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Optics and Lasers in Engineering 60 (2014) 3843

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Optics and Lasers in Engineering


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

Fiber sensor based on Lophine sensitive layer for nitrate detection


in drinking water
J.L. Camas-Anzueto a,n, A.E. Aguilar-Castillejos a, J.H. Castan-Gonzlez b, M.C. Lujpn-
Hidalgo b, H.R. Hernndez de Len a, R. Mota Grajales a
a
Departamento de Posgrado e Investigacin, Maestra en Ciencias en Ingeniera Mecatrnica, ITTG, Tuxtla Gutirrez, Chiapas, Mxico
b
Departamento de Posgrado e Investigacin, Maestra en Ciencias en Ingeniera Bioqumica, ITTG, Tuxtla Gutirrez, Chiapas, Mxico

art ic l e i nf o a b s t r a c t

Article history: A new characterization of Lophine as a sensitive layer to measure Nitrate in drinking water is presented
Received 26 March 2013 in this paper. The characterization was performed with a standard slide and a standard multimode ber
Received in revised form coated with a Lophine sensitive layer (2,4,5-Triphenylimidazol (C21H16N2)). Spectral characterization has
4 April 2014
been conducted in the wavelength range from 300 to 1100 nm. We have demonstrated that Lophine can
Accepted 6 April 2014
Available online 6 May 2014
be used as a ber sensor for the detection of Nitrate in drinking water. The sensing properties of the ber
sensor were analyzed at room temperature. Successful results were achieved when sensing Nitrate in the
Keywords: range between 1 mg/l and 70 mg/l. The response time was 20 ms and the recovery time was 40 ms.
Optical ber sensor & 2014 Elsevier Ltd. All rights reserved.
Lophine layer
Nitrate sensor
Environmental sensor

1. Introduction by Lalasangi et al. [11]. They showed that etched ber Bragg
grating (FBG) can work as a sensor to measure Nitrate concentra-
Currently, both the monitoring and the chemical analysis of tion by means of analyzing the Bragg wavelength shift as a
drinking water are of paramount importance to humanity in order response of variations in the concentration value. The FBG pro-
to prevent human diseases, although this requires careful planning posed is manufactured by the phase mask technique on a single
and fast and reliable methods to achieve useful results. Nitrate is mode GeB co-doped photosensitive ber. Determination of
one of the most important compounds that are measured to Nitrate based on the reduction of Nitrate in the presence of
determine water quality, and it cannot be detected unless chemical Zn/NaCl was reported by Narayana1 and Kenchaiah [12]. Here,
tests are used. This compound is an ionized form of Nitrogen sulfanilic acid was diazotized in an acidic medium and coupled
(NO3  ), and an important nutrient for all photosynthetic organ- with methylanthranilate to produce a colored dye with a max-
isms. If peopleinfants in particulardrink water with a high imum absorption at 493 nm. Detection of Nitrate and Nitrite by
concentration level of Nitrate, they can contract a disease called means of modication of the uorescence emission of suitable
methemoglobinemia. However, there are some chemical methods dyes can be integrated to a ber optical sensor [13]. Nitrites in the
for identifying Nitrate concentrations in drinking water. The task range between 1 and 1000 bbp were detected with a simple and
of performing Nitrate measurements in water is a complicated sensitive optical ber sensor, based on the evanescent wave
process that requires considering a number of factors in order to absorption [14]. A ber optical interrogator based on the colori-
achieve correct results. Therefore, optical ber sensors have metric technique for in-situ Nitrate detection in groundwater was
become an important solution for detecting chemicals in water proposed by Aulakh and Kaler [15]. The accuracy of color mea-
[14]. Methods to identify Nitrate concentrations in water have surement using this technique depends on the proper selection of
been reported in the literature, and some of these are electro- the complementary lter. Bedinkov et al. [16] reported a novel
chemical, ion chromatography, spectrophotometric, and UV reso- design for a potentiometric microsensor for a Nitrate ion based on
nance Raman spectroscopic [510]. A recent work on an optical doped polypyrrole lms. It is worth to mention that the maximum
ber sensor to detect Nitrate concentrations in water was reported Nitrate concentration limit in drinking waters recommended by
the World Health Organization is 50 mg/l.
In this paper, we present a new characterization of Lophine
n
Corresponding author. (2,4,5-Triphenylimidazol (C21H16N2)) as a sensitive layer for mea-
E-mail address: jcamas@ittg.edu.mx (J.L. Camas-Anzueto). suring and detecting Nitrate in drinking water. The sensitive layer

