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1.
cis-[Co(bipy)2(CN)2] complex was successfully prepared from the reaction of [Co(CN)2] with 2,2′-bipyridine in ethanol 96%. The product of complex synthesized was light brown crystal with percent yield of 75.86%.
The IR spectrum of this complex showed strong characteristics vibration band at 1471.9 and 1442.75 cm−1 for C=N stretching, 1664.57 cm−1 for C=C aromatic, 1600.9 cm−1 1 for HC=CH aromatic, 653.87 cm−1 for pyridine ring on 2,2′-bipyridine ligand, 3109.25 and 3080.32 cm−1 for C-H of aromatic ring. The thermogram of DTA-TG analysis showed 4 endothermic peaks at temperature of 53.4, 323.2, 444.2,
and 526.4°C, where the bond breaking of the complex occurred at different temperatures. The result of moment magnet measurement
of the complex showed that it was a high spin complex with moment magnet value of 3.68 BM, so it is a paramagnetic complex. 相似文献
2.
Sofia Nikolaou Daniela M. Tomazela Marcos N. Eberlin Henrique E. Toma 《Transition Metal Chemistry》2008,33(8):1059-1065
The polymetallic [Ru3O(CH3COO)6(py)2(BPE)Ru(bpy)2Cl](PF6)2 complex (bpy = 2,2′-bipyridine, BPE = trans-1,2-bis(4-pyridil)ethylene and py = pyridine) was assembled by the combination of an electroactive [Ru3O] moiety with a [Ru(bpy)2(BPE)Cl] photoactive centre, and its structure was determined using positive ion electrospray (ESI-MS) and tandem mass (ESI-MS/MS)
spectrometry. The [Ru3O(CH3COO)6(py)2(BPE)Ru(bpy)2Cl]2+ doubly charged ion of m/z 732 was mass-selected and subject to 15 eV collision-induced dissociation, leading to a specific dissociation pattern, diagnostic
of the complex structure. The electronic spectra display broad bands at 409, 491 and 692 nm ascribed to the [Ru(bpy)2(BPE)] charge-transfer bands and to the [Ru3O] internal cluster transitions. The cyclic voltammetry shows five reversible waves at −1.07 V, 0.13 V, 1.17 V, 2.91 V and
−1.29 V (vs SHE) assigned to the [Ru3O]−1/0/+1/+2/+3 and to the bpy0/−1 redox processes; also a wave is observed at 0.96 V, assigned to the Ru+2/+3 pair. Despite the conjugated BPE bridge, the electrochemical and spectroelectrochemical results indicate only a weak coupling
through the π-system, and preliminary photophysical essays showed the compound decomposes under visible light irradiation. 相似文献
3.
L. Tian N. Ren J. J. Zhang H. M. Liu S. J. Sun H. M. Ye K. Z. Wu 《Journal of Thermal Analysis and Calorimetry》2010,99(1):349-356
The two complexes of [Ln(CA)3bipy]2 (Ln = Tb and Dy; CA = cinnamate; bipy = 2,2′-bipyridine) were prepared and characterized by elemental analysis, infrared
spectra, ultraviolet spectra, thermogravimetry and differential thermogravimetry techniques. The thermal decomposition behaviors
of the two complexes under a static air atmosphere can be discussed by thermogravimetry and differential thermogravimetry
and infrared spectra techniques. The non-isothermal kinetics was investigated by using a double equal-double steps method,
the nonlinear integral isoconversional method and the Starink method. The mechanism functions of the first decomposition step
of the two complexes were determined. The thermodynamic parameters (ΔH
≠
, ΔG
≠
and ΔS
≠
) and kinetic parameters (activation energy E and the pre-exponential factor A) of the two complexes were also calculated. 相似文献
4.
H. X. Ma B. Yan Z. N. Li J. R. Song R. Z. Hu 《Journal of Thermal Analysis and Calorimetry》2009,95(2):437-444
The title compound 3,3-dinitroazetidinium (DNAZ) 3,5-dinitrosalicylate (3,5-DNSA) was prepared and the crystal structure has
been determined by a four-circle X-ray diffractometer. The thermal behavior of the title compound was studied under a non-isothermal
condition by DSC and TG/DTG techniques. The kinetic parameters were obtained from analysis of the TG curves by Kissinger method,
Ozawa method, the differential method and the integral method. The kinetic model function in differential form and the value
of E
a and A of the decomposition reaction of the title compound are f(α)=4α3/4, 130.83 kJ mol−1 and 1013.80s−1, respectively. The critical temperature of thermal explosion of the title compound is 147.55 °C. The values of ΔS
≠, ΔH
≠ and ΔG
≠ of this reaction are −1.35 J mol−1 K−1, 122.42 and 122.97 kJ mol−1, respectively. The specific heat capacity of the title compound was determined with a continuous C
p mode of mircocalorimeter. Using the relationship between C
p and T and the thermal decomposition parameters, the time of the thermal decomposition from initiation to thermal explosion (adiabatic
time-to-explosion) was obtained. 相似文献
5.
