Crystallization of Cocoa Butter in Cocoa Powder

Cocoa powder quality is determined by its color, flavor, dispersion, and flow properties, which can be controlled via tempering. Design of a cocoa powder tempering profile, however, requires that the mechanism of cocoa butter crystallization in cocoa powder be fully understood. Low-fat (8–12%) and high-fat (20–24%) cocoas were sourced from two commercial manufacturers at varying degrees of alkalization and compared with two commercial cocoa butters. Unrefined paired cocoa powders and cocoa butters sampled from the hydraulic press were also evaluated. Isothermal crystallization kinetics and polymorphism of cocoa powders and cocoa butters were compared at 18, 21, and 24 °C using a direct time-domain nuclear magnetic resonance method, differential scanning calorimetry, and x-ray diffraction. Crystallization was also studied under dynamic tumbling conditions. It was found that cocoa butter in cocoa powder was nucleated by the cocoa powder matrix and transitioned to higher-stability polymorphs more rapidly than bulk cocoa butters. High-fat cocoas also exhibited enhanced crystallization kinetics relative to low-fat cocoas, showing that differences in the cocoa microstructure may influence crystallization behavior. Notably, alkalization did not significantly affect the crystallization behavior of most cocoa powders. Finally, it was found that tumbling conditions led to crystallization of βV and that caking, especially of high-fat cocoas, could be reduced by a static low-temperature hold step prior to tumbling. Overall, these results demonstrated that crystallization of cocoa butter in cocoa powder is influenced both by the intrinsic attributes of the cocoa powder as well as the conditions of the tempering process.     

Crystallization Mechanisms and Rates of Cyclopentane Hydrates Formation in Brine

Clathrate hydrates most often grow at the interface between liquid water and another fluid phase (hydrocarbon) acting as a provider for the hydrate guest molecules, and some transfer through this shell is required for the hydrate growth to proceed, thus self‐limiting the reaction rate. An optical microscope and a horizontal reaction cell are utilized to capture the shell growth phenomenology and to estimate the hydrate layer growth rates from sequential pictures. Cyclopentane (CP) is chosen as the hydrate‐forming molecule to obtain hydrates at low pressure. Experimental hydrate layer growth rates are provided for the CP+brine system, using various combinations of salts and degrees of subcooling.     

Crystallization of calcium sulphate hemihydrate in concentrated phosphoric acid solutions

We aim to show the existence of agglomeration by measuring and modelling secondary nucleation and crystal growth rates of calcium sulphate hemihydrate, CaSO₄-0.5 H₂O, in concentrated phosphoric acid solutions. Using a batch crystallizer we measured the evolution of the population density as a function of supersaturation, H₂SO₄ excess and stirring rates. All experiments were carried out at 90 °C in solutions at 40 wt.% of P₂O₅, simulating the usual conditions for crystallizing hemihydrate in the industrial processes of phosphoric acid production. Nucleation and growth rates were calculated from the population number densities, using the moments analysis method. A model is presented for describing the crystallization process of hemihydrate. It is shown that secondary nucleation and growth rates are quadratic functions of supersaturation. H₂SO₄ concentrations affect supersaturation but at the same supersaturation the growth rates are not significantly different. Nucleation is independent of the stirring rate, whereas growth rates are slightly affected for stirring rates up to 500 rpm. Taking agglomeration into account, the moments method fits very well the experimental data.     

MO对B2O3-Al2O3-SiO2系统玻璃析晶性能的影响

研究了添加BaO、CaO、MgO对B2O3-Al2O3-SiO2系统玻璃析晶性能的影响。用DSC测试了玻璃的析晶温度，用XRD分析了玻璃析晶后的晶相组成，用SEM观察了析出晶粒的形貌特征。结果表明：BaO、CaO均可有效促进BAS玻璃的形成，而MgO易导致玻璃分相。MO-BAS玻璃的析晶温度在770～810℃之间。添加BaO时析出的主晶相为硼酸铝（Al18B4O33）和少量勃来石（Al16B6Si2O37），以针柱状晶为主。用CaO替代BaO，析出的主晶相不变，但析晶能力增加，以细小的粒状晶为主。添加MgO时析出的主晶相为偏硼酸铝（Al4B2O9）和勃来石，晶粒较粗大。     

(Zr0.67Ni0.33)100-xPdx(X=0、5、10、20)非晶合金的晶化行为

通过单辊快淬制备(Zr0.67Ni0.33)100-xPdx(x=0、5、10、20)非晶态合金,利用X射线衍射仪(XRD)、差示扫描量热仪(DSC)和高分辨电镜(HREM)研究了上述合金的晶化过程。结果表明,加入Pd后合金由1个晶化反应转变为2个晶化反应。当Pd的加入量为5at%时,初生相仍为Zr2Ni,随后部分残留非晶转变为Zr2Pd;当Pd的加入量达到10at%时,初生相为Zr2Ni和少量Zr2Pd并存;当Pd的加入量达到20at%时,初生相为明显的Zr2Pd。     

