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fully edited. Content may change prior to final publication. Citation information: DOI 10.1109/JIOT.2021.3069894, IEEE Internet of
Things Journal
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Manuscript submitted December 1, 2020. (Corresponding author: Fowzia Md Eshrat E. Alahi is with Shenzhen Institute of Advanced Technology,
Akhter.) Chinese Academy of Sciences, Shenzhen 518055, China (e-mail:
Fowzia Akhter, Hasin R. Siddiquei and S.C. Mukhopadhyay, are with Dept. ealahi@yahoo.com).
of Engineering, Macquarie University, Sydney, NSW 2109, Australia. (e-mail: Krishanthi Jayasundera is with University Technology Sydney, 15 Broadway,
fowzia.2k3@gmail.com;engr_hasin96@yahoo.com;subhas.mukhopadhyay@ Ultimo NSW 2007, Australia, <Krishanthi.Jayasundera@uts.edu.au>
mq.edu.au).
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problems [15]. Hence, it is necessary to have the best nitrate, II. MATERIALS AND METHODS
phosphate, and pH management in water used for farming for This section represents the fabrication procedure and
both economic and environmental reasons. experimental procedures for nitrate, phosphate concentrations,
There are numerous methods have been advised in analytical and pH level determination using the developed sensor in water
chemistry to determine the water contaminants, such as High- bodies.
performance liquid chromatography (HPLC) [16], UV-
spectroscopy [17], chromatography [18], and colorimetric A. Fabrication Procedure
methods [19] to detect nitrate and phosphate from water. The master mould is designed using Autodesk Fusion 360
Although these expensive systems provide highly accurate software and printed with Poly Lactic Acid (PLA) filament
results, they are time-consuming, complex to operate, and need using Dreamer 3D printer. At first, conductive ink is prepared,
daily care such as cleaning, storage, and maintenance [20]. mixing the MWCNTs powder and PDMS at a ratio of 10:2. The
Thus, it is essential to develop low-cost, low-power sensing optimum ratio is obtained by analyzing the variation of resultant
devices for detecting nitrate, phosphate, and pH accurately in conductivity with the change in concentrations. The analysis
different water bodies to ensure a sustainable world to live. shows that the electrodes' resultant conductivity changes with
Numerous researches have been done for determining the the variation of MWCNTs and PDMS ratio to a certain point.
contaminants of the water, such as nitrate, phosphate, chloride, After that, it reaches its saturation point. Therefore, a 10:2 ratio
magnesium, calcium, and pH [21- 23]. However, it still needs is finalized for developing electrodes of the sensor. Initially, the
high-sensitivity, low-power, low-cost, and easily operable conductive ink is cast on the moulds. This is followed by curing
sensors applicable to any environmental condition. Internet of the moulds at 70˚C for an hour to solidify the nanocomposites.
Things (IoT) enabled smart devices can also be used to monitor After that, PDMS is poured on the mould to form the substrate.
environments and water quality, making our lives accessible to A casting knife is used for adjusting the height of PDMS to
the digital world [24]. The inclusion of communication 1000 µm. The samples are then put inside a desiccator until the
protocols enables data transfer from the sensor node to the trapped air bubbles are removed. Finally, the sample is heated
server to further process and predict future trends [25]. at 70o C for three hours for solidification. Once the curing is
There are various materials available for developing the done, the samples are peeled off, and experiments are
substrates of the flexible sensors, including Polyethylene conducted after washing. The sensor consists of six pairs of
terephthalate (PET) [26], Polyimide [27], and interdigitated electrodes. The length of each electrode is 30 mm,
Polydimethylsiloxane (PDMS) [28]. Among them, PDMS has whereas the width is 1.5 mm. There is a 3 mm gap between two
been chosen in this research as it is biocompatible, successive electrodes. A good quality filament is a must to
hydrophobic, cost-effective. The interfacial bonds formed with ensure a smooth texture of the printed mould and making the
the sensors' electrodes and PDMS are outstanding [29]. Among sensor reproducible. PDMS and CNT powder should be mixed
the conductive materials (Carbon Nanotubes (CNTs), properly to ensure the sensor's conductivity. It is also essential
Aluminum, Gold, and Graphene), Multi-Walled Carbon to provide adequate attention to remove the trapped bubbles by
Nanotubes (MWCNTs) are utilized for developing electrodes desiccation. The schematic diagram of fabrication process is
because it has better bonding capability and higher electrical shown in Fig.1.
