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Copyright 2011 American Scientic Publishers
All rights reserved
Printed in the United States of America
SENSOR LETTERS
Vol. 9, 15, 2011
Side-Polished Optical Fiber Odor Sensor for VOC
Detection Based on Solvatochromism
Heng Yuan
1
, Se-Hyuk Yeom
1
, Jun-Woo Lim
2
, and Shin-Won Kang
3
1
School of Electrical Engineering and Computer Science, Kyungpook National University, Daegu, Republic of Korea
2
Kyungnam College University of Information and Technology, Busan, Republic of Korea
3
School of Electrical Engineering, College of IT Engineering, Kyungpook National University, Daegu, Republic of Korea
(Received: 13 November 2009. Accepted: 5 August 2010)
In this study, a new application of a side-polished optical ber device for detecting
volatile organic compounds (VOCs) was developed. Reichardts dye [2,6-diphenyl-4(2,4,6-
triphenylpyridinio)phenolate] (RDye) was used as a negative solvatochromic dye in the sensing
membrane. A UV-visible spectrophotometer and an optical spectrum analyzer AQ-6315 were used
to analyze the performance of the RDye solution and the sensor device, respectively. According to
the results, the sensitivity of the p-xylene gas was approximately 5.6 nm/ppm when the concentra-
tion was more than 0.4 ppm. The minimum sensing ability for p-xylene was approximately 20 ppb,
and the response time and recovery time were less than 60 s which was the setting scan period
set for the optical spectrum analyzer. By conducting future research, this method can be improved
to enable the detection of the type and the amount of VOCs with real-time monitoring.
Keywords: Odor Sensor, VOC, Reichardts Dye, Solvatochromism, Side-Polished Optical Fiber.
1. INTRODUCTION
VOCs are emitted not only from industries but also from
equipment used in our daily living, such as carpets,
garbage cans, and wall coatings. In the last decade, as we
have become more aware of the need for a healthy envi-
ronment, the demand for sensors for detecting pollutants
or hazardous substances is on the increase. In environ-
mental health research areas, the odor sensor for detect-
ing VOCs is one of the fastest developing technologies,
especially after many countries have brought out new laws
limiting VOCs in paints.
13
However, most of the VOC
odor sensor systems have a long response time or cannot
accurately detect the VOC concentration.
1, 4
Optical ber
sensor devices, on the other hand, have the advantages
of being extremely sensitive to measurements, immune to
electromagnetic interference, being mechanically exible,
sensitive at remote distances, capable of being multiplexed,
and more. This has interested many scientists and resulted
in some encouraging developments in the development of
devices for VOC detection.
5, 6
In this study, a side-polished optical ber sensor device
was used for VOC gas detection. We used Reichardts

Corresponding author; E-mail: swkang@knu.ac.kr


dye (RDye) which is a negative solvatochromic dye
synthesized by Christian Reichardt
7
and widely used for
chemical sensing applications.
2
It plays an important role
in the sensing membrane for VOC detection. After inves-
tigating the colorimetric properties of RDye mixed with
9 types of VOC solutions, we found that the RDye reacted
with 6 types of VOC gases, thus proving the feasibility
of a side-polished optical ber device for VOC sensing.
Furthermore, -xylene gas was selected for a quantity test.
The results were displayed on a optical spectrum analyzer
(AQ-6315).
2. MATERIALS AND PRINCIPLES
2.1. Side-Polished Optical Fiber Sensor Device
The side-polished optical ber sensor device consists of
a single-mode optical ber and a thin layer of sensing
membrane that works as a multi-mode planar waveg-
uide (PWG). The optical ber was polished on one side
down to the core. Hence, after the sensing membrane
was fabricated, two optic waveguides were formed and an
evanescent eld coupling was generated between the two
waveguides. For an optical wavelength of a specic value,
the effective refractive index of the PWG is in accordance
Sensor Lett. 2011, Vol. 9, No. 1 1546-198X/2011/9/001/005 doi:10.1166/sl.2011.1425 1
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Side-Polished Optical Fiber Odor Sensor for VOC Detection Based on Solvatochromism Yuan et al.
with the core of the optical ber. Thus, the energy trans-
mission between the optical ber and the PWG becomes
larger and can be regarded as a resonance phenomenon that
appears at specic optical wavelengths. A schematic dia-
gram of the side-polished optical ber structure is shown
in Figure 1.
