7936
18, SEPTEMBER 15, 2019
Paper-Sensors for Point-of-Care Monitoring of
Drinking Water Quality
Nilanjan Mandal, Shirsendu Mitra, and Dipankar Bandyopadhyay
Abstract— Contamination of water bodies due to the disposal
of natural and anthropogenic pollutants is one of the major
global concerns in the recent times. Regular on-spot monitoring
of water quality has become mandatory wherein diverse classes of
materials such as organic, inorganic, heavy metals, or biological
wastes are detected employing standard protocols. However, most
of the existing laboratory techniques are either costly and/or
time consuming owing to the process involving the expert driven
sophisticated analysis techniques. Herein, we report the develop-
ment of three paper based colorimetric sensors for the on-spot
quantitative detection of the levels of fluoride (F− ), lead (Pb2+),
and pH in drinking water. The variations in the color-intensities
of the paper sensors with the variation in the concentration
of fluoride (F− ), lead (Pb2+), and pH were converted into
electronic signals to enable the development of a point-of-care-
testing (POCT) device. For this purpose, initially, the sensors were
characterized and calibrated with known concentrations of con-
taminates before successful validations with real samples. There-
after, the sensors were illuminated with a light emitting diode
from one side while the transmitted rays passing through the
sensor was captured by a light dependent resistor (LDR) from the
other side. The variation in the color intensity of the paper-sensor
with the contaminant loading was found linearly varying with
the resistance of the LDR. The sensor was then translated into
a specific, stable and user friendly POCT device, which enabled
inexpensive spot detection of pollutants in drinking water.
Index Terms— Optical sensors, water pollution, optical device
fabrication, electric resistance, light emitting diode (LED),
photodetectors.
I. I NTRODUCTION
R EAL-TIME measurements of diverse hazardous envi-
ronmental pollutants have become one of the major
research focus in the recent years owing to their significance
in the mitigation of many long-term health hazards [1], [2].
In this regard, of late, the portable, low-cost, and user-friendly
point-of-care-testing (POCT) devices are envisioned to play a
pivotal role [3]–[5]. Among the other important environmental
markers, POC detections of the various pollutants in various
water sources [6]–[8] have perhaps taken the center stage
Manuscript received March 2, 2019; revised May 11, 2019; accepted
May 15, 2019. Date of publication May 27, 2019; date of current version
August 15, 2019. This work was supported by the Ministry of Electronics
and Information Technology (MeitY) grant no. 5(9)/2012-NANO, Government
of India. The associate editor coordinating the review of this paper and
approving it for publication was Dr. Gymama Slaughter. (Corresponding
author: Dipankar Bandyopadhyay.)
The authors are with the Centre for Nanotechnology, Indian Institute
of Technology Guwahati, Guwahati 781039, India (e-mail: nilanjan.
mandal@gmail.com; shirsenduofficial@gmail.com; dipban@iitg.ac.in).
This paper has supplementary downloadable multimedia material available
at http://ieeexplore.ieee.org provided by the authors. The Supplementary
Material contains a word document named as “Paper-Sensors for Point-of-
Care Monitoring of Drinking Water Quality_ESI,” that contains the supporting
information for the main manuscript named “Paper-Sensors for Point-of-Care
Monitoring of Drinking Water Quality.” This material is 1.17 MB in size.
Digital Object Identifier 10.1109/JSEN.2019.2919269
1558-1748 © 2019 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.
IEEE SENSORS JOURNAL, VOL. 19, NO.
of attention owing to their far reaching implications related
to the global health. For example, soluble or insoluble inor-
ganic [9] and organic contaminants [9], heavy metal ions [9],
biological (BOD) [10], [11] and chemical (COD) [11], [12]
oxygen demands, and pathogens [13] are now expected to
be detected on-spot with the help of commercially available
POCT devices [14]. Although, in this direction a substantial
progress has been made in the past few decades [15], a number
of issues still remain unaddressed.