conductivity with PDMS [30]. This research discusses the
fabrication, and application of a novel MWCNTs/PDMS sensor
for nitrate, phosphate, and pH detection in water bodies. The
mobility and behaviour of the nutrient ions in the water change
when temperature changes [31]. Therefore, the sensitivity of the
sensor towards temperature is also studied. It also explains a
portable sensing system's design and development process to
monitor the farm's water quality. The portable system has the
Internet of Things (IoT) capability, which will help check the
gradients of the water's nutrients and pH level. Irrespective of
the farm's time and place, the farmer will be getting feedback
from the experts if any sudden environmental variations occur
inside the farm.
This article is divided into four sections. A brief introduction
of the proposed research is discussed in section I; the materials
and methods, including the fabrication process, working
principle, and experimental setup, design of the portable
system, are discussed in section II. The experimental outcomes
and development of the calibration standards are included in
section III. The research conclusion has been provided in
Section IV of the paper. Fig. 1. Schematic diagram of the sensor fabrication process.
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The operating mechanism of the proposed sensor and parallel water for consecutive measurement. It is then dried for ten
plate capacitor is similar. When a low-amplitude alternating minutes for successive measurement. Finally, the experimental
voltage is applied between the excitation and sensing results are analyzed for developing calibration standards of
electrodes, an electric field initiates between them. The electric nitrate, phosphate, and pH from water samples.
field bulges out from the sensing electrode to the excitation
electrode due to the planar structure. This electric field changes
as soon as the material under test (MUT) is kept close to this
generated electric field. As a result, the values of the
impedances change. The MUT characteristics are analyzed in
this research by studying the variation of the electric field
properties. The sensor's operating principle are shown in Fig. 2.
Fig.2. Sensor’s working principle. Fig. 3. Experimental setup for nitrate and phosphate detection.
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TABLE I
TRAINING DATASET MATRIX
Nitrate Phosphate T pH Z R ϴ
0.1 0.1 5 1.71 Z1 R1 ϴ1
0.1 0.1 5 3.47 Z2 R2 ϴ2
- - - - - - -
- - - - - - -
0.1 0.1 10 1.71 Z5 R5 ϴ5
0.1 0.1 10 3.47 Z6 R6 ϴ6
- - - - - - -
- - - - - - -
0.1 1 5 1.71 Z17 R17 ϴ17
0.1 1 5 3.47 Z18 R18 ϴ18
- - - - - - -
- - - - - - -
1 0.1 5 1.71 Z65 R65 ϴ65
1 0.1 5 3.47 Z66 R66 ϴ66
Fig.5. Connection diagram of the proposed system.
- - - - - - -
- - - - - - -
10 10 20 10.49 Zn Rn ϴn (n=256)
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the allocated channel. During this Arduino program III. RESULTS AND DISCUSSIONS
development, the spreading factor (SF) is set to 7 for the fastest This section represents the sensor responses towards
data transmission. This Thingspeak server can be accessed from temperature, nitrate, phosphate concentrations, pH level and the
any location. This will allow the agronomist to monitor the real-
methods for developing the calibration standards to calculate
time data for early detection of any ecological risk. Lora
nitrate, phosphate concentrations and pH value in unknown
Communication protocol is used for data transmission in the
samples.
proposed system as it consumes the least power and provides
broad coverage compared to other communication A. The Response towards Temperature, Nitrate, Phosphate,
protocols[43] such as Zigbee [44] and WiFi [45]. A and pH
rechargeable battery is used rather than using the one-time This research aims to develop a portable nitrate, phosphate
battery to be charged whenever unused. It will reduce the cost
sensing, and pH system applicable to indoor and outdoor
of the system when used in the long-term.
