An improved approach for evaluating the semicrystalline lamellae of starch granules by synchrotron SAXS

Zhang, Binjia, Xie, Fengwei, Wang, David K., Zhao, Siming, Niu, Meng, Qiao, Dongling, Xiong, Shanbai, Jiang, Fatang, Zhu, Jie and Yu, Long (2017) An improved approach for evaluating the semicrystalline lamellae of starch granules by synchrotron SAXS. Carbohydrate Polymers, 158 29-36. doi:10.1016/j.carbpol.2016.12.002

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Author Zhang, Binjia
Xie, Fengwei
Wang, David K.
Zhao, Siming
Niu, Meng
Qiao, Dongling
Xiong, Shanbai
Jiang, Fatang
Zhu, Jie
Yu, Long
Title An improved approach for evaluating the semicrystalline lamellae of starch granules by synchrotron SAXS
Journal name Carbohydrate Polymers   Check publisher's open access policy
ISSN 0144-8617
1879-1344
Publication date 2017-02-20
Year available 2016
Sub-type Article (original research)
DOI 10.1016/j.carbpol.2016.12.002
Open Access Status File (Author Post-print)
Volume 158
Start page 29
End page 36
Total pages 8
Place of publication Kidlington, Oxford, United Kingdom
Publisher Pergamon Press
Language eng
Subject 1605 Organic Chemistry
2507 Polymers and Plastics
2505 Materials Chemistry
Abstract A fitting method combined with a linear correlation function was developed as an improved approach for the SAXS analysis of the semicrystalline lamellae of starch granules. Using a power-law function with two Gaussian plus Lorentz functions, the SAXS pattern was resolved into sub-patterns of the net lamellar peak and the power-law scattering plus scattering background (PL + B). The ratio of the net lamellar peak area (A) to the total scattering area (A) was proposed equal to the proportion of the lamellae within the starch granule (P). Along with this fitting method, we obtained a better profile of linear correlation function, with the elimination of the interference of non-lamellar amorphous starch (i.e., amorphous growth rings). Then, we could accurately calculate the lamellar parameters, e.g., P, the thicknesses of semicrystalline (d), crystalline (d) and amorphous (d) lamellae, and the volume fraction (φ) of crystalline lamellae within semicrystalline lamellae. Quantitative analysis revealed that P was positively correlated with the crystallinity (X) of starch. It was confirmed that the distribution of lamellar thickness was more important than the starch botanical origin in affecting the validity of the developed fitting method. We also proposed a criterion to test the validity of the proposed method. Specifically, the total SAXS pattern should be mostly tangent to the profile of PL + B at a high q tail (close to 0.2 Å).
Formatted abstract
A fitting method combined with a linear correlation function was developed as an improved approach for the SAXS analysis of the semicrystalline lamellae of starch granules. Using a power-law function with two Gaussian plus Lorentz functions, the SAXS pattern was resolved into sub-patterns of the net lamellar peak and the power-law scattering plus scattering background (PL + B). The ratio of the net lamellar peak area (Apeak) to the total scattering area (Atotal) was proposed equal to the proportion of the lamellae within the starch granule (PSL). Along with this fitting method, we obtained a better profile of linear correlation function, with the elimination of the interference of non-lamellar amorphous starch (i.e., amorphous growth rings). Then, we could accurately calculate the lamellar parameters, e.g., PSL, the thicknesses of semicrystalline (d), crystalline (dc) and amorphous (da) lamellae, and the volume fraction (φc) of crystalline lamellae within semicrystalline lamellae. Quantitative analysis revealed that PSL was positively correlated with the crystallinity (Xc) of starch. It was confirmed that the distribution of lamellar thickness was more important than the starch botanical origin in affecting the validity of the developed fitting method. We also proposed a criterion to test the validity of the proposed method. Specifically, the total SAXS pattern should be mostly tangent to the profile of PL + B at a high q tail (close to 0.2 Å−1).
Keyword Granule
Methodology
Semicrystalline lamellae
Starch
X-ray scattering
Q-Index Code C1
Q-Index Status Provisional Code
Grant ID 2662016QD008
201604
2014FJ1008
Institutional Status UQ

Document type: Journal Article
Sub-type: Article (original research)
Collections: School of Chemical Engineering Publications
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