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Keywords = Wide-Angle X-ray Scattering (USAXS/SAXS/WAXS)

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23 pages, 32973 KB  
Article
From Nucleation to Fat Crystal Network: Effects of Stearic–Palmitic Sucrose Ester on Static Crystallization of Palm Oil
by Fien De Witte, Ivana A. Penagos, Davy Van de Walle, Andre G. Skirtach, Koen Dewettinck and Filip Van Bockstaele
Foods 2024, 13(9), 1372; https://doi.org/10.3390/foods13091372 - 29 Apr 2024
Cited by 4 | Viewed by 2505
Abstract
Palm oil (PO), a semi-solid fat at room temperature, is a popular food ingredient. To steer the fat functionality, sucrose esters (SEs) are often used as food additives. Many SEs exist, varying in their hydrophilic-to-lipophilic balance (HLB), making them suitable for various food [...] Read more.
Palm oil (PO), a semi-solid fat at room temperature, is a popular food ingredient. To steer the fat functionality, sucrose esters (SEs) are often used as food additives. Many SEs exist, varying in their hydrophilic-to-lipophilic balance (HLB), making them suitable for various food and non-food applications. In this study, a stearic–palmitic sucrose ester with a moderate HLB (6) was studied. It was found that the SE exhibited a complex thermal behavior consistent with smectic liquid crystals (type A). Small-angle X-ray scattering revealed that the mono- and poly-esters of the SE have different packings, more specifically, double and single chain-length packing. The polymorphism encountered upon crystallization was repeatable during successive heating and cooling cycles. After studying the pure SE, it was added to palm oil, and the crystallization behavior of the mixture was compared to that of pure palm oil. The crystallization conditions were varied by applying cooling at 20 °C/min (fast) and 1 °C/min (slow) to 0 °C, 20 °C or 25 °C. The samples were followed for one hour of isothermal time. Differential scanning calorimetry (DSC) showed that nucleation and polymorphic transitions were accelerated. Wide-angle X-ray scattering (WAXS) unraveled that the α-to-β′ polymorphic transition remained present upon the addition of the SE. SAXS showed that the addition of the SE at 0.5 wt% did not significantly change the double chain-length packing of palm oil, but it decreased the domain size when cooling in a fast manner. Ultra-small-angle X-ray scattering (USAXS) revealed that the addition of the SE created smaller crystal nanoplatelets (CNPs). The microstructure of the fat crystal network was visualized by means of polarized light microscopy (PLM) and cryo-scanning electron microscopy (cryo-SEM). The addition of the SE created a finer and space-filling network without the visibility of separate floc structures. Full article
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22 pages, 8785 KB  
Article
Insights in the Structural Hierarchy of Statically Crystallized Palm Oil
by Fien De Witte, Ivana A. Penagos, Kato Rondou, Kim Moens, Benny Lewille, Daylan A. Tzompa-Sosa, Davy Van de Walle, Filip Van Bockstaele, Andre G. Skirtach and Koen Dewettinck
Crystals 2024, 14(2), 142; https://doi.org/10.3390/cryst14020142 - 30 Jan 2024
Cited by 8 | Viewed by 2610
Abstract
Palm oil (PO) is still widely used for the production of all types of food products. Due to its triacylglycerol (TG) composition, PO is semisolid at ambient temperature, offering possibilities for many applications. In order to tailor the fat crystal network for certain [...] Read more.