http://dx.doi.org/10.1016/j.optlaseng.2014.04.001
0143-8166/& 2014 Elsevier Ltd. All rights reserved.
J.L. Camas-Anzueto et al. / Optics and Lasers in Engineering 60 (2014) 3843 39

consists of Lophine Immobilized in a PolyVinylChloride (LIPVC)


polymeric matrix. Previous characterization of LIPVC was per-
formed on a standard slide to research its behavior with different
Nitrate concentrations in drinking water, and then the LIPVC was
deposited on an optical ber where the coating was removed from
a 1 cm section. The best result of the LIPVC was obtained when
this contained 20 mg of Lophine, which is presented in the
following sections. We demonstrate that without removing the
cladding of the optical ber, the ber sensor showed excellent
sensitivity and was able to measure Nitrate concentrations
between 1 mg/l and 70 mg/l in drinking water. Measurements of
both the response time and recovery time were in the order of
20 ms and 40 ms respectively, which show they are faster than
other known measuring methods. The proposed ber sensor is
suitable for being used for measuring Nitrate in drinking water.

2. Sensitive layer preparation

Lophine is an organic material and the most representative


chemiluminescent compound, and known as Imidazoles [17,18].
To use Lophine as a sensitive layer element, it was necessary to
immobilize it in plasticized PVC, which interacts efciently with Fig. 1. (a) Lophine sensitive layer deposited on slide and (b) Lophine sensitive layer
the aqueous environment, and at the same time works as a deposited on optical ber.
waterproof material. The proposed mixture of PVC can be found
in the Ref. [19], and it is used to immobilize the Lophine to obtain Nitrate Concentration Photodetector
LIPVC. This mixture for the preparation of the LIPVC was LPS-830-FC 1 mg/l to 70 mg/l S120C
obtained from a batch of 80 mg of poly(vinyl chloride), 160 l of Laser diode FC-Connector FC-Connector
driver
tributylphosphate and 20 mg of Lophine dissolved in 2 ml of
freshly distilled TetraHydrofuran (THF). The LIPVC was prepared
PM-320E
with different concentrations of Lophine and was deposited on Powermeter
Pure Water
slides and optical ber to characterize and obtain the best results Graded Index Fiber
in the detection of Nitrates. It was necessary to adjust the Lophine Petri container
dimension of the slide and to introduce it into a standard spectro-
Fig. 2. Optical ber sensor in transmission conguration.
photometer plastic cell to achieve the corresponding characteriza-
tion in the spectrophotometer. To deposit the sensitive layer on
the optical ber, the coating was removed in a 1 cm section, and conguration, and the LIPVC deposited on a multimode optical
the exposed cladding was sterilized. Isopropyl Alcohol Level was ber. It consists of a 1-m length multimode optical ber GIF-50,
used for cleaning the optical ber in special cleaning cloths and with a typical wavelength from 750 nm to 1450 nm. The ber
immediately the LIPVC was introduced in the sterile area for sensor has standard FC connectors at both ends. The multimode
periods from 2 to 3 min in direct contact. When Lophine is optical ber was coated around the ber in a 1 cm section with
deposited, its distribution presents micro-ramications of crystals LIPVC. A LPS-830-FC Fiber Pigtailed Laser Diode was used as the
[20,21]. The manufacturing process of the ber sensor has some optical source. This laser diode has a central wavelength of
common points particularly after the curing process where the 830 nm, and a maximum power of 10 mW. A S122C photodetector
sensitive layer is dipped into the mixture. Thermal curing is was used for optical detection. This photodetector offers a fast
necessary in order to harden the LIPVC and x it onto the ber. response for a precise low-power measurement from 50 nW to
The curing process is also essential to evaporate all the organic 40 mW, and a wavelength from 200 nm to 1100 nm with 1 nW of
solvents that are present in the solution. Finally, traces of THF were resolution. The PM320E Benchtop Optical Power and Energy Meter
removed, leaving the LIPVC only at the cladding of the optical equipment is set up to measure the optical power of laser diodes
ber. Fig. 1 shows schematics of both LIPVC deposited on the or other monochromatic or near monochromatic light sources and
slide and on the multimode optical ber (GIF125-100, GIF50 and the energy of pulsed light sources. The drinking water sample was
AFS105-125Y). However, the best results that are presented in the pure water from Aldrich Sigma Chemical, with a molecular weight
next section of this paper were achieved with the GIF-50 ber. of 18.02 g/mol, and is used only for laboratory research purposes.
Characterization is performed at controlled room temperature,
because Lophine has thermochromic properties. [22,23].
4. Results and discussion

