scholarly journals A nearly on-axis spectroscopic system for simultaneously measuring UV–visible absorption and X-ray diffraction in the SPring-8 structural genomics beamline

2016 ◽  
Vol 23 (1) ◽  
pp. 334-338 ◽  
Author(s):  
Miyuki Sakaguchi ◽  
Tetsunari Kimura ◽  
Takuma Nishida ◽  
Takehiko Tosha ◽  
Hiroshi Sugimoto ◽  
...  

UV–visible absorption spectroscopy is useful for probing the electronic and structural changes of protein active sites, and thus the on-line combination of X-ray diffraction and spectroscopic analysis is increasingly being applied. Herein, a novel absorption spectrometer was developed at SPring-8 BL26B2 with a nearly on-axis geometry between the X-ray and optical axes. A small prism mirror was placed near the X-ray beamstop to pass the light only 2° off the X-ray beam, enabling spectroscopic analysis of the X-ray-exposed volume of a crystal during X-ray diffraction data collection. The spectrometer was applied to NO reductase, a heme enzyme that catalyzes NO reduction to N2O. Radiation damage to the heme was monitored in real time during X-ray irradiation by evaluating the absorption spectral changes. Moreover, NO binding to the heme was probedviacaged NO photolysis with UV light, demonstrating the extended capability of the spectrometer for intermediate analysis.

Author(s):  
Naveen Thakur ◽  
Nikesh Thakur ◽  
Viplove Bhullar ◽  
Saurabh Sharma ◽  
Aman Mahajan ◽  
...  

Abstract Titanium dioxide (TiO2) nanofibers were synthesized by electrospinning to optimize the photocatalytic action efficiency. The synthesis of the fibers was carried out at four different wt% concentrations: 8, 9, 10 & 11% of polymer polyvinylpyrrolidone (PVP). The TiO2 fibers were further calcined at 700 °C to get powder form. The uncalcinated and calcined TiO2 nanofibers were characterized by using X-Ray diffraction (XRD), Raman spectroscopy, Scanning electron microscopy (SEM) and UV-Visible spectroscopy. Raman spectroscopy confirmed the rutile phase of the calcined TiO2nanofibers in powder form with a crystallite size of 34–38 nm. The surface morphology of the uncalcinated and calcined TiO2 nanofibers was examined by SEM and the fiber diameter found to be 360–540 nm. The optical bandgap of the calcined TiO2 nanofibers was found in the range of 3.29–3.24 eV. The photocatalytic activity of the TiO2 nanofibers as examined for uncalcinated and calcined nanofibers, methyl orange (MO) dye degraded up to 98 and 78%, respectively in 180 min under the exposure of UV light. Uncalcinated TiO2 nanofibers were found more suitable for degradation of MO dye as compared to calcined nanofibers.


2019 ◽  
Vol 34 (3) ◽  
pp. 242-250 ◽  
Author(s):  
J. Anike ◽  
R. Derbeshi ◽  
W. Wong-Ng ◽  
W. Liu ◽  
D. Windover ◽  
...  

Structural characterization and X-ray reference powder pattern determination have been conducted for the Co- and Zn-containing tridymite derivatives Ba(Co1−xZnx)SiO4 (x = 0.2, 0.4, 0.6, 0.8). The bright blue series of Ba(Co1−xZnx)SiO4 crystallized in the hexagonal P63 space group (No. 173), with Z = 6. While the lattice parameter “a” decreases from 9.126 (2) Å to 9.10374(6) Å from x = 0.2 to 0.8, the lattice parameter “c” increases from 8.69477(12) Å to 8.72200(10) Å, respectively. Apparently, despite the similarity of ionic sizes of Zn2+ and Co2+, these opposing trends are due to the framework tetrahedral tilting of (ZnCo)O4. The lattice volume, V, remains comparable between 626.27 Å3 and 626.017 (7) Å3 from x = 0 to x = 0.8. UV-visible absorption spectrum measurements indicate the band gap of these two materials to be ≈3.3 and ≈3.5 eV, respectively, therefore potential UV photocatalytic materials. Reference powder X-ray diffraction patterns of these compounds have been submitted to be included in the Powder Diffraction File (PDF).


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Honghui Teng ◽  
Shukun Xu ◽  
Dandan Sun ◽  
Ying Zhang

Fe-doped TiO2nanotubes (Fe-TNTs) have been prepared by ultrasonic-assisted hydrothermal method. The structure and composition of the as-prepared TiO2nanotubes were characterized by transmission electron microscopy, X-ray diffraction, and UV-Visible absorption spectroscopy. Their photocatalytic activities were evaluated by the degradation of MO under visible light. The UV-visible absorption spectra of the Fe-TNT showed a red shift and an enhancement of the absorption in the visible region compared to the pure TNT. The Fe-TNTs were provided with good photocatalytic activities and photostability and under visible light irradiation, and the optimum molar ratio of Ti : Fe was found to be 100 : 1 in our experiments.


2012 ◽  
Vol 502 ◽  
pp. 164-168
Author(s):  
Ling Xu ◽  
Han Mei Hu ◽  
Hai Yan Xu

Novel mace-like (wolf-teeth clubs) CdS nanostructures were successfully prepared on a large scale using CdCl2•2.5H2O and NH2CSNH2 as starting materials through a convenient mixed-solvothermal route. The as-synthesized products were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDX), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and UV-visible absorption spectroscopy. The experimental results reveal that the morphology of CdS products was greatly affected by the volume ratio of anhydrous ethanol and distilled water. The possible mechanism for the formation of mace-like CdS nanostructures is simply discussed.


