Sensors and Actuators A 205 (2014) 5862

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Sensors and Actuators A: Physical

journal homepage: www.elsevier.com/locate/sna

Conducting polymer coated optical microber sensor

for alcohol detection
Yeong Siang Chiam a , Kok Sing Lim b , Sulaiman Wadi Harun b ,
Seng Neon Gan a , Sook Wai Phang a,
a
b

Department of Chemistry, Faculty of Science, University of Malaya, 50603 Kuala Lumpur, Malaysia
Photonics Research Centre, Department of Physics, University of Malaya, 50603 Kuala Lumpur, Malaysia

a r t i c l e

i n f o

Article history:
Received 12 April 2013
Received in revised form 21 October 2013
Accepted 24 October 2013
Available online 1 November 2013
Keywords:
Polyaniline
Microber sensor
Alcohol
Wavelength shift

a b s t r a c t
In this study, an optical microber sensor coated with conducting polymer, polyaniline (PAni) is investigated as a detector for alcohols. PAni was synthesized by chemical oxidation method and dioctyl sodium
sulfosuccinate (AOT) was used as the dopant. PAni was then coated onto the microber by drop coating
method. The proposed sensor exhibits wavelength shift in the output spectrum in response to various
types of alcohols at different concentrations. The output response can be associated with the solution
refractive index and number of alkyl substituent of alcohol. Furthermore, this sensor also shows excellent
repeatability in the detection. In conclusion, a conducting polymer based microber optical sensor for
alcohol detection with simple, low cost and effective set-up was successfully achieved in this study.
2013 Published by Elsevier B.V.

1. Introduction
Fiber optic sensors have attracted a great deal of interest due
to their excellent performance in numerous sensing applications
include chemistry, biomedicines and environmental engineering
[14].
Generally, ber optics sensors can be divided into two categories, namely extrinsic and intrinsic sensors. With extrinsic
sensors, light is emitted from the ber and is blocked or reected
back into the ber-optic system such as optodes. While for intrinsic
ber, light is transported at internal sensing system [5]. In this type
of sensors, modications are made at the structure of optical ber
such as ber cladding removal and tapered bers.
The operating principle of most electrical based chemical sensors is based on electrical conductivity of the chemical analytes
which is a function of the amount of ions in solution. The measured electrical conductivity is then translated into the degree of
ion concentration. However, this technique is susceptible to electrical interference, corrosion to the sensor [6]. Therefore, optical based
sensors are preferable due to their many promising properties such
as non-invasive nature, immunity to electromagnetic interference,
high sensitivity, compact size, low cost, possibility of real time monitoring and remote sensing [7,8]. Besides, these sensors can also be
used for refractive index measurement [9,10] in which only a small
volume of sample is required. The principle of the measurement

Corresponding author. Tel.: +60 3 79674122; fax: +60 3 79674193.

E-mail address: pinkyphang@gmail.com (S.W. Phang).
0924-4247/$ see front matter 2013 Published by Elsevier B.V.
http://dx.doi.org/10.1016/j.sna.2013.10.025

is based on the between the guided light in the single mode ber
with surrounding medium. The resonant wavelength varies with
different refractive index of the surrounding medium. Therefore,
this sensor can also be employed for chemical sensing and liquid
concentration measurement. Subsequently, optical measurement
can be highly appealing. However, the drawback of this system is
its strong dependence on temperature which can be eliminated
through incorporating a temperature control into the system or
adopting temperature discriminative conguration [11].
Optical microber devices are well known as low-loss silica
waveguides in the forms of loops [12], knots [13], or coils [14,15],
and have been demonstrated for different applications include adddrop lters [16], lasing systems [1719], nonlinear optical systems
[20], and sensing devices [21,22]. Due to the small diameter of
microber, the evanescent eld in the surrounding of microber
is large and thus the microber devices are sensitive to changes in
of the surrounding medium, particularly the refractive index (RI)
of the medium. Ultraviolet (UV) light detection using microber
device has been demonstrated by coating the knot area of the device
with photoresponsive liquid crystal, which refractive index can be
inuenced by UV light irradiated on the device. As a result, the output spectrum of the device shifts when exposed to the UV light
[23].
Applying the voltage on the rod tunes the spectral signal resonating from the microber ring resonator. The operating principle
of optical microber sensors is followed the path whereby light
measurement is taken based on the resonant coupling of the light
guided by the single mode ber. Response to external physical,
chemical, biological, or other inuences will have effects on the

