scholarly journals Progress of robotized systems for crystallography for beamlines and laboratories

2014 ◽  
Vol 70 (a1) ◽  
pp. C788-C788
Author(s):  
Jean-Luc Ferrer ◽  
Xavier Vernede ◽  
Yoann Sallaz-Damaz ◽  
Christophe Berzin ◽  
Michel Pirocchi ◽  
...  

Development of 6-axis robotic arm based systems for protein crystallography automation is now expending rapidly. From the seminal work accomplished on beamline FIP-BM30A (ESRF) in 2000' to the present developments, robot based systems significantly changed the crystallography experiment strategy. They open possibilities for new strategies, give a high flexibility to the experimental setup, and make automation and remote control much easier. The robotized platform on which are based our present developments, named G-Rob, plays as a fully integrated, multi-purpose automated and remotely controlled diffractometer for beamlines and laboratories. G-Rob integrates several functions: classical sample changer; goniometer for frozen samples or capillaries [1], including frozen sample transfer from a storage Dewar; crystallization trays handling for in situ screening and data collection on crystallization plates and microchips [2]; powder diffraction; beam monitoring; on line crystal fluorescence/absorption; crystal harvesting; Etc. Thanks to its tool changer, the robot arm can go automatically from one application to another. G-Rob can be easily upgraded with new functions. Several G-Rob systems, both at synchrotrons (ESRF, LNLS, BNL) or as laboratory in-house systems (EPFL, CBS) are now available for the crystallography community. Among the last results obtained with G-Rob are: (i) Automated structure resolution at room temperature, for the analysis of protein dynamic; (ii) Automated structural screening for the fragment based drug design strategy. New functions are also under development, such as the remote controlled robotized crystal harvesting [3]. Such manipulations of individual crystals with the robot closes the gap for fully remote, and in the future fully automated, operation of crystallography pipeline.

2009 ◽  
Vol 42 (6) ◽  
pp. 1206-1208 ◽  
Author(s):  
D. Lian ◽  
I. P. Swainson ◽  
L. M. D. Cranswick ◽  
R. Donaberger

Inexpensive model robots are a viable option for automation of simple, repetitive tasks and can be solutions when space restriction and funding are issues, both factors that may eliminate more advanced robots from consideration. A simple-to-program, inexpensive robotic arm has been integrated in a sample changer for room-temperature experiments on a neutron powder diffractometer. In spite of the limited precision inherent in a model, servo-controlled robot, a very reproducible overall system can be made. Simple `tricks' such as incorporating self-centering mechanisms,e.g.mechanically self-centering designs and magnets, can produce central forces that eliminate the need for high precision from the robot arm.


1996 ◽  
Vol 429 ◽  
Author(s):  
N. I. Morimoto ◽  
J. W. Swart

AbstractA single wafer cluster tool was developed. It is composed of a central robot arm wafer handler and three processing chambers: a RF PECVD chamber, a microwave after glow RPECVD chamber and a rapid thermal annealing chamber. The tool is designed to allow high flexibility, with in-situ multi-sequential processing capability. An in depth study of the deposition of silicon oxide by PECVD was performed. As unique features, it handles TEOS vapor without a carrier gas and it includes a double stage gas distribution system. The films were characterized by means of: ellipsometry, FTIRS, RBS, AES, SIMS, stress and etch rate in diluted (1:100) HF solution. Good uniformity (>98 %) was obtained. The results show that the quality of the films is most influenced by the wafer temperature and flux of oxygen. For the best condition, the following results were obtained: deposition rate of 370 nm/min., refraction index of 1.46, stoichiometry of 2.0, intrinsic stress of 1.3×109 dyn/cm2, carbon content below the AES and SIMS detection limit and low OH content. We also propose a model that fits our results.


Author(s):  
César D. Fermin ◽  
Dale Martin

Otoconia of higher vertebrates are interesting biological crystals that display the diffraction patterns of perfect crystals (e.g., calcite for birds and mammal) when intact, but fail to produce a regular crystallographic pattern when fixed. Image processing of the fixed crystal matrix, which resembles the organic templates of teeth and bone, failed to clarify a paradox of biomineralization described by Mann. Recently, we suggested that inner ear otoconia crystals contain growth plates that run in different directions, and that the arrangement of the plates may contribute to the turning angles seen at the hexagonal faces of the crystals.Using image processing algorithms described earlier, and Fourier Transform function (2FFT) of BioScan Optimas®, we evaluated the patterns in the packing of the otoconia fibrils of newly hatched chicks (Gallus domesticus) inner ears. Animals were fixed in situ by perfusion of 1% phosphotungstic acid (PTA) at room temperature through the left ventricle, after intraperitoneal Nembutal (35mg/Kg) deep anesthesia. Negatives were made with a Hitachi H-7100 TEM at 50K-400K magnifications. The negatives were then placed on a light box, where images were filtered and transferred to a 35 mm camera as described.


