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1. Determine the X-axis and the Y-axis of the spectrum.

The X-axis of an IR spectrum is labeled


as "Wavenumber" and ranges in number from 400 on the far right to 4,000 on the far left. The X-
axis provides the absorption number. The Y-axis is labeled as "Percent Transmittance" and
ranges in number from 0 on the bottom and 100 at the top.

2.Determine the characteristic peaks in the IR spectrum. All IR spectra contain many peaks.
However, determine the large peaks on the spectrum because they will provide the data
necessary to read the spectrum.

3. Determine the regions of the spectrum in which the characteristic peaks exist. The IR
spectrum can be segregated into four regions. The first region ranges from 4,000 to 2,500. The
second region ranges from 2,500 to 2,000. The third region ranges from 2,000 to 1,500. The
fourth region ranges from 1,500 to 400.

4. Determine the functional groups absorbed in the first region. If the spectrum has a
characteristic peak in the range of 4,000 to 2,500, the peak corresponds to absorption caused by
N-H, C-H and O-H single bonds.

5. Determine the functional groups absorbed in the second region. If the spectrum has a
characteristic peak in the range of 2,500 to 2,000, the peak corresponds to absorption caused by
triple bonds.

6. Determine the functional groups absorbed in the third region. If the spectrum has a
characteristic peak in the range of 2,000 to 1,500, the peak corresponds to absorption caused by
double bonds such as C=O, C=N and C=C.

7. Compare the peaks in the fourth region to the peaks in the fourth region of another IR
spectrum. The fourth is known as the fingerprint region of the IR spectrum and contains a large
number of absorption peaks that account for a large variety of single bonds. If all the peaks in an
IR spectrum, including those in the fourth region, are identical to the peaks of another spectrum,
then you can be assured that the two compounds are identical.

FTIR allows the qualitative analysis of variations in surface chemistry of natural fibers after
treatment. FTIR spectra of untreated, alkali-treated and NaOH-then-Al2(SO4)3 treated abaca fibers
are
shown in Figure 7a–c. In addition, Figure 7d describes the spectra of dried precipitate or residues
from the spent solution after the Al2(SO4)3 treatment of abaca fibers. Note that the spectra in these
figures were offset vertically to observe the difference more clearly. Table 4 shows the observed
bands
in FTIR spectra and their assignments to functional groups. In general, untreated abaca fiber showed
loss of functional groups based on the comparison of its FTIR spectrum to that of the NaOH-treated
fibers. Peaks that receded in the treated fibers over frequencies 1510 cm−1, 1430 cm−1 and 1250
cm−1
could entail loss of phenolic groups, signifying removal of large amount of lignin and pectin whose
structure is a phenolic polymer. Another visible difference was observed at 1740 cm−1 due to C=O
stretching vibration which is a characteristic band of hemicellulose [42]. The disappearance of this
band indicates the dissolution of hemicellulose after the alkali pretreatment. However there is no
evidence indicating complete removal of these impurities. The decrease in tensile strength of the
samples could be attributed to these extractions. In addition, characteristic peak of Al(OH)3 at 990
cm−1
corresponding to Al–O bonds [43] was observed in the spectra of NaOH-then-Al2(SO4)3 treated
abaca
fiber, and the precipitate or residues from the spent solution. Thus, the FTIR results confirm the
possible formation of Al(OH)3 during neutralization and its deposition on the abaca surface.

Untreated
Treated
The peak intensity reduction found at around 1230cm-1 (C-O) of the acetyl group in lignin
component for 1% and 2% of treated sugar palm fibre was associated with the mercerisation of
lignocellulosic fibres [50]. Mercerisation removed the waxy layer, adhesive pectins and
hemicelluloses that bind the fibre bundles to each other and to the pectin and hemicellulose rich
sheats of the core [41]. The vibration peak at around 1580cm-1 to 1590cm-1 (C-C) associated with
the benzene ring of lignin reduced as the alkali treated concentration increased. In addition, the
vibration peak of C-H stretched at 2900cm-1 in cellulose and hemicellulose that was present in the
untreated fibre became weak, indicating that the part of the hemicellulose was removed [47].
Besides cleaning and modifying the fibre surface, alkali treatment reduces the hydrogen bonding
due to the removal of the hydroxyl groups (-OH) by reacting with sodium hydroxide [51, 52].
The hydroxyl groups are also involved in hydrogen bonding with the carboxyl groups, perhaps
also with the fatty acids that are available on the fibre surface of sugar palm fibres. Thus, for this
test, it was indicated by the reduction and broadening of the peaks around 3200cm-1. Figure 7
shows a typical reaction of sodium hydroxide with a natural fibre [53].
Fibre-OH + NaOHFibre-O-Na++ H2O + surface impurities
Figure 7. Chemical reaction of natural fibre with NaOH solution.

Broad and weak absorption


bands are observed at 3600–3400 cm_1 due to the
stretching vibrations of hydroxyl (OH) groups. The
absorption bands at 2917 and 2846 cm _1 are due to
the C–H symmetric stretching of the methylene (CH2
and CH3) groups. A very intense band is observed at
1717 cm_1 due to the carbonyl (C¼O) stretching from
the ester linkage. The bands at 1598, 1580 and
1493 cm_1 are attributed to the C¼C stretching vibrations
within the aromatic ring. The small intensity
bands at 1450 and 1379 cm _1 are reasoned due to the
asymmetrical and symmetrical vibrations of the methyl
(CH3) group. The strong band at 1238 cm _1 exists due
to the torsional vibrations of CH2 groups. The bands at
1116 and 1065 cm_1 are assigned to the C–O stretching
and C–O–C asymmetric stretching vibrations, respectively.
The bands at 981, 742 and 700 cm _1 exist due to
the C_H out-of-plane bending of trans _CH¼CH_,
¼C_H out-of-plane bending of aromatic ring and
¼C_H out-of-plane bending in singly substituted aromatic
ring, respectively.23–25
The spectra of untreated and treated fiber UPE
composites are both shown in Figure 15 and are
observed to be near similar to the spectra of UPE.
The stretching vibration bands (3600–3440 cm_1) for
OH group in the Borassus fiber/UPE composites
were much broader than that of the UPE. This possibly
suggests the occurrence of hydrogen bonding
between fibers and UPE. For composites, the peak
intensity of the C¼O group at 1717 cm _1 was relatively
higher than that of UPE. This indicates that
covalent bonding has taken place through an esterification
reaction between the fiber OH groups and
polyester COOH groups. However, in the chemically
modified fiber composites, the peak for C¼O groups
at 1717 cm_1 was more intense than the untreated
fiber composites. It appears that due to the removal
of wax and hemicellulose materials from the surface
of the fibers, the number of available OH groups and
reactive sites increased on the fiber surface for greater
esterification with UPE. Other researchers have also
reported similar observations for hemp-polyester
composites

AA-treated fibers reinforced PLA composites (C3, C4, and C5) are better than C1 and C2 to
reduce water absorption. This is due to the AA treatment coating the fiber surface, hence
decreasing the water absorption of the composites themselves [11, 27]. As expected, the acrylic
acid treatment leads to the decrease in the water sorption in the composites. Nevertheless, the
difference in water absorption was not clearly shown with different AA treatment. The order of
decreasing water absorption is as follows: NaOH < Untreated < AA. In addition, the reaction
scheme of acrylic acid with coconut coir fibers is shown in Fig. 4. The reaction result can be seen
from FTIR, which is shown at peak at 2850 cm-1. This peak -CH2- and -CH-group formation more
marked compared to untreated spectrum [27].

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