Real‐time X‐ray powder diffraction investigations on cocoa butter. II. The relationship between melting behavior and composition of β‐cocoa butter

Malssen, Kees van; Peschar, R.; Schenk, H.

doi:10.1007/bf02525449

Cited by 46 publications

(32 citation statements)

References 5 publications

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“…DSC pans were stored for different time periods (from 5 min to 10 days) in incubators set at 24°C prior to melting in the DSC at a rate of 5°C/min. The polymorphic state of the studied samples was related to the melting ranges published by van Malssen et al 5,6 crystal network. 43,44 The structural strength of a fat crystal network will be greatly affected by the interactions between the microstructural features (both primary and secondary), as well as the size of crystal structures present and the solid fat content of the network.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

Crystallization Dynamics of Shear Worked Cocoa Butter

Campos

Marangoni

2014

Crystal Growth & Design

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Control of heat and mass transfer conditions during chocolate manufacture is a critical factor influencing product quality and performance. The molecular basis for specific tempering protocols developed by the chocolatiers, and used widely by the food industry, is poorly understood. Here we show that cooling and shear rates applied during cocoa butter crystallization affect the incorporation of specific triacylglycerol (TAG) molecular species onto the surface of growing seed crystals, thus affecting the different structural levels in a cocoa butter crystal network. In this work, the effects of shear work on the different structural levels in cocoa butter are determined. Results from this research show different compositions during the early stages of static crystallization at different cooling rates. In other words, there is selective attachment of TAG species onto growing crystal surfaces, leading to fractional crystallization. With the application of shear, differences between cooling rates became negligible. Shear appears to enhance the formation of mixed crystal in the growing crystals, leading to faster crystallization kinetics, the formation of a higher number of smaller crystals, and a mechanically stronger crystal network. ■ INTRODUCTIONIn the manufacturing of chocolate products, the molten chocolate mass is processed under specific shear and cooling conditions with the aim of crystallizing cocoa butter into an ordered crystalline structure. Cocoa butter is chocolate's main fat component; therefore, its structure will directly affect the product's final physical properties such as contraction, snap, gloss, melting properties, and bloom resistance. This controlled crystallization is known as tempering. The purpose of tempering is to produce 1−3% of the desired highly ordered β V seed crystals, which will subsequently serve as nuclei for the rest of the mass to crystallize. 1−4 If molten chocolate mass were to be cooled directly at cooling tunnel or ambient temperatures, cocoa butter would crystallize in the metastable α II and β′ III−IV forms. 5−8 This results in a dull, soft, low melting point chocolate, prone to bloom.During tempering, the chocolate mass is cooled to 27−29°C to induce nucleation of both stable and unstable crystals. The temperature is then raised to 30−33°C to promote transformation of seed crystals to the stable β V form and melt unstable crystals. The temperature set points used vary by recipe. The tempered chocolate mass is then rapidly cooled to complete crystallization of the fat phase, yielding chocolate with desired quality attributes. 1−4 All methods of tempering, from small-hand tempering to large industrial scales, involve controlled cooling and some element of shear. Shear improves heat and mass transfer of molten cocoa butter, helping overcome kinetic barriers for nucleation and growth. 9 Shorter induction times for crystallization in cocoa butter 10 and chocolate 11,12 when processed under shear suggest that shear affects nucleation. The effect of shear on secondary nucleati...

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Section: ■ Results and Discussionmentioning

confidence: 99%

Crystallization Dynamics of Shear Worked Cocoa Butter

Campos

Marangoni

2014

Crystal Growth & Design

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“…In the present study, they were considered as a single crystalline element in the interpretation of the results (Sato, 2001). Using X-ray diffraction, Van Malssen et al (1996) also had difficulties to distinguish the polymorphs III and IV and even questioned the independent existence of these crystalline forms. Loisel et al (1998), using dSC (scanning rate equal to 0.1 °C/min), found that crystallization of form IV begins before the complete crystallization of form III, which causes an overlap effect or close proximity of the corresponding peaks.…”

Section: Polymorphic Transitions (Dsc)mentioning

confidence: 89%

Physicochemical properties of Brazilian cocoa butter and industrial blends. Part II Microstructure, polymorphic behavior and crystallization characteristics

