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Bioresource Technology 99 (2008) 13591367

Extraction and characterization of chitin and chitosan

from local sources
Entsar S. Abdou a, Khaled S.A. Nagy a, Maher Z. Elsabee b,*

a
Food Technology Research Institute, Agriculture Research Center, Cairo 12631, Egypt
b
Department of Chemistry, Faculty of Science, Cairo University, Cairo 12631, Egypt

Received 20 November 2006; received in revised form 27 January 2007; accepted 30 January 2007
Available online 26 March 2007

Abstract

Chitin has been extracted from six dierent local sources in Egypt. The obtained chitin was converted into the more useful soluble
chitosan by steeping into solutions of NaOH of various concentrations and for extended periods of time, then the alkali chitin was heated
in an auto clave which dramatically reduced the time of deacetylation. Chitin from squid pens did not require steeping in sodium hydrox-
ide solution and showed much higher reactivity towards deacetylation in the autoclave that even after 15 min of heating a degree of
deacetylation of 90% was achieved. The obtained chitin and chitosan were characterized by spectral analysis, X-ray diraction and
thermo gravimetric analysis.
 2007 Elsevier Ltd. All rights reserved.

Keywords: Chitin extraction; Local sources; Deacetylation conditions; Characterization

1. Introduction solubility, higher reactivity and higher anity towards sol-

Chitin, a naturally abundant polymer consists of 2-acet-
amido 2-deoxy-b-D-glucose through a b(1 ! 4) linkage. In
spite of the presence of nitrogen, it may be regarded as cellu-
lose with hydroxyl at position C-2 replaced by an acetamido
group. Like cellulose, it functions as structural polysaccha-
rides. Its natural production is inexhaustible; arthropods,
by themselves, count more than 106 species from the
1.2 106 of total species compiled for animal kingdom, con-
stitute permanent and large biomass source. Chitin is a
white, hard, inelastic, nitrogenous polysaccharide and the
major source of surface pollution in coastal areas.
Chitin is usually isolated from the exoskeletons of crus-
taceans and more particularly from shrimps and crabs
where a-chitin is produced (Minke and Blackwell, 1978;
Austin et al., 1989). Squid is another important source of
chitin in which it exists in the b form which was found to
be more amenable for deacetylation. It also shows higher
*
Corresponding author. Tel.: +20 26352316.
E-mail address: mzelsabee@yahoo.com (M.Z. Elsabee).
vents and swelling than a-chitin due to much weaker inter-
molecular hydrogen bonding ascribable to the parallel
arrangement of the main chains (Pawadee et al., 2003;
Gardner and Blakwell, 1975; Hunt and Elsherief, 1990;
Chandumpaia et al., 2004).
Many authors (Tolaimate et al., 2000, 2003; Pawadee
et al., 2003; Gardner and Blakwell, 1975; Hunt and Elsher-
ief, 1990; Chandumpaia et al., 2004; Acosta et al., 1993;
Rege and Block, 1999; Galed et al., 2005; Paulino et al.,
2006) have tackled the problem of extracting chitin from
its natural sources followed by its deacetylation to obtain
the much more useful material chitosan.
Potential and usual applications of chitin, chitosan and
their derivatives are estimated to be more than 200 (Sand-
ford, 1989; Ravi Kumar, 2000). This wide range of applica-
tions include cosmetics, agriculture, food, biomedical, and
textile, as chelating agents and renement industrial eu-
ents (Rathke and Hodson, 1994; Chassarya et al., 2005).
The production of chitosan from crustacean shells
obtained as a food waste is economically feasible, especially
if it includes the recovery of carotenoids. The shells contain

