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1.
以铜试剂(NaEt2dtc•3H2O)和邻菲咯啉(o-phen•H2O) 与水合氯化铽(TbCl3•3.75H2O)在无水乙醇中制得了三元固态配合物.化学分析和元素分析确定其组成为Tb(Et2dtc)3(phen).IR光谱研究表明配合物中Tb3+与NaEt2dtc中的硫原子双齿配位,同时与phen的氮原子双齿配位.用Calvet微热量计测定了298.15 K下液相生成反应的焓变ΔrHmθ(l),为(-21.819±0.055) kJ•mol-1,通过热化学循环计算了固相生成反应焓变ΔrHmθ(s),为(128.476±0.675) kJ•mol-1.改变反应温度,研究了液相生成反应的热动力学.用精密转动弹热量计测得配合物的恒容燃烧能ΔcU为(-17646.95±8.64) kJ•mol-1,经计算其标准燃烧焓ΔcHHmθ和标准生成焓ΔfHmθ分别为(-17666.16±8.64) kJ•mol-1和(-1084.04±9.49) kJ•mol-1. 相似文献
2.
改进文献方法,以铜试剂(NaEt2dtc·3H2O)和邻菲咯啉(o-phen·H2O)与低水合氯化钬(HoCl3·3.58H2O)在无水乙醇中反应,制得三元固态配合物.化学分析和元素分析确定该配合物的组成为Ho(Et2dtc)3(phen).IR光谱表明配合物中Ho3 与3个NaEt2dtc中的6个硫原子双齿配位,同时与o-phen中的2个氮原子双齿配位,可推测其配位数为8.用微量热量计测定了298.15 K下液相生成反应的焓变△rHm (1),为(-14.697±0.0376)kJ·mol-1,通过合理的热化学循环计算了固相生成反应焓变△rHm (s),为(117.504±0.619)kJ·mol-1;改变反应温度,研究了配合物的液相生成反应的热力学性质.配合物的恒容燃烧能△cU用精密转动弹热量计测定为(-18687.64±8.22)kJ·mol-1,其标准燃烧焓△cHm 和标准生成焓△fHm 经计算分别为(-18706.85±8.22)和(-70.01±9.37)kJ·mol-1. 相似文献
3.
Four ternary solid complexes were synthesized with sodium diethyldithiocarbamate (NaEt2dtc)(b), 1,10-phenanthroline (o-phen) (c) and hydrated lanthanide chlorides in absolute ethanol by an improved reported method. The complexes were identified as the general formula of RE(Et2dtc)3(phen) (RE=La, Pr, Nd, Sm) by chemical and elemental analyses. IR spectra of the complexes showed that the RE3+ was coordinated with sulfur atoms of NaEt2dtc and nitrogen atoms of o-phen. The constant-volume combustion energies of complexes, ΔcU, were determined by a precise rotating-bomb calorimeter at 298.15 K. The standard enthalpies of combustion, ΔcHm?, and standard enthalpies of formation, ΔfHm?, were calculated for these complexes, respectively. 相似文献
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A ternary solid complex Lu(Et2dtc)3(phen) has been obtained from the reaction of hydrated lutetium chloride with sodium diethyldithiocarbamate
(NaEt2dtc), and 1,10-phenanthroline (o-phen·H2O) in absolute ethanol. IR spectrum of the complex indicates that
Lu3+ binds with sulfur atom in the Na(Et2dtc)3 and nitrogen atom in the o-phen. The enthalpy change of liquid-phase reaction of formation of the complex,
ΔrHmӨ (l), was determined to be (-32.821 ± 0.147 ) kJ·mol-1 at 298.15 K by an RD-496 Ⅲ type heat conduction microcalormeter. The enthalpy change of the solid-phase reaction of formation of the complex,
ΔrHmӨ (s), was calculated to be (104.160 ± 0.168) kJ ·
mol-1 on the basis of an appropriate thermochemistry cycle. The thermodynamics of liquid-phase reaction of formation of the complex was investigated by changing the temperature of liquid-phase reaction. Fundamental parameters, such as the activation enthalpy (ΔH≠Ө), the activation entropy (ΔS≠Ө), the activation free energy (ΔG≠Ө), the apparent reaction rate constant (k), the apparent activation energy (E), the pre-exponential constant (A) and the reaction order (n), were obtained by combination the reaction thermodynamic and kinetic equations with the data of thermokinetic experiments. The molar heat capacity of the complex,
cm, was determined to be (82.23 ± 1.47) J·mol-1·K-1 by the same microcalormeter. The constant-volume combustion energy of the complex, ΔcU, was determined as (-17 898.228 ± 8.59) kJ·mol-1 by an RBC-Ⅱtype rotating-bomb calorimeter at 298.15 K. Its standard enthalpy of combustion,
ΔcHmӨ, and standard enthalpy of formation, ΔfHmӨ, were calculated to be (-17 917.43 ± 8.11) kJ·mol-1 and (-859.95 ±10.12) kJ·mol-1, respectively. 相似文献
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Er(PMAP)_9·2H_2O(PMAP=1-苯基-3-甲基-4-乙酰吡咯啉酮-5)属单斜晶系。空间群为P2_1/c,晶胞参数α=17,582(4),b=12.346(2),c=18.236(3),β=102.8(2)°,Z=4,R=0.06298。 相似文献
10.
