NMR超微量探头的新进展

介绍了超微量探头的新进展,这种设计独特的探头与过去的微量探头完全不同,它可将很小体积的样品(<40μL)100%地保留在接受线圈的有效范围内,运用魔角旋转校正谱线加宽,这是常规匀场方法难以纠正的,产生的结果使小体积样品灵敏度高,线形好,是以前的微量探头无法达到的.本文列举了文献中对这类探头在均相与非均相微量样品中的应用实例和用11mg未知样测定INADEQUATE谱并与FRED软件相结合完成¹³C骨架归属的情况.     

布鲁克新一代NMR自动调谐探头

所有的分析仪器总是不断追求进一步提高自动化程度,例如在有机合成和药物化学方面,为了适应大量筛选工作的需要,组合化学应运而生,对仪器自动化的要求更高.在这个领域里,NMR是个关键的分析技术,首当其冲地面对这些要求.作为主要的分析仪器生产厂家,布鲁克公司的承诺是——永远不断创新.最近,布鲁克公司推出用计算机控制的自动调谐和匹配的新一代NMR探头,就是又一个明显的例子.这种新探头,不仅满足了用户对NMR谱仪不断提高的要求,同时,使分子结构的测定和验证接近于完全自动化.     

具有独立探头的3ω技术测量固体热导率

设计并制作了一种适用于3ω技术的独立探头.提出了利用基于这种独立探头的3ω技术进行固体热导率测量的原理和方法.与传统3ω技术相比,基于独立探头的3ω技术具有探测器使用寿命长、不再对样品表面有光滑要求的优势,并且实现了对样品热导率的无损测量.对几种标准样品的热导率进行测试的结果表明,基于独立探头的3ω技术在表征块状固体及...     

基于压缩感知/重采样的NMR噪声抑制新方法

发展高灵敏检测方法是分析化学的永恒主题之一,提高信号强度和降低噪声水平是增强灵敏度的根本途径.在核磁共振波谱(NMR)分析中,通常采用高磁场强度的谱仪或复杂的脉冲实验方法来提高信号强度,或通过使用超低温探头来降低噪声水平,但这无疑会提高实验成本或增加实验难度.相较而言,利用数据后处理方法辨识和抑制噪声,是更为经济的提高信噪比(SNR)的途径.因此,该文在前期研究中发展的基于统计学中重采样原理的数据后处理方法(NASR)的基础上,通过引入压缩感知(CS)技术,对重采样方法进行了优化改进,所发展的NMR数据处理新方法(CS_NASR)可有效排除主观因素影响,提高处理结果的鲁棒性.     

低温NMR探头的应用

在过去10年中研发新核磁共振探头一直是制造者争夺的活跃领域. 最近，因其灵敏度的巨大提高，低温冷却探头得到人们格外的关注. 利用这一技术可大量节省谱仪机时. 对于低γ核可直接测定天然丰度样品而不必标记，这远比节省机时更为重要. 本文评述了针对5～10 Hz优化2 mg天然丰度噁唑烷酮抗菌素eperezolid的 CIGAR-HMBC-¹H-¹⁵N谱的比较，一个是采自美国瓦里安公司的5 mm低温探头，另一个是采自瓦里安公司传统室温3 mm 梯度三共振探头. 利用低温探头大约10 min就可记录到大部份¹H-¹⁵N远 程相关，26 min可观察到几乎所有的远程共振. 而在同样条件下使用3 mm传统梯度反式三共振探头无法得到有用的谱图，要想取得相同的结果须累加约18 h.     

一种多层压电结构:迭层换能器

在目前的换能器设计技术中,为了提高换能器的带宽,普遍采用重背衬技术。但是,重背衬的使用,使得换能器的灵敏度有较大的损失。近年来压电复合材料的应用使得换能器的性能大为改进。如何进一步提高压电换能器的灵敏度是Chofflet和Fink这篇文章的研究重点。     

二茂铁基化合物的ESR研究进展

二茂铁基化合物因具有独特的氧化还原、电、光、磁和催化性能,而被广泛研究与应用.电子自旋共振(ESR)技术是观察物质顺磁性最直接的手段,在研究二茂铁基化合物的电子结构、电子转移和分子间相互作用等方面具有独特的优势.ESR技术还具有灵敏度高、样品处理简单、直接检测不破坏样品等优点.该文综述了二茂铁基化合物的ESR研究进展.     

光纤水听器灵敏度测试研究

研制了一套简单可行的光纤水听器灵敏度校准装置,提出了一种简便的测量方法——比对法:将标准压电水听器探头和光纤水听器探头置于同一声场中，并将两探头的输出同时接到数字示波器上进行比对测量.研究表明,振动系统中的盛水容器具有一定的壁厚（>10 mm或1/10桶的外径）时，可将振动系统的谐振峰移出工作频段范围（3~1000 Hz）外.利用此装置结合比对法,校准系统简单，校准速度快,实验的误差小于0.5 dB,能满足一般光纤水听器灵敏度的校准需求.     

