19F-NMR测定甲磺酸帕珠沙星样品中的氟

研究了19F-NMR技术测定甲磺酸帕珠沙星药物样品中氟的检测条件.优化了实验参数,选用三氟乙酸钠作为内标,重水与去离子水混合液作为溶剂的内标绝对法进行定量分析.测定了甲磺酸帕珠沙星药物样品中氟含量.实验表明,氟的加标回收率在99.2%-100.9%之间,标准偏差为0.00446%-0.0652%,相对标准偏差小于1.459%.     

19F-NMR外标法测定盐酸左氧氟沙星中的氟含量

本文研究了利用19F-NMR技术测定盐酸左氧氟沙星药物样品中氟的检测条件.优化了实验参数,选用三氟乙酸钠作内标,重水与去离子水混合液为溶剂.测定了对盐酸左氧氟沙星样品中氟含量.实验表明,氟的加标回收率在98.4%-100.6%之间,标准偏差为0.00214%-0.0489%,相对标准偏差小于1.124%.     

电子束曝光技术

近十几年以来,国内外广泛地进行了电子束技术在工业中的应用研究.其中,一部分已经成功地用于实际生产中,例如:电子束蒸发、电子束焊接以及利用扫描电子显微镜观察材料及器件特性等. 随着科学技术的发展,国内外对于电子束技术在微电子器件制造中的应用也相当重视.一些技术比较先进的国家大都已开展了电子束曝光技术的研究试制工作,并已取得成果.下面我们就讨论电子束曝光技术中的一些问题. 所谓电子束曝光就是利用电子加速系统将电子加速,并通过电磁透镜将其聚焦成细束,然后利用电磁场控制该束在工件上扫描以制出所需要的图案.这里我们所指的…     

19F固体核磁共振技术研究膜蛋白相互作用的进展

固体核磁共振技术因其可实现细胞膜环境中的蛋白质结构研究而广受关注.¹⁹F元素由于灵敏度高、天然丰度高,无生物背景等优点,被广泛应用于生物核磁共振技术中.氟标固体核磁共振技术常被用于细胞膜中蛋白质的相互作用研究,如：抗菌肽与细胞膜的相互作用、聚合膜蛋白结构分析等.此篇综述介绍了常用的蛋白质氟标修饰的实验方法,总结了常用的¹⁹F生物固体核磁共振实验技术,以及介绍了应用¹⁹F固体核磁共振研究膜蛋白的成功案例.此外,此篇综述讨论了¹⁹F固体核磁共振技术在蛋白质研究中的局限性.     

非晶态超导性

一、引 言 Buckel 和 Hilsch于1954年发表了他们对非晶态超导性所作的系统的研究工作[1].最近十几年不断发现许多非晶态材料超导临界温度比相应的结晶态材料有很大提高.其超导性也有一些新的特点,因此受到应用和基础研究方面的重视。至今已经发表了不少理论和实验研究工作,同时也提出不少问题,有待进一步从固体和超导性的理论以及实验方面进行研究。 本文中先介绍非晶态简单金属超导性的特点.超导性起因于电子声子相互作用,因此为了理解非晶态超导性的特点,在第三部分分析非晶态电声子相互作用,在第四节部分综述非晶态过渡金属超导性的特点…     

声学超构材料及其物理效应的研究进展

声学超构材料作为一种新型的人工结构材料,拥有天然材料所不具备的超常物理特性,进一步拓展了材料的声学属性.同时,声学超构材料可以实现对声波精准的、可设计的操控,以及许多新颖奇特的物理现象,如声准直、声聚焦、声场隐身、声单向传输、声学超分辨成像等,具有重要的理论研究意义和应用价值.另外,拓扑材料的研究已延伸至声学领域,声学超构材料的拓扑性质成为近年的研究热点,受到人们的广泛关注.其鲁棒性边界态具有缺陷免疫、背散射抑制的特性,应用潜力巨大.本文综述了近十几年来声学超构材料的研究概况,介绍了相关的代表性工作,包括奇异等效声学参数的超构材料、声学超构表面、吸声超构材料、声学超分辨成像、宇称时间对称性声学和拓扑声学等,阐述了声学超构材料的设计理念和方法,并对其技术挑战和应用前景进行了讨论和总结.     