For example, there is an immediate necessity of a POCT
device for the detection of fluoride (F− ) and/or lead (Pb2+ )
contaminations in the drinking water. As per the World Health
Organization (WHO) guidelines the maximum permissible
limits for F− is 1.5 ppm in the drinking water while for
Pb2+ the same is 0.05 ppm [9]. Higher levels of F− and/or
Pb2+ in water can cause fluorosis or lead poisoning [16].
Further, presence of excess F− and Pb2+ in drinking water
can also cause various other chronic ailments in associated
with skin, teeth and bone s [17], brain [18], [19], lungs and
heart [20], [21]. On the other hand, the WHO guidelines also
suggest that the pH of the water should be in range of 6.0 to
8.0 [9]. The pH of drinking water deviating from this range
can affect the mucin layer in the various parts of the digestive
system which in turn can harm the immune system of a
human body triggering many critical ailments [9]. Importantly,
many of the previous studies suggest that the lowering of pH
than the normal range in most of the commercially available
bottled mineral waters is one of the key reasons of old-age
osteoporosis across the globe [22].
Certainly, there is an immediate need of a POCT device,
which can immediately provide information about the F− ,
Pb2+ and pH levels in the drinking water. It may be noted
here that the conventional methods of determining these
constituents in water involve either optical [23], [24] or
electrochemical [25], [26] methodologies. Yet, most of these
methodologies are either costly and/or consume time and
require expertise for testing and analyses [27]. In this regard,
of late, the advent of micro or nanoscale technologies have
provided a glimmer of hope in the design and development
of economic, specific, stable, portable, fast, and user friendly
POCT devices to detect these pollutants. For example, the use
of diverse nanomaterials [28], [29], nanostructures [13] and
carbon allotropes [30] have led to quantitative detection of
dissolved F− , Pb2+ and pH of water. However, these sensors
are yet to be translated into POCT applications owing to their
higher cost of fabrication, requirement of expertise handing,
and time required for detection.
In view of this background, in the present study, we have
developed paper based colorimetric sensors to quantitatively
MANDAL et al.: PAPER-SENSORS FOR POINT-OF-CARE MONITORING OF DRINKING WATER QUALITY
Fig. 1. Images (a)-(c) schematically illustrate the steps of colorimetric sensor fabrication for F− , Pb2+ and pH, respectively, and their color change. Image
(d) shows the integration of LED and LDR with the sensor and subsequent measurement of the change in resistance using Arduino based POCT device for
the display of water quality.
detect F− , Pb2+ and pH levels in the drinking water. The use
of reagent coated paper sensors to develop the colorimetric
sensors has been inspired by a number of recent seminal
contributions [31], [32]. The use of paper as the substrate
enabled the making of a sensor, which is less complicated
to fabricate, of low cost, and easily disposable. The working
principle of the colorimetric sensor depends on the color
change due to the following specific reactions between, (a)
F− and iron (III) thiocyanate for fluoride sensing, (b) Pb2+
and 1,5-Diphenylthiocarbazone (dithizone) for lead sensing
and (c) protonated bromothymol blue (BTB) for pH sensing,
on the paper surface. While the reagents were coated on the
paper surface, the network of microchannels in paper enabled
immediate mixing with the analyte through capillary action,
leading to a fast chemical reaction and colorimetric response.
The variations in the color on the surface of the paper sensor
were detected with the help of a light emitting diode (LED)
and a light dependent resistor (LDR). The paper sensors were
illuminated with the LED from one side while the light trans-
mitting through the sensors were captured by the LDR [32].
The resistance of the LDR was found to vary monotonically
with the change in the concentration of dissolved F− , Pb2+ and
pH of the water sample. The sensors were found to be specific
and detect the unknown levels of F− , Pb2+ and pH of real
water samples when compared and contrasted with standard
methodologies. The sensors, LED, and LDR were integrated
in an Arduino platform to translate into a portable and user-
friendly POCT device for on-site, low-cost, and instantaneous
monitoring of water quality.
