Sensors and Actuators B 198 (2014) 4954

Contents lists available at ScienceDirect

Sensors and Actuators B: Chemical

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

Electromagnetic wave sensing of NO3 and COD concentrations for

real-time environmental and industrial monitoring
O. Korostynska , A. Mason, M. Ortoneda-Pedrola, A. Al-Shammaa
Built Environment and Sustainable Technologies (BEST) Research Institute, School of Built Environment, Liverpool John Moores University, Liverpool, UK

a r t i c l e i n f o a b s t r a c t

Article history: A novel electromagnetic sensor for real-time analyte composition analysis operating at GHz frequencies
Received 9 December 2013 is reported. The sensing element in a form of a gold pattern, printed on Rogers substrate, connected to a
Received in revised form 19 February 2014 Vector Network Analyser, and emits an electromagnetic eld which interacts with the sample under test.
Accepted 9 March 2014
This results in unique microwave spectra, which are specic to the analyte solution. The developed sys-
Available online 19 March 2014
tem conrmed the viability of using microwaves for real-time NO3 and chemical oxygen demand (COD)
monitoring as the reected signals represented by S11 parameters were unique for each solution type
Keywords:
and concentration, with clearly observed shifts in the resonant frequencies peaks and their amplitudes
Real-time measurements
Environmental monitoring
when placed in direct contact with 30 l of each solution. The system would be of benet to a broad
Water solutions range of environmental and industrial process monitoring applications, as it provides real-time infor-
Microwave sensors mation of both the solution type and its concentration, without the need for using additional chemicals
NO3 for testing. Moreover, the reported microwave sensing technique offers a cost-effective and sustainable
COD approach to current laboratory based methods of aqueous solutions analysis, since the sensors are robust
and reusable.
2014 Elsevier B.V. All rights reserved.

1. Introduction Water quality standards for different types of water sources

The implementation of The European Water Framework Direc-
tive has triggered the need for new methods and systems which
enable the real-time monitoring of chemical and biological pollut-
ants in water. The composition of the analyte solutions must be
determined with high accuracy for many applications, such as food
and pharmaceutical industries, chemical processing and environ-
mental monitoring, where the content of impurities in water is an
important factor [1].
Traditional methods of aqueous solutions composition moni-
toring are lab-based and include standard UVVis measurements,
mass spectrometry, ion-sensitive electrodes and amperometric
sensors [2,3]. On the other hand, a range of modern real-time mon-
itoring approaches exist; for example, bre-optic sensors, MEMs,
lab-on-chip sensors and biosensors [4]. It was also demonstrated
that micro-Raman spectroscopy can allow the determination of the
NaCl salt concentration of an aqueous solution with an error close
to 5% [5].
Corresponding author. Tel.: +44 151 2312294.
E-mail address: O.Korostynska@ljmu.ac.uk (O. Korostynska).
(lakes, rivers or oceans) vary due to different intended human
use and their ecosystems or environmental conditions. Thus,
monitoring of their contents must also vary dependent on the
situation. With continuous industrial developments, depleting nat-
ural water resources, increasing population and corresponding
increased demand on domestic and industrial water consumption,
it is getting more and more challenging for the water supply indus-
try to maintain the safety of water.
Water quality assessments are based on the analysis of the
physical, chemical and bacteriological parameters and require
customised apparatus and trained staff. Environmental water mon-
itoring includes measurements of physical characteristics (e.g.
pH, temperature, conductivity), chemical parameters (e.g. oxygen,
alkalinity, nitrogen and phosphorus compounds), and abundance
of certain biological taxa. Monitoring could also include assays of
biological activity such as alkaline phosphatase, tests for toxins and
direct measurements of pollutants such as heavy metals or hydro-
carbons [3]. The quality of treated wastewater is primarily dened
by the measurement of global parameters such as biological oxy-
gen demand (BOD), chemical oxygen demand (COD), total organic
carbon (TOC) and total suspended solids (TSS) [6].
Current measurements of nutrients, such as phosphorous,
ammonia and volatile fatty acids in water are mostly based on

