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1.
Hua-Guang Yu Yi Liu Zhi-Cheng TanJia-Xin Dong Teng-Jun ZouXiao-Ming Huang Song-Sheng Qu 《Thermochimica Acta》2003,401(2):217-224
An on-line solution-reaction isoperibol calorimeter has been constructed. The performance of the apparatus was evaluated by measuring the molar enthalpy of solution of KCl in water at 298.15 K. The uncertainty and the inaccurary of the experimental results were within ±0.3% compared with the recommended reference data. Using the calorimeter, the molar enthalpies of reaction for the following two reactions: LaCl3·7H2O(s)+2Hhq(s)+NaAc(s)=La(hq)2Ac(s)+NaCl(s)+2HCl(g)+7H2O(l) and PrCl3·6H2O(s)+2Hhq(s)+NaAc(s)=Pr(hq)2Ac(s)+NaCl(s)+2HCl(g)+6H2O(l), were determined at T=298.15 K, as −(78.3±0.6) and −(97.3±0.5) kJ mol−l, respectively. From the above molar enthalpies of reaction and other auxiliary thermodynamic quantities, the standard molar enthalpies of formation of La(hq)2Ac and Pr(hq)2Ac, at T=298.15 K, have been derived to be −(1535.5±0.7) and −(1536.7±0.6) kJ mol−l, respectively. 相似文献
2.
The product from reaction of lanthanum chloride seven-hydrate with salicylic acid and 8-hydroxyquinoline, La(C7H5O3)2·(C9H6NO), was characterized by IR, elemental analysis, molar conductance, and thermogravimetric analysis. The standard molar enthalpies of solution of [LaCl3·7H2O (s)], [2C7H6O3 (s)], [C9H7NO (s)] and [La(C7H5O3)2·(C9H6NO) (s)] in a mixed solvent of absolute ethyl alcohol, dimethyl formamide (DMF) and perchloric acid were determined by calorimetry to be [LaCl3·7H2O (s), 298.15 K] = −96.45 ± 0.18 kJ mol−1, [2C7H6O3 (s), 298.15 K] = 14.99 ± 0.17 kJ mol−1, [C9H7NO (s), 298.15 K] = −3.86 ± 0.06 kJ mol−1 and [La(C7H5O3)2·(C9H6NO) (s), 298.15 K] = −117.78 ± 0.11 kJ mol−1. The enthalpy change of the reaction
(1) 相似文献
3.
合成了高氯酸镨和咪唑(C3H4N2), DL-α-丙氨酸(C3H7NO2)混配配合物晶体. 经傅立叶变换红外光谱、化学分析和元素分析确定其组成为[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3. 使用具有恒温环境的溶解-反应量热计, 以2.0 mol•L-1 HCl为量热溶剂, 在T=(298.150±0.001) K时测定出化学反应PrCl3•6H2O(s)+2C3H7NO2(s)+C3H4N2(s)+3NaClO4(s)=[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s)+3NaCl(s)+5H2O(1)的标准摩尔反应焓为ΔrHmө=(39.26±0.11) kJ•mol-1. 根据盖斯定律, 计算出配合物的标准摩尔生成焓为ΔfHmө{[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s), 298.150 K}=(-2424.2±3.3) kJ•mol-1. 采用TG-DTG技术研究了配合物在流动高纯氮气(99.99%)气氛中的非等温热分解动力学, 运用微分法(Achar-Brindley-sharp和Kissinger法)和积分法(Satava-Sestak和Coats-Redfern法)对非等温动力学数据进行分析, 求得分解反应的表观活化能E=108.9 kJ•mol-1, 动力学方程式为dα/dt=2(5.90×108/3)(1-α)[-ln(1-α)]-1exp(-108.9×103/RT). 相似文献
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5.
Quan Shi Zhi-Cheng Tan You-Ying Di Bo Tong Zhi-Heng Zhang Li-Xian Sun 《The Journal of chemical thermodynamics》2006,38(12):1701-1705
Low-temperature heat capacity Cp,m of 2,6-dicarboxypyridine (C7H5NO4; CAS 499-83-2) was precisely measured in the temperature range from (80 to 378) K with a high precision automated adiabatic calorimeter. No phase transition or thermal anomaly was observed in this range. The thermodynamic functions [HT − H298.15] and [ST − S298.15] were calculated in the range from (80 to 378) K. The standard molar enthalpy of combustion and the standard molar enthalpy of formation of the compound have been determined, and , by means of a precision oxygen-bomb combustion calorimeter at T = 298.15 K. The thermodynamic properties of the compound were further investigated through differential scanning calorimeter (DSC) and the thermogravimetric (TG) analysis. 相似文献
6.
