Excess molar enthalpy of binary mixtures of hexane+ethyl benzene, <Emphasis Type="Italic">o</Emphasis>-xylene, <Emphasis Type="Italic">m</Emphasis>-xylene and <Emphasis Type="Italic">p</Emphasis>-xylene at 298.15 K

Summary This paper reports excess molar enthalpies of the binary systems hexane+ethyl benzene, hexane+o-xylene, hexane+m-xylene and hexane+p-xylene at 298.15 K and atmospheric pressure, over the whole composition range. The data was measured directly using a Calvet microcalorimeter. The excess magnitude was correlated to a Redlich-Kister type equation for each mixture. Also, we will discuss the results for the four mixtures studied here and by comparison with the same binary systems but containing propyl propanoate as first component. Finally, we will correlate our results with the Nitta-Chao and the three UNIFAC theoretical approximations.     

Thermochemical properties of benzoic acid derivatives VIII. Enthalpies of combustion and formation of o-, m-, and p- t-butylbenzoic acids

The enthalpies of formation in the crystalline state at 298.15 K of o-, m-, and p-t-butyl-benzoic acids have been determined by static-bomb calorimetry. Vapour-pressure determinations were made by the Knudsen-effusion technique and the sublimation enthalpies at the mean temperatures of the measurement ranges have been derived for the three acids. The values obtained are:

     

3.

Reactions of tetracarbonylcobaltate(-I) with chlorosilanes in ether solvents     

Brian K. Nicholson  Jim Simpson 《Journal of organometallic chemistry》1978,155(2):237-244

The reactions of NaCo(CO)₄ with Me_nSiCl_4?n (n = 0–3) in diethylether (Et₂O) and in tetrahydrofuran (THF) have been studied. Three distinct reaction pathways were recognised which depend on the acidity of the chlorosilane and basicity of solvent. Attack at the silicon centre via the Co atom of Co(CO)₄^? leads to formation of a SiCo bond; reaction involving a CO ligand of Co(CO)₄^? gives clusters R₃SiOCCo₃(CO)₉; and chlorosilane induced attack of Co(CO)₄^? on the solvent gives products derived from THF molecules.     

4.

Electrodeposition of cobalt on stainless steel foils. Preparation of57Co sources for Mössbauer experiments     

R. González-Ramírez  H. Jiménez-Domínguez  O. Solorza-Feria  E. Ordóñez-Regil  A. Cabral-Prieto  S. Bulbulian 《Journal of Radioanalytical and Nuclear Chemistry》1993,174(2):291-298

Conditions for the electrodeposition of⁵⁹Co and⁵⁷Co on stainless steel foils have been studied. A set of electrolytic parameters has been determined to get a reasonably good electrodeposited sample. The⁵⁷Co electrodeposited foil was then introduced in a quartz tube to be annealed in an argon flow. The final product was a 11 Ci Mössbauer source for college experiments which was succesfully tested by obtaining spectra of stainless steel and sodium nitroprusside.     

5.

Nitrosyl derivatives of tricobaltcarbon clusters     

Stephen B. Colbran  Brian H. Robinson  Jim Simpson 《Journal of organometallic chemistry》1984,265(2):199-204

The nitrosyl clusters PPN[YCCo₃(CO)₇(NO)] (Y = Me, Ph, COOH, (C₅H₅)Fe(C₅H₄)) have been prepared in high yield from the reaction of YCCo₃(CO)₉ with PPN(NO₂) in THF, acetone or acetonitrile. Spectroscopic evidence indicates the structure of the nitrosyl anions is derived from that of YCCo₃(CO)₉ by the replacement of two CO ligands on one cobalt atom by a linear, terminal nitrosyl group. The nitrosyl metallates are extremely sensitive to oxidation and attempts to protonate the anions resulted in the reformation of the parent YCCo₃(CO)₉, molecules. The oxidative electrochemistry of the ferrocene complex, PPN[(C₅H₅)Fe(C₅H₄CCo₃(CO)₇(NO)] is also discussed.     

6.

