scholarly journals A Novel Method to Maintain the Sample Position and Pressure in Differentially Pumped Systems Below the Resolution Limit of Optical Microscopy Techniques

2020 ◽  
pp. 000370282094279
Author(s):  
Christopher M. Goodwin ◽  
John D. Alexander ◽  
Matthew Weston ◽  
David Degerman ◽  
Mikhail Shipilin ◽  
...  

We present a new method to maintain constant gas pressure over a sample during in situ measurements. The example shown here is a differentially pumped high-pressure X-ray photoelectron spectroscopy system, but this technique could be applied to many in situ instruments. By using the pressure of the differential stage as a feedback source to change the sample position, a new level of consistency has been achieved. Depending on the absolute value of the sample-to-aperture distance, this technique allows one to maintain the distance within several hundred nanometers, which is below the limit of typical optical microscopy systems. We show that this method is well suited to compensate for thermal drift. Thus, X-ray photoelectron spectroscopy data can be acquired continuously while the sample is heated and maintaining constant pressure over the sample. By implementing a precise manipulator feedback system, pressure variations of less than 5% were reached while the temperature was varied by 400 ℃. The system is also shown to be highly stable under significant changes in gas flow. After changing the flow by a factor of two, the pressure returned to the set value within 60 s.

2021 ◽  
Vol 4 (1) ◽  
Author(s):  
Marc Benjamin Hahn ◽  
Paul M. Dietrich ◽  
Jörg Radnik

AbstractIonizing radiation damage to DNA plays a fundamental role in cancer therapy. X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. The results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further.


2021 ◽  
pp. 150898
Author(s):  
Makoto Takayanagi ◽  
Takashi Tsuchiya ◽  
Shigenori Ueda ◽  
Tohru Higuchi ◽  
Kazuya Terabe

2014 ◽  
Vol 70 (a1) ◽  
pp. C500-C500
Author(s):  
Yusuke Yamada ◽  
Naohiro Matsugaki ◽  
Masahiko Hiraki ◽  
Ryuichi Kato ◽  
Toshiya Senda

Crystallization trial is one of the most important but time-consuming steps in macromolecular crystallography. Once a crystal appears in a certain crystallization condition, the crystal is typically harvested from the crystallization drop, soaked into a cryoprotection buffer, flash-cooled with a liquid nitrogen or cold gas flow and finally evaluated its diffraction quality by an X-ray beam. During these long process, crystal may be damaged and the result from the diffraction experiment does not necessarily reflect a nature of the crystal. On in-situ diffraction experiment, where a crystal in a crystallization drop is directly irradiated to an X-ray beam, a diffraction image from a crystal without any external factors such as harvesting and cryoprotection and, as a result, a nature of crystal can be evaluated quickly. In the Photon Factory, a new table-top diffractometer for in-situ diffraction experiments has been developed. It consists of XYZ translation stages with a plate handler, on-axis viewing system with a large numeric aperture and a plate rack where ten crystallization plates can be placed. These components sit on a common plate and it is placed on the existing diffractometer table in the beamline endstation. The CCD detector with a large active area and a pixel array detector with a small active area are used for acquiring diffraction images from crystals. Dedicated control software and user interface were also developed. Since 2014, user operation of the new diffractometer was started and in-situ diffraction experiments were mainly performed for evaluations of crystallization plates from a large crystallization screening project in our facility. BL-17A [1], one of micro-focus beamlines at the Photon Factory, is planned to be upgraded in March 2015. With this upgrade, a new diffractometer, which has a capability to handle a crystallization plate, will be installed so that diffraction data sets from crystals in crystallization drop can be collected.


1999 ◽  
Vol 567 ◽  
Author(s):  
Masayuki Suzuki ◽  
Yoji Saito

ABSTRACTWe tried direct oxynitridation of silicon surfaces by remote-plasma-exited nitrogen and oxygen gaseous mixtures at 700°C in a high vacuum. The oxynitrided surfaces were investigated with in-situ X-ray photoelectron spectroscopy. With increase of the oxynitridation time, the surface density of nitrogen gradually increases, but that of oxygen shows nearly saturation behavior after the rapid increase in the initial stage. We also annealed the grown oxynitride and oxide films to investigate the role of the contained nitrogen. The desorption rate of oxygen from the oxynitride films is much less than that from oxide films. We confirmed that nitrogen stabilizes the thermal stability of these oxynitride films.


2016 ◽  
Vol 55 (8S2) ◽  
pp. 08PC02 ◽  
Author(s):  
Antonio T. Lucero ◽  
Young-Chul Byun ◽  
Xiaoye Qin ◽  
Lanxia Cheng ◽  
Hyoungsub Kim ◽  
...  

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