Synthesis and characterization of a new trimetallic compound (NH4)Ni2.4Co0.6O(OH)(MoO4)2•1.5H2O

2014 ◽  
Vol 29 (4) ◽  
pp. 379-382 ◽  
Author(s):  
Sandra Amaya ◽  
Johana Arboleda ◽  
Adriana Echavarría

A new trimetallic compound with formula (NH4)Ni2.4Co0.6O(OH)(MoO4)2•1.5H2O was obtained by hydrothermal synthesis. The solid was characterized by X-ray diffraction, thermal analysis (thermogravimetric analysis and differential thermal analysis), Fourier-transformed infrared spectroscopy, Laser Raman spectroscopy, and chemical analysis by atomic absorption, confirming the formation of the layered phase ϕy. Crystallographic studies showed that the compound obtained is trigonal with hexagonal unit-cell parameters, a = 6.0468 ± 0.0016 Å and c = 21.8433 ± 0.0001 Å, and space group R-3m.

2017 ◽  
Vol 72 (9) ◽  
pp. 677-685
Author(s):  
Teresa S. Ortner ◽  
Hubert Huppertz

AbstractThe praseodymium borate-nitrate Pr[B5O8(OH)(H2O)0.87]NO3·2H2O was obtained in a hydrothermal synthesis. It crystallizes monoclinically in the space groupP21/n(no. 14) with four formula units (Z=4) and unit cell parameters ofa=641.9(3),b=1551.8(7),c=1068.4(5) pm, withβ=90.54(2)° yieldingV=1.0643(8) nm3. The defect variant constitutes the missing member in the series of isostructural, early rare earth borate-nitrates of the compositionRE[B5O8(OH)(H2O)x]NO3·2H2O [RE=La (x=0; 1), Ce (x=1), Nd (x=0.85), Sm (x=0)]. In addition to powder and single-crystal X-ray diffraction data, the novel borate-nitrate was characterized through IR and Raman spectroscopy.


Crystals ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 812
Author(s):  
Noura Othman Alzamil ◽  
Ghareeba Mussad Al-Enzi ◽  
Aishah Hassan Alamri ◽  
Insaf Abdi ◽  
Amor BenAli

Two new nonmetal cation tetrafluoroborate phases [H3tren](BF4)3 (I) and [H3tren](BF4)3 HF (II) were synthesized by microwave-assisted solvothermal and characterized by single crystal X-ray diffraction, IR spectroscopy and thermal analysis DTA-TGA. [H3tren](BF4)3 is cubic (P213) with unit cell parameter a = 11.688(1) Å. [H3tren](BF4)3•HF is trigonal (R3c) with unit cell parameters a = 15.297(6) Å and c = 12.007(2) Å. Both (I) and (II) structures can be described from isolated tetrafluoroborate BF4- anions, triprotonated tris-(2-aminoethyl)amine (tren) [H3tren]3+. Phase (II) contains disordered BF4- tetrahedron and hydrofluoric acid.


1998 ◽  
Vol 12 (11) ◽  
pp. 427-431
Author(s):  
K. Jeyabalan ◽  
L. K. Kaliyaperumal ◽  
A. Sekar ◽  
J. Srinivas

Synthesis and characterization of A 2 CaCuO 5( A=Nd, Sm ) system is reported. Powder X-ray diffraction analysis shows that the compounds crystallizes in an orthorhombic crystal systems and the unit cell parameters are found to be a=6.399(9)Å, b=7.218(8) Å and c=12.167(17) Å for Nd 2 CaCuO 5 and a=5.872(8) Å, b=7.457(3) Å and c=12.682(18) Å for Sm 2 CaCuO 5.


2000 ◽  
Vol 55 (9) ◽  
pp. 882-886 ◽  
Author(s):  
Martin Jansen ◽  
Sascha Vensky

The silver(I,II,III) oxide clathrate Ag7O8HCO3 was synthesized by anodic oxidation of silver(I) in a suspension of Ag2CO3 in an aqueous AgF solution. The title compound was characterized by single crystal X-ray diffraction (cubic, Fm3̄m, a = 9.8085(3) Å, Z = 4), scanning electron microscopy, thermal analysis, IR spectroscopy, 1H-solid state-NMR and measurement of the magnetic susceptibility


Science ◽  
2017 ◽  
Vol 355 (6323) ◽  
pp. 374-376 ◽  
Author(s):  
Chong Zhang ◽  
Chengguo Sun ◽  
Bingcheng Hu ◽  
Chuanming Yu ◽  
Ming Lu

Pentazole (HN5), an unstable molecular ring comprising five nitrogen atoms, has been of great interest to researchers for the better part of a century. We report the synthesis and characterization of the pentazolate anion stabilized in a (N5)6(H3O)3(NH4)4Cl salt. The anion was generated by direct cleavage of the C–N bond in a multisubstituted arylpentazole using m-chloroperbenzoic acid and ferrous bisglycinate. The structure was confirmed by single-crystal x-ray diffraction analysis, which highlighted stabilization of the cyclo-N5ˉ ring by chloride, ammonium, and hydronium. Thermal analysis indicated the stability of the salt below 117°C on the basis of thermogravimetry-measured onset decomposition temperature.


Crystals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 466
Author(s):  
Loisangela Álvarez ◽  
Blanca Rojas de Gascue ◽  
Rolando J. Tremont ◽  
Edgar Márquez ◽  
Euclides J. Velazco

A new compound, Bi2O2CO3:Al, was synthesized by the coprecipitation method. The characterization was done by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), electronic scanning microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). The characterization methods allowed to identify the Bi2O2CO3:Al compound, such as the Al-doped Bi2O2CO3 by XRD, the anionic part (CO32−) by FTIR, and the presence of aluminum in the compound by XPS and EDX. It was confirmed to have a nanostructure like a nanosheet and a microstructure that resembles a type sponge by SEM.