1-苯基-3-甲基-七氟丁酰吡唑酮-5(PMHFP)及邻菲咯啉(phen)希土混配配合物的合成及性质研究 总被引:1,自引:1,他引:1
本文在乙醇中合成了PMHFP及phen与希土离子的三元配合物Ln(PMHFP)3·phen(Ln=La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y).通过化学分析,元素分析及电导分析确定了配合物的组成;研究了配合物的紫外、红光光谱;借助于差热-热重分析仪研究了所有配合物的挥发性质,测定了它们各自的起始挥发温度,探讨了用于希土分析的可能性. 相似文献
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A new biosensor method was developed to determine residual carbofuran in tomatoes in a rapid and convenient fashion based on immobilizing acetylcholinesterase (AChE) on an electrode modified by concanavalin A (Con A)/polydopamine (PDA)-reduced graphene oxide (RGO)-gold nanoparticle (GNP) nanocomposites. The specific binding between Con A and AChE was investigated by the Ellman method and cyclic voltammetry (CV). The synthesis of nanocomposites was monitored by ultraviolet-visible absorption spectroscopy, scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). The results showed that, due to the specific binding and good electrical conductivity, the biosensor had 2.2 times higher bioactivity, leading to high sensitivity with a low Michaelis constant of 0.10?mM. Parameters that affect the response of the biosensor, such as the pH, enzyme loading, ionic concentration, and inhibition time, were optimized. When used for the detection of carbofuran, this biosensor showed a wide range of applicability from 5?µg/kg to 40?µg/kg with a detection limit of 0.012?µg/kg. In addition, the biosensor demonstrated good recovery values of 101% and 90% for 10?µg/kg and 100?µg/kg of the analyte, good stability, high repeatability, and a rapid detection time of 20?min for carbofuran in tomatoes, which provides significant advantages for future analysis. 相似文献
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N. N. Aleinikov S. A. Kashtanov I. A. Pomytkin A. M. Sipyagin 《Russian Chemical Bulletin》1995,44(1):180-181
Bis(tetramethylammonium), bis(tetrabutylammonium), and bis(tetraphenylarsonium) dihydrohexaoxoxenonates(VIII) were obtained in an aqueous solution and in acetonitriie. The rate constants of their decomposition were determined.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 184–185, January, 1995.This work was carried out with financial support from the International Scientific Foundation (Grant REI 000). 相似文献
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The complexes [Ni(PEt
3)2
dtc]X (1) and Ni(PEt
3)Xdtc (2) (dtc=S2CNEt
2,X=Cl, Br, I) have been prepared. As conductivity, susceptibility, UV and IR measurements show, the cations [Ni(PEt
3)2
dtc]+ of1 and the complexes2 at ambient temperature have square-planar structure. We suppose there might exist an equilibrium for2 between square-planar and tetrahedral configuration. 相似文献
14.
《Journal of Coordination Chemistry》2012,65(18):1555-1566
Reaction of the N-(2-pyridyl)carbonylaniline ligand (L) with Cu(NO3)2, Cu(ClO4)2, Zn(ClO4)2, Ni(NO3)2 and PdCl2 gives complexes with stoichiometry [Cu(L)2(H2O)2](NO3)2, [Cu(L)2(H2O)2](ClO4)2, [Zn(L)2(H2O)2] (ClO4)2, [Ni(L)2(H2O)Cl](NO3) and PdLCl2. The new complexes were characterized by elemental analyses and infrared spectra. The crystal structures of [Cu(L)2(H2O)2](NO3)2, [Cu(L)2(H2O)2](ClO4)2, and [Zn(L)2(H2O)2](ClO4)2 were determined by X-ray crystallography. The cation complexes [M(L)2(H2O)2] contain copper(II) and zinc(II) with distorted octahedral geometry with two N-(2-pyridyl)carbonylaniline (L) ligands occupying the equatorial sites. The hexa-coordinated metal atoms are bonded to two pyridinic nitrogens, two carbonyl oxygens and two water molecules occupying the axial sites. Both the coordinated water molecules and uncoordinated amide NH groups of the N-(2-pyridyl)carbonylaniline (L) ligands are involved in hydrogen bonding, resulting in infinite hydrogen-bonded chains running in one and two-dimensions. 相似文献
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The synthesis of new inorganic pigments has been investigated with the goal of preparing heat stable and anticorrosive pigments.