Author(s):  
C. Jennermann ◽  
S. A. Kliewer ◽  
D. C. Morris

Peroxisome proliferator-activated receptor gamma (PPARg) is a member of the nuclear hormone receptor superfamily and has been shown in vitro to regulate genes involved in lipid metabolism and adipocyte differentiation. By Northern analysis, we and other researchers have shown that expression of this receptor predominates in adipose tissue in adult mice, and appears first in whole-embryo mRNA at 13.5 days postconception. In situ hybridization was used to find out in which developing tissues PPARg is specifically expressed.Digoxigenin-labeled riboprobes were generated using the Genius™ 4 RNA Labeling Kit from Boehringer Mannheim. Full length PPAR gamma, obtained by PCR from mouse liver cDNA, was inserted into pBluescript SK and used as template for the transcription reaction. Probes of average size 200 base pairs were made by partial alkaline hydrolysis of the full length transcripts. The in situ hybridization assays were performed as described previously with some modifications. Frozen sections (10 μm thick) of day 18 mouse embryos were cut, fixed with 4% paraformaldehyde and acetylated with 0.25% acetic anhydride in 1.0M triethanolamine buffer. The sections were incubated for 2 hours at room temperature in pre-hybridization buffer, and were then hybridized with a probe concentration of 200μg per ml at 70° C, overnight in a humidified chamber. Following stringent washes in SSC buffers, the immunological detection steps were performed at room temperature. The alkaline phosphatase labeled, anti-digoxigenin antibody and detection buffers were purchased from Boehringer Mannheim. The sections were treated with a blocking buffer for one hour and incubated with antibody solution at a 1:5000 dilution for 2 hours, both at room temperature. Colored precipitate was formed by exposure to the alkaline phosphatase substrate nitrobluetetrazoliumchloride/ bromo-chloroindlylphosphate.


Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  

Remote on-line electron microscopy is rapidly becoming more available as improvements continue to be developed in the software and hardware of interfaces and networks. Scanning electron microscopes have been driven remotely across both wide and local area networks. Initial implementations with transmission electron microscopes have targeted unique facilities like an advanced analytical electron microscope, a biological 3-D IVEM and a HVEM capable of in situ materials science applications. As implementations of on-line transmission electron microscopy become more widespread, it is essential that suitable standards be developed and followed. Two such standards have been proposed for a high-level protocol language for on-line access, and we have proposed a rational graphical user interface. The user interface we present here is based on experience gained with a full-function materials science application providing users of the National Center for Electron Microscopy with remote on-line access to a 1.5MeV Kratos EM-1500 in situ high-voltage transmission electron microscope via existing wide area networks. We have developed and implemented, and are continuing to refine, a set of tools, protocols, and interfaces to run the Kratos EM-1500 on-line for collaborative research. Computer tools for capturing and manipulating real-time video signals are integrated into a standardized user interface that may be used for remote access to any transmission electron microscope equipped with a suitable control computer.


2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.


2020 ◽  
Vol 74 (11) ◽  
pp. 866-870
Author(s):  
Lewis C. H. Maddock ◽  
Alan Kennedy ◽  
Eva Hevia

While fluoroaryl fragments are ubiquitous in many pharmaceuticals, the deprotonation of fluoroarenes using organolithium bases constitutes an important challenge in polar organometallic chemistry. This has been widely attributed to the low stability of the in situ generated aryl lithium intermediates that even at –78 °C can undergo unwanted side reactions. Herein, pairing lithium amide LiHMDS (HMDS = N{SiMe3}2) with FeII(HMDS)2 enables the selective deprotonation at room temperature of pentafluorobenzene and 1,3,5-trifluorobenzene via the mixed-metal base [(dioxane)LiFe(HMDS)3] (1) (dioxane = 1,4-dioxane). Structural elucidation of the organometallic intermediates [(dioxane)Li(HMDS)2Fe(ArF)] (ArF = C6F5, 2; 1,3,5-F3-C6H2, 3) prior electrophilic interception demonstrates that these deprotonations are actually ferrations, with Fe occupying the position previously filled by a hydrogen atom. Notwithstanding, the presence of lithium is essential for the reactions to take place as Fe II (HMDS)2 on its own is completely inert towards the metallation of these substrates. Interestingly 2 and 3 are thermally stable and they do not undergo benzyne formation via LiF elimination.


2021 ◽  
Author(s):  
Ruixue Zhang ◽  
Wanying Zhao ◽  
Zhenzhen Liu ◽  
Shanghai Wei ◽  
Yigang Yan ◽  
...  

In situ formed amorphous LiBH4·1/2NH3 on the surface of Al2O3 nanoparticles results in an enhanced ion conductivity of 1.1 × 10−3 S cm−1 at room temperature.


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