2018 ◽  
Vol 83 (02) ◽  
pp. 181-190
Author(s):  
Ian E. Grey ◽  
Erich Keck ◽  
Anthony R. Kampf ◽  
John D. Cashion ◽  
Colin M. MacRae ◽  
...  

AbstractSchmidite, Zn(Fe3+0.5Mn2+0.5)2ZnFe3+(PO4)3(OH)3(H2O)8 and wildenauerite, Zn(Fe3+0.5Mn2+0.5)2Mn2+Fe3+(PO4)3(OH)3(H2O)8 are two new oxidised schoonerite-group minerals from the Hagendorf-Süd pegmatite, Hagendorf, Oberpfalz, Bavaria, Germany. Schmidite occurs as radiating sprays of orange–brown to copper-red laths on and near to altered phosphophyllite in a corroded triphylite nodule, whereas wildenauerite forms dense compacts of red laths, terminating Zn-bearing rockbridgeite. The minerals are biaxial (+) with α = 1.642(2), β = 1.680(1), γ = 1.735(2) and 2Vmeas = 81.4(8)° for schmidite, and with α = 1.659(3), β = 1.687(3), γ = 1.742(3) and 2Vmeas = 73(1)° for wildenauerite. Electron microprobe analyses, with H2O from thermal analysis and FeO/Fe2O3 from Mössbauer spectroscopy, gave FeO 0.4, MgO 0.3, Fe2O3 23.5, MnO 9.0, ZnO 15.5, P2O5 27.6, H2O 23.3, total 99.6 wt.% for schmidite, and FeO 0.7, MgO 0.3, Fe2O3 25.2, MnO 10.7, ZnO 11.5, P2O5 27.2, H2O 24.5, total 100.1 wt.% for wildenauerite. The empirical formulae, scaled to 3 P and with OH– adjusted for charge balance are Zn1.47Mn2+0.98Mg0.05Fe2+0.04Fe3+2.27(PO4)3(OH)2.89(H2O)8.54 for schmidite and Zn1.11Mn2+1.18Mg0.05Fe2+0.08Fe3+2.47(PO4)3(OH)3.25(H2O)9.03 for wildenauerite. The two minerals have orthorhombic symmetry, space group Pmab and Z = 4. The unit-cell parameters from refinement of powder X-ray diffraction data are a = 11.059(1), b = 25.452(1) and c = 6.427(1) Å for schmidite, and a = 11.082(1), b = 25.498(2) and c = 6.436(1) Å for wildenauerite. The crystal structures of schmidite and wildenauerite differ from that of schoonerite in having minor partitioning of Zn from the [5]Zn site to an adjacent vacant tetrahedral site [4]Zn, separated by ~1.0 Å from [5]Zn. The two minerals are distinguished by the cation occupancies in the octahedral M1 to M3 sites. Schmidite has M1 = M2 = (Fe3+0.5Mn2+0.5) and M3 = Zn and wildenauerite has M1 = M2 = (Fe3+0.5Mn2+0.5) and M3 = Mn2+.


2014 ◽  
Vol 70 (10) ◽  
pp. 1372-1375 ◽  
Author(s):  
Shanghua Fan ◽  
Defeng Li ◽  
Joy Fleming ◽  
Yuan Hong ◽  
Tao Chen ◽  
...  

7-Keto-8-aminopelargonic acid synthase (KAPA synthase; BioF) is an essential enzyme for mycobacterial growth that catalyses the first committed step in the biotin-synthesis pathway. It is a pyridoxal 5′-phosphate (PLP)-dependent enzyme and is a potential drug target. Here, the cloning, expression, purification and crystallization of KAPA synthase fromMycobacterium smegmatis(MsBioF) and the characterization of MsBioF crystals using X-ray diffraction are described. The crystals diffracted to 2.3 Å resolution and belonged to the monoclinic space groupP21, with unit-cell parametersa= 70.88,b= 91.68,c= 109.84 Å, β = 97.8°. According to the molecular weight of MsBioF, the unit-cell parameters and the self-rotation function map, four molecules are present in each asymmetric unit with aVMvalue of 2.06 Å3 Da−1and a solvent content of 40.20%.


e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Ku Marsilla Ku Ishak ◽  
Zulkifli Ahmad ◽  
Hazizan Md Akil

AbstractChitosan was chemically modified with bulky structure, cis-5- norbornene-2,3-dicarboxylic anhydride and the characteristics of this modified chitosan was studied. Fourier Transform Infrared results show that the anhydride monomer was successfully bound to amine group of chitosan. Thermal analysis of the modified structure provides N-acylated chitosan with improved thermal stability whereas X-ray Diffraction Analysis reveals reduction in crystallinity level after modification. Scanning Electron Microscope micrograph shows the physical nature and microstructure of N-acylated chitosan with less agglomeration


2019 ◽  
Vol 70 (11) ◽  
pp. 3931-3934
Author(s):  
Irina Fierascu ◽  
Raluca Somoghi ◽  
Cristian Andi Nicolae ◽  
Nicolae Stanica ◽  
Radu Claudiu Fierascu

An inorganic/organic magnetic nanocomposite was synthesized and analytically characterized using X-ray fluorescence, X-ray diffraction, transmission electron microscopy and thermal analysis. The evaluation of the magnetic properties revealed that both the magnetite and the magnetite/chitosan nanocomposite are superparamagnetic with a paramagnetic component, having the saturation magnetization values of 48.04 emu/g, and 41.3 emu/g, respectively. The synthesized material is indented for the adsorption of two known commercial-available pesticides (active ingredients deltamethrin and thiamethoxam, respectively) from aqueous solutions.


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