Sensors and Actuators B 161 (2012) 818823

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Sensors and Actuators B: Chemical

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Cd concentration sensor based on ber grating technology

U.S. Raikar a, , A.S. Lalasangi a , Jyoti F. Akki a , Prasad Raikar b , K.G. Manohar c , T. Srinivas d ,
N.M. Badiger a , P. Radhakrishnan e
a

Department of Physics, Karnatak University, Dharwad 580003, Karnataka, India

KLEs College of Engineering & Technology, Belgaum, Karnataka, India
Laser & Plasma Technology Division, BARC, Mumbai 400085, India
d
Electrical Communication Engineering Department, Indian Institute of Science, Bengaluru 560012, Karnataka, India
e
International School of Photonics, Cochin University of Science & Technology, Cochin 682022, Kerala, India
b
c

a r t i c l e

i n f o

Article history:
Received 17 June 2011
Received in revised form 1 November 2011
Accepted 8 November 2011
Available online 26 November 2011
Keywords:
Fiber Bragg grating
Long period grating
Concentration sensor
Cadmium
Spectrum

a b s t r a c t
Fiber Bragg grating (FBG) and Long Period Grating (LPG) chemical sensors are one of the most exciting developments in the eld of optical ber sensors. In this paper we have proposed a simple and
effective chemical sensor based on FBG and LPG techniques for detecting the traces of cadmium (Cd) in
drinking water at ppm level. The sensitiveness of these two has been compared. Also, these results have
been compared with the results obtained by sophisticated spectroscopic atomic absorption and emission
spectrometer instruments.
For proper designing of FBG to act as a concentration sensor, the cladding region of the grating has been
etched using HF solution. We have characterized the FBG concentration sensor sensitivities for different
solutions of Cd concentrations varying from 0.01 ppm to 0.04 ppm and observed reected spectrum in
FBG and transmitted spectrum in LPG using Optical Spectrum Analyzer. Proper reagents have been used
in the solutions for detection of the Cd species. The overall shift in wavelength is 10 nm in case of LPG
and the shift of Bragg wavelength is 0.07 nm in case of FBG for 0.010.04 ppm concentrations.
2011 Elsevier B.V. All rights reserved.

1. Introduction
The accuracy in detection and determination of concentration
of chemicals/contaminants (especially in ppm/ppb level) present
in the ground water are very important to meet the drinking water
standards of World Health Organization (WHO). If the concentration of dissolved chemicals in water crosses its limit, it may lead to
harmful effects on human health. Out of many dissolved chemicals,
cadmium (Cd) is an important one. A very large amount of cadmium
is released into the environment every year (about 25,000 tons a
year). About half of this is released into rivers through weathering
of rocks and some cadmium is released into air, through forest res
and volcanoes. The rest of the cadmium is released through human
activities, such as manufacturing and zinc ore processing. Contamination of drinking-water may occur as a result of the presence of
cadmium as an impurity in the zinc galvanized pipes or cadmiumcontaining solders in ttings, water heaters, water coolers and taps.
Short-term consumption (over days or weeks) of high levels of cadmium (Cd) through drinking water can cause nausea, vomiting,

Corresponding author. Tel.: +91 836 2215316/2772550; fax: +91 8360 2747884;
mobile: +91 9480480079.
E-mail address: usraykar kud@yahoo.co.in (U.S. Raikar).
0925-4005/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2011.11.039

and diarrhea, while long-term (over years or decades) consumption

may cause kidney dysfunction and osteoporosis [1,2]. As per World
Health Organization, the maximum permissible limit of Cd in water
is 0.005 ppm. So, precise measurement of Cd in drinking-water at
low concentration is very important.
Many of the methods like chemical, electrochemical and spectroscopy methods are adopted in nding the concentration of
cadmium [2]. Atomic Absorption Spectroscopy (AAS) is one of
the techniques for determining the concentration of a particular
metal element within a sample. The sample is atomized in the
ame, through which radiation of a chosen wavelength is sent.
A disadvantage of the AAS technique is the non-linearity of the
calibration curves when absorbance becomes higher than 0.5. The
relative standard deviations are between 0.3 and 1% for absorbance
of 0.10.2. Detection limits for ame AAS vary enormously from
15 ppb to more than 1000 ppb. Some elements cannot be measured at all inductively coupled plasma (ICP) is another technique
used for the detection of trace metals in samples. But certain unstable elements require special facilities for handling the radioactive
fume of the plasma. Also, an ICP has difculty handling halogens.
Special optics for the transmission of the very short wavelengths
become necessary [2,3].
Fiber optic sensors offer numerous advantages over electric
transducers due to their small size, high sensitivity and possibility

