ESTABLISH CONCURRENT UV, VISIBLE, AND RAMAN SPECTROSCOPY AND X-RAY DIFFRACTION

这个子项目是利用资源的许多研究子项目之一。 由NIH/NCRR资助的中心拨款提供。对子项目的主要支持 子项目的首席调查员可能是由其他来源提供的， 包括美国国立卫生研究院的其他来源。为子项目列出的总成本可能 表示该子项目使用的中心基础设施的估计数量， 不是由NCRR赠款提供给次级项目或次级项目工作人员的直接资金。 目的：在最近的更新方案中提出的目标是：我们将改进现有的单晶UV/VIS显微分光光度测量设备，在X射线光束线上以基本无缝和常规的方式提供单晶的光谱，并发展单晶荧光光谱和单晶拉曼光谱。 结果我们目前在光束线X26-C上的配置包括一个带有ADSC Q210面探测器(从NSLS借来的)的晶体逻辑衍射仪，一个4DX光系统AB光学系统，一个Newport 75W Xe研究弧灯，一个Newport 200W汞(Xe)研究弧灯，一个运行在Linux操作系统上的光束线控制的海洋光学USB 4000 CCD分光光度计，以及一个Horiba Jobin-Yvon Inc.由两个二极管激光器(532和785 nm)组成的拉曼系统，每个激光专用的拉曼探头，IHR 550光谱仪和Synapse CCD探测器。我们已经为Horiba Jobin-Yvon订购了一台473 nm的半导体激光器和相关的拉曼探头，正在等待交付和安装。 X射线衍射和光学吸收数据采集完全集成在一起，并由光束线控制软件控制。光束线软件还增加了其他功能，包括实时跟踪特定波长的吸收变化，以及使用RADDOSE程序将帧编号转换为辐射剂量。结果直接链接到我们的数据库跟踪系统PXdb。拉曼系统完全正常运行，在X射线曝光前后定期收集振动光谱。目前，拉曼系统由Horiba-JY提供的基于Windows的LabSpec软件控制。 光学吸收光谱收集利用来自Xe或Hg(Xe)弧光灯光源的UV/Vis光(300-850 nm)。光被带到样品上，透射光通过石英光纤被带到分光光度计。15倍显微镜物镜基于施瓦茨抛物面镜片的设计，该镜片采用全反射原理，因此没有色差。光被聚焦到取决于物镜和它连接的光纤的直径的光斑大小。例如，入射光子通过50？m光纤聚焦到直径25？m的光斑，而光子通过由400？m光纤聚焦的75？m直径区域被收集。这种排列通常在不到一秒的时间内产生全范围的电子吸收光谱。 在进度报告条目中可以找到完整的描述。 计划吸收光谱我们通过购买Oriel汞(Xe)弧光灯光源，将我们的能力扩展到光谱的UV区域。两盏灯使用的弧光灯外壳将配备280 nm的切割式滤光片和滤光片支架，以延长光纤电缆的使用寿命。为了允许远程控制吸收光谱的收集，正在进行几项修改。购买的电动快门将控制弧光灯光源的输出。正在为聚焦和收集目标设计更多的快门。将对控制软件进行修改，使远程操作成为现实。 衍射仪-Q210区域探测器将在不久的将来返回NSLS。之前在X25使用的Q315r探测器将安装在X26C。 非共振和共振拉曼光谱-我们订购了一台473 nm的激光器和探头。这将扩展我们的共振拉曼能力。在未来的一年里，拉曼数据收集的控制将被纳入CBass软件，并且操作将自动化。将开发工具，以实现物镜快门、激光快门、照明灯、房间灯等的远程计算机操作。 离线单晶光谱分析2010年初在X26-C机壳附近建造了一个离线光谱分析外壳，配备了光学台、衍射仪/测角仪和冷冻流。我们正在采购剩余的所需设备 单晶、荧光发射光谱荧光光谱是对电子吸收和拉曼光谱能力的补充。光源和探测仪器的各种选择正在调查中。 意义我们目前提供的技术在美国是独一无二的，并将在未来一年得到进一步加强。我们和我们的用户将解决的科学问题是美国大分子科学进步的核心。我们设想的国家资源将支持前所未有的、高度相关的研究。这些结果将为大分子原子结构、电子结构和化学之间的复杂关系提供急需的数据。这些数据将被该领域的大量国内和国际研究人员使用。我们的计划将使美国在这一领域处于领先地位。

This subproject is one of many research subprojects utilizing the resources provided by a Center grant funded by NIH/NCRR. Primary support for the subproject and the subproject's principal investigator may have been provided by other sources, including other NIH sources. The Total Cost listed for the subproject likely represents the estimated amount of Center infrastructure utilized by the subproject, not direct funding provided by the NCRR grant to the subproject or subproject staff. Objectives  The objectives stated in the recent renewal proposal are these: we will improve our current single crystal UV/Vis microspectrophotometry facility to provide optical spectra from single crystals in an essentially seamless and routine fashion at the X-ray beamline, and develop both single crystal fluorescence spectroscopy and single crystal Raman spectroscopy. Results  Our current configuration at beamline X26-C consists of a Crystal Logic diffractometer with an ADSC Q210 area detector (on loan from the NSLS), a 4DX-ray Systems AB optical system, a Newport 75W Xe research arc lamp, a Newport 200W Hg (Xe) research arc lamp, an Ocean Optics USB 4000 CCD-based spectrophotometer running through the beamline controls on a LINUX operating systems, and an Horiba Jobin-Yvon Inc. Raman system consisting of two diode lasers (532 and 785 nm), a Raman probe head specific for each laser, an IHR 550 spectrometer and Synapse CCD detector. We have ordered a 473 nm diode laser and associated Raman probe head for Horiba Jobin-Yvon and are awaiting delivery and installation. X-ray diffraction and optical absorption data collection are fully integrated and controlled by the beamline-control software. Additional capabilities have been added to the beamline software, including the ability to track in real-time absorption changes at specific wavelengths and to convert frame number to radiation dose using the RADDOSE program. The results are linked