scholarly journals Soft x-ray absorption spectroscopy of metalloproteins and high-valent metal-complexes at room temperature using free-electron lasers

2017 ◽  
Vol 4 (5) ◽  
pp. 054307 ◽  
Author(s):  
Markus Kubin ◽  
Jan Kern ◽  
Sheraz Gul ◽  
Thomas Kroll ◽  
Ruchira Chatterjee ◽  
...  
2019 ◽  
Vol 26 (1) ◽  
pp. 1-10 ◽  
Author(s):  
Bangjie Deng ◽  
Jiawei Yan ◽  
Qingmin Zhang ◽  
Yaodong Sang ◽  
Haixiao Deng

X-ray free-electron lasers (XFELs) have been widely used for applications such as X-ray crystallography and magnetic spin probes because of their unprecedented performance. Recently, time-resolved X-ray magnetic circular dichroism (XMCD) with ultrafast XFEL pulses have made it possible to achieve an instantaneous view of atomic de-excitation. However, owing to the narrow bandwidth and coherence of XFELs, X-ray absorption spectroscopy (XAS) and XMCD are time- and effort-consuming for both machine scientists and users of XFELs. In this work, an efficient scheme using a broadband XFEL pulse and single-shot X-ray spectrometer is proposed, in which the XAS and XMCD measurements can be accomplished with the same machine conditions. An evolutionary multi-objective optimization algorithm is used to maximize the XFEL bandwidth offered by the Shanghai Soft X-ray FEL user facility without additional hardware. A numerical example using MnO is demonstrated, showing that, by using approximately 1000 consecutive XFEL shots with a central photon energy of 650 eV and full bandwidth of 4.4%, precise spectral measurements for XAS and XMCD can be achieved. Additional considerations related to single-shot XAS and XMCD are discussed.


2014 ◽  
Vol 369 (1647) ◽  
pp. 20130337 ◽  
Author(s):  
Uwe Weierstall

X-ray free-electron lasers overcome the problem of radiation damage in protein crystallography and allow structure determination from micro- and nanocrystals at room temperature. To ensure that consecutive X-ray pulses do not probe previously exposed crystals, the sample needs to be replaced with the X-ray repetition rate, which ranges from 120 Hz at warm linac-based free-electron lasers to 1 MHz at superconducting linacs. Liquid injectors are therefore an essential part of a serial femtosecond crystallography experiment at an X-ray free-electron laser. Here, we compare different techniques of injecting microcrystals in solution into the pulsed X-ray beam in vacuum. Sample waste due to mismatch of the liquid flow rate to the X-ray repetition rate can be addressed through various techniques.


2012 ◽  
Vol 111 (1) ◽  
pp. 013715 ◽  
Author(s):  
P. Srivastava ◽  
S. Ghosh ◽  
B. Joshi ◽  
P. Satyarthi ◽  
P. Kumar ◽  
...  

2009 ◽  
Vol 6 (3) ◽  
pp. 268 ◽  
Author(s):  
Hsin-Liang Huang ◽  
H. Paul Wang ◽  
Edward M. Eyring ◽  
Juu-En Chang

Environmental context. Very fine phosphor ashes are discharged from particulate collection systems (such as bag houses) in the cathode ray tube or television disassembling processes. Effective recovery of ZnO and ZnS nanoparticles from the phosphor ash can be achieved by extraction with a room temperature ionic liquid. By synchrotron radiation X-ray absorption spectroscopy, the obtained molecular scale data turn out to be very useful in revealing speciation of zinc in the extraction process, which also facilitates the development of a simple nanoparticle recovery method. Abstract. An effective, simple method has been developed for the recovery of ZnO and ZnS nanoparticles from hazardous phosphor ash waste. Experimentally, zinc (77%) in the phosphor ash (that contains mainly zinc (91%)) can be recovered by extraction with a room temperature ionic liquid (RTIL) ([C4mim][PF6], 1-butyl-3-methylimidazolium hexafluorophosphate). Component fitted X-ray absorption near edge structure (XANES) spectra of zinc indicate that metallic zinc (Zn) (9%) in the phosphor ash can be dissolved to form a Zn2+–1-methylimidazole ([mim]) complex during extraction with the RTIL. ZnS and ZnO nanoparticles (60–61%) can also be extracted from the phosphor. Over the 298–523 K temperature range, desired ZnO/ZnS ratios (0.3–0.6) can be obtained since interconversion of ZnS to ZnO in the RTIL is temperature dependent. The Fourier transformed extended X-ray absorption fine structure (EXAFS) data also show that the nanosize ZnS extracted in the RTIL possesses a Zn–S bond distance of 2.33 Å with coordination numbers (CNs) of 3.6–3.7. At 523 K, in the RTIL, ~30% of the ZnS is oxidised to form octahedral ZnO (with a bond distance of 2.10 Å and a CN of 6.1) that may coat the surfaces of the ZnS nanoparticles. This work exemplifies the utilisation of X-ray absorption spectroscopy (EXAFS and XANES) to reveal speciation and possible reaction pathways in a nanoparticle extraction process (with a RTIL) in detail.


2009 ◽  
Vol 95 (13) ◽  
pp. 134102 ◽  
Author(s):  
D. P. Bernstein ◽  
Y. Acremann ◽  
A. Scherz ◽  
M. Burkhardt ◽  
J. Stöhr ◽  
...  

2014 ◽  
Vol 98 (4) ◽  
pp. 1156-1161 ◽  
Author(s):  
Iuliia Mikulska ◽  
Matjaz Valant ◽  
Iztok Arčon ◽  
Darja Lisjak

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