U.S. Raikar et al. / Sensors and Actuators B 161 (2012) 818823

of distributed measurements. The research eld in optical ber

grating technology has opened a new platform in both communication and sensor eld. These ber optics have originally
developed to multiple signals in optical networks and are now
being widely used in the eld of sensors, such as to measure strain,
temperature, pressure and as a chemical sensor [35]. Specically
ber grating sensors have attracted considerable attention.
Fiber gratings are categorized into two classes short period
grating (Bragg gratings) and long period gratings. In Bragg gratings,
coupling occurs between modes traveling in opposite direction. The
grating period in ber Bragg grating (FBG) is of the order of less than
100 m [6]. When a broadband light is connected to FBG a narrow
band of wavelength centered at one certain particular wavelength
known as Bragg wavelength B is reected. The FBG works on the
principle of reected wavelength B and is given by
B = 2 neff 

(1)

where neff is the effective refractive index of the core and  is

grating period.
Long period gratings (LPG) are the special class of ber gratings
in which the period of the index modulation is such that it satises
a phase matching condition between the fundamental core mode
and a forward propagating cladding mode of an optical ber. For a
long period grating, a periodic modulation of the index of refraction
in the ber core typically has a period in the range 100 m1 mm
and length of a few cm.
Principle of operation and some characteristics of long period
gratings are reported by Vengsarkar et al. in 1996 [7]. LPG promotes
coupling between the propagating core mode and co-propagating
cladding modes. The high attenuation of cladding modes results
in the transmission spectrum of the ber containing a series of
attenuation bands centered at discrete wavelengths, each attenuation band corresponding to the coupling to different cladding
mode. Phase matching between the mode propagating in the core
of the ber and a co-propagating cladding mode is achieved at the
wavelength m is [7].
)
m = (nco nm
cl

(2)

819

The unique sensitivity to the external refractive index of a long

period ber grating (LPFG) structure has invoked some discussion on using LPFGs for chemical/biochemical sensing. Patrick et al.
demonstrated that LPFGs could be used in effectively measuring the
concentration of ethylene, a principal compound, in the antifreezer
[13]. They fabricated LPFG of grating period 275 m could detected
a tiny change (less than 1%) in that concentration. Allsop and
co-workers [14] performed the detection of organic aromatic compounds in parafn by an LPFG sensor with optimized sensitivity.
They suggested that an LPFG approach in this application may be
more attractive than the conventional HPLC and UV spectroscopy
methods, as an LPFG could potentially offer in situ process control
measurements for oil renery industrial applications [14]. Many
chemical concentration sensors have been proposed previously
based on LPG by many workers [1518]. Cadmium was detected
from 1 to 8 ppb by PCS ber on the basis of surface plasmon resonances [19].
We demonstrated here the fabrication and design of ber grating based chemical sensor for Cd2+ in the range of 0.010.04 ppm.
A comparative study has been done for the results of these grating
sensors with results obtained using atomic absorption spectrometer (AAS) and inductively coupled plasma (ICP) for ground water
samples collected in this geological region.
2. Fabrication of ber gratings
2.1. Fabrication of FBG
Fabrication of a stable ber Bragg grating is very important.
External writing method was introduced by Meltz et al. using
holographic technique [20]. After this, two more techniques were
introduced, the phase mask technique by Hill et al. [21] and the
point-by-point technique by Malo et al. [22]. Out of three stable techniques, holographic technique and phase mask technique
are widely used all over world, leaving point-by-point technique
owing to its draw backs. For uniform grating fabrication phase
mask technique has many advantages over holographic technique.

where m is the peak wavelength of the resonance band between

the core mode and the cladding mode, nco and nm
are effective
cl
refractive index of the core mode and of the mth order cladding
mode respectively and  is the period of LPG. The minimum transmission of the attenuation bands is governed by the expression
[8].
Ti = 1 sin2 (m L)

