Editor's note: In the past forty years of reform and opening up, the preservation and restoration of cultural relics in the Palace Museum have made great progress. The paper was written by Vice President Song Jiro...Editor's note: In the past forty years of reform and opening up, the preservation and restoration of cultural relics in the Palace Museum have made great progress. The paper was written by Vice President Song Jirong who was in charge of cultural relics science and technology. It reviews the development of the Relic Hospital since the middle of the 20山 century, lists four restoration projects of cultural relics in the Palace Museum and discusses many academic achievements made in the protection of cultural relics in recent years by using modern analytical tools.展开更多
()*￡-1 -(4-Fluorobenzylidene)^l-(4-ethylphenyl)thiosemicarbazone was synthesized via the reaction of 4-(4-ethylphenyl)thiosemicarbazide and 4-fluorobenzaldehyde. The title compound was characterized by FTIR, and 13C ...()*￡-1 -(4-Fluorobenzylidene)^l-(4-ethylphenyl)thiosemicarbazone was synthesized via the reaction of 4-(4-ethylphenyl)thiosemicarbazide and 4-fluorobenzaldehyde. The title compound was characterized by FTIR, and 13C NMR, mass spectrometry and elemental analysis techniques. Structural property of the title compound was displayed by the X-ray single crystal diffraction. The title compound crystallized in triclinic space group Pl witli a=0.6494(4) nm,a=0.7971(5) nm, c=1.5492( 10) nm,a=83.690( 11)°,β=84.185(10)。γ=84.348(11)。molecular formula Ci6H16FN3S,Mr=301.39,V=0.7868(9) nm^3, Z=2, Dc=1.272 g/cm……3,^000)=316,“=0.213 mm-1, 5=1.02, 7?=O.O513, and cw7[Z>2o(Z)]=0.1662. The intennolecular interactions in the crystal structure were explained using the Hirshfeld surface and their associated two-dimensional fingerprint plots. The title compound showed C-H-S(l-x,-y,-z) and NH(1-y,-z) intermolecular interactions, and formed the supramolecular self-assemblies through R2^2(12) and R2^2(8) ring motifs. Shape index and curvediiess were performed to further understand some unique weak interactions, for instance, the weakπ…π stacking contacts in molecular structure witli difierent characteristic regions. Besides, the reduced density gradient(RDG) function provided a real-space function for discussing non-covalent interactions within molecule, such as hydrogen bonds, weak van der Waals interactions and attractive or repulsive effects.展开更多
A series of guanidine salts of 4,4＇-azo-l,2,4-triazol-5-one with guanidine（1）, aminoguanidine（2）, diaminoguanidine（3） and triaminoguanidine（4） was prepared. Compounds 2--4 were characterized by infrared（IR）...A series of guanidine salts of 4,4＇-azo-l,2,4-triazol-5-one with guanidine（1）, aminoguanidine（2）, diaminoguanidine（3） and triaminoguanidine（4） was prepared. Compounds 2--4 were characterized by infrared（IR） spectroscopy, elemental analysis and single-crystal X-ray diffraction. Thermal decomposition processes of compounds 1--4 were investigated by differential scanning calorimetry（DSC）, and all the compounds showed good thermal stability up to 190 ℃. Moreover, these four guanidine salts are more unstable with the increasing number of amino groups. Thermal stability parameters（Te,0 and Tb）and thermodynamic functions（△S≠, △H≠ and △G≠） for compounds 1-4 were calculated. The constant-volume combustion heats（AcU） for compounds 2--4 were determined and tended to increase with the increase of the number of amino groups. The calculated standard molar enthalpies of forma- tion（△ρH0m） of compounds 2-4 are -541.04, -178.67 and-83.08 kJ/mol, respectively. The impact sensitivities results indicate that these four energetic salts are less sensitive than 1,3,5-trinitrotriazacyccohexane（RDX） and 1,3,5,7- tetranitrotetraqza-cyclo-octane（HMX）.展开更多
[Zn（phen）3]·ZTO-6H2O（1） and [Cu（phen）3]·ZTO·6H2O（2） were synthesized by the reaction of ZnCNO3）2·6H2O/Cu（NO3）2·3H2O with 4,4-azo-1H-1,2,4-triazol-5-one（ZTO） and 1,10-phenanthrolin...[Zn（phen）3]·ZTO-6H2O（1） and [Cu（phen）3]·ZTO·6H2O（2） were synthesized by the reaction of ZnCNO3）2·6H2O/Cu（NO3）2·3H2O with 4,4-azo-1H-1,2,4-triazol-5-one（ZTO） and 1,10-phenanthroline（phen）. The two compounds were characterized by elemental analysis and IR spectrum analysis, respectively. Compound 1 was also characterized by single crystal X-ray diffraction analysis. For compound l, the coordination geometry around the Zn^2＋ is a distorted octahedron, with the bite angles of 76.7（3）°-77.6（4）° for all three phen ligands. Moreover, the thermal behaviors and thermal decomposition kinetics were studied and analyzed. Besides, thermal stability and safety parameters（TsADT, Tb） are 164.7 and 166.4℃ for compound 1, and 149.6 and 150.8℃ for compound 2, respectively.展开更多
The thermal behavior and non-isothermal decomposition kinetics of [Cu（en）2H2O]（FOX-7）2·H2O （en=ethylenediamine） were studied with DSC and TG-DTG methods.The kinetic equation of the exothermal process is dα...The thermal behavior and non-isothermal decomposition kinetics of [Cu（en）2H2O]（FOX-7）2·H2O （en=ethylenediamine） were studied with DSC and TG-DTG methods.The kinetic equation of the exothermal process is dα/dt=（10^17.92/β）4α^3/4exp（-1.688×10^5/RT）.The self-accelerating decomposition temperature and critical temperature of the thermal explosion are 163.3 and 174.8 ℃,respectively.The specific heat capacity of [Cu（en）2H2O]（FOX-7）2·H2O was determined with a micro-DSC method,with a molar heat capacity of 661.6 J·mol^-1·K^-1 at 25 ℃.Adiabatic time-to-explosion was also estimated as 23.2 s.[Cu（en）2H2O]（FOX-7）2·H2O is less sensitive.展开更多
文摘Editor's note: In the past forty years of reform and opening up, the preservation and restoration of cultural relics in the Palace Museum have made great progress. The paper was written by Vice President Song Jirong who was in charge of cultural relics science and technology. It reviews the development of the Relic Hospital since the middle of the 20山 century, lists four restoration projects of cultural relics in the Palace Museum and discusses many academic achievements made in the protection of cultural relics in recent years by using modern analytical tools.