II. M ATERIALS A ND M ETHODS
A. Materials
Ammonium thiocyanate, Iron (iii) Chloride, Bromothy-
mol blue, 1,5-Diphenylthiocarbazone (Dithizone), Sodium
7937
Fluoride, Lead (ii) Chloride, Potassium sodium tartrate,
Dimethyl formamide (DMF), Carbon tetra chloride (CCl4),
Sodium hydroxide, Hydrochloric acid, 125 mm filter paper
(grade 1), were obtained from Merck (India). The chemicals
above were of analytical grade and used without further
purification. The Milli-Q grade water was used in all the exper-
iments unless stated otherwise. The Arduino Uno R3 devel-
opment board, Liquid crystal display (LCD), resistors were
procured from Rhydo Labz (India). The samples solutions of
known concentrations of F− , Pb2+ and pH were prepared
by dissolving respective amounts of sodium fluoride, lead
chloride and hydrochloric acid and sodium hydroxide.
B. Sensor Fabrication
The schematic representation of sensor fabrication
for quantitative determination of fluoride Pb2+ , F− ,
pH and their respective sensing principle is shown in
Figures 1(a), (b), and (c). Whatmann filter paper (Grade 1)
was cut into 1 cm × 1 cm size, which was used as substrate
for the sensor fabrication. For the F− sensor, firstly, 0.1 M
of ammonium thiocyanate solution (w/v) and 0.1 M of iron
(iii) chloride solution (w/v) were mixed in equal amounts
to obtain a brick red colored iron (iii) thiocyanate solution
(v/v). Following this 60 μl of iron (iii) thiocyanate solution
was dispensed on each of the potassium sodium tartrate
coated paper pieces before vacuum dried at 37 ◦ C. For Pb2+
sensor, initially, the paper pieces were coated with 30 μl
of potassium sodium tartrate saturated solution and vacuum
dried at 37 ◦ C. Following this, 60 μl of 0.05% solution of
dithizone in CCl4 was dispensed on the paper pieces before
vacuum drying at 37 ◦ C. For the pH sensor, the paper pieces
were coated with 10 μl of 250 mM citric acid solution and
vacuum dried at 37 ◦ C. Following this, the sensors were
coated with 90 μl of 0.4% (w/v) of bromothymol blue in
7938
Fig. 2. The images (a) and (b) illustrates the UV Visible spectra and mechanism of the interaction between iron (iii) thiocyanate and fluoride. Images (c) and
(d) shows the UV Visible spectra and mechanism interaction between dithizone and lead. Images (e) and (d) illustrates the UV Visible spectra and mechanism
of interaction of bromothymol blue with different pH.
DMF and dried at 37 ◦ C. All the sensors fabricated were
stored in airtight condition until further use.
C. Characterization and Calibration
The colorimetric paper sensors were characterized for their
color intensity by placing them between a LED-LDR setup
as shown in Figures 1(a)-(d). The change in the electrical
resistance of the LDR due to the absorption of varying amount
of light, from the LED, resulting from the change in the
color intensity of the sensor was measured using setup using
Arduino Uno development board and LCD display as depicted
in Figure 1(d). The initial resistances of the unreacted sensors
of Pb2+ , F− , and pH were measured and termed as (R0i )
where, i = F− ,Pb2+ , pH, respectively. The resistances of the
sensors, after the addition of a 10 μL drop of sample solu-
tions containing different concentration of Pb2+ , F− , and pH,
were measured and denoted as ( R i ) where, i =F− ,Pb2+ , pH,
respectively.