(3)

where L is the length of the LPG and m is the coupling coefcient

for the mth cladding mode.
In the FBG, reected wavelength mainly depends on parameters like grating pitch and effective refractive index. When cladding
region is reduced along the length of grating region, the neff is
signicantly affected by surrounding refractive index (SRI) [8]. By
reducing the cladding part of ber, grating can be made to act as a
chemical sensor [9]. The change of wavelength due to the changes in
measurand is used for sensing applications. Our particular interest
is the use of FBGs as chemical sensors where the change of wavelength is induced by changing the chemical composition around
the sensor. In order to measure small changes in composition, it
is important for the optical mode to penetrate evanescently into
the surrounding solution. A sensing scheme for chemical sensing
was proposed based upon Bragg grating in- and out-coupling for
increased uorescence excitation [10]. A method of increased sensitivity to surrounding index by etching the ber close to the core
diameter was presented by Asseh et al. [11]. Sensors have been
developed for propylene glycol and sugar solutions down to 0.067%
and 0.027% respectively by the half etched FBG [12].

Fig. 1. Fabrication ber grating (a) Fiber Bragg grating and (b) long period grating.

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U.S. Raikar et al. / Sensors and Actuators B 161 (2012) 818823

Power (in W)

0.00003

0.00002

0.00001

0.00000
1546

1547

1548

1549

Wavelength (in nm)

Fig. 3. Transmitted spectrum of LPG.
Fig. 2. Reected spectrum of FBG.

We fabricated FBG using phase mask technique. Phase mask is a

diffractive element with one dimensional surface relief structure
fabricated on high-quality fused silica at surface transparent to
UV writing beam [23]. The prole of the periodic gratings is chosen such that when an UV beam is incident on the phase mask, the
zero order diffracted beam is suppressed and the diffracted plus
and minus rst orders are maximized. A near-eld fringe pattern
is produced by the interference of the plus and minus rst-order
diffracted beams. The period of the fringes is one-half that of the
mask. The interference pattern photo imprints a RI modulation in
the core of a photosensitive optical ber placed very near to the
phase mask (Fig. 1a).

A singlemode GeB co-doped photosensitive ber (Newport

F-SBG-15, with step index prole of NA 0.120.14, cladding diameter 125 1 m, and operating wavelength 1550 nm) is chosen to
form the FBG gratings in the core region. Acrylate buffer coating
surrounding cladding (about 56 cm) where the grating to be
written is stripped off and placed in-front of phase mask as shown
in Fig. 1a. UV beam from KrF laser (248 nm) is made to incident
on the ber through a phase mask. A grating period of 0.530 m
of length 1.5 cm is formed. When a broad band light source (JDS
Uniphase, 15301600 nm, 17 mW) is injected into one end of FBG,
the wavelength that satises Bragg condition is reected back
and the reected wavelength is collected using a 3 dB coupler and
characterized using optical Spectrum Analyzer (OSA) (Proximion
software) as in Fig. 2. The grating formation can be monitored

Fig. 4. Experimental set up for (a) ber Bragg grating and (b) long period grating.

U.S. Raikar et al. / Sensors and Actuators B 161 (2012) 818823

821

0.01 ppm
0.02 ppm
0.04 ppm
water

0.000020

Power in W

0.000016

0.000012

0.000008

0.000004

0.000000
1545.3

1545.6

1545.9

1546.2

1546.5

1546.8

1547.1

wavelength in nm
Fig. 5. Reected spectra of FBG for different concentrations of Cd solutions.

using Optical Spectrum Analyzer. The grating is formed in a

very small time interval of 20 s. The advantage of GeB co-doped
photosensitive ber is that the exposure time for grating formation
is remarkably reduced. The reected spectrum of FBG is shown
in Fig. 2, having a peak reectance of 75%, a centered wavelength
1546.96 nm (Bragg resonance wavelength), a band width (FWHM)
of 0.2 nm and peak power 30.16 W. The cladding of the grating
region was etched in 40% HF solution for about 60 min.
2.2. Fabrication of LPG
Fabrication of long period grating was made point by point
technique. The schematic diagram of fabrication of LPG is as in
Fig. 1b. The experiment conguration consisted of a computer controlled translational stage with optical beam scanner. A white light
source and spectrum analyzer [Agilent-86146B in built white light
source] in the range of 6001700 nm were used to monitor the
transmission spectrum as the grating was written. The singlemode
GeB photosensitive ber (Newport F-SBG-15, with step index prole of NA 0.120.14, cladding diameter 125 1 m, and operating
wavelength 1550 nm) is chosen to form long period grating. The
gratings of period 410 m have been made along the ber of length
1.4 cm using CO2 continuous laser having 10.6 m of output power
20 W. For grating of length of 1.4 cm totally 35 shots of laser
beam have given during grating formation. Fig. 3 shows the grating

