SABTUN ISMI KHASANAH

13/350642/PPA/04110
1. Chitosan Isolation
The degree of deacetylation was one of the most important
chemical parameters that influencing the performance of
chitin and chitosan in many of their applications. IR technique
can be used to measuring the intensity of absorption.

a.u
a)

b)
Wave bumber (cm-1)

Typical absorption and significant peaks shown in

Table 1. A characteristic broad band at 3448.72 cm -1
showed the stretching vibration of OH groups. The
chitin FTIR spectrum showed only one N-H2 peak formed
around
3271.27 cm-1, which suggested that there was a secondary
amide group. At the time, the lower intensity of the peak
observed in chitosan spectrum, it due to overlap among
vibrations of NH2 groups, -OH groups and intermolecular

hydrogen bonds as a result of addition of the amine group

concentration

in

deacetylation.

significant

peak

also

observed at 1651.07 cm-1 which indicated the presence of a

carbonyl group (C=O amide). In this area, the lower intensity
shown in chitosan spectrum due to decrease of C=O in amide
group by deacetylation.
Based on the spectra, degree of deacetylation can be
determined using absorbance ratio calculation of amide group
(1627.92 cm-1 or 1651.07 cm-1) and hydroxyl group (3448.72
cm-1). Calculation of DD in this study used baseline parameter
b that proposed by Huang et al. (2002). Standard of quality
parameter as chitosan was DD value that more than 75%. In
this study, DD value of chitin has 74.7% while the chitosan
has 78.4%.
Table 1. Absorptions bands for chitin and chitosan
sample
Wavenumber (cm-1)
Functional group
Chitin
Chitosan
OH vibration
3448.72
3448.72
N-H vibration
3271.27
3271.27
2
C-H SP vibration
3109.25
3109.25
C-H SP3 vibration
2885.51
2924.09 dan
2885.51
C=O vibration
1627.92
1651.07
NH2 vibration
1566.20
1566.20
-CH21381.03
1381.03
C-N vibration
1319.31
1319.31
C-O-C vibration
1072.42
1072.42
2. Determination of palm oil molecular weight

Detector responce

Time (min)

Figure 2. Chromatogram of the palm oil derivatization

Relative molecular weight of palm oil can be calculated
by determining the composition of fatty acid. Characterization
was done by derivative fatty acids to form volatile compounds
(esters) that can be analyzed using GC-MS. Chromatogram of
the derivatization result shown in Figure 2. Seven compounds
have observed with the greatest abundance shown in third
peak, appeared at a retention time of 41.533 minutes. The
third peak has m/z value 270 and base peak 74 showing
fragments of methyl palmitate (Figure 3). Fragmentation
pattern of methyl palmitate shown in Figure 4.

Abundance
(%)
m/z

Figure 3. Spectrogram of methyl palmitate

Figure 4. Mechanism of methyl palmitate fragmentation

Based on molecular ion and base peak of each
compounds in spectrogram, fatty acids composition in palm oil
can
be
known,
shown
in
Table 2. Composition percentage in table 2 can be used to
calculate relative molecular weight of palm oil. Relative
molecular
weight
in
this
study
was
842.9 g/mol.
Tabel 1. Fatty acid composition of palm oil
Persentase (%)
Palm oil
Palm oil
Molecula
standar
Fatty acid
r weight
(Ketaren,
1986)
Laurate acid
C12H24O2
1.88
Miristate
C14H28O2
2.69
1.1-2.5
acid
Palmityc
C16H32O2
42.69
40-46
acid
Lynoleat
C18H32O2
11.43
7-11
acid
Oleat acid
C18H34O2
37.49
39-45
Stearate
C18H36O2
3.81
3.6-4.7
acid