利用精密自动绝热热量计测定了Nd(Gly)2Cl3·3H2O在80-357K和Pr(Ala)3Cl3·3H2O在80-374K温区的热容. 根据两个化合物的热容计算出了相对于参考温度298.15K的热力学函数(HT?H298.15)和(ST?S298.15). 根据热重(TG)分析结果, 提出了这两个稀土化合物可能的热分解机理. 利用溶解-反应恒温热量计测定相关化合物的溶解焓并设计盖斯热化学循环, 计算出了两个化合物的标准摩尔生成焓. 相似文献
7.
采用熔融硼酸法在200 ℃下合成了一种具有层状结构的新型水合稀土多硼酸盐,Ln[B5O8(OH)2](Ln=Pr,Nd),并利用粉末X射线衍射技术确定了它的结构。Ln[B5O8(OH)2]晶体属于单斜晶系、P21/c空间群,它的基本构建单元(FBB)是由3个BO4和2个BO3组成的双三元环,[B5O12](2Δ+3T)。每一个FBB和邻近的4个FBB通过共用氧原子相连,形成了具有九元环窗口的层状硼酸根基团,稀土离子位于九元环中心附近。CSD:391317。 相似文献
8.
Two pure strontium borates SrB2O4·4H2O and SrB2O4 have been synthesized and characterized by means of chemical analysis and XRD, FT-IR, DTA-TG techniques. The molar enthalpies of solution of SrB2O4·4H2O and SrB2O4 in 1 mol dm−3 HCl(aq) were measured to be −(9.92 ± 0.20) kJ mol−1 and −(81.27 ± 0.30) kJ mol−1, respectively. The molar enthalpy of solution of Sr(OH)2·8H2O in (HCl + H3BO3)(aq) were determined to be −(51.69 ± 0.15) kJ mol−1. With the use of the enthalpy of solution of H3BO3 in 1 mol dm−3 HCl(aq), and the standard molar enthalpies of formation for Sr(OH)2·8H2O(s), H3BO3(s), and H2O(l), the standard molar enthalpies of formation of −(3253.1 ± 1.7) kJ mol−1 for SrB2O4·4H2O, and of −(2038.4 ± 1.7) kJ mol−1 for SrB2O4 were obtained. 相似文献
9.
Ke-Wei Lei Hai-Mei Feng Jun-Long Wen Tian-Pin Shu 《Monatshefte für Chemie / Chemical Monthly》2010,33(3):743-747
Abstract
The 18-metallacrown-6 metallamacrocycle [Fe6(pmshz)6(C4H9NO)6] has been synthesized by the self-assembly reaction of iron ions with N-substituted salicylhydrazide ligands. Six Fe(III) ions and six deprotonated N-propanoyl-4-methylsalicylhydrazide (H3 pmshz) ligands construct a planar 18-membered ring based on Fe–N–N–Fe linkage. Because of the coordination, the ligand enforces the stereochemistry of the Fe(III) ions as a propeller shape with alternating …ΔΛΔΛ… configurations. There is a strong antiferromagnetic exchange interaction between the paramagnetic iron centers. 相似文献10.
Hydrated strontium borate, SrB4O7·3H2O, has been synthesized and characterized by XRD, FT-IR, DTA-TG and chemical analysis. The molar enthalpy of solution of SrB4O7·3H2O in 1 mol dm−3 HCl(aq) was measured to be (21.15 ± 0.29) kJ mol−1. With incorporation of the previously determined enthalpies of solution of Sr(OH)2·8H2O(s) in [HCl(aq) + H3BO3(aq)] and H3BO3 in HCl(aq), and the enthalpies of formation of H2O(l), Sr(OH)2·8H2O(s) and H3BO3(s), the enthalpy of formation of SrB4O7·3H2O was found to be −(4286.7 ± 3.3) kJ mol−1. 相似文献
11.
