• Journal of the Korean Society of Clothing and Textiles
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• v.20 no.4
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• pp.682-689
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• 1996

A preparative method has been proposed for obtaining chitosan products which have a desired degree of deacetylation (DD, %) without much decrease in molecular weight. Deacetylation was prepared by two methods. The method I which was proposed by Domard etc. was that DMSO/thiophenol was used repeatedly only during the deacetylation, the method II was that DMSO/thiophenol was used after the alkali treatment. Then, effective deacetylation was performed by the method ll. To determine the degree of deacetylation, potentiometric titration method was adopted. According to the increase of DD, the viscosity average moleclar weght $(\overline{M\upsilon}$) and the DP of the chitosan products were decreased. The intensity of FT-lR peak appeared at $1655cm^{-1}, which was characteristic peak of amide I (Nacetyl secondary amide group), was gradually decreased with deacetylation. X-ray analysis showed that the lattice-spacing in the chitosan film increased with the degree of deacetylation, but the difference of the transparency of the chitosan products was not diverged significantly.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.28 no.4
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• pp.392-396
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• 1995

Chitosan was prepared from red snow crab (Chinonecetes japonicus) under various conditions of deacetylation (NaOH concentration, heating temperature, heating time and intermittent and repetition treatment). By measuring the degree of deacetylation and the molecular weight (Mw), effect of preparation condition was studied. As the concentration of NaOH increased in deacetylation process, for chitosan treated over $40\%$ NaOH, the rate of increase of the deacetylation of chitosan decreased, but the difference of Mw decrease was nearly constant. When treatment temperature increased from $130^{\circ}C$ to $150^{\circ}C$, the deacetylation degree increased only $3^{\circ}C\;from\;84\%\;to\;87\%,$ but Mw decreased from 267,000 to 85,800. The difference of Mw decrease of chitosan treated $130-150^{\circ}C$ was larger than that with $90-130^{\circ}C$. The deacetylation degree and Mw of the chitosan prepared by continuous treatment for 3 hrs was$84\%$ and 267,000. On the other hand those of chitosan with intermittent and repetition treatment for 3hrs was $93\%$ and 28,000. In order to increase the degree of deacetylation and inhibit depolymerizing, the intermittent and repetition treatment was found to be more effective than the continuous treatment.

• Fashion & Textile Research Journal
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• v.8 no.4
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• pp.458-464
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• 2006

The adsorption ability of heavy metal ions from the aqueous solution by chitosan, which it is well known natural biopolymer, has been investigated. The fundamental study in this research is focusing on the physicochemical adsorption utilizing the chitosan as a organic chelating adsorbent, adsorb especially heavy metal ions from the waste liquid solution. The adsorption ability of the chitosan between metal ions, having different characteristics with Mw of 188,600, 297,200, and 504,200 g/mol and degree of deacetylation (DD) of 86.92% and 100% were investigated targeting on the $Ni^{2+}$, $Co^{2+}$, $Zn^{2+}$, and $Pb^{2+}$ ions, respectively. The uptake of heavy metal ions with chitosan was performed by atomic absorption flame emission spectrophotometer (AAS) as conducted residual metal ions. It was found that chitosan has an strong adsorption capacity for some metals under certain conditions. Chitosan, which have 100% degree of deacetylation showed high adsorption recovery ratio and have an affinity for all kinds of heavy metals. In contrast, the molecular weight of chitosan was not completely affected on metal ion adsorption.