In the schematic diagram, P
I
and P
O
refer to the opti-
cal power at the input and output ports, respectively. J is
the thickness of the PWG. n
eo
and n
ef
are the effective
refractive index of the PWG and the optical ber, respec-
tively. If the mth-order mode of the resonance occurs, the
resonance wavelength \
m
is given by
8
\
m
=
2rJ(n
o
n
ef
)
1,2
mr +
1
+
2
(1)
where n
o
is the refractive index of PWG. 4
1
, 4
2
are
given by

i
(i =1, 2) =tan
1
(
(n
2
eo
n
2
i
)
(n
2
o
n
2
eo
)
(2)
where ( is the polarization-dependent constant (1 for TE
mode, n
2
0
/n
2
i
for TM mode) and n
i
is the refractive index
of the optical ber clad layer.
Therefore, the refractive index of the PWG and the opti-
cal ber play a decisive role in the side-polished optical
sensor device in determining the value of the resonance
wavelength. Because the refractive index of optical ber
is a constant, the sensing ability of this type of device
is determined by the refractive index of the PWG. In
other words, the resonance wavelength will shift with any
change in the refractive index of the PWG (sensing mem-
brane). This is the sensing principle of the side polished
optical ber sensor.
2.2. Sensing System
The VOC gas sensing system consists of a white light
source (AQ 4303B), an optical spectrum analyzer, gas
tanks (VOCs and N
2
), a mass ow controller (MFC), a
pump, a gas chamber, and a side-polished optical ber
sensor device, as shown in Figure 2.
The side-polished optical ber device was xed in the
gas chamber and was connected to a white light source and
an optical spectrum analyzer. Then, VOC gas was mixed
Fig. 1. Schematic diagram of the side-polished optical ber.
VOC
Light source
MFC
Gas chamber
Pump
Optical spectrum analyzer
Fig. 2. Schematic diagram of the sensing system.
with N
2
gas and let into the chamber. The concentration
was regulated by the MFC. As the sensing membrane that
contained the RDye came into contact with the VOC gas,
the refractive index of the PWG changed. This caused a
shift in the resonance wavelength according to Eq. (1).
This shift was detected by the optical spectrum analyzer,
located at the output port of optical ber, and the results
recorded.
3. EXPERIMENTAL DETAILS
3.1. Fabrication of Side-Polished
Optical Fiber Device
The side-polished optical ber device was fabricated using
the following process: a block of quartz measuring 5
10 25 mm was used as the base of the sensing device.
After a 160 nm-wide V groove was fabricated by a
mechanical slicer, a single-mode optical ber was xed in
the V groove as shown in Figure 3(a). The nal stage of
the sensing device fabrication process was the ber pol-
ishing. The fabricated device is shown in Figure 3(b).
(a)
(b)
Fig. 3. SEM images of the V groove and the fabricated device,
(a) SEM images of the V groove; (b) photo of the fabricated device.
2 Sensor Letters 9, 15, 2011
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Yuan et al. Side-Polished Optical Fiber Odor Sensor for VOC Detection Based on Solvatochromism
The sensing solution with 30 wt% PVP and 1.2 wt%
RDye was synthesized after RDye (SIGMA-ALDRICH)
and polyvinyl pyrrolidone (PVP) polymer pow-
der (SIGMA-ALDRICH) were dissolved in N,N-
dimethylacetamide (DMAC) solution.
The polished ber block was coated with the sensing
solution using a spin coater, and the device was dried
overnight. The thickness of the sensing membrane was
approximately several micrometers.