3. Experimental set up 4.1. Characterization of the LIPVC on a standard slide

The characterization of the LIPVC deposited on the slide was At this stage, sensitive layers of LIPVC with concentrations of
performed with a standard spectrophotometer plastic cell. The 10 mg, 20 mg and 30 mg of Lophine were prepared. Results
absorbance of the LIPVC was measured with a spectrophotometer indicate that the LIPVC layer containing 20 mg of Lophine is the
UV/vis (Beckman Coulter DU730). The characterization of the best for measuring Nitrate in water. The treatment samples were
absorbance was done to know the optimal concentration of obtained by preparing pure water samples with different concen-
Lophine to measure Nitrate in drinking water. Fig. 2 shows the trations of Nitrate, so it was prepared at 100 mg/l concentration,
experimental characterization of the ber sensor in transmission by using the Ofcial Mexican Standard methodology. To ensure
40 J.L. Camas-Anzueto et al. / Optics and Lasers in Engineering 60 (2014) 3843

that Nitrate samples were correct, a standard curve by plotting absorbance increases and an absorption peak at 319 nm appears,
absorbance at 220 nm against Nitrate concentrations was which is produced by Lophine absorption. This graph corroborates
obtained. Fig. 3 shows the curve with a linear increase with Adj. that Lophine is sensing Nitrate in water. Fig. 5a shows the spectral
R-Square of 0.98844. Then, we proceeded to measure the absor- absorbance from 300 to 1100 nm for different concentrations of
bance for each one in the wavelength range from 300 to 1100 nm Nitrate for 1 to 70 mg/l. As can be observed, the absorbance
without the LIPVC. These measurements are shown in Fig. 4. It increases according to the increase of Nitrate concentration in
can be observed that absorbencies of the treatment from 1 to water. Lophine absorption appears in all measurements. Fig. 5b
70 mg/l of Nitrate are around zero. However, when the LIPVC is shows a zoom of Fig. 5a in the wavelength range from 400 to
introduced into the treatment with 10 mg/l of Nitrate, the 1100 nm. This graph clearly shows the increase in absorbance
according to the Nitrate increase, which allows for the measure-
ment of Nitrate in any of these wavelengths. Fig. 6 shows the
Standard curve
2.5 =220 nm absorbance of the LIPVC as a function of different concentrations
of Nitrate. The values are taken from Fig. 5 at wavelengths of 550,
630 and 830 nm, and corroborate the hyperchromic effect. A linear
2.0
increase can be observed from 1 to 50 mg/l with an Adj. R-Square
Absorbance (AU)

Adj. R-Square of 0.95 and from 50 to 70 mg/l of 0.96. This graph corroborates
0.98844
1.5 that measurements can be performed in infrared, where the
optical bers transmission is reliable. Another important result
that has been found in the characterization of the LIPVC is a
1.0 bathochromic shift due to solvent effect; this is related to the
increase of Nitrate concentration. Fig. 7 shows a bathochromic
shift from 318 nm to 334 nm, which corresponds to 1 and 60 mg/l
0.5
respectively. From 1 to 40 mg/l the bathochromic shift was linear
with a wavelength shift from 318 to 332 nm with 0.35679 nm/
0 10 20 30 40 50 60 70 80
(mg/l), and from 40 to 60 mg/l it was from 332 to 334 nm with
Nitrate concentration (mg/l)
0.1 nm/(mg/l). In Figs. 57, an increasing absorbance behavior,
Fig. 3. Standard Nitrate curve. known as hyperchromic effect, can be observed. This effect is due
to the absorption characteristics of organic molecules in the
ultraviolet region, which depends on the electronic transitions
that can occur and on the effect of the atomic environment on the
Absorption peak
of Lophine =319 nm
transitions. For validation purposes, the pH measurement was
0.8
carried out in every sample of drinking water with different
0.7 concentrations of Nitrate. With this characterization, the LIPVC
0.6 i) Absorbance Measurement ensures the Nitrate measurement, since the pH values were from
Absorbance (AU)

without LI-PVC 7.1 to 7.5. A buffer solution to maintain a constant pH was used.
0.5 (1, 10, 20, 30, 40, 50, 60, 70 The absorbance change of the LIPVC is not signicant at 830 nm,
0.4 mg/l of Nitrate) and therefore ensures the measurement of Nitrate.
ii) Absorbance measurement
0.3 with LI-PVC
(10 mg/l of Nitrate) 4.2. Characterization of the ber sensor
0.2