0960-8524/$ - see front matter  2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2007.01.051
1360 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367
considerable amount of astaxanthin, a carotenoids that has
so far not been synthesized, and which is marked as a sh
food additive in aquaculture.
Chitosan itself was directly extracted from fungi by
alkaline and acid treatment (Rane and Hoover, 1993; Cai
et al., 2006; Suntornsuk et al., 2002; Chatterjee et al.,
2005). Some authors (Wang et al., 2006; Gagne and Simp-
son, 1993; Oh et al., 2000; Yang et al., 2000) have devel-
oped methods to use microorganisms or proteolytic
enzymes for the deproteinization of the crustacean chitin
wastes in this way a more economic production of chitin
and chitosan can be achieved.
The major procedure for obtaining chitosan is based on
the alkaline deacetylation of chitin with strong alkaline
solution. Isolation of chitin itself from dierent sources is
aected by the source. Generally the raw material is
crushed, washed with water or detergent and cut into small
pieces. The mineral content of the exoskeleton of the dier-
ent crustaceous is not the same and consequently dierent
treatments may be used. The present work is the rst sys-
tematic trial to investigate the extraction of chitin and
chitosan from dierent indigenous sources in Egypt.
2. Experimental part
2.1. Isolation of chitin
Chitin was isolated from six sources, two kinds of
shrimp (brown and pink) shells, two kinds of squid pens,
crabs shells and shells of fresh water lobster (craysh), Pro-
cambarus clarkii which is a species of freshwater craysh,
native to the south-eastern United States, but found also
on other continents, where it is often an invasive pest. It
is known variously as the red swamp crawsh, red swamp
craysh, Louisiana crawsh or Louisiana craysh. This
craysh is an intriguing species besides being a source for
chitin it is also an environmental problem in Egypt, the
craysh has become an abundant resident in the River Nile
because of its high reproduction rate and its strong adapt-
ability. This craysh is a voracious carnivore, preying upon
various crustaceans, mollusks and small sh, as well as
their eggs and fries causing thus a serious obstacle for
aquaculture industry. Other evidence shows that they feed
well upon some benthic vector snails, and so, it might be
used as a potential biological Schistosome control agent
if it is intentionally introduced into the irrigation and
drainage canals which are largely infested with these snails.
The raw materials were obtained in solid form from the
dierent sources, washed with water, desiccated at room
temperature and cut into small pieces. Demineralization
was carried out at room temperature using 1 M hydrochlo-
ric acid bathes. The number of bathes and their duration
were dependent upon the source; it was observed that the
emission of CO2 gas was more or less an important indica-
tor according to the studied species. It is for example strong
in case of crabs and shrimp and craysh and weak in case
of one kind of squid. De-proteinization was performed
using alkaline treatments with 1 M sodium hydroxide solu-
tions at 105110 C. This treatment was repeated several
times. The number of bathes depends on clarity of the solu-
tion; the absence of protein was indicated by the absence of
color of the medium at the end of the last treatment. Wash-
ing with distilled water was then carried out up to neutral-
ity after which the samples were dried.
At this stage, chitin isolated from squid pens is perfectly
white unlike those isolated from other sources which were
highly pink. Pigment traces responsible for color are
removed using a mild oxidizing treatment (KMnO4 + oxa-
lic acid + H2SO4). Reuxing in ethanol for 6 h was also
used to eliminate traces of protein and coloring materials.
Chitin content was determined from weight dierence of
the raw material and that of the chitin obtained after acid
and alkaline treatments.
2.2. Deacetylation of chitin
Preliminary experiments were carried out by reuxing
chitin in strong NaOH solution at normal atmosphere.
The experiments took more than 20 h producing low
deacetylation content and the reaction was accompanied
by drastic degradation of the nal chitosan. To avoid long
heating times, the reuxing in alkaline solution was tried in
an autoclave under two atmospheres pressure. The heating
lasted for several hours (1015 h) and still the resulting
chitosan was partially soluble in acetic acid indicating