3.2. Reaction Experiments of RDye
Mixed with VOCs
To investigate the refractive index changing of the RDye,
we dissolved the RDye in 4-ml of DMAC solution and
mixed with 1-ml samples of 9 types of VOC solutions:
methanol, propanol, ethanol, butanol, chloroform, DMF,
-xylene, benzene, and toluene, to fabricate 0.01 M RDye
solutions. After that, the change in the absorbing wave-
length and absorbance value were detected by the UV-
visible spectrophotometer under liquid phase.
Next, the VOC gas tests were prepared as follows.
Six types of VOC gasespropanol, butanol, chloroform,
-xylene, toluene, and hexanewere detected using the
same method, one by one. First, several drips of VOC
solutions were dropped near the side-polished optical ber
sensor device in the chamber, and then the chamber was
covered. As the VOC solutions evaporated, the color of
the sensing membrane that contained the RDye changed,
and the refractive index of the sensing membrane changed.
This caused a shift in the resonance wavelength that was
detected by the optical spectrum analyzer.
After the resonance wavelength shift experiment of
VOC gas sensing, -xylene gas was selected for use in the
quantity test. -xylene gases with a concentration range
from 0.01 to 1 ppm were detected in this experiment.
4. RESULTS AND DISCUSSION
4.1. Colorimetric Properties of RDye
Mixed with VOC Solutions
The change in the absorbing wavelength and absorbance
value of the RDye mixed with 9 types of VOC solutions
methanol, propanol, ethanol, butanol, chloroform, DMF,
-xylene, benzene, and toluenewere detected by a
UV-visible spectrophotometer. The results, shown in
Figures 4(a) and (b), show that RDye is very sensi-
tive to different VOCs, and a different VOC solutions
lead to different wavelength shifts and different degree of
absorbance, especially in solutions of methanol, propanol,
ethanol, and butanol.
The number of solutions in Figure 4(b) represents the
number in Figure 4(a). We set the DMAC solution (with
RDye and without VOCs) as the reference solution. In
Figure 4(b), we can see that after the VOC solutions
(a)
(b)
Fig. 4. Spectrum analyzes results of RDye mixed with VOC solutions,
(a) absorbance and wavelength results of RDye mixed with VOC solu-
tions; (b) variation of absorbance and wavelength after RDye mixed with
VOC solutions.
are added to the reference solution, not only had the
color changed, but also the optical absorbance (transmit-
tance). The negative absorbance means that the transmit-
tance increased, and the negative wavelength means that
the VOC gases cause a hypsochromic shift in the RDye.
The result is useful to recognize different VOC gases and
mixed VOC gases in future works.
According to Figure 4, -xylene has the least
absorbance changes of all the VOC solutions tested. There-
fore, because we focus on the wavelength shift between
RDye and VOC reaction, the -xylene gas was selected to
be used in the quantity test.
4.2. Resonance Wavelength Shift
Test of VOC Gas Sensing
Figure 5 shows the sensing results of the RDye-coated
side-polished optical ber for 6 types of VOC gases
propanol, butanol, chloroform, -xylene, toluene, and
hexane.
The results indicate that different VOCs lead to differ-
ent resonance wavelength shifts and different absorbance
Sensor Letters 9, 15, 2011 3
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Side-Polished Optical Fiber Odor Sensor for VOC Detection Based on Solvatochromism Yuan et al.
Fig. 5. Side-polished optical sensor device for VOC gases detection.
decrease. These results match the rst experiment results.
It means that, with the aid of RDye, the sensor device
can distinguish small differences of polarity from different
VOCs. Furthermore, the absorbance change means that the
clarity of the sensing membrane changed, which leads to a
change in energy of transmission between the optical ber
and the PWG.