Y.S. Chiam et al. / Sensors and Actuators A 205 (2014) 5862

light guided within the ber optic sensor [6]. Therefore, ber-optic
sensor with cladding modication is very attractive due to its large
dynamic range, high sensitivity, and superior integration with other
ber systems.
In 1960, Heeger et al. discovered that conducting polymer is a
new generation of polymer which displays the combined mechanical properties and processibility of polymer as well as the electronic
and optical properties of metals or semi-conductors. Conducting
polymer, while being organic polymer, has the unusual property
of possessing high electrical conductivity and exhibits a range
of properties from semiconductor to near-metallic behavior. Furthermore, they also display the optical properties of metals or
semi-conductors [24]. Some well known examples of conducting
polymers are polyaniline (PAni), polypyrrole (PPy) and polythiophine (PTh), which are being used as detection medium in ber
optic sensor.
Conducting polymer is used in optical sensors due to its many
advantages such as easy fabrication, excellent ambient stability,
rapid and reversible adsorption and desorption kinetics, has low
poisoning effect and low power consumption [25,26]. Besides,
conducting material such as PAni is independent on detecting environment such as surrounding temperature and air humidity while
traditional sensing material, metal oxide such as SnO2 and Fe2 O3
are highly dependent on detecting environment. This make the
conducting polymer favorable use as sensing material compared
with traditional material [26]. Furthermore, conducting polymer
sensor is light, cheap and interacts more favorably with organic
compounds compared with traditional material [27]. On the others
hand, PAni can shows multiple color change depending on its oxidation states. These macroscopic color changes can be used as an
indicator in optical sensing system [28].
In this study, an optical microber alcohol sensor fabricated
and experimentally investigated. This device is manufactured by
depositing PAni on a microber resonator, particularly at the
microber knot resonator the sensing area of the sensor which
is then used for the detection of alcohols of different concentrations. This proposed sensor is a simple, robust and low cost device
that can quantitate a measurable attribute and converts it into a
signal which can be read by an observer or by an instrument. Different types of alcohol such as methanol, ethanol, 1-propanol and
2-proapanol are examined in this study. Besides, alcohols with various concentrations are also being studied. From our knowledge, we
are the rst to report on this novel low cost and effective conducting
polymer-based optical sensor for alcohol detection.
2. Experimental
2.1. Chemicals
All the chemicals such as aniline (Ani), dioctyl sodium sulfosuccinate (AOT) and ammonium persulphate (APS) used were
procured from SigmaAldrich (USA) while hydrochloric acid (HCl)
used was from RCI Labscan (Thailand). Besides, methanol (CH3 OH),
ethanol (C2 H5 OH), 1-propanol and 2-propanol (C3 H7 OH) used were
purchased from SYSTERM (Malaysia). All the chemicals used were
analytical grade and were used without purication. Deionized
water was collected from Millipore water purication system. Preclean microscope glass slide with width and length of 75 mm and
25 mm, respectively, were used as substrate for the microber
structure during measurement.
2.2. Synthesis of polyaniline (PAni)
In the optical set-up, the sensing layer of coated ber is consisting of chemically oxidized PAni using Ani as monomer, AOT as

59

dopant and APS as oxidant. Ani was slowly added into the AOT solution and stirred for 2 h. It was followed by slow addition of APS into
the above solution. The polymerization reaction was carried out at
low temperature for 24 h. The resultant sample was washed with
distilled water to remove the unreacted AOT, APS and monomer.
Extraction and dilution were carried out to obtain the desired PAni
concentration.