Palm oil (PO) is still widely used for the production of all types of food products. Due to its triacylglycerol (TG) composition, PO is semisolid at ambient temperature, offering possibilities for many applications. In order to tailor the fat crystal network for certain applications, it remains imperative to understand the structural build-up of the fat crystal network at the full-length scale and to understand the effect of processing conditions. In this study, PO was crystallized under four temperature protocols (fast (FC) or slow (SC) cooling to 20 °C or 25 °C) and was followed for one hour of isothermal time. A broad toolbox was used to fundamentally unravel the structural build-up of the fat crystal network at different length scales. Wide-angle and small-angle X-ray scattering (WAXS and SAXS) showed transitions from α-2L to β’-2L over time. Despite the presence of the same polymorphic form (β’), chain length structure (2L), and domain size, ultra-small-angle X-ray scattering (USAXS) showed clear differences in the mesoscale. For all samples, the lamellar organization was confirmed. Both cooling speed and isothermal temperature were found to affect the size of the crystal nanoplatelets (CNPs), where the highest cooling speed and lowest isothermal temperature (FC and 20 °C) created the smallest CNPs. The microstructure was visualized with polarized light microscopy (PLM) and cryo-scanning electron microscopy (cryo-SEM), showing clear differences in crystallite size, clustering, and network morphology. Raman spectroscopy was applied to confirm differences in triglyceride distribution in the fat crystal network. This study shows that both cooling rate and isothermal temperature affect the fat crystal network formed, especially at the meso- and microscale. Full article
(This article belongs to the Special Issue Feature Papers in Crystals 2023)
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10 pages, 1822 KB  
Article
Phase Evolution and Textural Changes during the Direct Conversion and Storage of CO2 to Produce Calcium Carbonate from Calcium Hydroxide
by Meishen Liu and Greeshma Gadikota
Geosciences 2018, 8(12), 445; https://doi.org/10.3390/geosciences8120445 - 30 Nov 2018
Cited by 11 | Viewed by 6602
Abstract
The increasing use of energy resources recovered from subsurface environments and the resulting carbon imbalance in the environment has motivated the need to develop thermodynamically downhill pathways to convert and store CO2 as water-insoluble calcium or magnesium carbonates. While previous studies extensively [...] Read more.
The increasing use of energy resources recovered from subsurface environments and the resulting carbon imbalance in the environment has motivated the need to develop thermodynamically downhill pathways to convert and store CO2 as water-insoluble calcium or magnesium carbonates. While previous studies extensively explored aqueous routes to produce calcium and magnesium carbonates from CO2, there is limited scientific understanding of the phase evolution and textural changes during the direct gas–solid conversion routes to produce calcium carbonate from calcium hydroxide, which is one of the abundant constituents of alkaline industrial residues. With increasing interest in developing integrated pathways for capturing, converting, and storing CO2 from dilute flue gases, understanding the composition of product phases as they evolve is essential for evaluating the efficacy of a given processing route. Therefore, in this study, we investigate the phase evolution and the corresponding textural changes as calcium hydroxide is converted to calcium carbonate under the continuous flow of CO2 at an ambient pressure of 1 atm with continuous heating from 30 °C to 500 °C using in-operando wide angle X-ray scattering (WAXS), small angle X-ray scattering (SAXS), and ultrasmall angle X-ray scattering (USAXS) measurements. Full article
(This article belongs to the Special Issue Carbon Sequestration)
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14 pages, 3360 KB  
Article
Connecting the Morphological and Crystal Structural Changes during the Conversion of Lithium Hydroxide Monohydrate to Lithium Carbonate Using Multi-Scale X-ray Scattering Measurements
by Greeshma Gadikota
Minerals 2017, 7(9), 169; https://doi.org/10.3390/min7090169 - 14 Sep 2017
Cited by 20 | Viewed by 7066
Abstract
While CO2 storage technologies via carbon mineralization have focused on the use of earth-abundant calcium- and magnesium-bearing minerals, there is an emerging interest in the scalable synthesis of alternative carbonates such as lithium carbonate. Lithium carbonate is the carbonated end-product of lithium [...] Read more.
While CO2 storage technologies via carbon mineralization have focused on the use of earth-abundant calcium- and magnesium-bearing minerals, there is an emerging interest in the scalable synthesis of alternative carbonates such as lithium carbonate. Lithium carbonate is the carbonated end-product of lithium hydroxide, a highly reactive sorbent for CO2 capture in spacecraft and submarines. Other emerging applications include tuning the morphology of lithium carbonates synthesized from the effluent of treated Li-bearing batteries, which can then be reused in ceramics, glasses, and batteries. In this study, in operando Ultra-Small-Angle, Small-Angle, and Wide-Angle X-ray Scattering (USAXS/SAXS/WAXS) measurements were used to link the morphological and crystal structural changes as lithium hydroxide monohydrate is converted to lithium carbonate. The experiments were performed in a flow-through reactor at PCO2 of 1 atm and at temperatures in the range of 25–500 °C. The dehydration of lithium hydroxide monohydrate to form lithium hydroxide occurs in the temperature range of 25–150 °C, while the onset of carbonate formation is evident at around 70 °C. A reduction in the nanoparticle size and an increase in the surface area were noted during the dehydration of lithium hydroxide monohydrate. Lithium carbonate formation increases the nanoparticle size and reduces the surface area. Full article
(This article belongs to the Special Issue Carbon Capture and Storage via Mineral Carbonation)
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