19F NMR技术在蛋白质研究中的应用

因为¹⁹F核自身的特性,如自旋为1/2;丰度高(100%),具有与¹H相当的灵敏度;化学位移分布广且对环境敏感;绝大部分生物体内都不含¹⁹F因而无背景干扰等;¹⁹F NMR自诞生以来就成为非常有吸引力的研究手段. 现在,¹⁹F NMR已被广泛用于核磁共振成像、药物化学及生物大分子的研究,各个方面均有较多的相关文献综述. 该综述将集中讨论¹⁹F NMR在蛋白质研究中的应用,包括蛋白质¹⁹F标记方法,¹⁹F NMR在蛋白质结构、 动力学、蛋白质折叠、蛋白质与药物的相互作用及In-cell NMR中的应用.     

受激辐射损耗超分辨显微成像系统研究的新进展

由于受到衍射极限的影响,传统光学显微镜的分辨率被限制在半个波长左右.近二十年来出现了许多通过不同方法绕过光学衍射极限的超分辨成像技术,其中,受激辐射损耗显微(stimulated emission depletion microscopy,STED)通过引入一束环形损耗光来抑制荧光光斑外围荧光分子的发光,以达到减小点扩散函数的目的,实现超分辨成像.经过近些年的发展,STED系统无论从光束的产生、校准和扫描,还是最后的成像,都有了很大的发展.本文将简要介绍STED成像技术的基本原理,详述STED超分辨成像技术出现至今在光源、扫描及成像系统等方面的进展,以及在三维成像和多色成像方面的发展现状,STED技术与其他显微技术的结合.最后,本文对STED技术近几年的研究新进展进行了系统的论述,对STED技术未来的发展趋势进行了探讨.     

氟化高分子材料的光学特性及其应用

高分子材料在光电子领域是一种必不可少的材料。由于含氟化合物中分子吸收受到抑制及分子极化率降低等原因,导致氟化高分子材料在近红外光区具有优良的透明性,并且折射率很低,这对于高分子光学元件的设计具有重要意义。     

光学新分支——梯折光学

梯度折射率(下面简称梯折)光学,是近些年来引人注目的一门光学分支学科.它的发展已有一百多年的历史.Maxwell鱼睛透镜、Wood透镜、Luneburg透镜以及梯折透镜的研制成功都是梯折光学发展史上的重要里程碑.然而只有在近十几年来,随着计算机科学的发展;像差理论和计算方法的不断完善;梯折材料的研制成功以及测试方法的改进等,梯折光学才有可能在实际上有所应用.1979年美国召开了第一次梯折光学及其材料的专题会议,以后几乎每隔1—2年召开一次.使该课题成为国际上引人注目的一门光学分支学科.七十年代,中科院西安光机所在龚祖同教授和薛鸣球教授等的领导下开展的有关研究课题已取得了很大的成就,使梯折棒透镜在光纤通讯中开始实际应用.八十年代中,上海光学仪器研究所在庄松林研究员的领导下,进行了梯度折射率材料及其应用的研究,经过几年的努力,在材料的梯度深度和梯度大小方面取得了可喜的进展,并对光线在梯折介质中的传     

Short-range order and F ion diffusion inside the Pb1 − xAlxF2 + x solid solution Part I: F-NMR investigation

A ¹⁹F-NMR investigation of the Pb_{1 − x}Al_xF_{2 + x} (0 ≤ x ≤ 0.12) solid solution and of the ordered Pb₉Al₂F₂₄ phase is undertaken as a function of temperature. Several F⁻ ion groups become progressively mobile at the NMR time scale at increasing temperature, the first, (F_i)_pb and (F_n)_pb, are located in the surroundings of Pb²⁺ cations, the second ones, (F_rd)_AI and (F_ra)_Al, in that of Al³⁺ cations. Four types of fluoride ions are distinguished in the ¹⁹F-NMR spectra of rigid lattice at low temperature (T = 175 K) and the distribution of fluoride ions among the four sites is determined by deconvolution of the spectra registered. The sites occupied by the (F_n)_pb anions are identified with the normal anionic sites of the fluorite network, the others with different interstitial sites.     