本文利用水热合成方法,将稀土氧化物与邻苯二乙酸(H2pda)反应得到了2个新颖的稀土配位聚合物{[Ln2(pda)3(H2O)2]·2H2O}n(Ln=Nd(1),La(2))。测定了它们的晶体结构,并进行了X-射线单晶衍射、红外光谱、荧光光谱和热重分析等性质的表征。晶体结构测定表明这2个化合物为异质同晶化合物。属单斜晶系,C2/c空间群。晶体学参数分别为配合物1:a=2.62906(18)nm,b=1.61172(11)nm,c=0.78327(5)nm,β=93.173(5)°,V=3.3139(4)nm3,Z=4,F(000)=1840,μ=3.173mm-1,Dc=1.878g·cm-3,R1=0.0226,wR2=0.0609;配合物2:a=2.6271(14)nm,b=1.6149(8)nm,c=0.7966(4)nm,β=92.850(9),V=3.375(3)nm3,Z=4,F(000)=1816,μ=2.570mm-1,Dc=1.823g·cm-3,R1=0.0466,wR2=0.1416。化合物中邻苯二乙酸配体连接相邻的稀土金属离子,形成复杂的具有stp拓朴构型的三维网络结构。 相似文献
12.
A coordination polymer was synthesized by the reaction of CoCl2 with 1,2,4-triazole-5-one (TO) and charaterized by means of IR and TG–DTG. Single-crystal structure analysis showed that the complex crystallized in the monoclinic space group C2/c: a = 23.105(9) Å, b = 3.5683(2) Å, c = 13.589(6) Å, = 90°, β = 124.038(4)°, γ = 90°, V = 928.4(7) Å3, Z = 4. The standard molar enthalpy of formation of the complex was determined to be (−1034.28 ± 0.95) kJ mol−1. 相似文献
13.
选择分析纯邻苯二甲酸和浓氨水为反应物,合成了邻苯二甲酸氢铵.利用元素分析、FTIR和X-射线粉末衍射技术表征了它的组成和结构.用精密自动绝热热量计测定了它在78~400 K温区的摩尔热容,将该温区的摩尔热容实验值用最小二乘法拟合,得到摩尔热容(Cp,m)随折合温度(X)变化的多项式方程,利用此方程计算出该温区内每隔5 K的舒平热容值和相对于298.15K的各种热力学函数值.另外,依据Hess定律,通过设计合理的热化学循环,利用等温环境溶解-反应热量计分别测定所设计反应的反应物和产物在所选溶剂中的溶解焓,得到该反应的反应焓为△rHθm=(1.787±0.514)kJ·mol-1.最后,利用此反应焓和反应中其他物质的热力学数据计算出邻苯二甲酸氢铵的标准摩尔生成焓为:△fHθm[NH4(C8H5O4),s]=-(912.953±0.628)kJ·mol-1. 相似文献
14.
New hydrated lanthanide phthalates have been hydrothermally prepared with cerium and neodymium in different reaction media involving water or mixed water-ethanol solvent. The monohydrated Ln2(1,2-bdc)3(H2O) (Ln=Ce or Nd) and dihydrated Nd2(1,2-bdc)3(H2O)2 forms have been characterized by single-crystal analysis. Their structures consist of infinite inorganic chains of lanthanide-centered polyhedra linked to each other through the phthalate ligands in order to generate mixed organic-inorganic layered structure. The two hydrated structures differ by the number of terminal water species attached to the lanthanide cations, which induce symmetry change from a triclinic (Nd2(1,2-bdc)3(H2O)2) to an orthorhombic (Nd2(1,2-bdc)3(H2O)2) cell for neodymium whereas the cerium-based phase only exists in the monohydrated form, with two distinct symmetries (orthorhombic or triclinic). Structural comparisons with the other members of the lanthanide phthalate series with identical chemical formula are also discussed. Thermal X-ray diffraction experiment indicates that the transformation from dihydrate form into the monohydrated form does not occur during a heating process. 相似文献
15.
在140℃下,以3-溴-4-甲基苯甲酸和咪唑为配体,通过水热法在甲醇/水混合溶剂中反应24 h合成了锌(Ⅱ)配合物Zn(C3H4N2)2(C8H6O2Br)2。通过元素分析、红外光谱、热重分析和X射线粉末衍射对配合物进行了结构表征,同时用X射线单晶衍射分析确定了其晶体结构。结果表明,其晶体属单斜晶系,空间群为C2/c,晶胞参数:a=13.257(3),b=9.765(2),c=20.494(4),β=107.79(3)°,V=2526.3(9)3,Dc=1.655g·cm-3,μ=4.170mm-1,F(000)=1248,Z=4,最终残差因子R1=0.0552,wR2=0.1378。配合物为单核结构,中心锌(Ⅱ)离子与来自2个3-溴-4-甲基苯甲酸根的2个O原子及2个咪唑分子的2个N原子配位,形成了畸变的四方锥几何体。晶体内,分子间则通过N—H…O氢键作用在ab面形成了层状结构。研究了配合物的发光性质。 相似文献
16.