http://dx.doi.org/10.1016/j.snb.2014.03.030
0925-4005/ 2014 Elsevier B.V. All rights reserved.
50 O. Korostynska et al. / Sensors and Actuators B 198 (2014) 4954
off-line monitoring and imply low frequency data sampling and
delay between sampling and availability of the results [7]. How-
ever, in past years there has been a growing interest in the use of
on-line monitoring systems able to distinguish abnormal changes
from normal variations [8,9].
The term chemical oxygen demand is used to express the
amount of oxygen consumed during oxidation of a sample with
hot acid dichromate solution under dened conditions. This is a
standard test for wastewater quality control and it provides an esti-
mate of the oxidisable matter present in the sample [10]. The result
is usually expressed as milligrams of oxygen consumed per litre
of sample (mg/l). Several methods, mostly relying on respirome-
try, have so far been proposed for the quantitative characterization
of the COD fractions in terms of biodegradability, though most of
these procedures are quite time-consuming and generally require
acclimated biomass [11]. However, the standard reference method
for determination of COD has the following inconveniences: (i)
strong experimental conditions involved in the oxidation of organic
matter by potassium dichromate in sulphuric acid at high temper-
atures; (ii) use of catalysts such as silver sulphate, which increases
the cost of analysis; (iii) generation of residues such as chromium,
silver and mercury, which are harmful to the environment; and (iv)
low analytical speed, owing to the use of a digestion stage that lasts
from 2 to 3 h [10].
No single system available today can fully address the needs of
the customers in its ability to determine, in real time, the compo-
sition of water solutions to the desired sensitivity level, bearing
in mind the desire for system portability and cost-effectiveness.
Therefore, novel real-time monitoring techniques are necessary.
One technique potentially capable of meeting this current demand
is based on microwave sensing, as presented in this paper.
2. Electromagnetic wave sensing
Electromagnetic wave sensing at microwave frequencies is a
new technological approach which has been successfully used for
monitoring processes in various industrial applications including
solution concentrations [1], uid level measurements [12], mate-
rial moisture content [13,14], for continuous process monitoring
of biogas plants [15], for the determination of moisture content in
soil [16], in the food industry for the verication of the vegetable
oil types [17], for non-destructive evaluation of an activated carbon
[18], for monitoring of Pseudomonas aeruginosa concentration [19],
and in the healthcare industry [20], for example for real-time mon-
itoring of glucose in diabetic patients [21,22] and for non-invasive
monitoring of bodily uids [23,24].
Microwaves are largely used for material characterisation since
they easily propagate through low-loss dielectrics and the ampli-
tude of the electromagnetic wave reected by or transmitted
through a material strongly depends on the dielectric properties
of the material itself.
A microwave system is able to adequately trace multiple phases
in a complex uid ow. For example, an electromagnetic waves cav-
ity resonator was used to monitor the percentage volumes of each
phase (oil and gas) in the pipeline using the resonant frequencies
shifts that occur within the resonator [25,26].
However, the microwave planar printed patterns for various
sensing applications are increasingly used due to their versatil-
ity, at prole and low weight. Their design can be tailored to suit
particular applications, coupled with reliability and cost-efciency.
They are easily manufactured using common methods for printed
circuit board production, and their impedance can be matched to
the input line by altering the micro-strip line feed conguration.
The patch antenna represents the frequency-selective element of
a phase shift transistor oscillator. The active integrated antenna
frequency of operation is determined by both the patch geometry
and the electrical loads connected at the two microstrip ends [27].
For example, a coaxial-fed patch antenna suitable for non-
destructive porosity measurements in low-loss dielectric materials
has been reported [28]. The variation of the patch resonant fre-
quency when it is put on the surface of the material under test
was used to estimate the dielectric permittivity at 2.4 GHz ISM fre-
quency bands. The estimated porosity was in good agreement with
that obtained by the conventional mechanical measurements, and