H. X. Ma B. Yan Y. H. Ren Y. Hu Y. L. Guan F. Q. Zhao J. R. Song R. Z. Hu 《Journal of Thermal Analysis and Calorimetry》2011,103(2):569-575
3,3-Dinitroazetidinium (DNAZ) salt of perchloric acid (DNAZ·HClO4) was prepared, it was characterized by the elemental analysis, IR, NMR, and a X-ray diffractometer. The thermal behavior
and decomposition reaction kinetics of DNAZ·HClO4 were investigated under a non-isothermal condition by DSC and TG/DTG techniques. The results show that the thermal decomposition
process of DNAZ·HClO4 has two mass loss stages. The kinetic model function in differential form, the value of apparent activation energy (E
a) and pre-exponential factor (A) of the exothermic decomposition reaction of DNAZ·HClO4 are f(α) = (1 − α)−1/2, 156.47 kJ mol−1, and 1015.12 s−1, respectively. The critical temperature of thermal explosion is 188.5 °C. The values of ΔS
≠, ΔH
≠, and ΔG
≠of this reaction are 42.26 J mol−1 K−1, 154.44 kJ mol−1, and 135.42 kJ mol−1, respectively. The specific heat capacity of DNAZ·HClO4 was determined with a continuous C
p mode of microcalorimeter. Using the relationship between C
p and T and the thermal decomposition parameters, the time of the thermal decomposition from initiation to thermal explosion (adiabatic
time-to-explosion) was evaluated as 14.2 s. 相似文献
6.
Lucas Bomfim Bolzon Alexandre G. S. Prado 《Journal of Thermal Analysis and Calorimetry》2011,106(2):427-430
The protonation and deprotonation of the Nb2O5 surface has been followed in order to understand the reactions of surface of this catalyst. The simultaneous potentiometric
and conductometric titrations had been carried by using 50 mL of water suspension of Nb2O5 40 g L−1. The oxide was entirely deprotonated when adding 0.4 mL NaOH 1 mol L−1, and later titrated with 0.1 mol L−1. The titration had supplied K
1 and K
2 and the obtained values were 3.24 × 10−3 and 4.17 × 10−8, respectively. The zero point charge was pHpcz = 4.94. The thermodynamic studies were carried out by using 50 mL of a 40 g/L Nb2O5 aqueous suspension with the pH adjusted to pHPZC value. The suspension was titrated with 0.5 mol/L of HNO3 or NaOH for protonation or deprotonation studies, respectively, in an isoperibol calorimeter CSC ISC-4300. Thus, the obtained
thermodynamic values of the protonation and deprotonation of Nb2O5 were Δdp
G = −37.60 kJ/mol, Δdp
H = −23.72 kJ/mol and ΔdpS = 47 J/(mol K). 相似文献
7.
A. N. Mansurova R. I. Gulyaeva V. M. Chumarev V. P. Mar’evich 《Journal of Thermal Analysis and Calorimetry》2010,101(1):45-47
Homogeneous manganocolumbite (MnNb2O6) was synthesized from Nb2O5 and MnO oxides. Powder sample was orthorhombic with unit cell parameters: α = 0.5766 nm, b = 1.4439 nm, c = 0.5085 nm and V = 0.4234 nm3. Heat capacity over the temperature range of 313–1253 K was measured in an inert atmosphere with combined thermogravimetry
and calorimetry using NETZSCH STA 449C Jupiter thermoanalyzer. Melting point was 1767 ± 3 K, enthalpy of melting was 144 ± 4 kJ mol−1. Experimental heat capacity of MnNb2O6 is fitted to polynomial C
pm = 221.46 + 3.03 · 10−3 T + −39.79 · 105 T
−2 + 40.59 · 10−6 T
2. 相似文献
8.
Shu-Jing Sun Juan-Fen Wang Ning Ren Jian-Jun Zhang Hong-Mei Ye Shu-Ping Wang 《Structural chemistry》2012,23(1):79-89
Some binuclear lanthanide complexes with the general formula [Ln(2,3-DClBA)3bipy]2 (Ln = Sm(1), Eu(2), Tb(3), Dy(4), and Ho(5); 2,3-DClBA = 2,3-dichlorobenzoate; bipy = 2,2′-bipyridine) were synthesized and characterized by elemental analysis, molar
conductance, infrared, ultraviolet, luminescent spectroscopy, thermogravimetry, and different thermogravimetry (TG–DTG) techniques.
