Real‐time X‐ray powder diffraction investigations on cocoa butter. I. temperature‐dependent crystallization behavior

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

doi:10.1007/bf02525448

Cited by 65 publications

(71 citation statements)

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“…TAG mixtures also show differences in phase stability. For example, milk fat is β′-stable (6) while cocoa butter has β as the most stable phase (7,8).…”

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confidence: 99%

Crystal packing of a homologous series β′‐stable triacylglycerols

Langevelde

Malssen

Sonneveld

et al. 1999

J Americ Oil Chem Soc

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n = even) triacylglycerols which are β′-stable, Guinier X-ray powder diffraction photographs were used to determine cell parameters and space groups. The powder diffraction patterns are consistent with a pseudo-orthorhombic unit cell with space group Ic2a. Only one axis is changing as a function of chain lengthening. The experimental results were used to propose a β′-crystal packing for triacylglycerols. In contrast to earlier proposed β′-crystal structures, the acyl chains of this structure are not tilted with respect to the methyl-end group plane. Furthermore, with only one molecule in the asymmetric unit, overall orthogonal chain packing is obtained when the intramolecular acyl zigzag planes are parallel.Paper no. J8979 in JAOCS 76, 603-609 (May 1999)KEY WORDS: Crystal packing, fat, triacylglycerol, X-ray diffraction.Polymorphism of fats and triacylglycerols (TAG) is a permanent subject of research because it may have important implications for the manufacturing of many different food products such as chocolate and margarine. Pure TAG crystallize in the different polymorphic phases α, β, and/or β′ and sometimes even several different β′-and/or β-polymorphs exist (1,2). The different polymorphic phases and their variants can be distinguished by X-ray diffraction through typical reflections in the fingerprint region of the X-ray powder diagram (d-spacings from 3.0 to 6.0 Å) (3,4). Table 1 shows the characteristics of the X-ray patterns of the different phases. Depending on the TAG type the most stable phase is either β′ or β. De Jong and Van Soest (5) showed that TAG of the type C n C n+2 C n and C n C n+4 C n+2 (n = even) are normally β′-stable. Most other types are generally β-stable. TAG mixtures also show differences in phase stability. For example, milk fat is β′-stable (6) while cocoa butter has β as the most stable phase (7,8).The phase behavior of pure TAG as well as TAG mixtures is very complex. Their phase transitions are generally irreversible and depend on experimental circumstances such as temperature and time, and their thermal history as is demonstrated by memory effects (9). Knowledge of this behavior, particularly the β′ → β phase transition is very important, especially for the chocolate industry, since unwanted phase transitions of cocoa butter may cause fat bloom, a white appearance of fat crystals on the surface. Therefore, control of these transitions determine to a large extent the quality of chocolate products.Crystal structure information of the different phases is indispensable to understand the mechanism of these transitions. Unfortunately, so far only crystal structures of β-polymorphs of pure TAG have been reported (10-15), all [β-1,2,3-tridecanoyl-glycerol, or tricaprin, or C 10 C 10 C 10 (β-CCC); β-1,2,3-tridodecanoyl-glycerol, or trilaurin, or C 12 C 12 C 12 (β-LLL); β-1,2,3-trihexadecanoyl-glycerol, or tripalmitin, or C 16 C 16 C 16 (β-PPP); and β-2-11-bromoundecanoyl-1,3-didecanoyl-glycerol, or C 10 C 11 Br C 10 (β-CL Br C)] crystallizing in space group P -1. The molecules are i...

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“…TAG mixtures also show differences in phase stability. For example, milk fat is β′-stable (6) while cocoa butter has β as the most stable phase (7,8).…”

mentioning

confidence: 99%

Crystal packing of a homologous series β′‐stable triacylglycerols

Langevelde

Malssen

Sonneveld

et al. 1999

J Americ Oil Chem Soc

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“…Our CB samples also shows XRD patterns which look much like that of β-VI (Figure 1), while its melting point (31.43℃) was closer to β-V (30.8~33.8℃), as reported by Chapman et al (1971) and Wille and Lutton (2001). Malssen et al (1996) also observed that in some CB samples originated from twelve different countries, XRD patterns of β-phase are closer to those of β-VI but their m.p. resembled that of β-V.…”