Kinetics of nucleation and growth of L-sorbose crystals in a continuous MSMPR crystallizer with draft tube: Size-independent growth model approach

The experimental data concerning kinetics of a continuous mass crystallization in L-sorbose - water system are presented and discussed. Influences of L-sorbose concentration in a feeding solution and mean residence time of suspension in a working volume of laboratory DT MSMPR crystallizer on the resulting crystal size distributions, thus on the nucleation and growth kinetics, were determined. The kinetic parameter values were evaluated on the basis of size-independent growth (SIG) kinetic model (McCabe’s ΔL law). It was observed that within the investigated range of crystallizer productivity (220–2,200 kg of L-sorbose crystals m⁻³ h⁻¹), a crystal product of mean size Lm from 0.22 to 0.28 mm and CV from 68.8 to 44.0% was withdrawn. The values of linear growth rate show increasing trend (from 6.6·10⁻⁸ to 7.6·10⁻⁸ m s⁻¹) with the productivity enlargement (assuming constant residence time τ=900 s). Occurrence of secondary nucleation phenomena within the circulated suspension, resulting from the crystals attrition and breakage was observed. The parameter values in a design equation, matching linear growth rate and suspension density with nucleation rate were determined.     

Temperature-induced changes in morphology and microstructure of electrospun mullite nanofibers fabricated from a hybrid mullite sol

Mullite nanofibers with small diameter and high surface area are an ideal candidate as the reinforcements in composite materials, and have promising applications in the fields of catalysis, filtration, thermal storage and so forth. In this work, electrospun mullite nanofibers were successfully synthesized using a hybrid mullite sol. The morphology and microstructure of fibers calcined at different temperatures were investigated. The morphology of fibers synthesized at 900 °C is porous with coarse surface, and after crystallization it becomes compact with smooth surface. The densities of fibers increase with the increasing temperatures. At 1200 °C the surface of fibers becomes coarse again, as a result of the grain growth of mullite. The crystallization path of fibers was revealed that the Al-rich mullite (4Al₂O₃·SiO₂) together with amorphous silica formed at 1000 °C, changed into mullite with higher silica contents as temperature further increased, and finally transformed into a stable 3Al₂O₃·2SiO₂ phase at 1200 °C. During this crystallization process, the flow of amorphous silica phase and the formation of mullite crystal structure benefit the densification of fibers, leading to the resultant fibers with fine and compact microstructure. The present findings can provide a guideline for the preparation of the promising high-mechanical mullite nanofibers and the synthesized nanofibers display great potential as reinforcements in structural ceramic composites.     

Evidence of liquid water formation during methane hydrates dissociation below the ice point

Dissociation of small methane hydrate samples formed from water droplets of size 0.25-2.5 mm has been investigated below the ice melting point in the temperature range of 240-273 K, where the self-preservation effect is observed for bulk hydrates. The experiments included optical microscopy observations combined with P-T measurements of the dissociation conditions for the methane hydrates. For the first time, the formation of supercooled liquid water during the hydrate dissociation was reliably detected in the temperature range of 253-273 K. The formation of the liquid phase was visually observed. The induction time of the ice nucleation for the metastable liquid water depended from the dissociation temperature and a size of water droplets formed during the hydrate dissociation. It was found that in the temperature range of 253-273 K values of the dissociation pressure for the small hydrate samples fall on the extension of the water-hydrate-gas equilibrium curve into the metastable region where supercooled water exist. The average molar enthalpy of 51.7 kJ/mol for the dissociation of the small methane hydrate samples in the temperature range of 253-273 K was calculated using Clausius-Clapeyron equation. This value agrees with the enthalpy of dissociation of bulk methane hydrates into water and gas at temperatures above 273 K.     

铝膜沉积温度对铝诱导结晶化多晶硅薄膜性能的影响

以超白玻璃为衬底,采用热丝化学气相沉积法沉积初始非晶硅膜,经自然氧化形成二氧化硅层,最后利用磁控溅射 法在不同衬底温度下沉积铝膜,制备了glass/Si/SiO/Al叠层结构并对其进行铝诱导晶化形成多晶硅薄膜.用X射线衍射,光学显微镜和拉曼光谱对样品进行了分析.结果表明,铝诱导晶化制备的多晶硅薄膜的晶粒大小随着铝膜沉积...     

Effect of DAG on milk fat TAG crystallization

The effect of milk fat and standard DAG on the crystallization behavior of milk fat TAG (MF-TAG) was investigated. When milk fat DAG were added to MF-TAG at the 0.1 wt% level, crystallization was delayed. Racemic purity was shown to be an important factor in the ability of DAG to influence TAG crystallization. Only sn-1,2 isomers of blends of MF-TAG with 0.1 wt% of the racemic mixtures of dipalmitin and diolein increased the activation free energy barrier to MF-TAG nucleation (ΔG _c ) and delayed the subsequent crystallization process by increasing the crystallization induction time (τ_SFC) determined from solid fat content-time measurements. Although crystallization kinetics were affected, the properties of the resulting network structures remained unchanged upon addition of milk fat minor components at the 0.1 wt% level