19F-NMR Analysis of Primary and Secondary Amines Following Chemical Derivatization with Trifluoroacetic Anhydride

Five amines were reacted with trifluoroacetic anhydride (TFAA) as derivatization reagent and subsequently analyzed via ¹⁹F nuclear magnetic resonance (NMR) spectroscopy. The ¹⁹F-NMR spectra of derivatives of aniline, 2,4-dimethyl aniline, and 2-methoxy aniline produce a signal that are very close to TFAA. The peaks resulting from the reaction of TFAA with N-ethyl aniline and N-methyl aniline are shifted much farther downfield than any of the other signals. Optimal ¹⁹F-NMR sensitivity based upon T ₁ relaxation time was investigated for derivatization compound and flurbiprofen as internal standard in toluene. The calibration curve was linear for amines over the range of 9.0–100.0?mg?L^?1, with detection limit (S/N?=?3) of 2.6–2.9?mg?L^?1. Solid-phase extraction cartridges were investigated for preconcentration of water samples. The method was validated through spike and recovery for secondary amines from tap water sample.     

Uniform mixing of antiferromagnetism and high-temperature superconductivity in electron-doped layers of four-layered Ba(2)Ca(3)Cu(4)O(8)F(2): a new phenomenon in an electron underdoped regime

We report (63,65)Cu- and (19)F-NMR studies on a four-layered high-temperature superconductor Ba(2)Ca(3)Cu(4)O(8)F(2)((0234F(2.0)) with apical fluorine (F(-1)), an undoped 55 K superconductor with a nominal Cu(2+) valence on average. We reveal that this compound exhibits the antiferromagnetism (AFM) with a Néel temperature T(N)=100 K despite being a T(c)=55 K superconductor. Through a comparison with a related trilayered cuprate Ba(2)Ca(3)Cu(4)O(8)F(2)(0233F(2.0)), it is demonstrated that electrons are transferred from the inner plane (IP) to the outer plane (OP) in 0234F(2.0) and 0223F(2.0), confirming the self-doped high-temperature superconductivity (HTSC) having electron and hole doping in a single compound. Remarkably, uniform mixing of AFM and HTSC takes place in both the electron-doped OPs and the hole-doped IPs in 0234F(2.0).     

Recent results on the generation of new orientations during recrystallization

In the last years High Voltage Electron Microscopy and Beck-experiments have been used in Göttingen to elucidate the generation of new orientations during the anneal of a deformed metal single crystal. It is found on Al, Cu and dilute Cu-P solid solutions that nucleation always occurs in orientations of the deformation microstructure. During growth orientations change by multiple twinning to produce grain boundaries of lower energy. These are not always the most mobile ones except in some alloys. The influence of such a growth selection on texture is discussed.This summary is based on the careful work of and lively discussion with the Göttingen RX group of P. Wilbrandt, A. Berger, F. Ernst and U. Klement. It is supported by DFG.     

Nuclear magnetic resonance studies of surface interactions between trifluoromethanesulfonic acid and silica

The nature of the interaction between trifluoromethanesulfonic acid (triflic acid) and the surface groups of silica as a support has been investigated by¹H and¹⁹F-NMR studies. The¹⁹F-NMR spin-lattice relaxation time (T ₁) dependence on temperature suggests that the dominant relaxation mechanism for¹⁹F is a combination of spin-rotation (SR) interactions, one of which seems to be quenched by cage-like structures. This mechanism is activated by the treatment followed to stabilize the acid on silica. Hydrogen proton relaxation seems instead to be driven by dipolar interactions and the formation of hydrogen bridges. Activation energies have been estimated for various cases, assuming an Arrhenius-type temperature dependence for the correlation times of molecular motion. A linear dependence of¹H chemical shift on inverse temperature was also found, which is interpreted as thermal weakening of hydrogen bonding. The results support the conclusion that the stability of triflic acid on silica is due to the formation of strong hydrogen bridges between the sulfonic groups of triflic acid and the silica surface hydroxyls, provided a network structure similar to that observed for pure acid is obtained in which strong interactions between acid molecules occur. The acid seems to be organized as solid-like “drops” on the silica surface, which accounts for the long residence time on the silica surface.     