conditions. The temperature of the water varies significantly in
a practical scenario. As a result, the sensor’s performance
suffers due to temperature variations. Hence, the temperature
effect on the sensor's performance is studied initially. It is
carried out following the procedure based on prior research
[46]. The ions' mobility varies because of the change in
temperature, which causes variation in impedance. This
experiment's experimental setup is almost the same as Fig. 3,
which includes an IEC Hotplate (Cat no. 1920-001), a mercury
thermometer, HIOKI IM 3536 LCR meter, and a computer. The
deionized water temperature is varied from 5o C to 45o C using
IEC Hotplate, and the sensor's resistances, reactance, phase
angles and impedances are measured for 10 Hz ~ 100 kHz
frequency range. A mercury thermometer is dipped inside the
water for determining the actual temperature while taking this
measurement. The resistances of the sensor change
considerably in comparison to the change in reactance for
various temperatures. Therefore, the graph presenting the
change in resistance for various frequencies (Fig.8(a)) is
included in this article. The maximum sensitivity of the sensor
for temperature is calculated as 1.1974 Ω/℃. A frequency of
1.3 k Hz is selected as the operating frequency as it lies in the
sensitive region where all the temperatures are distinct. At this
frequency, the values of resistances are considered for finding
the correlation between the sensor's temperature and resistance.
Fig.8 (e) represents temperature and sensor's resistance
relationship. This curve is used for measuring temperature from
unknown water sample. The determination coefficient (R2) is
0.9902, which reveals a well-correlation between the
temperature and the sensor's resistance. Thus, temperature can
be measured using the following equation.
6×106 −𝑅𝑇
𝑇 (℃) = (2)
104539
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changes are attributed to the double-layer capacitance (Cdl), sensitivity for nitrate, phosphate, and pH level of the sensor are
adsorption capacitance (Cad), and solution resistance (Rs). The calculated as 1.9396 Ω/ppm ,0.8839 Ω/ppm and 1.0295 Ω,
sensor shows considerable changes towards nitrate solutions for respectively.
the whole range of frequency (10 Hz ~ 100kHz); for phosphate, The highest value of R2 is achieved by applying the linear fit
the prominent response is found between 10 Hz to 10 kHz, for nitrate, phosphate, and pH. These regression analyses are
whereas, for pH, the significant changes are found between 10 simple and easy. Therefore, these have been chosen for
Hz to 300 kHz. It is observed from the experimental outcomes covering the whole range of nitrate, phosphate concentrations,
that the change in resistance is more prominent in comparison and pH levels.
to reactance towards the sample solutions. Thus, variation in
107 −𝑅𝑠𝑒𝑛𝑠𝑒
resistance concerning frequency towards different nitrate and For nitrate, 𝐶𝑛𝑖𝑡𝑟𝑎𝑡𝑒 = (3)
364104
phosphate concentrations and pH levels are included here. The 5×106 −𝑅𝑠𝑒𝑛𝑠𝑒
calibration curves (Fig. 8 (e)) are also achieved based on the For phosphate, 𝐶𝑝ℎ𝑜𝑠𝑝ℎ𝑎𝑡𝑒 = (4)
165918
resistance values against various nitrate, phosphate 7×106 −𝑅𝑠𝑒𝑛𝑠𝑒
For pH level, 𝑃𝐻_𝑙𝑒𝑣𝑒𝑙 = (5)
193248
concentrations, and pH values.
While obtaining the calibration curve for measuring the Where, Cnitrate (ppm), Cphosphate (ppm) refer to the actual nitrate
unknown concentrations, a particular frequency is chosen, and phosphate concentrations, PH_level is the pH value,
which is common for all the tested solutions of nitrate, whereas Rsense (Ω) shows the sensor's real impedance.
phosphate, and pH. Hence, the calibration standards are
B. Reproducibility and repeatability of the sensor
developed at 1.3 kHz to determine nitrate, phosphate
concentrations, and pH values with the sensor's resistance. The Five sensors are fabricated initially for testing their
reproducibility. Their responses towards 10 ppm phosphate
(a) (b)
(c) (d)
(e)
Fig. 8. Sensor's response towards various (a) temperatures, (b) nitrate, (c) phosphate, and (d) pH for a frequency sweep (10 Hz~100 kHz), and (e) The functional
relationship between real part of impedance and temperature, nitrate, phosphate, and pH.