directly to our database tracking system, the PXdb. The Raman system is fully operational with vibrational spectra routinely collected before and after x-ray exposure. Currently, the Raman system is controlled by the Windows-based LabSpec software provided by Horiba-JY. The optical absorption spectra collection utilizes UV/vis light (300 - 850 nm) from either a Xe or a Hg (Xe) arc lamp source. The light is brought to the sample and the transmitted light brought to the spectrophotometer via through quartz optical fibers. The 15x microscope objectives are based upon the Schwarzschild parabolic mirror design, which uses an all-reflecting principle and are, therefore, free from chromatic aberration. The light is focused to a spot size that depends upon objective and the diameter of the optical fiber to which it is connected. For example, the incident photons are focused to 25 ¿m diameter spot through a 50 ¿m optical fiber, whereas photons are collected through a 75 ¿m diameter region focused by a 400 ¿m optical fiber. This arrangement yields full range electronic absorption spectra typically in less than one second. Find a full description in the Progress Report entry. Plans  Absorption spectroscopy  We have expanded our capabilities into the UV region of the spectrum through the purchase of an Oriel Hg (Xe) arc lamp source. The arc lamp housing used for both lamps will been fitted with a 280 nm cut-up filter and filter holder in order to extend the lifetime of the fiber optic cables. To allow for remote control over the collection of absorption spectra, several modifications are underway. A purchased motorized shutter will control the output at the arc lamp source. Additional shutters are being designed for both the focusing and collection objectives. The control software will be amended such that remote operations becomes a reality. Diffractometer - The Q210 area detector will be returned to the NSLS in the near future. The Q315r detector, previously used at X25, will be installed at X26C. Non-resonance and Resonance Raman Spectroscopy - We have ordered a 473 nm laser and probe head. This will expand our resonance Raman capabilities. In the coming year, control of Raman data collection will be incorporated into the CBASS software and the operations will be automated. Tools will be developed to allow for the remote, computerized operation of the objective shutters, laser shutters, illumination lamps, room lights, etc. Off-line single-crystal spectroscopy  An enclosure for off-line spectroscopy was constructed adjacent to the X26-C hutch in early 2010 and outfitted with an optical table, diffractometer/goniometer and cryostream. We are in the process of procuring the remaining required equipment Single Crystal, Fluorescence-Emission Spectroscopy  Fluorescence spectroscopy complements the electronic absorption and Raman spectroscopy capabilities. The various options for light sources and detection instruments are under investigation. Significance  The technologies we currently provide are unique in the United States, and will be enhanced further in the coming year. The scientific problems that we and our users will address are central to the progress of macromolecular sciences in the United States. The national resource we envision will support unprecedented, highly correlated studies. The results will provide much needed data on the complex relationships among macromolecular atomic structure, electronic structure and chemistry. These data will be used by the large number of national and international researchers in the field. Our plans will place the United States in a leadership position in this area.