2.3. Chemical characterizations

2.3.1. Fourier transforms infrared (FTIR) spectroscopy
FTIR spectroscopy of PAni was recorded using FT-IR spectrometer (Perkin Elmer RX 1 model) from wavelength range of
4004000 nm to conrm the chemical structure of PAni.

2.3.2. UV-vis spectroscopy

Ultravioletvisible (UVvis) spectroscopy of PAni was recorded
using UVVis spectrophotometer (UV-1650 PC model) in the wavelength range of 300900 nm to determine the conducting behavior
of PAni.

2.4. Preparation of tapered ber coated with PAni

In this study, single mode glass ber (SMF) was used. The optic
ber device composes of a microber knot resonator (MKR) in a
Sagnac loop reector. Using the ame brushing method, optical
microber with length of 56 cm is fabricated from an SMF. After
that, the microber knot resonator was made and xed at a diameter of 0.52.0 mm. Then, the microber structure was embedded in
Teon in order to maintain the physical structure and resonance
condition [29]. PAni solution was then deposited onto the MKR
region using drop coating method. The device was left to dry for
30 min.

2.5. Application of PAni based tapered ber in alcohol detection

Fig. 1a shows the optical set-up for microber sensor which laser
with wavelength of 1550 nm was used as a light source for the
microber device. This microber device consists of a microber
knot resonator which is coated with PAni. In the experiment, this
device is connected to a 3-port circulator so that the output wave
from the microber device can be circulated out of the system. The
incident wave, Ein enter into port 1 and exits through port 2 before
it enters the microber device. Then, the waves pass through a
coupler which splits the wave into two. The two waves counterpropagate in the Sagnac loop and enter the MKR (as shown in
Fig. 1b) through its two arms. Finally, the waves recombined at the
coupler and produces the output waves, Eout and it is routed out
from the device through port 3. The output wave is analyzed and
recorded using an optical spectrum analyser (OSA) [29]. To eliminate the temperature inuence on the microber, the experiment
is conducted in air-conditioned laboratory in which the temperature is regulated at 26 C. The microber device is placed on a
large aluminum optical table. This stabilizes the temperature of
the microber device and the wavelength uctuation is less than
0.02 nm/h.
This microber device which coated with PAni is used to study
alcohols at different concentrations such as 1%, 5%, 10%, 20% and
50%. The alcohols which were investigated in this study include
methanol, ethanol, 1-propanol and 2-propanol. Refractive indexes
for each alcohol with different concentration are recorded. The
optical property of PAni toward different types of alcohols was
analyzed by OSA.

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Y.S. Chiam et al. / Sensors and Actuators A 205 (2014) 5862

Fig. 1. (a) Optical set-up for microber sensor. (b) Microscope image of microber knot resonator (MKR). Inset shows the drawing of the MKR.

3. Results and discussion

3.1. Chemical characterizations
3.1.1. Fourier transform infra-red (FTIR) characterization
Fig. 2 shows the FTIR spectrum of the resulted PAni. The peaks at
1614 cm1 and 1460 cm1 are assigned to quinoid and benzenoid
rings vibration in the polymer chain, respectively. The absorption
band at 1614 cm1 also supports the presence of Ani repeating units
in the PAni chain being connected via a head-to-tail monomer coupling during polymerization. Furthermore, the peaks at 1291 cm1
and 1197 cm1 indicating the C N stretching in bipolaron polymer is highly doped and exist in the conducting form. The peaks
at 36003000 cm1 and 30002800 cm1 correspond to the N H
and C H stretching vibrations of PAni, respectively. The FTIR spectrum reveals the PAni exist in the emeraldine salt form [30,31].

Fig. 3. UV spectrum of PAni.

