Solid-Solid Synthesis, Characterization and Thermal Decomposition of Thiourea Complex of Antimony Trichloride

2012 ◽  
Vol 549 ◽  
pp. 126-130
Author(s):  
Guo Qing Zhong ◽  
Mei Gu ◽  
Yu Qing Jia
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Liquid State ◽  
Antimony Trichloride ◽  
Solid Complex ◽  
Solid Reaction ◽  
Thermal Decomposition Process ◽  
Monoclinic System ◽  
Thiourea Complex ◽  
Percentage Mass Loss

The solid complex of antimony trichloride with thiourea was synthesized by solid-solid reaction or liquid state reaction of antimony trichloride and thiourea. The formula of solid complex is all SbCl3[CS(NH2)2]3. The crystal structure of the complex belongs to monoclinic system and the lattice parameters are: a = 1.2426 nm, b = 1.6396 nm, c = 1.9254 nm and β = 96.24° for solid-solid reaction, and a = 1.2343 nm, b = 1.6585 nm, c = 1.9252 nm and β = 96.46° for liquid state reaction, respectively. The infrared spectra reveal that antimony ion in the complex is coordinated only by the sulfur atom of CS(NH2)2. The possible pyrolysis reactions in the thermal decomposition process of the complex, the experimental and calculated percentage mass loss were also given.

scholarly journals Solid-solid synthesis, characterization and thermal decomposition of a homodinuclear cobalt(II) complex

2015 ◽  
Vol 80 (11) ◽  
pp. 1391-1397 ◽  
Author(s):  
Di Li ◽  
Guo-Qing Zhong ◽  
Zhi-Xian Wu
Keyword(s):  
Thermal Decomposition ◽  
Raw Materials ◽  
Uv Spectra ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Monoclinic System ◽  
X Ray ◽  
Decomposition Processes ◽  
Elemental Analyses ◽  
Percentage Mass Loss

The homodinuclear cobalt(II) complex [Co2(dipic)2(H2O)5]?2H2O was synthesized with pyridine-2,6-dicarboxylic acid (H2dipic) and cobalt(II) acetate as raw materials by room temperature solid-solid reaction. The complex was characterized by elemental analyses, single crystal X-ray diffraction, X-ray powder diffraction, Fourier transform infrared spectroscopy, UV spectra, and thermogravimetry and differential scanning calorimetry. Its crystal structure belongs to monoclinic system and space group P2(1)/c. There are two types of the Co(II) ions, and they are all six-coordination, one Co(II) is coordinated by four carboxyl O atoms and two pyridine N atoms from two dipic2- anions, and another Co(II) is coordinated by five O atoms from five H2O molecules and one bridged carboxyl O atom from the dipic2- anion. The possible pyrolysis reactions in the thermal decomposition processes of the complex, the experimental and calculated percentage mass loss are also given.

scholarly journals Synthesis, Crystal Structure, and Thermal Decomposition of the Cobalt(II) Complex with 2-Picolinic Acid

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Di Li ◽  
Guo-Qing Zhong
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Picolinic Acid ◽  
Cobalt Acetate ◽  
Distorted Octahedral Geometry ◽  
Scanning Calorimetry ◽  
Monoclinic System ◽  
Cell Parameters ◽  
Composition And Structure ◽  
Final Residue

The cobalt(II) complex of 2-picolinic acid (Hpic), namely,[Co(pic)2(H2O)2]·2H2O, was synthesized with the reaction of cobalt acetate and 2-picolinic acid as the reactants by solid-solid reaction at room temperature. The composition and structure of the complex were characterized by elemental analysis, infrared spectroscopy, single crystal X-ray diffraction, and thermogravimetry-differential scanning calorimetry (TG-DSC). The crystal structure of the complex belongs to monoclinic system and space groupP2(1)/n, with cell parameters ofa=9.8468(7) Å,b=5.2013(4) Å,c=14.6041(15) Å,β=111.745(6)°,V=747.96(11) Å3,Z=2,Dc=1.666 g cm−3,R1=0.0297, andwR2=0.0831. In the title complex, the Co(II) ion is six-coordinated by two pyridine N atoms and two carboxyl O atoms from two 2-picolinic acid anions, and two O atoms from two H2O molecules, and forming a slightly distorted octahedral geometry. The thermal decomposition processes of the complex under nitrogen include dehydration and pyrolysis of the ligand, and the final residue is cobalt oxalate at about 450°C.