The single crystals of the complexes have been obtained except the complex 2 and their structures have been determined by single-crystal X-ray diffraction. The four complexes are isostructural and the
rare earth ions are all nine coordinated. The two rare earth ions in each complex are linked by two bridging bidentate and
two chelating-bridging tridentate carboxylate groups. Under ultraviolet light excitation, the europium and terbium complexes
exhibited characteristic red fluorescence of Eu3+ ion and green fluorescence of Tb3+ ion at room temperature. The non-isothermal kinetics was investigated by using the integral isoconversional non-linear (NL-INT)
and the Popescu methods. The mechanism functions of the first decomposition step of the complexes 3–5 were determined. Meanwhile, the thermodynamic parameters (ΔG
≠
, ΔH
≠, and ΔS
≠) at DTG peak temperatures were also calculated. 相似文献
9.
S. -X. Wang Z. -C. Tan Y. -S. Li L. -X. Sun Y. Li 《Journal of Thermal Analysis and Calorimetry》2008,92(2):483-487
Synthesis, characterization and thermal analysis of polyaniline (PANI)/ZrO2 composite and PANI was reported in our early work. In this present, the kinetic analysis of decomposition process for these
two materials was performed under non-isothermal conditions. The activation energies were calculated through Friedman and
Ozawa-Flynn-Wall methods, and the possible kinetic model functions have been estimated through the multiple linear regression
method. The results show that the kinetic models for the decomposition process of PANI/ZrO2 composite and PANI are all D3, and the corresponding function is ƒ(α)=1.5(1−α)2/3[1−(1-α)1/3]−1. The correlated kinetic parameters are E
a=112.7±9.2 kJ mol−1, lnA=13.9 and E
a=81.8±5.6 kJ mol−1, lnA=8.8 for PANI/ZrO2 composite and PANI, respectively. 相似文献
10.
Jiang-Yang Shao Ting Sun Qing-Yu Guo Hong Li Sheng Lan 《Transition Metal Chemistry》2011,36(5):499-504
A classical ruthenium(II) complex [Ru(bpy)2(dppz)]2+ (bpy = 2,2′-bipyridine, dppz = dipyrido[3,2-a:2′,3′-c]phenazine) was combined with guanine and single-walled carbon nanotubes
dispersed with DNA (SWCNTs-DNA) to prepare electrochemically tunable photoluminescence materials. These multi-component aggregates
were found to show enhanced luminescence by the electrocatalytic oxidation of guanine under the excitation of a continuous
wave green laser at a constant anodic potential via an electrode-solution interface. The results from this study provide a
significant foundation for better understanding of DNA-based luminescent devices. 相似文献
11.
One new metal – organic coordination framework formulated as [{Cu(4,4′-bipy)(CH3COO)2}·3H2O]n (1) (where 4,4′-bipy=4,4′-bipyridine) has been hydrothermally synthesised and characterised by elemental analysis, IR and electronic
spectroscopy, variable temperature magnetic moment measurement and single crystal X-ray diffraction study. Single crystal
X-ray analysis reveals that 1 is one dimensional polymeric compound in which acetate ligand shows both mono- and bidentate bonding mode, and 4,4′-bipy
acts as bridging ligand which supports the formation of infinite chains. The global feature of the χ
M
T vs. T curve in 1 is characteristic of moderate antiferromagnetic interaction and the best fit parameters from 300 down to 2 K are found as
J = −78.7 cm−1. 相似文献
12.
Nopsiri Chaiyo Rangson Muanghlua Surasak Niemcharoen Banjong Boonchom Panpailin Seeharaj Naratip Vittayakorn 《Journal of Thermal Analysis and Calorimetry》2012,107(3):1023-1029
The thermal transformation of Na2C2O4 was studied in N2 atmosphere using thermo gravimetric (TG) analysis and differential thermal analysis (DTA). Na2C2O4 and its decomposed product were characterized using a scanning electron microscope (SEM) and the X-ray diffraction technique
(XRD). The non-isothermal kinetic of the decomposition was studied by the mean of Ozawa and Kissinger–Akahira–Sunose (KAS)
methods. The activation energies (E
α) of Na2C2O4 decomposition were found to be consistent. Decreasing E
α at increased decomposition temperature indicated the multi-step nature of the process. The possible conversion function estimated
through the Liqing–Donghua method was ‘cylindrical symmetry (R2 or F1/2)’ of the phase boundary mechanism. Thermodynamic functions (ΔH*, ΔG* and ΔS*), calculated by the Activated complex theory and kinetic parameters, indicated that the decomposition step is a high energy
pathway and revealed a very hard mechanism. 相似文献
13.
