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51.
A. K. Galwey 《Journal of Thermal Analysis and Calorimetry》2005,82(2):423-437
Summary A representational model, proposed to account for the physical changes that accompany the melting of alkali halides, was described
in Part 1 [1]. The liquid is portrayed as undergoing continual dynamic structural reorganization of its constituent ions between
individual small domains, zones of various regular, crystal-type arrays. These alternative arrangements are stabilized by
the enthalpy of melting, which, in liquids, relaxes the restriction for solids that only the single, most stable, crystal
structure can be present. The dynamic character of the melt accounts for its fluid character and the loss of long-range order
[1, 2]. This model is extended here to consider the phase diagrams of binary, common ion, alkali halide mixtures comprehensively
reviewed in [3]. Factors determining whether each of these yields a eutectic, or a solid solution, on cooling are discussed
and several trends in the 70-phase diagrams are identified. Eutectic formation, involving maintenance of the liquid state
below the melting points of the pure components, is ascribed to the participation, in an extended dynamic equilibrium, of
additional domains having the regular structures characteristic of double salts. The known crystalline double binary halides
[3], Li/Cs or Rb/F, Cl, Br or I, melt at temperatures well below those of the simpler pure component salts. It is concluded
that the set/liq model for melting, proposed in [1, 2], accounts for some important properties of the phase diagrams presented
in [3]. 相似文献
52.
Differential
scanning calorimetry (DSC) is a thermal analytical tool for preformulation
studies. Extrapolated melting temperature (TP)
and heat of fusion (ΔHf)
can be used as parameters for optimizing the DSC performance. Two model pharmaceuticals
acetaminophen and nicotinamide are used in this study. Using a factorial design
for the experimental model and matrix analysis the results, the effect of
sample mass, heating rate and the nitrogen flow rate were evaluated on the
ΔHf values
and TP values. Two
levels for each of the procedural variables were used as a balanced experimental
design with two sample sizes, two heating rates and two nitrogen flow rates.
It was found that the change in the heating rate caused significant changes
in the ΔHf
values but not the Tp
values for acetaminophen. However, no significant effect was found for the Tp value but ΔHf value was affected to a
certain extent for nicotinamide. 相似文献
53.
Anna B. DenisovaVyacheslav Ya. Sosnovskikh Wim Dehaen Suzanne ToppetLuc Van Meervelt Vasiliy A. Bakulev 《Journal of fluorine chemistry》2002,115(2):183-192
Reaction of 2-hydrazinothiazoles 1 with 1-thienyl- and 1-furyl-1,3-butanediones 2a,b in methanol in the presence of hydrochloric acid mainly leads to a mixture of pyrazoles 3 and pyrazolines 4 or pyrazoles 3 and 5 in strong acidic conditions. Isomeric hydrazones 6 and pyrazolines 4 were formed and isolated in these reactions in the absence of hydrochloric acid. It has been shown that the regioselectivity in the reaction of diketones 2 with hydrazine 1 is governed by both the concentration of acid and the nature of substituents in the 1,3-diketones 2. Cyclization of hydrazones 6 is shown to occur under milder conditions than dehydration for pyrazolines 4. The new heterocyclic compounds were prepared and fully characterized by NMR spectra and by X-ray analysis for 3c. 相似文献
54.
The enthalpies of sublimation and fusion and triple-point temperatures of 2-bromo-. 3-bro-mo- and 4-bromobenzoic acids have been determined precisely by sublimation calorimetry, drop calorimetry and differential thermal analysis. The measurements of sublimation enthalpy of the three acids were made at 333, 348 and 363 K, respectively, using a Tian-Calvet microcalorimeter equipped with Knudsen effusion cells. The derived standard molar enthalpies of sublimation at 298.15 K are (95. 94±0. 41), (99. 20± 0.18), and (103. 08±0. 59) kJ · mol-1for the 2-bromo-, 3-bromo- and 4-bromobenzoic acids, respectively. In addition, the saturated vapour pressure of these compounds was also calculated on the basis of the sublimation experiments. The enthalpy of fusion, the triple-point temperatures and the mole fraction purities of the samples of the investigated substances were measured using the mean temperature version DTA apparatus developed by the CTM of the CNRS in Marseille. The triple-point temperature and the 相似文献
55.
56.
In this study, immunization with a vaccine consisting of multiple F(abt’)2 fragments of affinity-purified antitetanus toxoid antibodies covalently bound to a carrier protein successfully induced antitetanus
toxoid antibodies. Further studies showed that this vaccine preparation contained no biologically detectable tetanus antigen.
The induced antitetanus antibody (Ab1t’) titer was higher than the titer of antibodies binding control antigens. The immunizing
F(abt’)2 preparation did not elicit a secondary antitetanus response from mice primed with tetanus toxoid and, hence, appeared free
of tetanus epitopes. The specificity of Ab1t’ was established by absorption and inhibition with antigen. Immunization with
antitetanus F(abt’)2 (Ab1t’) fragments appears to have elicited naturally occurring autologous antitetanus toxoid antibody (Ab1t’) through an
idiotypic pathway. As predicted by network theory, anti-idiotype (Ab2) and antitetanus (Ab1t’) cycled reciprocally. Clonotypic
characterization of Ab1t’ using isoelectric focusing and affinity immunoblotting showed increases in Ab1t’ titer to be the
result of increased synthesis by limited subsets of antitetanus toxoid B-cell clones and not increased synthesis by multiple
clones, as is characteristic of antigen-driven Ab1 responses. Many Ab1 and Ab1t’ clonotypes had identical pIs, suggesting
that they either share V region genes or are the product of the same B-cell clones. These findings indicate that immunization
with polyclonal multivalent Ab1 preparations can trigger active synthesis of antibodies with the same specificity. The results
provide further evidence for naturally occurring idiotypic cascades that could be exploited for studies of catalytic antibodies. 相似文献
57.
58.
水溶性金属卟啉肿瘤靶向磁共振成像造影剂的研究 总被引:5,自引:0,他引:5
利用显微荧光-阿达玛变换三维图像分析研究了Cu-TSPP,Mn-TSPP,Cu-TMAP,Mn-TMAP4种水溶性金属卟啉人细胞间质进入肿瘤细胞内的富集过程,对金属卟啉的自旋-晶格驰豫性能(R1)的天空结果表明,Mn(Ⅱ)卟啉配合物的R1、值结Gd-DTPA提高1.5-2倍。 相似文献
59.
Measurement of the degree of crystallinity of the polymer matrix in a composite is complicated by the presence of the reinforcing additive. This is particularly the case in APC-2 in which as much as 70% can be carbon fibre. A First Law procedure, developed for determining the degree of crystallinity of PEEK, which involves direct measurement of the enthalpy changes associated with melting, crystallization and heat capacity changes, has found to be an effective method for the determination of the crystallinity of the PEEK matrix. The procedure has been applied to carbon fibre and glass fibre PEEK composites. 相似文献
60.
Nb4W13O47, a member of the solid solution series Nb8−nW9+nO47 (0?n?5), crystallizes in a threefold superstructure of the tetragonal tungsten bronze structure. While the oxidation of this reduced phase at TOX=1200 °C leads to a separation into the thermodynamically stable phases, lower oxidation temperatures result in products that comprise new structural elements and ordering variants. The characterization of the oxidation products obtained at TOX=1000 °C was performed by scanning transmission electron microscopy applying a high-angle annular dark field detector. At the selected imaging conditions (Z contrast), not only the metal positions are revealed by this technique but valuable additional information about the elemental distribution can be obtained simultaneously. 相似文献