66 EMULSIONS
butter has a higher likelihood of crystallizing than shea olein.
Visual inspection and pH The pH remained between 5.2 and 5.3 throughout the study, with no visual changes observed. The emulsions were stable under the tested conditions.
X-ray
XRD identified crystallization. Formulation A, with only Lipex SheaLiquid TR, showed no crystal peaks at any storage temperature (Figure 1). Therefore, the identified peaks are attributed to the addition of Lipex 102, which increased crystallinity. In the short-spacing for all emulsions,
including Formulation A, a broad area was observed, representing the emulsifier system to the greatest extent.15
In this study, a liquid
polyglucoside ester was used. A crystalline glucoside ester would have produced distinct peaks along with an amorphous area.16 Both WAXS (short space) and SAXS (long
space) characterized crystallization. Long space responses showed distinct peaks for triple chain (3L) and double chain (2L) packing, while short space peaks were weaker. Formulation B showed no crystallization
at 25°C. At 20°C, crystallization appeared after three months in the long spacing area (d-spacing of 44 Å), indicating double packing. The short spacing peak was too weak to determine the polymorphic form. At 20°C, formulations C and D showed
crystallization peaks after one week, with d-spacings of 3.9, 4.2, 34, 45, and 69 Å, indicating triple chain SOS in the beta prime phase.17 Tristearin in the beta phase crystallizes in double chain packing with a chain length of 45 Å.18
At
25°C, formulation C showed crystallization after one month (d-spacing of 45 Å) (Figure 2). Formulation D, with the highest Lipex 102,
showed double chain packing at 45 Å after one week, growing throughout the period. The 3-L packing appeared after three months.
Formulation A
■ 3 Months at 25°C
■ 3 Months at 20°C
■ Time Zero 0.100 1.000 10.000 Formulation B
■ 3 Months at 25°C
■ 3 Months at 20°C
■ Time Zero 0.100 1.000 10.000 100.000µm 0.1
Figure 4: Droplet size distribution. X-axis Droplet size (µm). Day 0 in the bottom and 3 months storage at 20 and 25 °C respectively at the top
PERSONAL CARE November 2025 1 10 100 100.000µm 0.1 1 10 100 Formulation C at 25°C
■ Months 3 ■ Months 1 ■ Week 1 ■ Day 1 ■ Time Zero
0.1 1 10 100 100.00 10.00 1.00 100.00 10.00 1.00
Figure 2: XRD for formulations C and D. Merged SAXS/WAXS diagrams where the x-axis represents the d-spacing for formulations C and D at 20 and 25°C. Day 0 in the bottom and 3 months storage at 20°C at the top. The X-axis shows distance in Angstrom
Formulation A■ Formulation B ■ Formulation C ■ Formulation D ■
18 16 14 12 10 8 6 4 2 0
-2 0.1 1 10 100 µm Figure 3: Particle size distribution. X-axis Particle size distribution (µm) for the freshly made formulations
Droplet size measurements On day one, all emulsions showed a monodisperse droplet size distribution, ranging from 1.4 to 2.1 µm (Figure 3). At 20°C and 25°C, formulations A and B
remained monodisperse. Formulation A’s droplet size was 1.5 µm initially and remained stable.
Formulation C at 20°C
■ Months 3 ■ Months 1 ■ Week 1 ■ Day 1 ■ Time Zero
1000µm 0.1 1 10 Formulation D at 25°C
■ Months 3 ■ Months 1 ■ Months 1 ■ Day 1 ■ Time Zero
1000µm
Figure 5: Droplet size distribution. X-axis Droplet size (µm). Day 0 in the bottom and three months storage at 20°C at the top
www.personalcaremagazine.com 100
Formulation B started at 1.9 µm and ended at 1.8 µm (20°C) and 1.7 µm (25°C) (Figure 4). Formulations C and D transitioned from monodisperse to polydisperse systems at both 20°C and 25°C (Figure 5). Formulation C started with a droplet size of 1.7 µm and developed a two-domain system (21.8 µm) at 20°C after
Formulation D at 20°C
■ Months 3 ■ Months 1 ■ Week 1 ■ Day 1 ■ Time Zero
1000µm 100.00 10.00 Formulation C at 25°C 1.00 100.00 10.00 Formulation D at 25°C 1.00 Formulation C at 20°C
■ Month 3 ■ Month 1 ■ Week 1 ■ Day 1 ■ Day 0 Formulation D at 20°C
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