文摘()*￡-1 -(4-Fluorobenzylidene)^l-(4-ethylphenyl)thiosemicarbazone was synthesized via the reaction of 4-(4-ethylphenyl)thiosemicarbazide and 4-fluorobenzaldehyde. The title compound was characterized by FTIR, and 13C NMR, mass spectrometry and elemental analysis techniques. Structural property of the title compound was displayed by the X-ray single crystal diffraction. The title compound crystallized in triclinic space group Pl witli a=0.6494(4) nm,a=0.7971(5) nm, c=1.5492( 10) nm,a=83.690( 11)°,β=84.185(10)。γ=84.348(11)。molecular formula Ci6H16FN3S,Mr=301.39,V=0.7868(9) nm^3, Z=2, Dc=1.272 g/cm……3,^000)=316,“=0.213 mm-1, 5=1.02, 7?=O.O513, and cw7[Z>2o(Z)]=0.1662. The intennolecular interactions in the crystal structure were explained using the Hirshfeld surface and their associated two-dimensional fingerprint plots. The title compound showed C-H-S(l-x,-y,-z) and NH(1-y,-z) intermolecular interactions, and formed the supramolecular self-assemblies through R2^2(12) and R2^2(8) ring motifs. Shape index and curvediiess were performed to further understand some unique weak interactions, for instance, the weakπ…π stacking contacts in molecular structure witli difierent characteristic regions. Besides, the reduced density gradient(RDG) function provided a real-space function for discussing non-covalent interactions within molecule, such as hydrogen bonds, weak van der Waals interactions and attractive or repulsive effects.
文摘A series of guanidine salts of 4,4＇-azo-l,2,4-triazol-5-one with guanidine（1）, aminoguanidine（2）, diaminoguanidine（3） and triaminoguanidine（4） was prepared. Compounds 2--4 were characterized by infrared（IR） spectroscopy, elemental analysis and single-crystal X-ray diffraction. Thermal decomposition processes of compounds 1--4 were investigated by differential scanning calorimetry（DSC）, and all the compounds showed good thermal stability up to 190 ℃. Moreover, these four guanidine salts are more unstable with the increasing number of amino groups. Thermal stability parameters（Te,0 and Tb）and thermodynamic functions（△S≠, △H≠ and △G≠） for compounds 1-4 were calculated. The constant-volume combustion heats（AcU） for compounds 2--4 were determined and tended to increase with the increase of the number of amino groups. The calculated standard molar enthalpies of forma- tion（△ρH0m） of compounds 2-4 are -541.04, -178.67 and-83.08 kJ/mol, respectively. The impact sensitivities results indicate that these four energetic salts are less sensitive than 1,3,5-trinitrotriazacyccohexane（RDX） and 1,3,5,7- tetranitrotetraqza-cyclo-octane（HMX）.
文摘[Zn（phen）3]·ZTO-6H2O（1） and [Cu（phen）3]·ZTO·6H2O（2） were synthesized by the reaction of ZnCNO3）2·6H2O/Cu（NO3）2·3H2O with 4,4-azo-1H-1,2,4-triazol-5-one（ZTO） and 1,10-phenanthroline（phen）. The two compounds were characterized by elemental analysis and IR spectrum analysis, respectively. Compound 1 was also characterized by single crystal X-ray diffraction analysis. For compound l, the coordination geometry around the Zn^2＋ is a distorted octahedron, with the bite angles of 76.7（3）°-77.6（4）° for all three phen ligands. Moreover, the thermal behaviors and thermal decomposition kinetics were studied and analyzed. Besides, thermal stability and safety parameters（TsADT, Tb） are 164.7 and 166.4℃ for compound 1, and 149.6 and 150.8℃ for compound 2, respectively.
基金Supported by the National Natural Science Foundation of China（Nos. 21241003, 20803058）, the Science and Technology Research and Development Program of Shaanxi Province, China（No.2013K02-25） and the Education Committee Foundation of Shaanxi Province, China（No.2013JK0697）.
文摘The thermal behavior and non-isothermal decomposition kinetics of [Cu（en）2H2O]（FOX-7）2·H2O （en=ethylenediamine） were studied with DSC and TG-DTG methods.The kinetic equation of the exothermal process is dα/dt=（10^17.92/β）4α^3/4exp（-1.688×10^5/RT）.The self-accelerating decomposition temperature and critical temperature of the thermal explosion are 163.3 and 174.8 ℃,respectively.The specific heat capacity of [Cu（en）2H2O]（FOX-7）2·H2O was determined with a micro-DSC method,with a molar heat capacity of 661.6 J·mol^-1·K^-1 at 25 ℃.Adiabatic time-to-explosion was also estimated as 23.2 s.[Cu（en）2H2O]（FOX-7）2·H2O is less sensitive.