0.1 Having thoroughly characterized LIPVC to different Nitrate con-


0.0 0.0 centrations, we proceeded to deposit it in three different types of
multimode bers. Therefore the best result was obtained with the
-0.1 multimode ber optic GIF-50. At this stage, three samples of LIPVC
300 400 500 600 700 800 900 1000 1100 1200
were prepared with different concentrations of Lophine, 10 mg, 20 mg
Wavelength (nm)
and 30 mg. Fig. 8a shows the output power of the ber sensor as a
Fig. 4. (i) Absorbance at different Nitrate concentrations without LIPVC and function of Nitrate concentrations in drinking water. As can observed,
(ii) absorbance of 10 mg/l of Nitrate with LIPVC. the best result was obtained when the LIPVC contained 20 mg of

Absorption peak
of Lophine Absorbance measurement
1.4
1.3 Absorbance measuremente 20 mg of Lophine
0.25 70
1.2 20 mg of Lophine
Nitrate concentration
1.1 Nittrate concentration 40 60 (mg/l)
Absorbance (AU)

0.20
Absorbacne (AU)

1.0 mg/l
0.9 1 30
0.8 10
0.15
0.7 20
30 20 50
0.6
40 0.10
0.5 50
0.4 10
60
0.3 70) 0.05
0.2
0.1 1
0.00
0.0
300 400 500 600 700 800 900 1000 1100 400 500 600 700 800 900 1000 1100
Wavelength (nm) Wavelength (nm)

Fig. 5. (a) Spectral absorbance of the LIPVC as a function of the Nitrate concentration and (b) zoom from 400 to 1100 nm to visualize the absorbance increase.
J.L. Camas-Anzueto et al. / Optics and Lasers in Engineering 60 (2014) 3843 41

Lophine. This is because 10 mg of Lophine surrounding the optical from 20 to 30 mg/l it decreased 49 mW. The output power had a
ber is not enough to interact with the propagating evanescent eld, minimum rate of reduction in the range of Nitrate concentration from
while with 30 mg of Lophine, overlapped crystals are formed, and 10 to 30 mg/l. In addition, from 30 up to 70 mg/l, the output power
some of these crystals do not interact with the evanescent eld and was linear and decreased from 4.039 mW to 2.6 mW. The power
therefore there is no contribution to the sensitivity of the sensor. In difference (P) between the output power for 1 mg/l and 70 mg/l was
addition, when the LIPVC contained 20 mg, the initial output power P1.97 mW. When the LIPVC layer contained 30 mg of Lophine,
was 4.6312 mW, and it was when the drinking water contained 1 mg/l the output power did not have a signicant change. It can be observed
of Nitrate. The sensor exposure time was 300 s in each measurement that from 1 mg/l to 50 mg/l the output power had a variation of
to verify the output power stability. It can be observed that the output 55 mW. However, with 60 mg/l, a drastic decrease from 4.3 mW to
power decreases when the Nitrate concentration increases. Although 3.6 mW was observed. Fig. 8b shows a zoom of the graph with 10 mg
the decrease of the output power is not linear, its behavior suggests of Lophine. Here, the behavior of the output power is not linear and
that it can be used as a ber sensor to measure Nitrate in drinking presents a P 0.16 mW. Therefore, atypical behavior was observed
water. From 10 to 20 mg/l the output power decreased 24 mW, and

Measurement of Nitrate Concentration in Real time


Absorbance measurement Pure
0.30 20 mg of Lophine Water GIF-50 with 20 mg
0.35
+ 1 mg of Lophine
550 nm = 830 nm

Output Power (A. U.)


0.25
630 nm
+ 10 mg
0.30
Absorbance (AU)

850 nm + 20 mg
0.20
+ 30 mg -3 ml
0.25
+ 40 mg -3 ml
0.15
+ 50 mg -3 ml
0.20
0.10 + 60 mg -3 ml
-3 ml
0.15
0.05
-3 ml

0.10
+ 70 mg
0.00
0 10 20 30 40 50 60 70 80 0 200 400 600 800 1000 1200
Nitrate Concentration (mg/l) Time (s)

Fig. 6. Absorbance at three xed wavelengths as a function of Nitrate concentration. Fig. 9. Output power in the sensor at different concentrations of Nitrate in water.

Bathochromic
1.5 318 shift 334
Hyperchromic 336
1.4
70 effect 334
1.3
1.2 30 332
Abosorbance (AU)

1.1 Bathocromic
Wavelength (nm)

1.0 330 shift


0.9 20
328
0.8
0.7 10 326
0.6
324
0.5 Adj. R-Square
0.4 322 0.99464
0.3 1
320
0.2
0.1 318
0.0
316
300 310 320 330 340 350 360 0 10 20 30 40 50 60
Wavelength (nm) Nitrate concentration (mg/l)

Fig. 7. Absorption peak of Lophine with bathochromic shift.

