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Sub-millisecond time-resolved SAXS using a continuous-flow mixer and X-ray microbeam.使用连续流混合器和 X 射线微束实现亚毫秒时间分辨 SAXS。
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用于溶液中生物大分子X射线散射的MacCHESS设施升级。

Upgrade of MacCHESS facility for X-ray scattering of biological macromolecules in solution.

作者信息

Acerbo Alvin Samuel, Cook Michael J, Gillilan Richard Edward

机构信息

Macromolecular Diffraction Facility of the Cornell High Energy Synchrotron Source (MacCHESS), Cornell University, 161 Synchrotron Drive, Ithaca, NY 14853, USA.

出版信息

J Synchrotron Radiat. 2015 Jan;22(1):180-6. doi: 10.1107/S1600577514020360. Epub 2015 Jan 1.

DOI:10.1107/S1600577514020360
PMID:25537607
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC4294029/
Abstract

X-ray scattering of biological macromolecules in solution is an increasingly popular tool for structural biology and benefits greatly from modern high-brightness synchrotron sources. The upgraded MacCHESS BioSAXS station is now located at the 49-pole wiggler beamline G1. The 20-fold improved flux over the previous beamline F2 provides higher sample throughput and autonomous X-ray scattering data collection using a unique SAXS/WAXS dual detectors configuration. This setup achieves a combined q-range from 0.007 to 0.7 Å(-1), enabling better characterization of smaller molecules, while opening opportunities for emerging wide-angle scattering methods. In addition, a facility upgrade of the positron storage ring to continuous top-up mode has improved beam stability and eliminated beam drift over the course of typical BioSAXS experiments. Single exposure times have been reduced to 2 s for 3.560 mg ml(-1) lysozyme with an average quality factor I/σ of 20 in the Guinier region. A novel disposable plastic sample cell design that incorporates lower background X-ray window material provides users with a more pristine sample environment than previously available. Systematic comparisons of common X-ray window materials bonded to the cell have also been extended to the wide-angle regime, offering new insight into best choices for various q-space ranges. In addition, a quantitative assessment of signal-to-noise levels has been performed on the station to allow users to estimate necessary exposure times for obtaining usable signals in the Guinier regime. Users also have access to a new BioSAXS sample preparation laboratory which houses essential wet-chemistry equipment and biophysical instrumentation. User experiments at the upgraded BioSAXS station have been on-going since commissioning of the beamline in Summer 2013. A planned upgrade of the G1 insertion device to an undulator for the Winter 2014 cycle is expected to further improve flux by an order of magnitude.

摘要

溶液中生物大分子的X射线散射是结构生物学中越来越受欢迎的工具,并且从现代高亮度同步辐射源中受益匪浅。升级后的麦克斯生物小角X射线散射站现位于49极摆动器光束线G1处。与之前的光束线F2相比,通量提高了20倍,使用独特的小角/广角X射线散射双探测器配置,可实现更高的样品通量和自主X射线散射数据采集。这种设置实现了从0.007到0.7 Å(-1)的组合q范围,能够更好地表征较小的分子,同时为新兴的广角散射方法提供了机会。此外,正电子储存环升级为连续注入模式,提高了光束稳定性,并消除了典型生物小角X射线散射实验过程中的光束漂移。对于浓度为3.560 mg/ml的溶菌酶,单次曝光时间已缩短至2 s,在吉尼埃区域的平均品质因数I/σ为20。一种采用低背景X射线窗口材料的新型一次性塑料样品池设计,为用户提供了比以前更纯净的样品环境。与样品池结合的常见X射线窗口材料的系统比较也已扩展到广角范围,为不同q空间范围的最佳选择提供了新的见解。此外,该站还对信噪比水平进行了定量评估,以便用户估计在吉尼埃区域获得可用信号所需的曝光时间。用户还可以使用一个新的生物小角X射线散射样品制备实验室,该实验室配备了基本的湿化学设备和生物物理仪器。自2013年夏季光束线调试以来,用户一直在升级后的生物小角X射线散射站进行实验。计划在2014年冬季将G1插入装置升级为波荡器,预计通量将进一步提高一个数量级。