Foundations of retention in partition chromatography

The connection between the observable output in column chromatography (retention time, retention volume, retention factor, separation factor, etc.) and system properties (hold-up volume, pressure, temperature, isotherm behavior, etc.) is discussed from a practical and mechanistic perspective for gas–liquid chromatography, reversed-phase liquid chromatography, supercritical fluid chromatography, micellar electrokinetic chromatography, and capillary electrochromatography. The unifying feature of these techniques is that retention can be described by a partition model, although not always exclusively. When over simplistic system models are used to explain variation in retention parameters they frequently mask the true reasons for poor repeatability and difficulties in transfer between system. Methods employing relative retention afford higher precision but may contain residual uncorrected errors. For those systems with several separate mechanisms contributing to retention the effective retention parameters can no longer be interpreted by simple partition models. The broadly based and practically focused material in this article affords an illustration of the often complicated relationship between system properties and retention, and the dangers that lurk in simplified retention models if the validity of their underlining approximations is not appropriate for the system under study.     

Degradation of polycaprolactone in supercritical fluids

The degradation of polycaprolactone (PCL) was studied in subcritical and supercritical toluene from 250 to 375 °C at 50 bar. The degradation was also investigated in various solvents like ethylbenzene, o-xylene and benzene at 325 °C and 50 bar. The effect of pressure on degradation was also evaluated at 325 °C at various pressures (35, 50 and 80 bar). The variation of molecular weight with time was analyzed using gel permeation chromatography and modeled using continuous distribution kinetics to evaluate the degradation rate coefficients. PCL degrades by random chain scission in subcritical conditions (250-300 °C) and by chain end scission (325-375 °C) in supercritical conditions in toluene. The degradation of PCL in other solvents at 325 °C was by chain end scission under both subcritical and supercritical conditions indicating that the mode of scission depends on the temperature and not on the supercriticality of the solvent. The thermogravimetric analysis of PCL was investigated at various heating rates (2-24 °C/min) and the activation energy was determined using Friedman, Ozawa and Kissinger methods. It was shown that PCL degrades by random scission at lower temperatures and by chain end scission at higher temperatures again indicating that the mode of scission is dependent on the temperature.     

Supercritical fluid extraction of flumetralin in tobacco

Summary This work evaluates the level of Flumetralin residues in real tobacco samples. Conventional extraction methods were compared with SFE methods in both static and dynamic modes using CO₂ and CO₂ with modifier. Additionally, in the dynamic SFE mode, different collection approaches, such as collection at room temperature without solvent, collection at room temperature in the presence of solvent (hexane) and collection in an ice bath, without solvent, were studied. SFE showed itself to be a promising extraction technique for pesticide residues in tobacco samples.     

红外烤漆机理及轮毂模拟烤漆实验研究

我国汽车、拖拉机及家电等行业的烤漆装机功率约为１６０万ｋＷ,能耗大、能源利用率低而质量差,工件不干亟待解决．文中阐述了红外强化烤漆的机理并利用新研制的高温定向电阻带辐射器对汽车轮毂进行了强化模拟烤漆实验研究并进行了理论计算,结果表明高温定向近距离辐射及优化布置辐射器是缩短烤漆周期、节约能源及确保烤漆质量的重要途径之一．     

Combining ultrasound,vacuum and/or ethanol as pretreatments to the convective drying of celery slices

This work studied three emerging approaches to improve the convective drying (50 °C, 0.8 m/s) of celery. Celery slices of 2 mm thick were pretreated for 5 min using ultrasound (32 W/L, 40 kHz), vacuum (75 kPa vacuum pressure) and ethanol (99.8% v/v, as drying accelerator) applied individually or in combination. To evaluate individual effects of ultrasound and vacuum, the treatments were also performed with distilled water or air medium, respectively. Moreover, the cavitational level was characterized in each condition. Drying kinetics was evaluated tending into account the drying time required by each treatment and the Page’s model parameters. In addition, microstructural effects and shrinkage were evaluated. As results, ethanol combined with ultrasound significantly improved drying kinetics reducing drying time by around 38%. However, vacuum pretreatment did not affect drying kinetics even in combination with ethanol and/or ultrasound. Microstructural evaluation did not evidence cell disruption, suggesting changes in intercellular spaces, pores and/or cell wall permeability. The use of ethanol and vacuum showed a greater effect on shrinkage after pretreatment and after drying, respectively. In conclusion, at the studied conditions, the drying acceleration by vacuum and ultrasound is lower compared to the effect produced using ethanol.     

加热方式对真空冷冻干燥热质传递机理的影响

1引言真空冷冻干燥（简称真空冻干）是多孔介质在低温低压下相变界面移动的耦合传热传质过程，其数学模型带有典型的非线性，难于精确求解［‘，2］。从应用上而言，真空冻干具有设备投资高，能耗大，干燥时间长的缺点。能量的供应即加热方式、升华水汽的流动条件、物料的输运性质是影响真空冻干性能的主要因素间。本文以牛肉的真空冷冻干燥过程为例，建立过程的非稳态数学模型，利用数值求解的结果，结合实验分析，研究了通过千层的辐射加热和通过冻结层的导热加热条件下真空冻干过程中传热传质的机理，分析了加热方式对缩短干燥时间的影响…     

谷物的红外辐射振动流化优化传热传质机理研究

在与工业设备相仿的螺旋提升红外辐射振动流化模拟干燥机与热风固定床中，研究了谷物玉米的干燥特性，分析了物料的干燥动力学的实验规律，阐明了红外辐射振动流化高效、优质优化传热传质的机理。