共路径光相干成像系统光纤探头的研究

本文提出了基于楔形光纤以及端面成角度光纤的共路径光相干成像系统探头,实现背向散射信号在其端部的共路径相位干涉,从而获得待测件断面成像信息.首先,建立了共路径光相干成像系统光路及探头相位干涉的理论模型,分析了各光纤探头尺寸与干涉信号强度、系统性能的关系.其次,分别设计出楔形光纤、端面成角光纤探头,开展了共路径光路干涉实验,搭建了工作波长为1 550 nm的共路径光路测试系统.然后,根据不同待测样品的散射率,设计并研制了不同角度的楔形光纤探头,分析了不同尺寸的光纤探头对系统性能的影响,针对不同样品开展了固定探头探测实验.实验结果表明,楔形光纤端部可直接对输出光聚焦,照射在被测样品上,且其端面成一定角度时,可调节输出分光比,实现对参考信号的调节,提高了系统信噪比.为进一步开展共路径光相干成像系统的研究奠定了基础.     

高效液相核磁共振仪联用技术及微量探头技术在天然产物分析中的应用

以下工作在VARIAN公司的INOVA 500 MHz仪器上完成，使用了高灵敏度的LC-NMR联用探 头及先进的WET脉冲序列进行溶剂峰压制. 通过运用高效液相-核磁共振仪联用技术及微量探头技术对几个天然产物混合物进行分析，展示了高效液相-核磁共振联用（HPLC-NMR）技术及微量探头技术在天然产物分析中的优势，既高效，快速，微量. 二者结合使用，使得用NMR技术分析天然产物混合物变得切实可行.     

Electro-optical detection of ZnO-Based unbalanced fabry-perot resonators

Zinc oxide films prepared by magnetron sputtering are introduced to the electro-optical detection to improve the voltage sensitivity. With the help of large piezoelectric effect, ZnO films make up for the deficiency of the low electro-optical coefficient. In this paper, we illustrated the mechanism of piezo-induced enhancements, and measured the electric signals on the line of coplanar waveguides. This method breaks through the limit of material species for optoelectronically responsive sensing, and shows promising applications in optical detection.     

All-optical mass sensing with coupled mechanical resonator systems

With the small mass, large quality-factor and high frequency, mechanical resonators (MRs) will ultimately find usage in a broad range of applications, such as electrometry, optomechanical/electromechanical signal processing, and mass detection. In this review, we focus on a particular MR application: mass sensing in an all-optical domain. Compared to the mass detection based on the electrical techniques, we have proposed an optical protocol to weigh the external particles deposited onto the surface of a mechanical resonator. This protocol, which is so far the first method to deal with the mass sensing in an all-optical domain, is based on some coupled mechanical resonator systems. Here we review our recent optical mass sensors comprehensively. These all-optical mass sensors have the potential to break through the limitation of frequency restriction and to enhance the sensitivity of mass detection.     

Improving the Sensitivity of Forward Light Scattering Technique to Large Particles

The detection of a small number of large particles whose size lies outside the required size distribution is important in the processing of many materials when those particles result in the deterioration of the product quality. Laser diffraction, which is a very popular technique for on-line monitoring and process control, has, however, limited sensitivity to those few large particles. This paper deals with the improvement of this sensitivity. The fluctuations of the signal received by the detectors were analyzed by both experiment and simulation. Two statistical approaches, cross-correlation and principal component analysis (PCA), were applied. A detection procedure is proposed which is based on the combination of sweep selection through PCA and an appropriate deconvolution of the selected sweeps. The preliminary experiments with Al₂O₃ powder showed an improved sensitivity to the large particles.     

High-accuracy mass spectrometry with stored ions

Like few other parameters, the mass of an atom, and its inherent connection with the atomic and nuclear binding energy is a fundamental property, a unique fingerprint of the atomic nucleus. Each nuclide comes with its own mass value different from all others. For short-lived exotic atomic nuclei the importance of its mass ranges from the verification of nuclear models to a test of the Standard Model, in particular with regard to the weak interaction and the unitarity of the Cabibbo–Kobayashi–Maskawa quark mixing matrix. In addition, accurate mass values are important for a variety of applications that extend beyond nuclear physics. Mass measurements on stable atoms now reach a relative uncertainty of about 10^-11${10}^{-11}$. This extreme accuracy contributes, among other things, to metrology, for example the determination of fundamental constants and a new definition of the kilogram, and to tests of quantum electrodynamics and fundamental charge, parity, and time reversal symmetry. The introduction of Penning traps and storage rings into the field of mass spectrometry has made this method a prime choice for high-accuracy measurements on short-lived and stable nuclides. This is reflected in the large number of traps in operation, under construction, or planned world-wide. With the development and application of proper cooling and detection methods the trapping technique has the potential to provide the highest sensitivity and accuracy, even for very short-lived nuclides far from stability. This review describes the basics and recent progress made in ion trapping, cooling, and detection for high-accuracy mass measurements with emphasis on Penning traps. Special attention is devoted to the applications of accurate mass values in different fields of physics.     