Fig. 7. Bragg wavelength vs concentration.

transmission spectrum. Diffraction of core guided light into

cladding modes produces characteristic transmission minima or
dip. This writing method using focused CO2 laser is highly controllable and is applicable to ordinary telecommunication ber.
3. Experimental setup and sensor test
A schematic diagram of the proposed FBG and LPG based concentration sensor the experimental set up is shown in Fig. 4a
and b respectively. Different solutions of cadmium in the range
0.01 ppm0.04 ppm are prepared by dissolving CdSO4 (Aldrich)
in distilled water (Aldrich). 4 mL solutions are taken into different test tubes. To each Cd concentration solution, reagents
N,N-dimethylaformamide and thiourea are added in appropriate
volumes and let it stand for 5 min to complete reaction to take place.
Now, FBG/LPG is completely immersed in these solutions taken in
special glass cells designed in the laboratory. In each case reected
wavelength (B ) is recorded for FBG shown in Fig. 5 and transmission spectrum of LPG shows in Fig. 6. At the end of each sample
measurement, the grating was cleaned with acetone repeatedly,
followed by drying properly, so that the original spectrum of FBG
and LPG was obtained. The graph of wavelength versus solution
concentration is plotted for FBG and LPG Figs. 7 and 8 respectively
used to determine the concentration of Cd in drinking water.
4. Results and discussion
The spectral response of change in wavelength with concentration is shown in Figs. 7 and 8. In the experiment, the reected Bragg
wavelength and LPG resonance wavelengths were monitored while
samples with different concentrations of cadmium were in contact
with the grating. From the reected spectrum in FBG and transmission spectrum in LPG, it is found that with increasing concentrations
of cadmium, the sensitive attenuation bands shows blue shift with
respect air surrounding medium. The FBG and LPG exhibited a total
blue shift of approximately 0.07 nm and 10 nm respectively, when

Table 1
Slope, intercept and correlation coefcient from Figs. 7 and 8.

Fig. 6. Transmitted LPG spectra for different concentrations.

Parameter

Fig. 5

Fig. 6

Slope
Intercept
Correlation coefcient

1.57617
1546.15 nm
0.91376

0.24
1.3312 m
0.93918

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U.S. Raikar et al. / Sensors and Actuators B 161 (2012) 818823

Table 2
Concentration of Cd in test sample measured using different techniques.
Chemical species

FBG sensor (ppm)

LPG sensor (ppm)

Atomic absorption spectrometer (ppm)

Inductive coupled plasma (ppm)

WHO standard (ppm)

Cadmium

0.001

0.002

0a

<0.03b

0.005

a
b

Measurements were made in USIC (University Scientic Instrument Center, Karnatak University, Dharwad, India).
Measurements were made at MetChem Laboratories, Bangalore (India Pvt. Ltd.).

Experimental Data
Linear Fit

wavelength in micrometer

1.332

Acknowledgement
Authors are thankful to DAE-BRNS for providing grants (No.
2006/34/22-BRNS/2801).

1.330

References

1.328

1.326

1.324

1.322
0.00

0.01

0.02

0.03

0.04

Concentration in ppm
Fig. 8. LPG resonance dips wavelength vs concentration.