3.1.2. Ultravioletvisible (UVvis) characterization

Refer to the UV spectrum on Fig. 3, the peak observed at 353 nm
is correspond to * transition of benzenoid rings. The shoulder peak appears at 434 nm is due to the localized polaron bands
of protonated PAni while the strong absorption peak appears at
755 nm indicates the conducting emeraldine salt phase of doped
PAni [30]. FTIR spectrum in Fig. 2 and UVvis spectrum in Fig. 3
conrm the polymerization of PANi. Since the microber structure
is in the scale of micrometer, an optical microscope equipped with a
CCD camera is used to observe and capture the image of PAni coated
microber device. The above gure shows that the PAni has been
deposited onto the MKR. The electrical conductivity measurement
has been carried out and the measured conductivity of the PAni
lm is 1 102 S/cm2 .
3.2. Application of PAni coated microber in alcohols detection

Fig. 2. FTIR spectrum of PAni.

Fig. 4 shows the output spectra of PAni coated microber device

before and after its immersion in 1% of n-propyl alcohol. Based on
Fig. 4, there is a wavelength shift for PAni coated microber from

Y.S. Chiam et al. / Sensors and Actuators A 205 (2014) 5862

61

Fig. 7. Output response of the sensor to the refractive indices of different alcohols.
Fig. 4. Wavelength shift before and after immersion in 1% of n-propyl alcohol during
optical measurement.

Fig. 5. Electrostatic interaction beween PAni and n-propyl alcohol.

Fig. 8. Recycle ability of PAni coated microber toward 5% ethanol.

Fig. 6. Wavelength shift during optical measurement for different types of alcohols.

1540.42 nm (before immersion) to 1539.87 nm (after immersion).

This wavelength shift is due to electrostatic interaction between
the partial positive amine group ( NH+ ) from PAni backbone and
the partial negative charge of hydroxyl group ( OH ) from alcohol solution (Fig. 5). Due to this electrostatic interaction, PAni
backbone is restricted from twisting by the hydroxyl group with
different alkyl substituent which cause solvachromic effect and
thus decrease the dihedral angle between adjacent aromatic rings
of the polymer. This theory is proposed by Ginder et al. through
theoretical consideration [32,33].
The transformation from the planar to the tetrahedral structure will signicantly twist the torsion angle between the aromatic
groups of PAni due to the steric hindrance of the aromatic groups.
The increase in the band gap signicantly reduce the absolute
coefcient of solvent and cause the solvachromic shift. Thus, the
excitation peak of PAni after immersion in alcohol solution shift to
the lower wavelength or hysochromoc shift (blue shift) and appear
at higher energy compare to the excitation peak of the PAni before
immersion in alcohol solution [34].
From wavelength shift obtained in Fig. 6, the increase of carbon
atoms in the alkyl group of alcohol molecules (methanol, ethanol,
1-propanol and 2-propanol) will increase the effect of steric

hindrance and cause red shift to be more pronounced in the optical

measurement. With increasing of carbon atoms in the alkyl group,
steric hindrance effect will weaken the electrostatic interaction
between the NH+ groups from PAni backbone with the hydroxyl
group of alcohol. From methanol to propanol, this effect significantly increases the dihedral angle between adjacent aromatic
rings of PAni. Hence, the increase in band gap signicantly reduce
the absolute coefcient of solvent and cause the solvachromic shift.
Thus, increasing size of alkyl group for alcohol molecules will cause
an increase in bathochromic shift (red shift) in optical measurements [35].
Fig. 7 shows that the refractive index is proportional to the concentration of alcohols. With increasing concentration, wavelength
shows a bathochromic shift (red shift) during optical measurement.
The increase in alcohol concentrations (from 1% to 30%) significantly increases the refractive index of the solution and effective
refractive index at the microber. The change in effective refractive index of the microber causes wavelength shift in the output
spectrum of the microber sensor. The relationship between wavelength shift and refractive index change in the solution can be
well explained with a linear expression,  = kn where  is
the wavelength shift, n is the refractive index change and k is the
sensitivity coefcient.
From Fig. 7, it shows that refractive index increases with the
increment of alcohol concentration. Besides, optical measurement
shows increase in the wavelength shift with increasing in alcohol
concentration (Refer Fig. 6). Thus, the wavelength shift is directly
proportional to the refractive index of each alcohol.
According to Plancks constant formula, E = hc/, as the wavelength increase, the energy required for electron transition
between PAni and alcohol will be less which results to a red shift
(bathochromic shift) in the absorbance spectrum.
PAni coated microber shows good recyclability in alcohol
detection as shown in Fig. 8. According to Fig. 8, there is a constant