The synthesis is based on a thermal procedure making use of the reversible transformation of cyclo-tetraphosphates(V) to higher
linear phosphates(V). New binary condensed phosphates were synthesized based on the results of thermal analysis. These compounds
represent new environmentally-friendly special pigments.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
16.
Rhodium(III), palladium(II) and platinum(II) complexes of Bis(o-aminobenzenesulfonyl)ethylenediamine
New complexes of the formulae K3[RhL
3]·2 H2O, [PdL]·H2O and [M(LH2)Cl2] [whereM = Pd, Pt andLH2 = bis(o-aminobenzenesulfonyl)ethylenediamine] have been prepared and characterized by conductivity measurements, thermogravimetric analysis, X-ray powder patterns and IR, Ligand Field and1H-NMR spectroscopy.
Rhodium(III), Palladium(II)- und Platin(II)-Komplexe mit Bis(o-aminobenzolosulfonyl)ethylendiamin (Kurze Mitteilung)
Zusammenfassung Neue Komplexe der allgemeinen Formeln K3[RhL 3]·2H2O, [PdL]·H2O und [M(LH2)Cl2] mitM = Pd, Pt undLH2 = Bis(o-aminobenzolosulfonyl)ethylendiamin wurden dargestellt und mit Konduktionsmessungen, thermogravimetrischen Analysen, Röntgenstrukturanalysen, IR, Ligandfeld- und1H-NMR-Spektroskopie charakterisiert.相似文献
17.
手性二噁唑啉吡啶铁和镍配合物的制备与表征 总被引:1,自引:0,他引:1
Tridentate bis(oxazolinylpyridine)(1) reacted with nickel chloride or ferrous chloride in anhydrous ethanol to form bis(oxazolinylpyridine) Nickel(Ⅱ) and Iron(Ⅱ) complexes. The stable solid complexes were characterized with IR, UV, MS, XPS and elemental analysis. No stable complexes were formed with bidentate bis(oxazoline)(2) ins- tead of bis(oxazolinylpyridine). 相似文献
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IntroductionTheabilityofdithiocarbamate(dtc)bindingtometalshasbeenknownformanyyears .Itformschelateswithvirtu allyalltransitionmetals.1Thebidentateanionisalsowellknownasabridgebetweentwotransitionmetalcenters.2 Wa ter solubledialkyldithiocarbamatecomplexes… 相似文献
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A selective method has been developed for extraction chromatographic studies of aluminium(III) and its separation from several metal ions with a chromatographic column containing N-n-octylaniline (liquid anion exchanger) coated on silanized silica gel as a stationary phase. The aluminium(III) was quantitatively extracted with the 0.065 mol/L N-n-octylaninine from 0.013 to 0.05 mol/L sodium succinate at a flow rate of 1.0 mL/min. The extracted metal ion has been recovered by eluting with 25.0 mL of 0.05 mol/L hydrochloric acid and estimated spectrophotometrically with aurintricarboxylic acid. The effects of the acid concentration, the reagent concentration, the flow rate and the eluting agents have been investigated. The log-log plots of distribution coefficient (KdAl(III)) versus N-n-octylaniline concentrationin 0.005 and 0.007 mol/L sodium succinate gave theslopes 0.5 and 0.7 respectively and showed theprobable composition of theextracted species was 1:1 (metal to amine ratio) and the nature of extracted species is [RR''NH2+ Al succinate2-] org. .The extraction of aluminium(III) was carried out in the presence of various ions to ascertain the tolerance limit of individual ions. Aluminium(III) has been separated from multicomponent mixtures, pharmaceutical samples and synthetic mixtures corresponding to alloys. A scheme for mutual separation of aluminium(III), indium(III), gallium(III) and thallium(III) has been developed by using suitable masking agents. The method is fast, accurate and precise. 相似文献
20.
Damir A. Safin Maria G. Babashkina Michael Bolte Łukasz Szyrwiel Axel Klein Henryk Kozlowski 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):1739-1745
The reaction of the potassium salt of the N-(thio)phosphorylated thioureas AdNHC(S)NHP(O)(OiPr)2 (HLI , Ad = Adamantyl) and MeNHC(S)NHP(S)(OiPr)2 (HLII ) with Co(II) and Zn(II) in aqueous EtOH leads to [MLI,II 2] chelate complexes. They were investigated by UV-vis, 1H and 31P NMR spectroscopy, and microanalysis. The molecular structures of [MLI 2] were elucidated by single crystal X-ray diffraction analysis. The metal centers in both complexes are found to be in a distorted-tetrahedral O2S2 environment formed by the C=S sulfur atoms and the P=O oxygen atoms of two deprotonated LI ligands. The photoluminescence properties of [ZnLII 2] are also reported. 相似文献