low deacetylation extent.
Kurita (2001) has indicated that deacetylation of chitin
can be highly facilitated by steeping in strong sodium
hydroxide solution at room temperature before heating.
This approach was then adapted and the eect of steeping
time on the feasibility of deacetylation was investigated.
3. Determination of the deacetylation percent
3.1. Potentiometric titration
Chitosan (0.5 g) was dissolved in 25 ml of 0.1 M stan-
dard HCl aqueous solution. The solution was then toped
up to 100 ml with distilled water and calculated amount
of KCl was added to adjust the ionic strength to 0.1. The
titrant was a solution of 0.05 M NaOH. pH meter was used
for pH measurements under continuous stirring. The
titrant was added until the pH value reached 2.00, the stan-
dard NaOH was then added stepwise and the pH values of
solution were recorded and a curve with two inection
points was obtained.
The dierence of NaOH solution volumes between these
points corresponds to the acid consumed for salication of
the amine groups of chitosan and allows the determination
of DDA% of the chitosan.
The DA was calculated from the relation (Broussignac,
1968):
 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367
1  161Q
DDA%
1 42Q
where Q = NDV/m, DV is the volume of NaOH solution
between the two inection points (in l), N is the concentra-
tion of NaOH (in mol/l in this paper 0.05 mol/l) and m is
the dry weight of chitosan (in g).
3.2. Elemental analysis
The DDA% value of chitosan samples was calculated
from the following formula (Kasaai et al., 2000; Jiang
et al., 2003):
6:857  C=N
DDA%
1:7143
where C/N is the carbon/nitrogen ratio measured from the
elemental composition of the chitosan samples.
3.3. Fourier transform infrared FTIR spectroscopy
The FTIR spectra were measured in KBr pellets in the
transmission mode in the range 4004000 cm1 using Per-
kinElmer 2000 spectrophotometer. The DDA of the sam-
ples were calculated from the IR spectra following the
method in Ref. (Brugnerottoa et al., 2001).
The bands at 1650 and 1320 cm1 were chosen to mea-
sure the DA. As internal reference, the intensities at 3450
and 1420 cm1 were evaluated. The absorption band ratios
involving the reference at 3450 cm1 had poorer t. The
absorption ratio A1320/A1420 shows superior agreement
between the absolute and estimated DA-values according
to Brugnerottoa et al. (Brugnerottoa et al., 2001) and there-
fore was adapted in this work:
DA% 31 : 92  A1320 =A1420  12 : 20; r 0 : 990
3.4. NMR method
Hirari et al. (Hirari et al., 1991) reported the chemical
shift of methyl protons in acetamide group to appear at
2.07 ppm in acidic deuterium oxide solutions while the
methyl group of glacial acetic acid appears at 2.12 ppm
(The Aldrich Library of NMR Spectra). Therefore, the
peak around 2.1 ppm in the spectra (Fig. 1) can be safely
assigned to the methyl protons in the acetamide group,
and that around 2.2 ppm is due to the methyl group in ace-
tic acid moiety. The chemical shift is aected by solvent,
concentration and temperature, and taking these into
account, one can explain the dierence between the chem-
ical shift value reported by Lavertu (lavertu et al., 2003)
and those reported here.
In the obtained spectra, the dierence in chemical shifts
between peaks at about 2.1 and 2.2 ppm is constant (about
0.15 ppm) within experimental errors. The setting of TMS
peak to be 0 ppm is sometimes slightly aected by opera-
tional and spectral variations, and for peaks with many
1361
Fig. 1. 1HNMR spectrum of chitosan derived from pink shrimp (0.5 h
heating in autoclave and 1 day steeping in 40% NaOH).
spikes as in our case, the reproducibility might be lowered.
Therefore, it can be safely stated that the chemical shift for
amide methyl protons can be set to 2.06 ppm and that for
acetic acid moiety to 2.21 ppm.
It is described (Hirari and Lavertu) that the peak at
4.9 ppm is assigned to C1 proton of glucosamine unit in
chitosan and the peaks in 34 ppm to C2C6 protons of
glucosamine and N-acetylglucosamine units. They also
showed that C1 proton of N-acetylglucosamine unit
appears around 4.6 ppm, and this peak is overlapped with
the strong solvent peak in our spectra and can be seen as a
shoulder in the representative example shown in Fig. 1 for
pink shrimp chitosan obtained after 0.5 ppm heating in the
autoclave the chitin was steeped for 1 day in 40% NaOH
solution.
For the determination of the degree of deacetylation
(DDA) the method of Lavertu was adapted in which
 