Figure 2 illustrates the UV-Visible spectroscopic results. The
Figure 2(a) illustrates the UV-Visible spectra of the interaction
between iron (iii) thiocyanate and fluoride. In the plot the
blue curve represents the UV-Visible spectra for the iron (iii)
thiocyanate whose absorption peak is at 295 nm while the red
curve represents the fading of the color product of the reaction
whose absorption peak is at 290 nm [33]. It is well known that
F− on interaction with brick red coloured iron (iii) thiocyanate
gives colourless iron (iii) fluoride, as shown in the figure 2(b).
In this regard, the specific reaction can be written as,
Fe (SCN)3 +6NaF →[FeF6 ]3− +6Na+ + 3(SCN)−
Figure 2(c) demonstrates the UV-Visible spectra of the inter-
action between dithizone and Pb2+ . In the plot the blue
IEEE SENSORS JOURNAL, VOL. 19, NO. 18, SEPTEMBER 15, 2019
curve represents the UV-Visible spectra of the dithizone whose
absorption peak is at 445 nm and 620 nm, respectively,
whereas the red curve represents the pinkish Pb2+ (ii) dithi-
zone a new absorption peak is formed whose value is 533 nm
[34], [35]. The structural changes of the dithizone due to
complexation with Pb2+ is as shown in Figure 2(d). The
specific reaction can be written as,
PbCl2 + 2C13 H12 N4 S →Pb(C13 H12 N4 S)2 + 2Cl−
Figure 2(e) shows the UV-Visible spectra of the bromothy-
mol blue in lower pH (blue curve) whose absorption peak is at
427 nm whereas at higher pH (red curve) its absorption peak
being 600 nm [36]. The bromothymol blue in its protonated
form is yellow in colour. The colour changes to greenish blue
to dark blue as the deprotonation of bromothymol blue occurs
due to increase of alkaline pH which is shown in Figure 2(f).
In this regard, the specific reaction can be written as,
OH−
C27 H28 Br 2 O5 S −→ (C27 H26 Br 2 O5 S)2−
The stability of the Pb2+ , F− , and pH sensors have been
provided in the Section I of Electronic Supporting Informa-
tion (ESI). Further, the influence of humidity and temperature
on the readings of the sensor have also been illustrated in
the Section II of the ESI. For comparison with standard
methods of detection of the level of pollutants, we employed
UV-Vis Spectroscopy for F− , Atomic absorption spectroscopy
(AAS) for Pb2+ , and pH meter for pH, which has been
illustrated in the Section III of the ESI. The Section IV
of the ESI shows the performance of the proposed sensors
as compared to the previously available ones. The Section V
MANDAL et al.: PAPER-SENSORS FOR POINT-OF-CARE MONITORING OF DRINKING WATER QUALITY
Fig. 3. Plots (a) – (c) show the variation in the normalized resistance change (R0i /R i ) with the fluoride concentration (C F ) in water, lead concentration
(C P b ) in water and pH of water, respectively. Images (d)-(f) illustrate the color change of the F − , Pb 2+ and pH sensors, respectively, due to the change in
concentrations as written at the bottom.
and Section VI of the ESI discusses the Raman, FTIR and
the NMR characterization studies.
III. R ESULTS A ND D ISCUSSIONS
A. Sensing Mechanism
The initial resistance , R 0i of the F− sensor was recorded
from the LDR when light was irradiated on the sensor from
an LED light source before the water sample was dispensed.
Thereafter, final resistance R i the F− sensor was measured
after dispensing of various concentration of F− sample in
water ranging from 1.0 – 10 ppm. It was observed that
when the sample containing F− was dispensed on the sensor
surface discoloration occurred due to the reaction resulting
in increased transmission of light to the LDR, which in turn
resulted in a decrease of R i . The Figure 3(a) demonstrates
the variation in the normalized resistance R 0i /R i with the
concentration of fluoride in water sample , C F The R 0i /R i
was found to linearly and monotonically decrease with C F in
the water sample.
The images in the Figure 3(d) illustrate the visual increase
in the discoloration of the sensor surface due to increase in
the C F in the water sample dispensed on the sensor surface.