Cytotoxic and NF-κB inhibitory sesquiterpene lactones from Piptocoma rufescens     

Ren Y  Acuña UM  Jiménez F  García R  Mejía M  Chai H  Gallucci JC  Farnsworth NR  Soejarto DD  Carcache de Blanco EJ  Kinghorn AD 《Tetrahedron》2012,68(12):2671-2678

Six new (1-6) and eight known germacranolide-type sesquiterpene lactones, along with several known phenylpropanol coumarates and methylated flavonoids, were isolated from the leaves of Piptocoma rufescens, collected in the Dominican Republic. The new compounds were identified by analysis of their spectroscopic data, with the molecular structure of 3 being established by single-crystal X-ray diffraction. The absolute configurations of the sesquiterpene lactones isolated were determined from their CD and NOESY NMR spectra, together with the analysis of Mosher ester reactions. Bioassay screening results showed the majority of the sesquiterpene lactones isolated (1-13) to be highly cytotoxic toward the HT-29 human colon cancer cell line, with the most potent compound being 15-deoxygoyazensolide (10, IC(50), 0.26 μM). In addition, several of the sesquiterpene lactones exhibited NF-κB (p65) inhibitory activity.     

7.

Simplified model for mass diffusivity estimation based on dynamic pendant drop volume analysis     

Vargas Pedro  Guerrero Junior  Jiménez Maria  Zabala Damelys 《Heat and Mass Transfer》2012,48(1):93-98

We present a simplified correlation for calculating the dissolved gas moles in a pendant drop during the diffusion time, for several drop shapes. After this correlation is determined, the Yang and Gu (Ind Eng Chem Res 44:4474–4483, 2005) dynamic pendant drop volume analysis (DPDVA) method for calculation of mass diffusivity from the pendant drop volume variation against time can be used. We solved the differential equation in cylindrical coordinates for the mass transfer model of the gas diffusion into the liquid inside the pendant drop, using a different characteristic length (L_C), instead of the outer radius of the syringe needle (r_n) used in Yang and Gu (Ind Eng Chem Res 44:4474–4483, 2005) for defining the dimensionless variables. L_C is the relationship between the pendant drop volume and its mass transfer surface area at the initial conditions. The generalized correlation saves time, simplifies the method application and the deviations in the diffusion coefficient calculation respect to the complete Yang and Gu model are below 6%.     

8.

Raman Spectroscopy Analysis of a Playing Card from the 18th Century     

A. C. Prieto  M. Avella  O. Martínez  J. Jiménez  J. L. Alonso  I. Sánchez 《光谱学快报》2013,46(2):114-117

We present the characterization, by means of three complementary experimental techniques (optical microscopy [OM], scanning electron microscopy equipped with energy dispersive X-Ray spectroscopy [SEM-EDX], and micro-Raman spectroscopy [µRaman]), of a card belonging to a deck of the Spanish pattern made in Perú at the time of Virreinato de Perú (18th century). The objective is to obtain detailed information on the pictorial palette used for the decoration of the cards, where two basic colors, red and green, are seen. Small samples from both colored regions were analyzed.     

9.

Creep mechanism of gas-pressure-sintered silicon nitride polycrystals I. Macroscopic and microscopic experimental study     

D. Gómez-García  M. Jiménez-Melendo  A. Domínguez-Rodríguez ‡ 《哲学杂志》2013,93(31):3375-3386

The creep behaviour and microstructure of two silicon nitride ceramics have been investigated. Compressive creep tests were performed at temperatures between 1450 and 1700°C at stresses between 6 and 90?MPa in an Ar atmosphere. The creep behaviour was characterized by a stress exponent lower than one for both materials, with an average value n?≈?0.6 over the whole range of stresses and temperatures, and with apparent activation energies between 470 and 530?kJ?mol^?1. The study of the microstructural evolution revealed the absence of dynamic grain growth and, in some cases, evidence of grain rearrangement. Partial coalescence of cavities was observed only at the highest stress, but this did not result in accelerated creep.     

10.