Section: Resultsmentioning

confidence: 73%

“…Polymorphism is defined as the ability of a substance to exist in more than one crystalline form in a crystal lattice (Oh and Swanson, 2006). This polymorphism, is a critical step in chocolate making, and has been studied extensively in the last century (Wille and Lutton, 1966;Chapman et al, 1971;Malssen et al, 1996;Schenk and Peschar, 2004). Several techniques such as differential scanning colorimetery, light microscopy, pulsed nuclear magnetic resonance, and X-ray diffractometer (XRD) have been used to determine polymorphic structures of lipids (Guthrie et al, 2005).…”

Section: Introductionmentioning

confidence: 99%

“…Several techniques such as differential scanning colorimetery, light microscopy, pulsed nuclear magnetic resonance, and X-ray diffractometer (XRD) have been used to determine polymorphic structures of lipids (Guthrie et al, 2005). Among these methods, XRD is a powerful tool, which provides direct structural information for identifying the types of crystals (Malssen et al, 1996;Langevelde et al, 2001;Schenk and Peschar, 2004;Guthrie et al, 2005). The technique shows at least five different crystalline forms with different characteristic patterns; γ, α, β′ and β (V, VI), in CB (Figure 1).…”

Section: Introductionmentioning

confidence: 99%

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Fat Bloom and Polymorphism in Chocolate Prepared with Modified Tea Seed Oil

Sahari

Zarringhlami²,

Barzegar³

et al. 2013

jtsr

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In order to produce cocoa butter replacer (CBR), tea seed oil was modified with enzymatic interesterification. The modified product was then added to dark chocolate formulation as a replacement for 10%, 15% and 20% of cocoa butter (CB) to study fat bloom formation and polymorphic structure in these samples.Keywords Fat bloom; Polymorphism; Chocolate; Modified tea seed oil Practical ApplicationsAccording to our results, higher levels of fat bloom occurred in the chocolate sample without CBR (chocolate containing 100% CB, CBCH), compared with other chocolate samples. However, among the chocolates containing enzymatic interesterified sample (EIS) at various levels of 10%, 15% and 20%, the chocolate sample containing 10% of EI (EICH) showed lower fat bloom development during storage period (20 days). The results of polymorphic structure evaluation using X-ray diffractometer (XRD) showed new β-crystalline form with the XRD pattern close to that of β-VI and the m.p. appeared similar to β-V in CB. Also, XRD pattern of EIS showed β′-crystalline form in this sample. Presence of two crystalline forms (β and β′) in the EICH revealed that, adding 10% of the CBR prepared in the current study to chocolate formulation had probably no adverse effect on β-crystal formation in the chocolate sample.

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“…Real time XRD studies using laboratory X-ray diffractometers have been carried out to observe the evolving crystalline structure in cocoa butter in both static (Van Malssen et al, 1996, 1996a and sheared crystallisation (Sonwai, 2002). Synchrotron XRD offers improved resolution, rapid data collection and simultaneous small (SAXS) and wide (WAXS) angle measurements, corresponding to the long and short range spacing in the crystal lattice .…”

Section: Introductionmentioning

confidence: 99%

Development of a single droplet freezing apparatus for studying crystallisation in cocoa butter droplets

Talhat

Lister

Moggridge

et al. 2015

Journal of Food Engineering

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a b s t r a c tThe single droplet freezing apparatus described by Pore et al. (2009), which allows crystallisation to be monitored in situ by X-ray diffraction, was modified to allow rapid switching of coolant gas and monitoring by video microscopy. The apparatus was used to study drops of cocoa butter undergoing simulated spray freezing at high cooling rates, e.g. 130 K/min. The transformation of an Ivory Coast cocoa butter to the Form V polymorph was significantly faster in drops ($40 h) than in static bulk samples (10 days) crystallised under isothermal conditions. Phase transformation was observed from Forms I/ II ? III ? IV ? melt ? V, with Form V crystallising directly from the melt at 28.6°C. Numerical simulations of the temperature evolution within the droplet established that the drops are not isothermal, explaining why nucleation was initially observed in the lower (upstream) part of the droplet.

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Real‐time X‐ray powder diffraction investigations on cocoa butter. I. temperature‐dependent crystallization behavior

Cited by 65 publications

References 11 publications

Crystal packing of a homologous series β′‐stable triacylglycerols

Crystal packing of a homologous series β′‐stable triacylglycerols

Fat Bloom and Polymorphism in Chocolate Prepared with Modified Tea Seed Oil

Development of a single droplet freezing apparatus for studying crystallisation in cocoa butter droplets

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