Ribeiro¹,

Basso²,

Gonçalves³

et al. 2012

Grasas y Aceites

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The microstructural behavior of industrial standardized cocoa butter samples and cocoa butter samples from three different Brazilian states is compared. The cocoa butters were characterized by their microstructural patterns, crystallization kinetics and polymorphic habits. The evaluation of these parameters aided in establishing relationships between the chemical compositions and crystallization behavior of the samples, as well as differentiating them in terms of technological and industrial potential for use in tropical regions.<br><br>En este trabajo se presenta el comportamiento de la microestructura y la cristalización de mantecas de cacao representativas de las mezclas industriales, y de la manteca de cacao original de tres regiones geográficas diferentes de Brasil. Las muestras se evaluaron de acuerdo a la microestructura, la cinética de cristalización y el comportamiento polimórfico. La evaluación de estos parámetros nos permite establecer relaciones entre la composición química y el comportamiento de la cristalización de las muestras, así como las diferencias sobre la adecuación del potencial tecnológico e industrial para su aplicación en las regiones tropicales

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“…By contrast, using only DSC, Huyghebaert and Hendrickx [6] found all six of Wille and Lutton's forms and gave the conditions required to reproduce them. Van Malssen et al [7] suggested the existence of only one b 0 polymorph -an amalgam of form III and IV. They also argued that forms V and VI were not unique polymorphs, but rather different sub-phases [8].…”

Section: Introductionmentioning

confidence: 99%

Raman spectroscopy of the polymorphic forms and liquid state of cocoa butter

Bresson

Rousseau

Ghosh

et al. 2011

Euro J Lipid Sci & Tech

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Raman spectroscopy was used to characterize the polymorphs and liquid state of cocoa butter, with emphasis placed on the evolution of the ester carbonyl stretching region (1800–1700 cm−1), along with complementary analysis and comparison of the Raman‐active CC (1200–1000 cm−1), CC (1660 cm−1), CH (3000–2700 cm−1) and CH2 (1500–1250 cm−1) vibrational modes. Unique Raman signatures were obtained for all cocoa butter polymorphs, with their identity confirmed using DSC and XRD. The ester carbonyl region permitted polymorph discrimination due to differences in the number of modes, their relative frequencies and their full‐widths at half‐maximum. The CC stretching modes, which provided insight into the trans/gauche content, were polymorph‐independent. CH stretching generally increased with polymorph stability, indicating the dominance of antisymmetric CH methylene vibrations as the cocoa butter crystal lattice became more ordered. The change in the intensities of the CH stretching bands used to probe the order–disorder transition of forms IV, V and VI hinted at pre‐melt structural changes mostly in forms IV and V. Overall, Raman spectroscopy clearly demonstrated that the different functional groups studied could be characterized independently, allowing for the understanding of their role in cocoa butter polymorphism.Practical applications: Fat bloom is the unwanted, uncontrolled re‐crystallization or polymorphic transition of CB form V crystals into form VI normally caused by the migration of lower‐melting fats (e.g. in centre‐filled products) and/or temperature fluctuations during storage. In its mildest form, it appears as an overall dulling of the chocolate surface. In its extreme form, the appearance of the chocolate deteriorates significantly with the development of distinct white patches. Though forms V and VI can be clearly distinguished via XRD, we present evidence that Raman spectral characterization of the ester carbonyl stretching (1800–1700 cm−1), CC (1200–1000 cm−1), CC (1660 cm−1), CH (3000–2700 cm−1) and CH2 (1500–1250 cm−1) vibrational modes yields distinct liquid–solid and polymorph‐dependent differences in CB. From a practical standpoint, the unique signatures associated with forms V and VI offer novel possibilities in the study of fat bloom formation, such as the development of predictive tools.

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Real‐time X‐ray powder diffraction investigations on cocoa butter. II. The relationship between melting behavior and composition of β‐cocoa butter

Cited by 46 publications

References 5 publications

Crystallization Dynamics of Shear Worked Cocoa Butter

Crystallization Dynamics of Shear Worked Cocoa Butter

Physicochemical properties of Brazilian cocoa butter and industrial blends. Part II Microstructure, polymorphic behavior and crystallization characteristics

Raman spectroscopy of the polymorphic forms and liquid state of cocoa butter

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