• Fashion & Textile Research Journal
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• v.5 no.1
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• pp.71-76
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• 2003

Three different types of chitosan were prepared from red crab shells to study anti-microbial activity of chitosan on pathogenic bacteria, MRSA(Methicillin-resistant. Staphylococcus aureus), Water-insoluble chitosan, whose degree of deacetylation is kept over 90% and molecular weights are 20,000, 500,000, 150,000, 80,000, and 40,000, respectively. Water-soluble chitosan, whose degree of deacetylation is about 48% and molecular weights are 200,000 and 80,000. Water-soluble chitosan, whose degree of deacetylation is 82% and molecular weight is 3,900. The anti-microbial activities of three types of chitosan were investigated by Tube Dilution Technique(TDT) and Agar Plate Smear Method(APSM). And the following conclusions are made ; Chitosan having 5 different types of M.W chitosan (over 90% deacetylation) showed similar anti-microbial activities at over 0.05% concentration. Especially, chitosan having M.W 40,000 150,000 showed the excellent anti-microbial activity. The anti-microbial activity of chitosan was enhanced when the chitosan/acetic add solution was aged for 7days. The anti-microbial activity of chitosan was only shown at chitosan/acetic acid solution. The anti-microbial activity was not detected in chitosan solution dissolved in neutral pH water. Therefore, it can be concluded that the anti-microbial activity was due to NH3+ cationic ion of chitosan in acidic aqueous solution.

• Fashion & Textile Research Journal
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• v.5 no.5
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• pp.529-538
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• 2003

Chitosan should be satisfied a certain Mw range for the final application, Low molecular weight chitosan(LMWC) can be acquired by depolymerizing high molecular weight starting chitosan. Using $H_2O_2$ in depolymerizing chitosan is very effective and reproducible in controlling Mw of resulting LMWC. However, $H_2O_2$ can break glycoside linkage of chitosan and oxidize some $-NH_2$ groups in chitosan. It has been reported that decrease in DA(degree of deacetylation) of LMWC prepared by $H_2O_2$. However, any quantitative data of decrease in DA has not been reported yet. In this study, DA of initial chitosan and DA of $H_2O_2$ treated chitosan were measured and the change in DA of chitosan upon $H_2O_2$ treatment were investigated. Change in DA was very different upon $H_2O_2$ treatment condition. LMWC also showed DA change upon time passage. Pre-swelling treatment of initial chitosan and low ratio of $H_2O_2$/chitosan prevented a decrease in DA significantly. Yellowing of LMWC was detected upon time passage, however, decrease in DA was minimal (around 1%).

• Journal of Environmental Health Sciences
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• v.27 no.1
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• pp.36-43
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• 2001

Chitosans were prepared from red crab chitin under various alkali treatment conditions(different alkali concentrations, reaction times and temperatures) and theirphysicochemical properties were investigated. The nitrogen content and deacetylation degree of red crab chitin were 6.15% and 22.17A%, respectively. By the IR spectra, red crab and reference chitin showed the sharp bands at 1650 $cm^{-1}$ / and 1550 $cm^{-1}$ /, which are characteristic of chitin. The nitrogen contents of prepared chitosans ranged from 6.19~7.48%. Thedeacetylation degree was increased from 63~76% and 48~78% with increasing reaction time and temperature, whereas viscosity was decreased. The nitrogen content and yield of red crab chitosan perpared from chitin with 50% NaOH, 1:25(w/v) for 3.0 hr at 120$cm^{-1}$ / were 7.26% and 85.0%, respectively. and viscosity, deacetylation degree and molecular weight, 67.0 mPa.s, 75.0% and 6.5$\times$10$^{5}$ Dalton, respectively. From the IR spectra, the amide absorption bands of red crab and reference chitosan became very weak, similarly. And at solid state $^{13}$ C-NMR spectra, C=O(carbonyl carbon) signals absent, whereas $CH_3$(methyl carbon) was residues. Chemical shift of $^{13}$ C-NMR spectra of red crab and reference chitosans were in good agreement with slight experimental deviation.

• Korean Journal of Food Science and Technology
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• v.31 no.2
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• pp.558-563
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• 1999

Response surface methodology was used for monitoring physicochemical properties of chitosan with preparation of chitosan. Deacetylation degree of chitosan was in proportion to NaOH concentration for deacetylation of chitosan. The solubility of chitosan was maximized in 52% (concentration of NaOH), $109^{\circ}C$ (deacetylation temperature) and 123 min (deacetylation time). Viscosity of chitosan was mainly influenced by concentration of NaOH, and was greatly decreased with the increase of concentration of NaOH. The optimum condition ranges for preparation of chitosan was $52{\sim}54%$ NaOH, $100{\sim}115^{\circ}C$ in deacetylation temperature and $100{\sim}140\;min$ in deacetylation time.