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concentrations are recorded. The outcomes are summarized in pH values in various water samples with more than 95%
Table II. It is found that all the sensors exhibit similar accuracy. The 5% measurement error is because of other
performances with a maximum RDS of around 1.5%. minerals' presence in the sample water. However, the accuracy
Therefore, it can be confirmed that the proposed fabrication can be further improved by preparing mixed samples with
technique promotes outstanding reproducibility. additional water quality parameter such as calcium,
magnesium, and dissolved oxygen and training the system with
TABLE II more data using a high memory-based microcontroller board.
TESTING REPRODUCIBILITY OF THE SENSOR
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D. Data Storage into Thingspeak Cloud Server cost, low-power portable system responds quickly, which is
within 1 second. Another essential feature of the proposed
The LoRa connectivity is included in the proposed system sensor is reliability in determining pH level, nitrate, and
so that the farmers can check the nutrients levels and transfer phosphate concentrations with RSD less than 3%. The design
the data in the Thingspeak channel for storing and sharing with and application of a portable smart sensing system for
the experts. The agronomist can review the collected data
monitoring water quality in real-time are also explained.
immediately in the IoT server. This will allow them to
Inclusion of the K-NN machine learning algorithm enhanced
understand the trend and advise the farmers accordingly from
the applicability in real-sample with 95% accuracy. The
any remote location. Therefore, the portable system is taken to
the Macquarie University Creek two times (morning and implementation cost of the system is about 150 US dollar which
afternoon) daily for a week to study its water quality, and data includes the purchase of electronic consumables in small
are transferred to Thingspeak as shown in Fig. 13. The numbers. However, the overall cost can be reduced
concentration of nitrate and phosphate is below 3 ppm. The significantly when product is developed in large numbers. The
temperature is varied from 10o~15oC. The concentrations of proposed sensor patch and the smart portable system are highly
nitrate and phosphate are not too high, interprets the quality of potential to develop a complete and efficient water quality
water is good. The pH value varies from 8.0 ~8.5, which defines surveillance system in real-time. This will enable early
the water is alkaline. As the pH level does not change detection of environmental hazards and provide time for an
significantly, the organisms can live and grow adequately in the effective countermeasure. Anyone can use this portable system
creek water. This developed system will substantially impact on with minimal training. This is an ideal system for a regular
taking decisions, making farms smart enough to adapt more evaluation of contaminants level.
quickly to changing conditions. Remotely monitoring the farm The low-cost sensor's performance will be enhanced further
conditions and infrastructure helps saving time, labour, and by introducing the selectivity for nitrate, phosphate, pH, and
cost, enabling farmers to focus on other things. temperature as a coating or reliable sensing materials in future
(a) (b)
(c) (d)
o
Fig.13. (a) Temperature ( C), (b) Nitrate concentration (ppm), (c) Phosphate concentration (ppm), and pH level data transferred into the Thingspeak cloud server.
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learning assisted stimulus identification for non-invasive personal care funds from the Chinese Academy of Sciences (CAS) and the
diagnostics", Material Advances, vol. 2818, 2020.
National Natural Science Foundation of China (NSFC), and the
[40] D. Adidrana and N.Surantha, "Hydroponic Nutrient Control System based
on Internet of Things and KNearest Neighbors", in Proc. IEEE
Ministry of Science and Technology (MOST) for the Foreign
International Conference on Computer, Control, Informatics and its Youth Project as a Principal Investigator (PI). He has research
Applications (IC3INA), Tangerang, Indonesia,, 23-24 Oct. 2019. interests in sensor design and fabrication, robust neural
[41] J. Vitola, F. Pozo, D.A. Tibaduiza ,and M. Anaya, "A sensor data fusion interface, and neural recording/stimulation devices for
system based on k-Nearest Neighbor pattern classification for structural biomedical applications.
health monitoring applications", Sensors, vol. 417, 2017.
[42] The Things Network (2020, Nov 22). [Online]. Available:
https://www.thethingsnetwork.org/ Dr. Krishanthi P. Jayasundera graduated
[43] J.Botero-Valencia, L. Castano-Londono , D. Marquez-Viloria, and M. from University of Peradeniya, Sri Lanka
Rico-Garcia, "Data reduction in a low-cost environmental monitoring with honours degree in Chemistry. She
system based on LoRa for WSN", IEEE Internet of Things Journal, vol.6, obtained her both Master and PhD in
no.2, pp.3024-3030, 2019.