Synthesis and Characterization of a Fluorinated Phenolic Resin/phenolic Resin Blend

Fluorine atoms were introduced into the molecular chain of a phenolic resin (PR) by a two-step acid synthesis process to improve its thermal and hydrophobic properties. The successful synthesis of a fluorinated phenolic resin/phenolic resin blend (F-PR/PR) was proven by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance 19F (¹⁹F-NMR). The thermal properties of F-PR/PR were analyzed by differential scanning calorimetry (DSC) and thermo gravimetric analysis (TGA) and the results indicate that the F-PR/PR had good thermal stability. The hydrophobic properties of PR were effectively modified as demonstrated by the water drop contact angles. The flexural and tribological properties of F-PR/PR were also investigated. The fluorine atom, by virtue of its electronegativity, size and bond strength with carbon, can be used to create composites from F-PR/PR with remarkable properties. For comparison, two other resin blends were also synthesized.     

具有CF2=CF结构的化合物中19F NMR化学位移的计算

系统总结和分析前人对19F NMR化学位移研究成果的基础上,对19F NMR化学位移的规律进行研究,最终确定用回归分析中的最小二乘法来确定计算19F NMR化学位移的公式,并用F检验法对所得计算公式进行检验,给出了具有CF2=CF结构的化合物中19F NMR化学位移的计算公式δcal=B+△α+△β,该公式的置信度为9...     

Carbon-13 and Fluorine-19 NMR Spectroscopy of the Supramolecular Solid p-tert-Butylcalix[4]arene ·α,α,α-trifluorotoluene

The supramolecular 1 : 1 host–guest inclusion compound, p-tert-butylcalix[4]arene ·α,α,α-trifluorotoluene, 1, is characterized by ¹⁹F and ¹³C solid-state NMR spectroscopy. Whereas the ¹³C NMR spectra are easily interpreted in the context of earlier work on similar host–guest compounds, the ¹⁹F NMR spectra of solid 1 are, initially, more difficult to understand. The ¹⁹F{¹H} NMR spectrum obtained under cross-polarization and magic-angle spinning conditions shows a single isotropic resonance with a significant spinning sideband manifold. The static ¹⁹F{¹H} CP NMR spectrum consists of a powder pattern dominated by the contributions of the anisotropic chemical shift and the homonuclear dipolar interactions. The ¹⁹F MREV-8 experiment, which minimizes the ¹⁹F–¹⁹F dipolar contribution, helps to identify the chemical shift contribution as an axial lineshape. The full static ¹⁹F{¹H} CP NMR spectrum is analysed using subspectral analysis and subsequently simulated as a function of the ¹⁹F–¹⁹F internuclear distance (D_FF = 2.25 ± 0.01 Å) of the rapidly rotating CF₃ group without including contributions from additional libration motions and the anisotropy in the scalar tensor. The shielding span is found to be 56 ppm. The width of the centerband in the ¹⁹F{¹H} sample-spinning CP NMR spectrum is very sensitive to the angle between the rotor and the magnetic field. Compound 1 is thus an attractive standard for setting the magic angle for NMR probes containing a fluorine channel with a proton-decoupling facility.     

19F NMR的特点

¹⁹F的磁旋比和相对灵敏度接近质子;¹⁹F NMR化学位移范围可达 δ 1 000,谱图分辨率高;¹⁹F NMR对环境因素较氢谱远为敏感、复杂,可反映出化合物结构的细微差别. 由于正常生物体内含氟成分很少,干扰小,因此在生物医学研究中引入氟代物进行¹⁹F NMR研究有特殊意义. 对氟化物的¹⁹F NMR化学位移和偶合常数的范围也分类作了总结.