2012 ◽  
Vol 585 ◽  
pp. 224-227
Author(s):  
Anand Kumar ◽  
Ali Vazid ◽  
Sushil Kumar

Polyaniline (PANI) has been synthesized by chemical oxidative polymerization technique with potassium dichromate oxidant in aqueous hydrochloric acid medium. After polymerization, the polymer so prepared is doped with ferrous sulphate, a transition metal salt, with tetrahydrofuran and water as solvents. The undoped/doped samples were characterized by various techniques such as UV-visible spectroscopy, FTIR spectroscopy, X-ray diffraction and dc conductivity measurements. UV-visible absorption studies revealed the presence of cation/polaron transitions and the presence of direct optical transitions. FTIR studies provide information regarding structural changes in the backbone of PANI with doping concentration. X-ray diffraction patterns of powdered polymer composites showed amorphous nature as mostly conducting polymers exhibit. The dc conductivity of PANI-ferrous sulphate composites were measured by two probe method in pellet form at room temperature (300 K) and found to increase with temperature showing the semiconductor behavior of synthesized polymer composites


2021 ◽  
Author(s):  
Nejeh Hannachi ◽  
Thierry ROISNEL ◽  
Faouzi HLEL

Abstract A new non-centrosymmetricorganotin (IV) hybrid compoundC5H14N2 [SnCl6] 2H2O was determined by single crystal X-ray diffraction at 150(2) K. Its crystal structure was solved by single crystal X-ray diffraction reveling that compound crystallizes in the orthorhombic system with Pbca space group with the following lattice parameters: a = 12.1486 (15) Å, b= 15.4571 (17) Å, c = 16.7610 (18) Å with Z = 8. The bonding between inorganic and organic entities in the compounds is realized by hydrogen bonding O−H…O ,O−H…Cl , NH • • • Cl, N-H…Cl and O−H…Cl. Finally,UV-visible absorption measurements exhibit two absorption bands (226 nm and 262 nm).The optical band gap (Eg) is deduced to be 3.46 Ev.


2019 ◽  
Vol 14 (11) ◽  
pp. 1523-1531
Author(s):  
Manjit Kaur ◽  
Rakesh Dogra ◽  
Narinder Arora ◽  
Navjeet Sharma ◽  
Rajesh Kumar

AC transport properties and dielectric response of sandwich geometry (Ag/CuPc/Ag) of CuPc(CuPc) thin films deposited using thermal evaporation technique have been studied within frequency range 1 Hz–10 KHz and in temperature range 303–383 K. Scanning electron microscope (SEM) investigations of these films reveal fiber like morphology. Crystalline natures of CuPc films have been characterized using X-ray diffraction for different temperatures. The molecular orientations in films for different substrate temperatures have been confirmed by Raman spectroscopy. The optical band gaps calculated from the UV–Visible absorption spectra is found to lie in the range 3.01–3.15 eV. Electrical conductivity of CuPc films increases with increase of temperature. The hole mobility values of CuPc films at different temperatures have been calculated using negative differential susceptance (–ΔB) technique. Both capacitance and dielectric constant have been found to decrease with the increase of frequency and temperature.


2015 ◽  
Vol 1123 ◽  
pp. 227-232 ◽  
Author(s):  
Iqriah Kalim Susanto ◽  
Ardiansyah Taufik ◽  
Rosari Saleh

Nanocomposite Fe3O4-CuO-ZnO with different molar ratio of Fe3O4:CuO:ZnO were synthesized using sol-gel method and characterized by X-ray diffraction, energy dispersive X-ray spectroscopy, field emission scanning electron microscope, UV-visible diffuse reflectance spectroscopy and vibrating sample magnetometer. The characterization results manifested that the combination of Fe3O4, CuO and ZnO nanoparticles was successful. The photocatalytic activity of nanocomposite with the molar ratio of 1:1:5 was more effective in the degradation of methylene blue under UV light irradiation than pure Fe3O4, CuO, ZnO. The role of photoactive species involved in the photocatalytic reaction was studied and found that holes play the most important role in photodegradation of methylene blue.


2004 ◽  
Vol 60 (3) ◽  
pp. 315-324 ◽  
Author(s):  
M. A. Fernandes ◽  
D. C. Levendis

Structural changes that occur during the [2 + 2] photodimerization of the metastable α′-polymorph of ortho-ethoxy-trans-cinnamic acid at 293 K are presented here. Crystals of the α′-polymorph were first stabilized by exposing the α-polymorph to UV light for a short period of time at 343 K. The photodimerization reaction was then carried out at 293 K and observed in situ by single-crystal X-ray diffraction. The α′-polymorph contains three molecules in the asymmetric unit, labelled A, B and C, which are arranged to form two potential reaction sites. The intermolecular distance between the C=C bonds of molecules A and B (making up the AB site) is 3.6 Å, and these were observed to undergo photodimerization at 293 K. The corresponding distance between centrosymmetrically related C=C bonds in the CC site (made up of C molecules) is 4.6 Å, and these remain unreacted even after 60 h irradiation at 293 K. The crystal of the final product, which corresponds to a 66.7% conversion (only two out of three molecules in the asymmetric unit take part in the photodimerization reaction at 293 K), contains an ordered arrangement of the photodimer and unreacted monomer. The crystal retains many structural features of the original monomer crystal, including carboxylic acid hydrogen bonds and C—H...O interactions. Single-crystal X-ray diffraction was used to monitor changes in the unit-cell parameters, reacting molecules and molecular conformations as the reaction progressed. The conformation of the photodimer obtained from the solid-state reaction differs from that of the photodimer obtained by recrystallization from solution.


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