Organic Chemistry from Kanazawa
[44] Zigbee Alliance(2020, Nov 10). [Online]. Available:
https://zigbeealliance.org/ University, Japan. She worked as post-
[45] Wi-Fi Alliance (2020, Nov 22). [Online]. Available: https://www.wi-
doctoral researcher at Massey University
fi.org/ nearly 14 years in New Zealand involving
[46] M.E.E. Alahi, L. Xie, S.C. Mukhopadhyay, and L. Burkitt, "A various projects focused on the chemical
temperature compensated smart nitrate-sensor for agricultural industry", synthesis of architecturally interesting molecules which have
IEEE Trans. on industrial electronics, vol.64, no.9, pp. 7333-7341, 2017. biological, environmental and /or medicinal
significance. Currently, she is working as Senior Researcher
Fowzia Akhter has completed B. Sc. in with University Technology Sydney, Australia. She specialises
Electrical and Electronic Engineering in Organic chemistry, Bio-sciences, sensitivity analysis using
from Khulna University of Engineering NMR, HPLC, SPR and so on. She has published over 30 papers
and Technology (KUET), Bangladesh in in different international journals and conference proceedings,
2008 and received her M.Sc in edited 5 books and 10 conference proceedings.
Communication Engineering from
International Islamic University Malaysia Dr. Subhas Chandra Mukhopadhyay is
(IIUM), Malaysia in 2012. Due to her working as a Professor of Mechanical/
excellent result during Masters, she received Rector's Award Electronics Engineering, Macquarie
which is one of the most prestigious awards for postgraduate University, Australia and is the Discipline
students of IIUM. Upon completion of M.Sc, she joined Linton Leader of the Mechatronics Engineering
University College, Malaysia as a lecturer. He served there Degree Programme. His fields of interest
before joining Macquarie University for her Ph.D. in 2017. Her include Smart Sensors and sensing
research interests include MEMS-based gas sensors, flexible technology, instrumentation techniques,
sensors, smart sensing systems, Internet of things, optics and wireless sensors and network (WSN),
photonics. Internet of Things (IoT), wearable sensors etc. He has
supervised over 40 postgraduate students and over 100 Honours
Hasin R. Siddiquei has completed B. Sc. students. He has examined over 60 postgraduate theses. He has
in Electrical and Electronic Engineering published over 400 papers in different international journals
from Rajshahi University of Engineering and conference proceedings, written 7 books and 42 book
and Technology (RUET), Bangladesh and chapters and edited seventeen conference proceedings. He has
received his M.Sc in Communication also edited thirty books with Springer-Verlag and twenty five
Engineering from International Islamic journal special issues. He has organized over 20 international
University Malaysia (IIUM), Malaysia. conferences as either General Chairs/co-chairs or Technical
During M.Sc, he developed a MEMS biosensor for detecting Programme Chair. He has delivered 353 presentations
DF-1 cells. After completion of M.Sc, he worked at including keynote, invited, tutorial and special lectures. He is
Infrastructure University Kuala Lumpur (IUKL), Malaysia as a a Fellow of IEEE (USA), a Fellow of IET (UK), a Fellow of
lecturer and Uttara University (UU), Bangladesh as a senior IETE (India), a Topical Editor of IEEE Sensors journal, and an
lecturer. Currently, he is working with Prof. Subhas associate editor of IEEE Transactions on Instrumentation and
Mukhopadyay as a visiting researcher at Macquarie University. Measurements. He is a Distinguished Lecturer of the IEEE
Sensors Council from 2017 to 2022. He is the Founding Chair
Md. Eshrat E. Alahi has received a Ph.D. of the IEEE Sensors Council New South Wales Chapter. More
in Engineering from Macquarie details can be available at
University, Sydney, Australia. He is http://web.science.mq.edu.au/directory/listing/person.htm?id=
currently working as a Post-Doctoral smukhopa
Research Fellow at Shenzhen Institutes of
Advanced Technology (SIAT), Chinese
Academy of Sciences. He has published
more than 35 research papers, including SCI journals,
conference proceedings, and book chapters. He has got research
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