以乙酰丙酮(Hacac)、邻菲咯啉(phen)、硝酸根为配体,8-羟基喹啉为酸度调节剂合成出一个系列的镧系轻稀土四元配合物Ln(NO3)2(phen)2(CH3COCHCOCH3)(Ln=La,Ce,Pr,Nd,Sm)。配合物的结构与性质由元素分析,IR,1HNMR和TGA等表征。单晶Ce(NO3)2(phen)2(CH3COCHCOCH3)·H2O结构经由X射线衍射仪分析表明,晶体属单斜晶系,空间群P21/n,晶胞参数为a=1.11017(8)nm,b=0.98401(7)nm,c=1.34453(10)nm,β=102.0530(10)°,V=1.43641(18)nm3,Dc=1.715g·cm-3,Z=2,F(000)=742。配合物呈单核结构,中心离子Ce髥配位数为10。 相似文献
17.
合成了无水乳酸配合物(NH4)2[Sr(C3H5O3)4]。用X射线单晶衍射仪对该配合物的晶体结构进行了表征,确定了其组成、空间结构和配位方式。绘制了配合物的Hirshfeld表面和2D指纹图,揭示了分子间的相互作用以及该配合物具有多个配位位点和较强的配位活性。根据相关的晶体数据计算出了该配合物的晶格能及其对应阴离子的摩尔体积,计算得到该配合物的晶格能为2742.9 kJ·mol-1。用等温环境反应-溶解量热计测量了该配合物在298 K超纯水溶剂中的溶解焓。根据Pitzer电解质溶液理论,在298 K下获得了该配合物的无限稀释摩尔溶解焓△sHm∞和Pitzer参数,确定该配合物的△sHm∞为(114.01±0.04) kJ·mol-1。计算了该配合物的表观相对摩尔焓(ΦL)以及不同浓度下溶质和溶剂的相对偏摩尔焓(L1和L2)。最后,根据晶格能和△sHm∞设计了热化学循环,并计算出了阴离子的水合焓值。热重和微商热重曲线进一步揭示了该配合物的结构。 相似文献
18.
本文利用水热合成方法,将稀土氧化物与邻苯二乙酸(H2pda)反应得到了2个新颖的稀土配位聚合物{[Ln2(pda)3(H2O)2]·2H2O}n(Ln=Nd(1),La(2))。测定了它们的晶体结构,并进行了X-射线单晶衍射、红外光谱、荧光光谱和热重分析等性质的表征。晶体结构测定表明这2个化合物为异质同晶化合物。属单斜晶系,C2/c空间群。晶体学参数分别为配合物1:a=2.629 06(18)nm,b=1.611 72(11)nm,c=0.783 27(5)nm,β=93.173(5)°,V=3.313 9(4)nm3,Z=4,F(000)=1 840,μ=3.173 mm-1,Dc=1.878 g·cm-3,R1=0.022 6,wR2=0.060 9;配合物2:a=2.627 1(14)nm,b=1.614 9(8)nm,c=0.796 6(4)nm,β=92.850(9)°,V=3.375(3)nm3,Z=4,F(000)=1 816,μ=2.570 mm-1,Dc=1.823 g·cm-3,R1=0.0466,wR2=0.1416。化合物中邻苯二乙酸配体连接相邻的稀土金属离子,形成复杂的具有stp拓朴构型的三维网络结构。 相似文献
19.
A.S. Monayenkova A.A. Popova L.A. Tiphlova Y.V. Gorushkina A.V. Tsoi I.P. Romanova V.A. Alyoshin 《Thermochimica Acta》2005,430(1-2):83-86
The enthalpies of reactions between alkaline-earth cuprates M2CuO3 (M = Ca, Sr) and hydrochloric acid were measured in a hermetic swinging calorimeter at 298.15 K. The M2CuO3 samples were prepared by solid-phase synthesis from calcium or strontium carbonate and copper oxide and characterized by X-ray powder diffraction, EDX and wet analysis. The standard enthalpies of formation obtained for the cuprates, −1431 ± 4 kJ mol−1 for Ca2CuO3 and −1374 ± 3 kJ mol−1 for Sr2CuO3, are discussed and compared with previous experimental and assessed values. 相似文献