Ling Pei Meiya Li Jun Liu Benfang Yu Jing Wang Dongyun Guo Xingzhong Zhao 《Journal of Sol-Gel Science and Technology》2010,53(2):193-198
Ferroelectric thin films of Nd and Mn co-doped bismuth titanate, Bi3.15Nd0.85Ti3−x
Mn
x
O12 (BNTM) (x = 0–0.1), were fabricated on Pt/TiO2/SiO2/Si(100) substrates by a sol–gel technique. The BNTM films had a polycrystalline perovskite structure and uniform and dense
surface morphologies. A lattice distortion was observed in the BNTM films due to Mn ion doping. The ferroelectric measurement
of the films indicated that the values of coercive field (E
c
) decreased gradually with the increase of the Mn content (x), however, the remanent polarization (P
r
) increase firstly and then decrease with the increase of x. The sample with x = 0.05 had optimum electrical properties and a maximum 2P
r
value. The 2P
r
and 2E
c
values of the film at a maximum applied electric field of 400 kV/cm were 38.3 μC/cm2 and 180 kV/cm, respectively. Moreover, this BNTM capacitors did not show fatigue behaviors after 1.0 × 1010 switching cycles at a frequency of 1 MHz, suggesting a fatigue-free character. The main reason for the increase of the 2P
r
and the decrease of the 2E
c
might be attributed to the lattice distortion in BNTM films due to Mn ion doping. 相似文献
14.
Bin Peng Hui Chao Bin Sun Feng Gao Liang-Nian Ji Jian Zhang 《Transition Metal Chemistry》2007,32(2):271-277
Two novel cobalt(III) mixed-polypyridyl complexes
[Co(bpy)2(dpta)]3+ and [Co(bpy)2(amtp)]3+ (bpy = 2,2′-bipyridine, dpta = dipyrido-[3,2-a;2′,3′-c]-thien-[3,4-c]azine, amtp = 3-amino-1,2,4-triazino[5,6-f]-1,10-phenanthroline)
have been synthesized and characterized. The interaction of CoIII complexes with calf thymus DNA was investigated by spectroscopic and viscosity measurements. Results suggest that the two
complexes bind to DNA via an intercalative mode. Moreover, CoIII complexes have been found to promote the photocleavage of plasmid DNA pBR322 under irradiation at 365 nm. The mechanism studies
reveal that hydroxyl radical (OH•) is likely to be the reactive species responsible for the cleavage of plasmid DNA by [Co(bpy)2(dpta)]3+ and superoxide anion radical (O
2
•−
) acts as the key role in the cleavage reaction of plasmid DNA by [Co(bpy)2(amtp)]3+. 相似文献
15.
S. Vidhisha Kotha Laxma Reddy K. Ashwini Kumar Yata Praveen Kumar S. Satyanarayana 《Transition Metal Chemistry》2010,35(8):1027-1034
This article describes the synthesis of a polypyridyl ligand, namely 2-(2, 5-dimethoxyphenyl)-1H-imidazo[4,5-f]1,10-phenanthroline (DMPIP) and its Ru(II) complexes, namely [Ru(bipy)2DMPIP]2+ (1), [Ru(dmb)2DMPIP]2+ (2) and [Ru(phen)2DMPIP]2+ (3) ((bipy = 2,2′-bipyridine, dmb = 4,4′-dimethyl-2,2′-bipyridine, phen = 1,10-phenanthroline). The complexes were characterized
by elemental analysis, plus IR, 1H-NMR and 13C [1H]-NMR spectra. The interactions of the complexes with calf thymus DNA were investigated. The results indicate that the three
complexes can intercalate into DNA. Under irradiation at 365 nm, all three complexes promote the photocleavage of plasmid
pBR 322 DNA. Inhibitor studies suggest that singlet oxygen plays a significant role in the cleavage mechanism for the complexes. 相似文献
16.
