-based fluorescent probes
Xilang Jin Likai Hao Mengyao She Martin Obst Andreas Kappler Bing Yin Ping Liu Jianli Li Lanying Wang Zhen Shi 《Analytica chimica acta》2015
Here we present the first examples of fluorescent and colorimetric probes for microscopic TBT imaging. The fluorescent probes are highly selective and sensitive to TBT and have successfully been applied for imaging of TBT in bacterial Rhodobacter ferrooxidans sp. strain SW2 cell-EPS-mineral aggregates and in cell suspensions of the marine cyanobacterium Synechococcus PCC 7002 by using confocal laser scanning microscopy. 相似文献
80.
Seta Noventa Jvan Barbaro Malgorzata Formalewicz Claudia Gion Federico Rampazzo Rossella Boscolo Brusà Massimo Gabellini Daniela Berto 《Analytica chimica acta》2015
This work validated an automated, fast, and low solvent- consuming methodology suited for routine analysis of tributyltin (TBT) and degradation products (dibutyltin, DBT; monobutyltin, MBT) in biota samples. The method was based on the headspace solid-phase microextraction methodology (HS-SPME), coupled with gas chromatographic separation and tandem mass-spectrometry (GC–MS/MS). The effectiveness of the matrix-matched signal ratio external calibration was tested for quantification purposes. The exclusion of matrix influences in the calibration curves proved the suitability of this versatile quantification method. The method detection limits obtained were of 3 ng Sn g−1 dw for all the analytes. The analysis of references materials showed satisfying accuracy under optimum calibration conditions (% recovery between 87–111%; |Z-scores|<2). The repeatability RSD% and intra-laboratory reproducibility RSD% were lower than 9.6% and 12.6%, respectively. The work proved the remarkable analytical performances of the method and its high potential for routine application in monitoring organotin compounds (OTC). 相似文献