• Journal of the Korean Society of Clothing and Textiles
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• v.28 no.6
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• pp.807-818
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• 2004

The antibacterial activities of several types of chitosan were measured against Staphylococcus aureus and evaluated for their application to antibacterial textile finishing. The ％ reduction of bacteria of the chitosans prepared in our laboratory were between 72 and 87%. The two water-soluble chitosans with molecular weights 1,000 and 3,000 did not show antibacterial activities. The deacetylation of chitosan was appeared to increase antibacterial activity. The ％ reduction in bacterial density of the 86％-deacetylated chitosan solution was 56% where that of the 76％-deacetylated chitosan solution was only 17％ at 0.1% chitosan concentration. Molecular weights of the chitosans seemed not to affect antibacterial activities of chitosans. The antibacterial activity of the acid-soluble, 86%-deacetylated chitosan with 4 cps showed 98% of the ％ reduction at the level of 0.2％ chitosan. The ％ reduction of bacteria of this chitosan was higher at the higher concentration of acetic acid in the chitosan-bacterial mixture. The antibacterial activity was increased with the pH change over the range of 4.0 to 6.5. The 100% of the ％ reduction of bacteria was achieved within 4 hour incubation of the chitosan-bacterial mixture. According to the data obtained from the above experiments, the four chitosans among the six prepared in our laboratory were proved to be valuable for antibacterial textile finishing.

• Biotechnology and Bioprocess Engineering:BBE
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• v.4 no.1
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• pp.26-31
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• 1999

The advantages of the organism Streptomycs griseus HUT 6037 is that the chitinase and chitosanase using chitinaceouse substrate are capable of hydrolyzing both amorphous and crystalline chitin and chitosan. We attempted to investigate the optimization of induction protocol for high-level production and secretion of chitosanase and the influence of chitin and partially deacetylated chitosan sources (75∼99% deacetylation). The maximum specific activity or chitinase has been found at 5 days cultivation with the 48 hours induction time using colloidal chitin as a carbon source. To investigate characteristic of chitosan activity according to substrate, we used chitosan with various degree of deacetylation as a carbon source and found that this strain accumulates chitosanase in the culture medium using chitosanaceous substrates rather than chitinaceous substrates. The highest chitosanase activity was also presented on 4 days with 99% deacetylated chitosan. The partially 53% deacetylated chitosan can secrete both chitinase and chitosanase which was defined as a soluble chitosan. The specific activities of chitinase and chitosanase were 0.89 at 3 days and 1.33 U/mg protein at 5 days, respectively. It indicate that chitosanase obtained from S. griseus HUT 6037 can hydrolyze GlcNAc-GlcN and GlcN-GlcN linkages by exo-splitting manner. This activity increased with increasing degree of deacetylation of chitosan. It is the first attempted to investigate the effects of chitosanase on various degrees of deacetylations of chitosan by S. griseus HUT 6037. The highest specific activity of chitosanase was obtained with 99% deacetylated chitosan.

• Proceedings of the SOHE Conference
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• 1997.12a
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• pp.33-37
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• 1997

Cotton fabric was treated with chitosan solution by pad-dry(-cure) method to impart antimicrobial properties. Four chitosans of different degree of deacetylation(DAC: 65~95％) with similar molecular weight(ca. 50, 000) and one chitosan oligomer(MW 1, 800, DAC 86％) were used. Antimicribial activity against Staphylococcus aureus was evaluated by the Shake Flask Method. Treated fabrics were laundered up to 20 times according to AATCC Test Method 60-1986 and antimicrobial activity of laundered fabrics was evaluated. The antimicrobial activity was increased with the concentration and DAC of chitosan used. And the cured samples showed better durability to laundering than not-cured samples. Crosslinker and binder decreased the antimicrobial activity of fabrics treated with chitosan oligomer and were not effective to improve the durability to washing.