隧穿磁阻传感器研究进展

传感器作为物联网技术的基石,在人们的生产生活中发挥着重大作用.其中,基于隧穿磁阻效应(tunneling magnetoresistance, TMR)的磁传感器具有灵敏度高、尺寸小、功耗低等优点,在导航定位、生物医学、电流检测和无损检测等领域具有极大的应用前景.本综述以TMR传感器技术路线的发展为核心,囊括了从基本传感单元到三维空间磁场检测,再到实际应用的多个研究重点.首先,介绍了TMR传感器发展历程并阐明其基本工作原理,讨论了提高单个传感单元磁隧道结输出线性度的方法.接下来,详细介绍了传感器的重要电路结构—惠斯通电桥,以及制备TMR全桥结构的多种工艺方法.进一步,从三维空间磁场检测这一市场需求入手,深入讨论了基于TMR传感器的三维传感结构的设计和制备方法.同时,以传感器灵敏度和噪声水平这两大基本性能为切入点,列举了TMR传感器性能的优化方案.最后,本文对TMR传感器的应用展开了详细介绍,以自旋麦克风,生物传感器两个新兴应用为例,对TMR传感器未来在物联网中的发展和应用进行了展望.     

催化化学发光分析系统研究进展

催化化学发光是分子通过催化剂表面时被氧气氧化过程中产生的一种光辐射现象。在过去的三十几年里,催化化学发光技术发展迅速,特别是在传感器方面快速发展,成为一项新型分析检测技术,在公众安全、排放检测、环境保护等方面发挥了巨大的作用。基于催化发光技术设计的传感器具有检测限低、灵敏度高、快速、仪器简单易操作、易实现小型化,便携等优点,在无机小分子气体及易挥发有机物的分析检测中展现了其独特的优势。应用于催化发光的催化材料发展至今已达上千种,囊括了金属、金属氧化物,非金属氧化物、硫化物、硒化物、金属盐类、有机物、陶瓷玻璃类等各类材料;复合材料的应用丰富了催化材料的种类;纳米新材料的引入为其发展提供了新的契机;材料的形貌等也得以深入研究。催化发光新技术也不断发展,催化发光与其他技术(雾化、分离富集、等离子体等)联用的发展,静态催化发光技术、多级催化发光技术、循环催化发光技术等的开发应用进一步提高了催化法光分析系统的灵敏度与选择性,拓展了催化发光的应用范围。本文综述了近年来催化发光的催化材料、联用技术及其他新技术的发展,并对其发展趋势进行了展望。     

The Progress on Cataluminescence-Based Analytical SystemSCIEI北大核心CSCD

Cataluminescence(CTL) is a phenomenon of light radiation generated when analyte moleculars were oxidized by catalyst. In the past few decades, CTL has developed rapidly and become a promising detection technique, especially in gas sensing, and has attracted much attention of researchers for its potential versatile applications in emission control, public safety, and environmental protection. The analytical system based on CTL has low detection limit, high sensitivity and simple instrument which easy to operate, which shows huge advantages in the detection of inorganic gases and volatile organic compounds. The library of sensing materials has been greatly enriched to thousands kinds, which contains metals, metal/non-metal oxides, sulfide, metal salts, organic compounds, ceramic, glass and other types of materials; Composite materials have been developed; The decreasing of material dimensions to nanoscale provided new opportunities for its development; The morphology of material has also been explored. Some novel hyphenated techniques based on CTL coupled to other techniques including preconcentration/sepration, nebulization, plasma have been developed, as well as some new CTL technique including static CTL, cyclic CTL and ect. Thanks to development of sensing material and the appearance of these novel techniques, the selectivity and sensitivity of CTL system has been improved, and the range of CTL application has been extended. In this article, the progress made in the field of cataluminescence, especially in latest developments of analytical applications were reviewed. The catalysts used in CTL, the recent novel CTL techniques were sumerized. The future of the cataluminescence was also forecasted.     

A two-step hydrothermally grown ZnO microtube array for CO gas sensing

Tubular ZnO microstructure arrays were fabricated on a large scale by a two-step hydrothermal method. The porous ZnO tubular structures were then used to construct a gas sensor for CO detection. The microtube array gas sensor showed sensitive response to different concentration of CO with an optimum temperature of 250 °C. Because of the large surface to volume ratio, the sensitivity of the microtube arrays was about twice of that of the ZnO rods. Our results indicate that this simple two-step method for fabrication of large-scale tubular microstructure arrays can be potentially used in gas sensor applications with improved performance. PACS 81.07.Bc; 78.55.Et; 07.07.Df     

Characteristic X-ray production by heavy ion bombardment as a technique for the examination of solid surfaces

Over the past few years, intense effort has been expended on studying the physical processes responsible for the production of characteristic X-rays during heavy ion/atom collisions. It is considered timely at this stage to assess one of the applications of this work, viz., the use of heavy ions to detect elements at or near to surfaces. It emerges that one of the advantages of the technique is its ability to detect light elements with high sensitivity and to examine the depth distribution of implanted elements. As an example of its application, evidence is presented for the detection of sulphur on the surfaces of copper, nickel and stainless steel.