Synthesis and characterization of cassava starch nanocrystals by hydrolysis method

Cassava starch nanocrystals (CSN) has not been reported in open literature, although other starches such as rice, corn, potato and bean were widely used as the main material. Thus, the objective of this research was to investigate the possibility of synthesizing high yield of CSN at different concen...

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Main Author:	Md. Shahrodin, Nur Shazrynda
Format:	Thesis
Language:	English
Published:	2014
Subjects:	TP Chemical technology
Online Access:	http://eprints.utm.my/id/eprint/50837/1/NurShazryndaMdShahrodinMFChE2014.pdf
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spelling	my-utm-ep.508372020-07-13T02:17:05Z Synthesis and characterization of cassava starch nanocrystals by hydrolysis method 2014-06 Md. Shahrodin, Nur Shazrynda TP Chemical technology Cassava starch nanocrystals (CSN) has not been reported in open literature, although other starches such as rice, corn, potato and bean were widely used as the main material. Thus, the objective of this research was to investigate the possibility of synthesizing high yield of CSN at different concentrations of sulphuric acid (H2SO4). The physical, chemical and thermal properties of synthesized CSN was also investigated. Synthesized CSN was prepared by hydrolysing native cassava starch (NCS) with several concentration of H2SO4 (2.8 M, 3.0 M, 3.2 M and 3.4 M). The acid hydrolysis process took 5 days with continuous stirring speed of 300 to 400 rpm, with constant temperature of 37 °C. The hydrolysed solution of CSN underwent a centrifuging process with distilled water until it was neutralized to make sure that no acid residues remain in the CSN solution. The CSN precipitate was dried in an oven over night at 60 °C. The highest yield (1.1 %) produced was from 3.4 M CSN. Morphological test by transmission electron microscopy indicated that the samples have been destructed and degraded to be nanocrystals with a size range of 5 - 20 nm. X-ray diffraction (XRD) and 13C nuclear magnetic resonance (13C NMR) were used to indicate the type of crystallinity for both NCS and CSN. XRD illustrated that NCS was a C – type patterns, however after hydrolysed (CSN), the crystallinity changed to B – type crystalline starch. This result was also proven in 13C NMR resonance pattern. Fourier transform infrared (FTIR) spectra showed a few peaks shifted after hydrolysis, most of the changes were due to the hydrogen bonding in starch molecules which proved that there were alteration in the inter and intra-molecular hydrogen bonding of starch molecules. The thermal properties showed that glass transition temperature (Tg) was gradually increased as the concentration of the acid increased. This was due to the more energy needed to disrupt crystalline structures which were formed during synthesis process. 2014-06 Thesis http://eprints.utm.my/id/eprint/50837/ http://eprints.utm.my/id/eprint/50837/1/NurShazryndaMdShahrodinMFChE2014.pdf application/pdf en public http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:86920 masters Universiti Teknologi Malaysia, Faculty of Chemical Engineering Faculty of Chemical Engineering
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	TP Chemical technology
spellingShingle	TP Chemical technology Md. Shahrodin, Nur Shazrynda Synthesis and characterization of cassava starch nanocrystals by hydrolysis method
description	Cassava starch nanocrystals (CSN) has not been reported in open literature, although other starches such as rice, corn, potato and bean were widely used as the main material. Thus, the objective of this research was to investigate the possibility of synthesizing high yield of CSN at different concentrations of sulphuric acid (H2SO4). The physical, chemical and thermal properties of synthesized CSN was also investigated. Synthesized CSN was prepared by hydrolysing native cassava starch (NCS) with several concentration of H2SO4 (2.8 M, 3.0 M, 3.2 M and 3.4 M). The acid hydrolysis process took 5 days with continuous stirring speed of 300 to 400 rpm, with constant temperature of 37 °C. The hydrolysed solution of CSN underwent a centrifuging process with distilled water until it was neutralized to make sure that no acid residues remain in the CSN solution. The CSN precipitate was dried in an oven over night at 60 °C. The highest yield (1.1 %) produced was from 3.4 M CSN. Morphological test by transmission electron microscopy indicated that the samples have been destructed and degraded to be nanocrystals with a size range of 5 - 20 nm. X-ray diffraction (XRD) and 13C nuclear magnetic resonance (13C NMR) were used to indicate the type of crystallinity for both NCS and CSN. XRD illustrated that NCS was a C – type patterns, however after hydrolysed (CSN), the crystallinity changed to B – type crystalline starch. This result was also proven in 13C NMR resonance pattern. Fourier transform infrared (FTIR) spectra showed a few peaks shifted after hydrolysis, most of the changes were due to the hydrogen bonding in starch molecules which proved that there were alteration in the inter and intra-molecular hydrogen bonding of starch molecules. The thermal properties showed that glass transition temperature (Tg) was gradually increased as the concentration of the acid increased. This was due to the more energy needed to disrupt crystalline structures which were formed during synthesis process.
format	Thesis
qualification_level	Master's degree
author	Md. Shahrodin, Nur Shazrynda
author_facet	Md. Shahrodin, Nur Shazrynda
author_sort	Md. Shahrodin, Nur Shazrynda
title	Synthesis and characterization of cassava starch nanocrystals by hydrolysis method
title_short	Synthesis and characterization of cassava starch nanocrystals by hydrolysis method
title_full	Synthesis and characterization of cassava starch nanocrystals by hydrolysis method
title_fullStr	Synthesis and characterization of cassava starch nanocrystals by hydrolysis method
title_full_unstemmed	Synthesis and characterization of cassava starch nanocrystals by hydrolysis method
title_sort	synthesis and characterization of cassava starch nanocrystals by hydrolysis method
granting_institution	Universiti Teknologi Malaysia, Faculty of Chemical Engineering
granting_department	Faculty of Chemical Engineering
publishDate	2014
url	http://eprints.utm.my/id/eprint/50837/1/NurShazryndaMdShahrodinMFChE2014.pdf
_version_	1747817545940860928

Synthesis and characterization of cassava starch nanocrystals by hydrolysis method

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