Output Power Measurement


5.0 at 830 nm wavelength
Multimode Fiber 4.64
Output power at 830 nm wavelength
GIF-50 4.62 Fiber sensor :GIF-50 with 10 mg
4.5
4.60 of Lophine
O utput P ow er (m W )
Output Power (mW)

4.58
4.0
4.56
4.54
3.5
4.52
10 mg
20 mg 4.50
3.0
30 mg
4.48

2.5 4.46
4.44
0 10 20 30 40 50 60 70 80 10 20 30 40 50 60 70

Nitrate concentration (mg/l) Nitrate Concentration (mg/l)

Fig. 8. (a) Output power in the ber sensor with 10 mg, 20 mg, and 30 mg of Lophine and (b) zoom of the graph with 10 mg of Lophine.
42 J.L. Camas-Anzueto et al. / Optics and Lasers in Engineering 60 (2014) 3843

10.72 10 ms/div
Pure Water
10.70
Pure Water Response Pure Water
10.70 Time

Output Power (A.U.)

O u tp u t P o w e r (A . U .)
Response time
10.68
10.68 20 ms
Recovery
Time 10.66
10.66

10.64
10.64 Nitrate
Concentration Nitrate Concentration
70 mg/l
10.62 10.62 70 mg/l

10.60 10.60
75 175 225 275 325 5 45 85 125 165
Time (ms) Time (ms)

Fig. 10. (a) Response and recovery time curve of the sensor and (b) zoom of the response time.

between 1 and 10 mg/l, 30 and 40 mg/l, and 50 and 60 mg/l of Nitrate used as a sensitive layer on a ber sensor for the detection of
concentration. The P for 1 mg/l and 70 mg/l was 159 mW. Therefore Nitrate in drinking water. The best results were obtained when the
the atypical behavior of the output power suggests that 10 mg of LIPVC was deposited in a multimode ber GIF-50. Therefore, the
Lophine on the LIPVC is not reliable to be used as a sensitive layer of ber sensor was successfully used for Nitrate detection in water
the ber sensor. Finally, the results presented so far corroborate that for the rst time as far as the author's knowledge is concerned.
the best result is obtained when the LIPVC contains 20 mg of Measuring Nitrate concentrations in water from 1 mg/l to 70 mg/l
Lophine. was sufcient for achieving successful results. It was also found
Fig. 9 shows the measurement of Nitrate in-situ with contin- that the best response time of the ber optic sensor was 20 ms and
uous addition of Nitrate in drinking water. Pure water as drinking its recovery time was 40 ms, and this is a very important para-
water was the initial sample, and after that, volumes of 3 ml of meter to use as a ber sensor in-situ.
water with different concentrations of Nitrate were added. The
rst arrow indicates how the Nitrate concentrations in water were
added. It can be observed that the output power began to decrease Acknowledgments
from 0.35 mW to 0.12 mW when the sample contained 70 mg/l of
Nitrate. After that, volumes of 3 ml of water with Nitrate were This work was supported by FOMIX-CHIAPAS CHIS-2008-08-
extracted. It can be observed that the output power increased 105817 Project.
when the water was extracted. It is necessary to mention that
Nitrate concentrations for each 3 ml sample of water extracted References
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2011;18(1):1448. Hector Ricardo Hernandez De Leon is a researcher at Department of Electrical &
Electronics Engineering of Institute of Technology Tuxtla Gutierrez, Chiapas, Mexico
(ITTG). He is Electronics Engineer by the National Polytechnic Institute of Mexico
City (IPN). He obtained an MSc and PhD in Automated Systems at the National
Institute of Applied Sciences INSA-Toulouse-France. His research interests are
Jorge Luis Camas Anzueto received the PhD degree from Instituto Nacional de intelligent control and diagnosis of drinking water plants.
Astrofsica ptica y Elctrnica (INAOE), Puebla. Mxico in 2004. He is currently a
researcher in Maestra en Ciencias en Ingeniera Mecatrnica (MCIM) of the
Instituto Tecnolgico de Tuxtla Gutirrez, Chiapas, Mxico. His research interests
include optical ber, ber sensors, and optoelectronics.
Rafael Mota Grajales is a researcher from Instituto Tecnolgico de Tuxtla Gutirrez,
Chiapas. His master degree was obtained from Instituto Tecnolgico de Laguna,
Coahuila. Actually, he is studying the PhD from Universit Claude Bernard Lyon,
France. His research interests are instrumentation and manufacturing process.
Aldo Esteban Aguilar Castillejos received his electronic engineering degree from
the Instituto Tecnolgico de Tuxtla Gutirrez (ITTG), in 2009. He received the MS