H4:9
DDA %  100
H4:9 H2:06=3
Based on these, one can calculate DDA unequivocally
from the obtained NMR spectra.
NMR and potentiometric titration were found to be the
most reliable methods and the values reported here are usu-
ally the average of these methods.
3.5. Viscosity measurements
The viscosities of all prepared chitosan samples (except
the insoluble samples) were measured using an Ostwald
capillary viscometer and the intrinsic viscosities were deter-
mined, the solvent was 5% acetic acid and 0.1 M KCl the
obtained intrinsic viscosity was used to calculate molecular
1362 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367

weight for the prepared samples from the MarkHouwink
Sakurada relation:
g KM a
where K and a are constants which were determined in the
literature by many authors. K = 1.38 104 and a = 0.85
(Gamzazade et al., 1985), and K = 2.14 103 and
a = 0.657 (Pankaj et al., 1999) another values were
K = 1.4 104 and a = 0.83 (Wan et al., 2003). Another
formula for squid chitosan has been adapted (Chan-
dumpaia et al., 2004) with K = 8.93 104 a = 0.71.
Due to the variation of the K and a constants it seemed
reasonable to use the intrinsic viscosity data [g] directly
since converting it to molecular weight values will yield
the same behavior pattern in addition to the variation in
the values of the constants.
3.6. X-ray diraction
X-ray diraction analysis (XRD) was applied to detect
the crystallinity of the extracted samples of chitin and their
corresponding chitosan. A Scintag powder diractometer
was used for this purpose between 2h angles of 5 and
40. Ni-ltered Cu Ka-radiation was used as the X-ray
source. The relative crystallinity of the polymers was calcu-
lated by dividing the area of the crystalline peaks by the
total area under the curve.
3.7. NMR
Nuclear magnetic resonance NMR spectra were mea-
sured using JNMAl 300, Jeol spectrometer at 300 MHz in
D2O in which drops of DCl was added to enhance
solubility.
3.8. Thermal analysis
Thermo-gravimetric analysis TGA was carried out using
Shimadzu TGA-50H instrument at a heating rate of 10 C/
min under nitrogen atmosphere.
4. Results and discussion
Table 1 contains data of the percent of chitin present in
As seen from Table 1 two types of squid pens were used,
one which was opaque white in color (CT) and was found
to consist almost of CaCO3, while the other pens were
transparent and much smaller in size with very small
amount of carbonates and more than double the chitin
content of any other source (SQ). The chitin content in
Craysh (CF) ranging about 2021% warrants its use as
an economic way of producing chitin on an industrial scale
due to the availability and the low price of the source.
The chitin extracted from squid pen was found to be
much more amenable to deacetylation than that from
shrimp, crab and craysh. That is why the eect of steeping
on deacetylation was studied only for the four a-chitin i.e.
that from shrimp, crabs and craysh.
4.1. Eect of steeping time on DDA% of chitosan
The extracted chitin was heated into an autoclave after
being steeped in sodium hydroxide solution of various con-
centrations at a solid: liquor ration of 1:20. The eect of
steeping time in 40% NaOH solution and heating in auto-
clave (at 2 atmosphere pressure) is illustrated in Fig. 2.
From Fig. 2, it can be seen that after 1 day steeping in
the NaOH solution, the deacetylation takes only 1 h to
yield high DDA reaching almost 92% for the craysh chitin
while 4 days steeping led to further increase in the DDA up
to 9297%. Therefore, the use of the autoclave leads to dra-
matic reduction in the time of deacetylation and conserva-
tion of energy.
4.2. Eect of NaOH concentration on the DDA% of chitosan
To study the eect of alkaline concentration of the
steeping solution on the DDA%, dierent concentrations
of sodium hydroxide solutions (10%, 20%, 30% and 40%
(w/w) were used for steeping of chitin for 24 h) the reaction
time in the autoclave was kept at 0.5 h. It was found that
the DDA% increases as the concentration of NaOH
increases and Fig. 3 shows the DDA% as a function of
98
BS
RS
96 CF
CR

the exoskeleton of dierent local sources. 94

Table 1
DDA%

Percent of chitin in dierent local sources 92

Source % Of % Of % Of
CaCO3 protein chitin 90
Brown shrimp (penaeus aztecus) 48.97 29.50 21.53
shells (BS) 88
Pink shrimp (penaeus durarum) 42.26 34.02 23.72
shells (PS) 86
Cuttlesh pens (CT) 88.48 6.12 5.40 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
Squid pens (SQ) 4.74 46.23 49.00
Steeping time, days
Crabs shells (CR) 66.58 16.68 16.73
Craysh shells (CF) 63.94 15.46 20.60 Fig. 2. Eect of steeping time in 40% NaOH upon the DDA% after
The values depicted above are the average value of 35 experiments. heating in an autoclave for 1 h.
 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367 1363

100 96
BS
PS 94
CF
80 CR 92

90
60
DDA%

DDA%
88

86
40
84
BS
82 PS
20
CF
80 CR

0 78
10% 20% 30% 40% 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
NaOH wt % Time, h

Fig. 3. Eect of NaOH concentration of the steeping bath on the DDA% Fig. 5. Eect of the heating time in autoclave on DDA% of the dierent
after heating for 1 h in the autoclave. sources using 40% NaOH and steeping time 1 day.