Two new neodymium complexes, [Nd2(abglyH)6(2,2′-bipy)2(H2O)2] · 4H2O 1 and {[Nd(abglyH)3(H2O)2] · (4,4′-bipy) · 7H2O}n
2 (abglyH2 = N-P-acetamidobenzenesulfonyl-glycine acid, 2,2′-bipy = 2,2′-bipyridine, 4,4′-bipy = 4,4′-bipyridine), have been synthesized and
their structures have been measured by X-ray crystallography. In 1, nine-coordinated Nd(III) ions are bridged by two syn–syn bidentate and two tridentate bridging carboxylate groups from four different abglyH− anions to form dinuclear motifs, which are further connected into a 3-D supramolecular framework via hydrogen bonds between
the binuclear motifs and the uncoordinated water molecules. In 2, eight-coordinated Nd(III) ions are linked by six carboxylate groups adopting a syn–syn bidentate bridging fashion to form a 1-D inorganic–organic alternating linear chain. These polymeric chains generate microchannels
extending along the a direction, and these cavities are occupied by discrete tetradecameric water clusters, which interact with their surroundings
and finally furnish the 3-D supramolecular network via hydrogen bonds. At the same time, π–π stacking interactions between
benzene rings from abglyH− anions also play an important role in stabilizing the network. 相似文献
17.
E. Vessally M. Nikoorazm A. Esmaili H. Ghoudarzi Afshar 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2011,85(4):631-635
Thermal internal energy gaps, ΔE
s−t; enthalpy gaps, ΔH
s−t; Gibbs free energy gaps, ΔD
s−t, between singlet (s) and triplet (t) states of R2C4H2M (M = C, Si, and Ge) were calculated at B3LYP/6-311++G** level of theory. The ΔG
s−t of R2C4H2C was increased in the order (in kcal/mol): R = −CH3 (−10.51) > −H (−9.59) > i-Pr (−9.51) > t-Bu (−8.98). While, the ΔG
s−t of R2C4H2Si and R2C4H2Ge were increased in the order (in kcal/mol): −CH3 (17.01) > i-Pr (15.30) > −H (15.26) > t-Bu (14.35) and -H (22.79) > −CH3 (22.69) > i-Pr (21.66) > t-Bu (21.01), respectively. 相似文献
18.
S. K. Tripathi Balbir Singh Patial Nagesh Thakur 《Journal of Thermal Analysis and Calorimetry》2012,107(1):31-38
Differential scanning calorimetry data at different heating rates (5, 10, 15 and 20 °C min−1) of Se70Te15In15 chalcogenide glass is reported and discussed. The crystallization mechanism is explained in terms of recent analyses developed
for use under non-isothermal conditions. The value of Avrami exponent (n) indicates that the glassy Se70Te15In15 alloy has three-dimensional growth. The average values of the activation energy for glass transition, E
g, and crystallization process, E
c, are (154.16 ± 4.1) kJ mol−1 and (98.81 ± 18.1) kJ mol−1, respectively. The ease of glass formation has also been studied. The reduced glass transition temperature (T
rg), Hruby’ parameter (K
gl) and fragility index (F
i) indicate that the prepared glass is obtained from a strong glass forming liquid. 相似文献
19.
Soraia Meghdadi Mehdi Amirnasr Mohammad H. Habibi Ahmad Amiri Fatemeh Ahmadi Keiko Kihara Takayoshi Suzuki Hamid Reza Bijanzadeh 《Transition Metal Chemistry》2008,33(7):879-886
The structure, spectroscopic, and electrochemical properties of [Co{(BA)2pn}(L)2]ClO4 complexes, where (BA)2pn = N,N′-bis(benzoylacetone)-1,3-propylenediimine dianion and the two ancillary ligands (L) are pyridine, py (1), and 4-methylpyridine, 4-Mepy (2), have been investigated. These complexes have been characterized by elemental analyses, IR, UV–Vis and 1H-NMR spectroscopy. The crystal structure of [Co{(BA)2pn}(py)2]ClO4 (1) has been determined by X-ray diffraction. The coordination geometry around cobalt(III) is best described as a distorted
octahedron. The electrochemical reduction of these complexes at a glassy carbon electrode in acetonitrile solution indicates
that the first reduction process corresponding to CoIII–CoII is electrochemically irreversible, which is accompanied by the dissociation of the axial N(py)–cobalt bonds. This process
becomes quasi-reversible upon the addition of excess py ligands. The second reduction step of CoII/I shows reversible behavior and is not influenced by the nature of the axial ligands.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
20.
E. Styczeń W. K. Jóźwiak M. Gazda D. Wyrzykowski Z. Warnke 《Journal of Thermal Analysis and Calorimetry》2008,91(3):979-984
Thermal decomposition of compounds consisting of tetrahalogenocuprate(II), [CuBrnCl4−n]2− (n=0–4) anions and a tetraethylammonium cation has been studied using TG-FTIR, TG-MS, DTA and DTG techniques. The measurements
were carried out in an argon and air atmospheres over the temperature range 293-1073 K. The products of the thermal decomposition
were identified by IR and Far Infrared (FIR) spectroscopy as well as X-ray powder diffractometry. 相似文献