4.3. Quantity Test of P-Xylene Gas Sensing
The results of the quantity test of -xylene gas sensing are
shown in Figure 6. In order to express the result clearly,
the results at the concentrations of 0, 0.2, 0.4, 0.6, and
0.8 ppm were selected and compared. And a resonance
wavelength of close to 800 nm was selected. According
to the results, the resonance wavelength showed a hyp-
sochromic shift property as the concentrations of -xylene
increased. On the other hand, compared to the wavelength Fig. 6. Quantity test of -xylene gas sensing.
4 Sensor Letters 9, 15, 2011
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Yuan et al. Side-Polished Optical Fiber Odor Sensor for VOC Detection Based on Solvatochromism
Table I. The resonance wavelength shift value according to the con-
centration of -xylene.
Concentration of -xylene (ppm) Wavelength shift (nm)
0.01 0
0.02 0.04
0.04 0.12
0.06 0.2
0.08 0.28
0.1 0.34
0.2 0.6
0.4 1
0.6 2
0.8 3.1
1 4.4
shift, the intensity changes were so small that they can be
ignored for low concentration VOC detection. The results
matched those of Figures 4 and 5. In future works, the
intensity change experiments will be prepared together
with the wavelength shift experiments. This is valuable for
studies of mixed VOCs detection.
According to the result, the sensitivity of the side-
polished optical ber sensor device for -xylene was
approximately 5.6 nm/ppm, with a concentration of more
than 0.4 ppm. Below the concentration of 0.4 ppm, the
sensitivity was weak. The sensing limit of -xylene gas
concentration was approximately 20 ppb in this experi-
ment. The data are shown in Table I.
At the same time, the response time and recovery time
were less than 60 s. which was the setting scan period of
the optical spectrum analyzer that we set.
5. CONCLUSION
This study reported a new application of a side-polished
optical ber device for VOC gas detection. RDye, a widely
used negative solvatochromic dye with a hypsochromic
shift in the UV/VIS absorption band, with increasing sol-
vent polarity, was the most important part of the sensing
membrane. Four tasks were undertaken in this study: the
fabrication process of a side-polished optical ber device,
the colorimetric properties of RDye mixed with VOC
solutions, the resonance wavelength shift experiments for
6 types of VOC gases using the side-polished optical ber
device and the quantity test for -xylene gas detection.
The results were detected by an optical spectrum analyzer
located at the output port of the optical ber.
According to the results, the sensing system shows high
sensitivity for different VOCs. Even though the sensitiv-
ity of the -xylene gas in reacting with RDye is much
weaker than other VOCs, it still has a wavelength shift of
5.6 nm/ppm with a minimum value of detection of approx-
imately 20 ppb. The response time and the recovery time
were less than 60 s. which was the setting scan period of
the optical spectrum analyzer. We believe that any sensor
device produced using the same fabrication process under
the same conditions would show good stability.
In the future, we plan to use other VOC gases in mixed
gas experiments prepared using different sensing mem-
branes and side-polished optical ber sensor device array
methods.
Acknowledgments: This work was supported by Korea
Science and Engineering Foundation (KOSEF) grant
funded by the Korea government (MEST) (No. 2009-
0063405).
References and Notes
1. N. A. Rakow and K. S. Suslick, Nature 406, 710 (2000).
2. J. H. Krech and S. L. Rose-Pehrsson, Anal. Chim. Acta 341, 53
(1997).
3. K. S. Suslick, N. A. Rakow, and A. Sen, Tetrahedron 60, 11133
(2004).
4. Y. Q. Chen and C. J. Lu, Sen. Actuator, B 135, 492 (2009).
5. S. Zheng, L. N. Binh, and G. P. Simon, J. Lightwave Technol. 13, 244
(1995).
6. A. Cusano, M. Consales, A. Crescitelli, M. Penza, P. Aversa, C. D.
Veneri, and M. Giordano, Carbon 47, 782 (2009).
7. C. Reichardt, Chem. Rev. 94, 2319 (1994).
8. R. Vallee and G. He, J. Lightwave Technol. 11, 1196 (1993).
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