100
the concentration of the steeping bath before heating in the
autoclave. It seems that below 40% sodium hydroxide con- 98
centration the steeping has little eect. While Fig. 4 shows
how reactive the b-chitin towards deacetylation since even 96
30% NaOH can achieve up to 90% DDA even without pre-
94
DDA%

treatment in NaOH.
92
4.3. Eect of the heating time in autoclave on DDA% of 90
chitosan
88 CT
The eect of the reaction time on the DDA% of chitin SQ
86
from dierent sources in the autoclave using 40% NaOH
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
and a steeping time of 1 day is shown in Fig. 5.
Time, h
It seems that the craysh chitin is relatively more reac-
tive than the other forms of chitin. The chitin extracted Fig. 6. Eect of reaction time in the autoclave on the DDA% for the
from squid pen required no steeping and it readily under- b-chitin form squid pens, using 40% NaOH.
goes deacetylation in the autoclave to high values of
DDA as shown in Fig. 6. Even after 15 min, the degree highly dependent on both the DDA% and the molecular
of deacetylation reaches 8789%. weight of the polymer. Therefore, after investigating the
It has been established that chitin and chitosan have eect of the dierent parameters on the DDA%, it is essen-
many biological and biomedical applications which are tial to see how the dierent procedures aect the molecular
weight of the nal chitosan polymer. The molecular weight
120
was determined by measuring the intrinsic viscosity in 5%
100
acetic acid solution where the chitosan was freely soluble.
Figs. 7 and 8 illustrate how the intrinsic viscosity of the
80 obtained chitosan is aected by the reaction time in the
autoclave and the time of steeping in 40% NaOH solution
DDA%

60 prior to heating. As a representative example the equation

of (Wan et al., 2003) K = 1.4 104 and a = 0.83 has been
40 used to calculate the molecular weight since it is the most
recent one; the chitosan of CF after 0.5 h in the autoclave
20
CT
has a molecular weight of 8.13 105 was reduced to
SQ 4.60 105 after heating for 2.5 h. Heating time has more
0 pronounced eect on the viscosity than the steeping time
10% 20% 30% 40% which has almost an erratic eect as shown in Fig. 9 while
NaOH wt% the reaction time is always followed by gradual decrease in
Fig. 4. Eect of NaOH concentration on the extent of hydrolysis of the viscosity. The same trend was found for the case of b-chitin
b-chitin from the two types of squid pens. from squid pen, a gradual decrease of viscosity with
1364 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367

12 heating time in the autoclave has been observed in 40%

BS
PS NaOH solution the molecular weight (K = 8.93 104
CF
10
CR
a = 0.71 (Chandumpaia et al., 2004)) was reduced from
6.4 105 to 3.9 105 after heating for 0.25 h and 1.25 h,
8 respectively, for SQ sample.
[] dl/g

6 4.4. FTIR

4 A representative example of chitin and its chitosan is

given in Fig. 10. The DDA was calculated as was explained
2 in the experimental part using the ratio of the bands at
1320 and 1420 cm1.
0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.5. X-ray diraction
Reaction Time, h
X-ray diraction (XRD) analysis was applied to detect
Fig. 7. Eect of the reaction time in the autoclave on the intrinsic viscosity
[g] values of the chitosan obtained from the a-chitin, using 40% NaOH the crystallinity of the isolated chitin and the obtained
and steeping for 1 day. chitosan. Relative mass crystallinity of the dierent chitin
and chitosan are listed in Table 2. The structure of a-chitin

8
BS
PS
CR
7
CF

6
[] dl/g

2
1 day 2 days 3 days 4 days
Steeping Time, days

Fig. 8. Eect of the steeping time on the intrinsic viscosity of chitosan

after heating for 1 h in the auto clave in 40% NaOH solution.