Table 3
Detection limits for Cd.
AAS (ng/mL)

ICP (ng/mL)

1 (0.001 ppm)

2 (0.002 ppm)

the surrounding medium was gradually changed from water to

0.04 ppm of cadmium.
We can determine the concentration of Cd in these samples using graph of reected and transmitted wavelength versus
concentration by interpolating the graph Figs. 7 and 8. From
Figs. 7 and 8 the shift in wavelength is linear with correlation factors of 0.91376 and 0.93918. The interpolated graph data are
given in Table 1. The concentration of Cd in collected water sample is found to be 0.001 ppm with FBG and 0.002 ppm with LPG. A
comparative study has been done using atomic absorption spectrometer (AAS) and inductively coupled plasma (ICP) spectrometer
and the results are found to be in agreement. The results are given
in Table 2. Table 3 provides information on detection limits for Cd
element by ame atomic absorption and ICP atomic emission.
5. Conclusions
We have fabricated and designed a highly sensitive grating sensor using BGe co-doped ber to detect the traces of Cd in drinking
water. Fiber Bragg grating and long period grating sensors can be
used for measuring the cadmium in water with good sensitivity in
the lower concentration range. From the results, the sensitivity of
chemical sensor by LPG is high compared with FBG. The advantage
of this type of sensor is its simplicity in construction, high sensitivity in lower concentrations and ease of use. We believe a better
sensitivity of our designed sensor can be achieved by optimization
of some key parameters such as grating length, RI prole of the
core, optical design and modifying the grating surface with gold
nanoparticles.

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Biographies
U.S. Raikar is a Professor, Department of Physics, Karnatak University, Dharwad,
Karnataka state, India. He obtained post graduation from Karnatak University Dharwad, M.Phil (1990) and Ph.D. (1994) degree from Shivaji University, Kolhapur. His
main areas of research interest are Spectroscopy and Fiber Optics. He is a member

U.S. Raikar et al. / Sensors and Actuators B 161 (2012) 818823

for IEEE Photonics Society and life member for many scientic organizations across
the world. He is reviewer for many International Journals.
A.S. Lalasangi obtained M.Sc. in 1999 and M.Phil in 2005 degree from Karnatak
University, Dharwad, Karnataka state, India. Now pursuing Ph.D. under the guidance
of Prof. U.S. Raikar.
Jyoti F. Akki obtained her post graduate degree from Karnatak University, Dharwad, India in year 2006. Now working for doctoral degree at Karnatak University,
Dharwad, under the guidance of Dr. U.S. Raikar.
Prasad Raikar obtained graduation from National Institute of Technology, Mysore
in the year 2009. M.Tech. degree from KLEs college of Engineering and Technology,
Belgaum. His elds of interest are Machine Design and Sensors.
K.G. Manohar is Scientic Ofcer H, at Laser and Plasma Technology Division of
Bhabha Atomic Research Center, Mumbai, India. Also he is Professor at Homi Bhabha
National Institute, Mumbai. He obtained his Ph.D. from University of Mumbai in 1992
and carried out his Post-Doctoral work at University of Kaiserslautern, Germany
(19931994). His research interests are Laser Spectroscopy, Laser Cooling and Trapping and Laser & Optics Technology.
T. Srinivas is Associate Professor in Department of Electrical Communication Engineering Department, Indian Institute of Science, Bengaluru, India. His main area of

823

research interest is Optical Communication more specically Photonics Integrated

Circuits. And his work is focused on PBG, MOEM Sensors, micro ring resonator,
Fiber Bragg Grating (FBG) Arrays, Wavelength Division Multiplexing (WDM) network Architecture. Srinivas obtained Ph.D. from Indian Institute of Science (IISc) in
1993 and has been Post Doctoral Research fellow at Toyohashi University of Technology, Japan during 19921996. He is member of IEEE Photonics and IEEE Com Soc
Society.
N.M. Badiger is a Professor, Department of Physics, Karnatak University, Dharwad,
Karnataka state, India. He obtained post graduation and Ph.D. in 1988 from Karnatak University Dharwad. His main area of research interest is Nuclear Reaction
and Radiation. He is awardee of DAE fellowship and 3rd world academy of science
Italy.
P. Radhakrishan is a Professor and Director of International School of Photonics and also the Director of the Center of Excellence in Lasers and Optoelectronic
Sciences, Cochin University of Science and Technology, Kochi, Kerala, INDIA. His
research interests include laser technology, laser spectroscopy, and ber optic sensors. Ph.D. degree received from Cochin University of Science and Technology in
1986. He has been a lecturer at the Cochin College from 1979 to 1988. He is the
present President of the Photonics Society of India and life member of Indian
Laser Association, Indian Association of Physics Teachers and the Indian Physics
Association.