Synthesis, Crystal Structure and Thermal Decomposition of a New Energetic Potassium Salt of dihydridobis(3-nitro-1,2,4-triazolyl) Borate

2020 ◽  
Vol 24 (9) ◽  
pp. 1042-1047
Author(s):  
Wang Guodong ◽  
Liu Yucun ◽  
Liu Guoqing ◽  
Jing Suming ◽  
Liao Longyu
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Potassium Salt ◽  
X Ray Diffraction ◽  
Ozawa Method ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Parameters ◽  
Potassium Borohydride ◽  
Crystal Density

A new energetic organic potassium salt of dihydridobis (3-nitro-1,2,4-triazolyl) borate was synthesized from 3-nitro-1,2,4-triazole and potassium borohydride at 110 °C, and structurally characterized by elemental analysis, IR spectra, 13C NMR and singlecrystal X-ray diffraction. Results show that the crystal belongs to monoclinic system with space group of p21 / C and cell parameters of a = 10.335 (8) Å, B = 10.812 (8) Å, C = 9.821 (8) Å, α = 90 ˚, β = 106.470 (13), γ = 90 °, z = 4. Its crystal density is 1.755g/cm3. Thermal properties were studied with TG-DTA and DSC. There was only one sharp decomposition peak temperature of 270 °C at the heating rate of 10 °C/ min-1. The activation energies EK = 48.0kJ/mol-1 and EO = 49.8kJ/mol-1 were calculated by the Kissinger method and Ozawa method respectively (CCDC: 1975139).

ChemInform Abstract: BaN3Cl: Synthesis, Crystal Structure, Vibrational Spectra and Thermal Decomposition of Barium Azide Chloride.

ChemInform ◽  
2009 ◽  
Vol 40 (2) ◽  
Author(s):  
Bjoern Blaschkowski ◽  
Harald Balzer ◽  
Hans-Lothar Keller ◽  
Thomas Schleid
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Vibrational Spectra

scholarly journals Kinetic Analysis of the Thermal Decomposition of Iron(III) Phosphates: Fe(NH3)2PO4 and Fe(ND3)2PO4

2020 ◽  
Vol 21 (3) ◽  
pp. 781
Author(s):  
Isabel Iglesias ◽  
José A. Huidobro ◽  
Belén F. Alfonso ◽  
Camino Trobajo ◽  
Aránzazu Espina ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Kinetic Analysis ◽  
Room Temperature ◽  
Isoconversional Methods ◽  
Iron Phosphate ◽  
Dihydrogen Phosphate ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Group A

The hydrothermal synthesis and both the chemical and structural characterization of a diamin iron phosphate are reported. A new synthetic route, by using n-butylammonium dihydrogen phosphate as a precursor, leads to the largest crystals described thus far for this compound. Its crystal structure is determined from single-crystal X-ray diffraction data. It crystallizes in the orthorhombic system (Pnma space group, a = 10.1116(2) Å, b = 6.3652(1) Å, c = 7.5691(1) Å, Z = 4) at room temperature and, below 220 K, changes towards the monoclinic system P21/n, space group. The in situ powder X-ray thermo-diffraction monitoring for the compound, between room temperature and 1100 K, is also included. Thermal analysis shows that the solid is stable up to ca. 440 K. The kinetic analysis of thermal decomposition (hydrogenated and deuterated forms) is performed by using the isoconversional methods of Vyazovkin and a modified version of Friedman. Similar values for the kinetic parameters are achieved by both methods and they are checked by comparing experimental and calculated conversion curves.

scholarly journals Thermal behavior and decomposition kinetics of rifampicin polymorphs under isothermal and non-isothermal conditions

2010 ◽  
Vol 46 (2) ◽  
pp. 343-351 ◽  
Author(s):  
Ricardo Alves ◽  
Thaís Vitória da Silva Reis ◽  
Luis Carlos Cides da Silva ◽  
Silvia Storpírtis ◽  
Lucildes Pita Mercuri ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Thermal Behavior ◽  
Melting Process ◽  
Decomposition Process ◽  
Stable Form ◽  
Thermal Decomposition Process ◽  
Mean Values ◽  
Conversion Level ◽  
Polymorphic Forms ◽  
Crystalline Forms

The thermal behavior of two polymorphic forms of rifampicin was studied by DSC and TG/DTG. The thermoanalytical results clearly showed the differences between the two crystalline forms. Polymorph I was the most thermally stable form, the DSC curve showed no fusion for this species and the thermal decomposition process occurred around 245 ºC. The DSC curve of polymorph II showed two consecutive events, an endothermic event (Tpeak = 193.9 ºC) and one exothermic event (Tpeak = 209.4 ºC), due to a melting process followed by recrystallization, which was attributed to the conversion of form II to form I. Isothermal and non-isothermal thermogravimetric methods were used to determine the kinetic parameters of the thermal decomposition process. For non-isothermal experiments, the activation energy (Ea) was derived from the plot of Log β vs 1/T, yielding values for polymorph form I and II of 154 and 123 kJ mol-1, respectively. In the isothermal experiments, the Ea was obtained from the plot of lnt vs 1/T at a constant conversion level. The mean values found for form I and form II were 137 and 144 kJ mol-1, respectively.

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