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Unraveling the Wide Variation in the Thermal Behavior of Crystalline Sucrose Using an Enhanced Laboratory Recrystallization Method
Crystal Growth & Design ( IF 3.8 ) Pub Date : 2018-01-04 00:00:00 , DOI: 10.1021/acs.cgd.7b01526
Yingshuang Lu 1 , Danielle L. Gray 2 , Leilei Yin 3 , Leonard C. Thomas 4 , Shelly J. Schmidt 5
Affiliation  

Recently, we found that sucrose from beet sources exhibited only one large endothermic DSC peak, whereas sucrose from most cane sources exhibited two peaks. Thus, our objective was to unravel the cause of this wide variation in thermal behavior by investigating both commercial and recrystallized sucrose samples, using a variety of analytical techniques, including DSC, HPLC, SXRD, and Micro-CT. With the aid of recrystallization method enhancements and compositional changes, sucrose crystals were intentionally altered to produce a variety of thermal behaviors, including DSC curves exhibiting one or two endothermic peaks or a single peak with either a low (144 °C) or a high (190 °C) Tmonset value. SXRD results for all sucrose crystals studied were consistent with the known structure of sucrose. Thus, polymorphism is not the cause of thermal behavior variation, but rather, the variation is attributed to the influence of occlusion composition and chemistry on thermal decomposition. Micro-CT supported this assertion by revealing the development of large cavities within the sucrose crystal during heat treatment when occlusion composition and chemistry was conducive to thermal decomposition (e.g., low ash content and pH), but showed impeded cavity formation when occlusions contained inhibitory attributes (e.g., high ash content, sulfite, or water removal via grinding).

中文翻译:

使用增强的实验室重结晶方法揭示结晶蔗糖热行为的广泛变化

最近,我们发现甜菜来源的蔗糖仅表现出一个大的吸热DSC峰,而大多数甘蔗来源的蔗糖则表现出两个峰。因此,我们的目标是通过使用包括DSC,HPLC,SXRD和Micro-CT在内的多种分析技术,研究商业和重结晶的蔗糖样品,来揭示热行为如此广泛变化的原因。借助重结晶方法的增强和成分变化,蔗糖晶体被有意地改变以产生多种热行为,包括DSC曲线显示一个或两个吸热峰或一个低(144°C)或高( 190°C)Tmonset值。所有研究的蔗糖晶体的SXRD结果与已知的蔗糖结构一致。因此,多态性不是热行为变化的原因,而是该变化归因于吸留成分和化学成分对热分解的影响。Micro-CT通过揭示在闭塞过程中蔗糖晶体内大孔的形成(当闭塞的成分和化学成分有利于热分解(例如,低灰分和pH))时支持了这一论断,但是当闭塞包含抑制属性时,则表明了空腔的形成受到阻碍(例如,高灰分,亚硫酸盐或通过研磨去除水)。
更新日期:2018-01-04
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