13C direct detected COCO-TOCSY: a tool for sequence specific assignment and structure determination in protonless NMR experiments     

Balayssac S  Jiménez B  Piccioli M 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2006,182(2):325-329

A novel experiment is proposed to provide inter-residue sequential correlations among carbonyl spins in (13)C detected, protonless NMR experiments. The COCO-TOCSY experiment connects, in proteins, two carbonyls separated from each other by three, four or even five bonds. The quantitative analysis provides structural information on backbone dihedral angles phi as well as on the side chain dihedral angles of Asx and Glx residues. This is the first dihedral angle constraint that can be obtained via a protonless approach. About 75% of backbone carbonyls in Calbindin D(9K), a 75 amino acid dicalcium protein, could be sequentially connected via a COCO-TOCSY spectrum. 49 [Formula: see text] values were measured and related to backbone phi angles. Structural information can be extended to the side chain orientation of aminoacids containing carbonyl groups. Additionally, long range homonuclear coupling constants, (4)J(CC) and (5)J(CC), could be measured. This constitutes an unprecedented case for proteins of medium and small size.     

1 [2] [3] [4] [5] [6] [7] [8] [9] [10] [11] 下一页 » 末  页»

	$\text{ΔH}{}_{\mathrm{f}}{}^{\mathrm{o}}\text{(c, 298.15 K)/kJ mol}{}^{\mathrm{?1}}$	$\text{ΔH}{}_{\mathrm{s}}\text{/kJ mol}{}^{\mathrm{?1}}$
o-t-butylbenzoic acid	476.2 ± 1.9	99.8 ± 0.4	(at 314.6 K)
m-t-butylbenzoic acid	504.3 ± 1.6	103.0 ± 0.5	(at 326.5 K)
p-t-butylbenzoic acid	502.9 ± 1.7	103.8 ± 0.4	(at 334.1 K)

Reactions of tetracarbonylcobaltate(-I) with chlorosilanes in ether solvents

The reactions of NaCo(CO)₄ with Me_nSiCl_4?n (n = 0–3) in diethylether (Et₂O) and in tetrahydrofuran (THF) have been studied. Three distinct reaction pathways were recognised which depend on the acidity of the chlorosilane and basicity of solvent. Attack at the silicon centre via the Co atom of Co(CO)₄^? leads to formation of a SiCo bond; reaction involving a CO ligand of Co(CO)₄^? gives clusters R₃SiOCCo₃(CO)₉; and chlorosilane induced attack of Co(CO)₄^? on the solvent gives products derived from THF molecules.     

Electrodeposition of cobalt on stainless steel foils. Preparation of57Co sources for Mössbauer experiments

Conditions for the electrodeposition of⁵⁹Co and⁵⁷Co on stainless steel foils have been studied. A set of electrolytic parameters has been determined to get a reasonably good electrodeposited sample. The⁵⁷Co electrodeposited foil was then introduced in a quartz tube to be annealed in an argon flow. The final product was a 11 Ci Mössbauer source for college experiments which was succesfully tested by obtaining spectra of stainless steel and sodium nitroprusside.     

Nitrosyl derivatives of tricobaltcarbon clusters

The nitrosyl clusters PPN[YCCo₃(CO)₇(NO)] (Y = Me, Ph, COOH, (C₅H₅)Fe(C₅H₄)) have been prepared in high yield from the reaction of YCCo₃(CO)₉ with PPN(NO₂) in THF, acetone or acetonitrile. Spectroscopic evidence indicates the structure of the nitrosyl anions is derived from that of YCCo₃(CO)₉ by the replacement of two CO ligands on one cobalt atom by a linear, terminal nitrosyl group. The nitrosyl metallates are extremely sensitive to oxidation and attempts to protonate the anions resulted in the reformation of the parent YCCo₃(CO)₉, molecules. The oxidative electrochemistry of the ferrocene complex, PPN[(C₅H₅)Fe(C₅H₄CCo₃(CO)₇(NO)] is also discussed.     

