## 3 Results and Discussion  
### Spectral Characteristics Overview for Samples Measured with XRD  
Four polymorphic forms (including the original, untreated control group) of cocoa butter were determined from XRD (Figure 3). The pattern of sample A was closed to type II (\(\alpha\) type), whilst sample B and C patterns were closed to type V (\(\beta\) type) and III (\(\beta^{\prime}\) type) in the studies of [PERSON] and [PERSON] (1966) [8] and [PERSON] et al. (2015) [42], respectively. Regarding sample A, the observation of \(\alpha\) type was consistent with the study of [PERSON] et al. (2015), who observed the single peak at 21.0\({}^{\circ}\) in the wide-angle region (WAXS) obtained from XRD spectra [42]. [PERSON] and [PERSON] (1966) stated that type II (\(\alpha\) type) products would be obtained when the melted cocoa butter was rapidly frozen and stored for several minutes to an hour at 0 \({}^{\circ}\)C [8]. [PERSON] and [PERSON] (2003) mentioned that the transient metastable \(\gamma\) and \(\alpha\) phases were generated when the temperature was below \(-\)15 \({}^{\circ}\)C [39]. However, only \(\alpha\) type was observed in the current study, which may be due to the unstable property of \(\gamma\) type as well as the longer storage time (23-d storage) before measurement [40]. The \(\alpha\) phase was reported to be much more stable than the \(\gamma\) phase and easily formed either by a transformation from the unstable \(\gamma\) or directly from the melt [42; 43; 44; 8; 40]. The \(\gamma\) phase was reported as the least stable of all encountered solid phases and could stay unchanged for at least 10 days only when the preset solidification temperature was lower than \(-\)10 \({}^{\circ}\)C [40]. [PERSON] and [PERSON] (2003) claimed that the \(\gamma\) phase could be detected only after 2 days of crystallization at \(-\)15 \({}^{\circ}\)C or \(-\)20 \({}^{\circ}\)C. When the temperature increased, it transformed into \(\alpha\) type in a short time [39]. For that reason, it is difficult to define the exact melting point of the \(\gamma\) phase, and its melting or disappearing range was estimated to be around \(-\)8 to +5 \({}^{\circ}\)C [40]. [PERSON] et al. (1996) mentioned that the \(\alpha\) type was generated with a cooling rate of 360 \({}^{\circ}\)C/min [45]. Several authors pointed out the rapid freezing of the melted cocoa butter facilitated the \(\alpha\)-type crystallization generation [3; 8; 39]. However, little information on detailed processing and cooling rates was provided. This is the first study that offers specific information on how different types of crystallization are generated under different procedures with distinguished cooling rates, which could be of practical use for the chocolate industry. Although the \(\alpha\) phase is stable, it is unstable at temperatures above 6 \({}^{\circ}\)C and will transfer to \(\beta^{\prime}\) type (form III and IV) at most an hour [40]. Figure 2: Flowchart of the experiments. With regard to sample B, the XRD spectra (Figure 3b) agreed with the observation from [PERSON] et al. (2015) [42], who found the WAXS peak at 19.2\({}^{\circ}\) 2\(\theta\) was more intensive and a 1.3\({}^{\circ}\) and 2.7\({}^{\circ}\) doublet formed in the range of the small angle region (SAXS) at 27.1 \({}^{\circ}\)C after 2309 min [42]. Similar patterns were observed, and Sample B was defined as \(\beta\) (V) type in accordance with the study of [PERSON] and [PERSON] (1966) [8]. As mentioned above, the ability to induce the formation and stabilization of certain polymorphic forms in cocoa butter is vital to producing chocolate with a fairly good quality. The presence of form V (\(\beta\) type) is in high demand as chocolate in this phase presented the desirable characteristics such as gloss, snap, and bloom resistance [4; 7; 9; 46].