A higher discoloration led to the transmittance of higher
amount of LED light through the paper surface, which led
to a higher reduction in the electrical resistance of the LDR
7939
when theC F was higher in the water sample. The Figure 3(b)
demonstrates the variation in the normalized resistanceR0i /R i
with C P b in water. The R 0i /R i was found to increase with
C P b n the water sample. The images in the Figure 3(e)
illustrate the visual increase in the pink color intensity of the
sensor surface due to increase in C P b in the water sample
dispensed on the sensor surface. A higher pink coloration led
to the transmittance of lower amount of LED light through
the paper surface, which led to a increase in the electrical
resistance of the LDR when C P b was higher in the water
sample. The calibration for the pH sensor was performed
after dispensing of various samples of water having pH in
the range of 6.0 – 8.0. Once the sample was dispensed on
the sensor surface, a greenish blue coloration occurred due
to the reaction, which resulted in the decreased transmission
of light through the paper surface to the LDR. Figure 3(a)
demonstrates the variation in R 0i /R i with pH of water samples.
The images in the Figure 3(d) illustrate the visual increase
in the greenish blue coloration on the sensor surface due to
increase in pH of the water sample dispensed on the sensor
surface. The Section VII of the ESI discusses the interference
performance of the proposed sensors in presence of other
contaminant ions.
Fig. 4 show a typical POCT device for the water qual-
ity monitoring. We tested a range of water samples with
unknown levels of F − , Pb2+ and pH, which are plotted
7940
Fig. 4. Image shows a POCT device for monitoring of F − , Pb 2+ and pH
of water.
as solid red triangular, circular and square symbols on the
plots (a) – (c) in the Fig. 3 respectively. The plots suggest
that the POCT device could detect the levels of these pollu-
tants with reasonable accuracy when compared with standard
methodologies.
IV. C ONCLUSIONS
In summary, we report the development of three paper sen-
sors for the on-spot detection of F − , Pb 2+ and pH in
the drinking water. The colorimetric sensors show monotonic
variation in the color with the loading of F − , Pb 2+ and
pH in the water sample, which was detected with the help of
an electronic arrangement. The sensors were illuminated with
LED before the transmitted rays through them was captures
in an LDR. The variation in the resistance of LDR was
found to monotonically vary with the F − , Pb 2+ and pH
loading in the water sample. The LED-sensor-LDR combi-
nation was integrated with and Arduino circuit to develop
an economic, specific, stable, portable, fast, and user friendly
POCT device, which enabled spot detection of pollutants in
drinking water.
ACKNOWLEDGMENT
We also gratefully thank the support from Central Instru-
mental Facility, IIT Guwahati for the access to the character-
ization facilities. We are also grateful to Rupam Sinha for his
contributions.
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7941
Nilanjan Mandal received the B.Tech. degree in
biotechnology from the Haldia Institute of Technol-
ogy (HIT), India, in 2009, and the M.Tech. degree in
bioelectronics from Tezpur University (TU), India,
in 2012.
He is currently a Research Scholar with the Centre
for Nanotechnology, Indian Institute of Technology
Guwahati, India.
Shirsendu Mitra received the B.Sc. degree in chem-
istry and the B.Tech. degree in chemical engineering
from the University of Calcutta, India, in 2010 and
2013, respectively.
He is currently a Research Scholar with the
Department of Chemical Engineering, Indian Insti-
tute of Technology Guwahati, India.
Dipankar Bandyopadhyay received the B.Sc.
degree in chemistry from the University of Calcutta,
India, in 1995, the B.Tech. degree in chemical
engineering from the University of Calcutta, India,
in 1998, and the M.Tech. and Ph.D. degrees from
the Indian Institute of Technology Kanpur, Kanpur,
India, in 2001 and 2009, respectively.
He is currently a Professor with the Department
of Chemical Engineering, Indian Institute of Tech-
nology Guwahati, India, where he is also the Head
of the Centre of Centre for Nanotechnology.