Cytotoxic and NF-κB inhibitory sesquiterpene lactones from Piptocoma rufescens

Six new (1-6) and eight known germacranolide-type sesquiterpene lactones, along with several known phenylpropanol coumarates and methylated flavonoids, were isolated from the leaves of Piptocoma rufescens, collected in the Dominican Republic. The new compounds were identified by analysis of their spectroscopic data, with the molecular structure of 3 being established by single-crystal X-ray diffraction. The absolute configurations of the sesquiterpene lactones isolated were determined from their CD and NOESY NMR spectra, together with the analysis of Mosher ester reactions. Bioassay screening results showed the majority of the sesquiterpene lactones isolated (1-13) to be highly cytotoxic toward the HT-29 human colon cancer cell line, with the most potent compound being 15-deoxygoyazensolide (10, IC(50), 0.26 μM). In addition, several of the sesquiterpene lactones exhibited NF-κB (p65) inhibitory activity.     

Simplified model for mass diffusivity estimation based on dynamic pendant drop volume analysis

We present a simplified correlation for calculating the dissolved gas moles in a pendant drop during the diffusion time, for several drop shapes. After this correlation is determined, the Yang and Gu (Ind Eng Chem Res 44:4474–4483, 2005) dynamic pendant drop volume analysis (DPDVA) method for calculation of mass diffusivity from the pendant drop volume variation against time can be used. We solved the differential equation in cylindrical coordinates for the mass transfer model of the gas diffusion into the liquid inside the pendant drop, using a different characteristic length (L_C), instead of the outer radius of the syringe needle (r_n) used in Yang and Gu (Ind Eng Chem Res 44:4474–4483, 2005) for defining the dimensionless variables. L_C is the relationship between the pendant drop volume and its mass transfer surface area at the initial conditions. The generalized correlation saves time, simplifies the method application and the deviations in the diffusion coefficient calculation respect to the complete Yang and Gu model are below 6%.     

Raman Spectroscopy Analysis of a Playing Card from the 18th Century

We present the characterization, by means of three complementary experimental techniques (optical microscopy [OM], scanning electron microscopy equipped with energy dispersive X-Ray spectroscopy [SEM-EDX], and micro-Raman spectroscopy [µRaman]), of a card belonging to a deck of the Spanish pattern made in Perú at the time of Virreinato de Perú (18th century). The objective is to obtain detailed information on the pictorial palette used for the decoration of the cards, where two basic colors, red and green, are seen. Small samples from both colored regions were analyzed.     

Creep mechanism of gas-pressure-sintered silicon nitride polycrystals I. Macroscopic and microscopic experimental study

The creep behaviour and microstructure of two silicon nitride ceramics have been investigated. Compressive creep tests were performed at temperatures between 1450 and 1700°C at stresses between 6 and 90?MPa in an Ar atmosphere. The creep behaviour was characterized by a stress exponent lower than one for both materials, with an average value n?≈?0.6 over the whole range of stresses and temperatures, and with apparent activation energies between 470 and 530?kJ?mol^?1. The study of the microstructural evolution revealed the absence of dynamic grain growth and, in some cases, evidence of grain rearrangement. Partial coalescence of cavities was observed only at the highest stress, but this did not result in accelerated creep.     

13C direct detected COCO-TOCSY: a tool for sequence specific assignment and structure determination in protonless NMR experiments

A novel experiment is proposed to provide inter-residue sequential correlations among carbonyl spins in (13)C detected, protonless NMR experiments. The COCO-TOCSY experiment connects, in proteins, two carbonyls separated from each other by three, four or even five bonds. The quantitative analysis provides structural information on backbone dihedral angles phi as well as on the side chain dihedral angles of Asx and Glx residues. This is the first dihedral angle constraint that can be obtained via a protonless approach. About 75% of backbone carbonyls in Calbindin D(9K), a 75 amino acid dicalcium protein, could be sequentially connected via a COCO-TOCSY spectrum. 49 [Formula: see text] values were measured and related to backbone phi angles. Structural information can be extended to the side chain orientation of aminoacids containing carbonyl groups. Additionally, long range homonuclear coupling constants, (4)J(CC) and (5)J(CC), could be measured. This constitutes an unprecedented case for proteins of medium and small size.