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Y.S. Chiam et al. / Sensors and Actuators A 205 (2014) 5862

wavelength shift before and after detection of alcohol. This PAni

coated microber device shows a good recycle ability. This sensor
can be useful for the monitoring of alcohol concentration and quality control in drug synthesis in the pharmaceutical and biomedical
industry.
4. Conclusion
A simple optical sensor is demonstrated as a device to detect
various alcohols namely methanol, ethanol, 1-propanol and 2propanol of different concentrations. The study indicates red shift in
the output spectrum with increasing steric effect and concentration
of alcohol. This is due to the increase in dihedral angle and average
band gap in conjugated polymer system, which cause the lower
energy receive by PAni ber. On the other hand, this PAni coted
microber sensor exhibits high sensitivity and good repeatability
(10 times) in detection of alcohol.
Acknowledgements
The authors would like to thanks University of Malaya for providing nancial support such as the UMRG grant (RP008C-13AFR),
ERGS grant (ER003-2012A), PPP grant (PV143-2012A) and HIR
grant (UM.C/625/1/HIR/181) in completing this studies.
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Biographies
Yeong Siang Chiam received her B.Sc. degree in Chemistry from Chemistry Department, University of Malaya in 2011. Currently, she is pursuing her M.Sc. degree at
the same department. Her current research interest is conducting polymers.
Kok Sing Lim received his B.Eng. degree from the Department of Electrical Engineering, Faculty of Engineering, University of Malaya, Malaysia, and Ph.D. with the
Photonics Research Centre, University of Malaya, Malaysia in 2008 and 2012, respectively. He is currently a senior lecturer at University of Malaya. His current research
interests include optics of microber devices, in-ber gratings, ber-optic sensors
and ber lasers.
Sulaiman Wadi Harun received the B.E. degree in electrical and electronics system
engineering from the Nagaoka University of Technology, Nagaoka, Japan, in 1996,
and the M.Sc. and Ph.D. degrees in photonics from the University of Malaya, Kuala
Lumpur, Malaysia, in 2001 and 2004, respectively. He is currently a full professor
at Photonics Research Centre, University of Malaya. His current research interests
include ber-optic active and passive devices.
Seng Neon Gan received his B.Sc., M.Sc. and Ph.D. degrees in chemistry from the University of Malaya, Kuala Lumpur, Malaysia. He is the member of American Chemical
Society and Royal Society of Chemistry. Furthermore, he is also the fellow of Malaysia
Scientic Association and Institute Kimia Malaysia. He is currently a professor at
University of Malaya. His current research interests include polymer chemistry,
chemistry of catalysis, bioplastics, material processing technology, bio-compatible
materials as well as waste management and utilization.
Sook Wai Phang received the B.Sc. degree in Chemical Technology and M.Sc. degree
in Chemistry from Universiti Kebangsaan Malaysia in 2002 and 2004, respectively.
She worked as a chemistry lecturer at Inti International University in 2004. She completed her PhD degree in Engineering (Polymer) from Yamagata University, Japan in
2008. Currently, she is a senior lecturer at the Chemistry Department, Faculty of Science, University of Malaya. Her research interests include synthesis of conducting
polymers and their applications in ber optic sensors, chemical sensors, microwave
absorbers, solar cell, etc.