14
CT
SQ
12

10
[] dl/g

8
Fig. 10. FTIR spectra of CF upper curve chitosan lower curve chitin.
6

2 Table 2
Crystallinity of chitin and chitosan (X-ray analysis)
0 BS chitin PS chitin CT chitin SQ chitin CR chitin CF chitin
0.5 1.0 1.5 2.0 2.5 3.0 3.5 chitosan chitosan chitosan chitosan chitosan chitosan
Time, h Crystallinity (%)
64 66 66.6 48.9 70.82 43.15 59.22 41.78 59.86 40.99 56.94 36.43
Fig. 9. Eect of the reaction time in the autoclave on the intrinsic viscosity
[g] values of the chitosan obtained from b-chitin using 40% NaOH and no Crystallinity percent was calculated by dividing the area of the crystalline
steeping. peaks by the total area under the curve.
 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367 1365

has been determined by Minke and Blackwell (Minke and
Blackwell, 1978) using X-ray diraction analysis, based on
the intensity data from deproteinized lobster tendon.
Least-squares renement shows that adjacent chains have
alternating sense (i.e. are antiparallel). In addition, there
is a statistical distribution of side-chain orientations, such
that all the hydroxyl groups form hydrogen bonds. The
unit cell is orthorhombic. The chains form hydrogen-
bonded sheets linked by C@OHN bonds are approxi-
mately parallel to the a-axis, and each chain has an

Fig. 11. X-ray diraction patterns of (a) a-chitin from (1) BS (2) PS (3) CR (4) Cray Fish (b) the corresponding chitosan.

Fig. 12. X-ray diraction patterns of (a) b-chitin from (1) CT (2) SQ (b) the corresponding chitosan.
1366 E.S. Abdou et al. / Bioresource Technology 99 (2008) 13591367

O-3 0 HO.5 intra-molecular hydrogen bond, similar to

that in cellulose. The results indicate also that a statistical
0.000
mixture of CH2OH orientations is present, equivalent to
half oxygen on each residue, each forming inter- and -0.002
intra-molecular hydrogen bonds. As a result, the structure

DTGA
contains two types of amide groups, which dier in their -0.004
hydrogen bonding, and account for the splitting of the
amide I band in the infrared spectrum. The Inability of this -0.006
chitin polymorph to swell on soaking in water is explained
by the extensive intermolecular hydrogen bonding. -0.008
CF, chitosan
In Fig. 11, the X-ray diraction patterns of the obtained CF Chitin
a-chitin (A) and the corresponding hydrolyzed chitosan (B) -0.010
are given. All chitin samples show strong reections at 2h 0 100 200 300 400 500 600
around 910 and 2h of 2021 and minor reections at Temperature, C
higher 2h values e.g. at 26.4 and higher. The band at
and is due to Fig. 14. DTA curves for chitosan and chitin from CF.
9.9 corresponds to a d spacing of 8.92 A
the incorporation of bound water molecules into the crystal
lattice (Ogawa et al., 1992). The reection at 2h 19.420
(Harish Prash- 5. Conclusion
corresponds to a d spacing of about 4.41 A
anth et al., 2002). Generally, the sharpness of the bands are
Chitin has been extracted from dierent sources indige-
higher in the chitin samples than in their chitosan analogue
nous for Egypt. It was found that Craysh which constitute
with slight decrease in the crystallinity percent. Fig. 12
a pollution hazard in Egypt could be an economic source of
illustrates the chitin and chitosan obtained from squid pens
chitin. The obtained chitin was hydrolyzed using an auto-
(b-chitin) the band at 2h 9.9 decreases after deacetylation
clave after being steeped in strong sodium hydroxide solu-
followed by dramatic decrease in crystallinity percent as
tion for dierent period of time which reduced the
seen in Table 2.
deacetylation time dramatically to produce chitosan with
reasonably high molecular weight, and high deacetylation
4.6. Thermal analysis
percent. It has also been shown that b-chitin is much more
amenable to deacetylation than the a form.
TGA curves of chitin and chitosan are shown in Fig. 13
The chitin and chitosan have been characterized as to
as representative examples. Two endothermic peaks are
their degree of deacetylation and their relative degree of
observed. The rst peak appears around 9099 C corre-
crystallinity was measured by X-ray diraction method.
sponds to loss of water. The second one emerges at about
The thermal behavior of the obtained polymers revealed
303 C in chitosan and at about 372 C in the correspond-
that they both decompose by two step patterns and that
ing chitin as seen in the DTA curves in Fig. 14. All the
chitin is more thermally stable than chitosan.
extracted samples showed similar trend; the chitin has
higher thermal stability than the corresponding chitosan.
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