the mean percent error was less than 13.5%.
To clarify the principle behind electromagnetic wave sensing
suggested in this work for measuring the type and concentration
of analyte solutions, it is worth mentioning that microwave sensors
in the form of planar printed patterns operate based upon the fact
that an object under test, e.g. a water sample or piece of plastic,
when placed into the vicinity or in direct contact with a microwave
sensor, interacts with the electromagnetic waves in a unique man-
ner, which can be specically correlated with the properties of this
material. In particular, the sensing is based on interaction of prop-
agating or resonating modes within the material under test. By
considering how reected (S11 ) microwave signals vary at discrete
frequency intervals, the change in the signal can be linked to the
amount and type of material under test. The response of the sensor
manifests itself as a resonant frequency change, attenuation of the
signal or as a phase shift.
3. Experimental procedure
3.1. Analyte solutions preparation
A range of solutions with various concentrations of NO3 and
COD in the mg/l range were prepared to verify the potential of
the microwave sensing approach to distinguish between different
solutions and to measure their concentrations in real time.
To verify the analyte composition, COD measurements were
performed in Hach Lange cuvettes, as it is a standardised method
broadly used and which produces easily comparable results.
Hach Lange COD cuvette test LCK314 (Hach Lange, UK) for chem-
ical oxygen demand is commonly used to indirectly measure the
amount of organic compounds in water. This specic test has a
range of 15150 mg/l O2 . It follows the chromsulphoric acid method
and it provides differentiation between tests and measuring ranges
by means of colour-coding, which then are read in a spectropho-
tometer. Specically, oxidisable substances react with sulphuric
acidpotassium dichromate solution in the presence of silver sul-
phate as a catalyst. Chloride is masked by mercury sulphate. The
reduction in the yellow coloration of Cr6 + is evaluated. The cuvette
containing pre-dosed reagents were incubated at 148 C for 2 h,
and then the measurements with the spectrophotometer were per-
formed.
Similarly, a number of analyte solutions with different con-
centrations of nitrate were prepared. Hach Lange nitrate cuvette
test LCK340 (Hach Lange, UK) was used, which follows the
2,6-dimethylphenol method. Nitrate ions in solutions containing
sulphuric and phosphoric acids react with 2,6-dimethylphenol
to form 4-nitro-2,6-dimethylphenol. The samples placed in the
cuvettes were incubated at room temperature for 15 min and then
were read in the spectrophotometer to determine NO3 concentra-
tion.
Notably, NO3 and COD solutions were tested separately to reveal
the nature of the electromagnetic wave sensor response to these
solutions. Having conrmed the ability of the developed system
to differentiate between the solution types and to detect its con-
centration, the next challenge is to test the system response to
the water samples with mixture of pollutants. Taking into account
 O. Korostynska et al. / Sensors and Actuators B 198 (2014) 4954
Fig. 1. Design of a microwave sensing pattern with SMA connector.
endless amount of possible water pollutants combination, the cur-
rently ongoing research is application-specic, where solution with
known composition is tested with a particular industrial or envi-
ronmental scenario in hand.
3.2. Electromagnetic sensor design and measurement setup
The design of any microwave sensor is the key parameter that
regulates its performance. A Sensor with the structure shown
in Fig. 1 operating at microwave frequencies was designed on a
Rogers substrate, dielectric constant 3.4 at 10 GHz, with 35 m
thick gold layer serving as a ground plane and a top pattern in
the form of interdigitated (IDE) electrodes. This versatile design
combines ease of manufacturing with the desired functionality.
Notably, Au patterns are particularly suitable for measuring analyte
solutions as Au does not chemically react with them. The sensing
area was 5 8 mm2 .
A distinct feature of IDE type sensors is their superior sensitivity
to change close to the sensor surface, with this sensitivity decaying
rapidly with distance away from the surface. This is advantageous
as it reduces signicantly the chance of undesirable factors inu-
encing sensor response.
The microwave sensor was attached to a Rohde and Schwarz
ZVA24 vector network analyser (VNA) via a coaxial cable, as pictured
in Fig. 2. A Molex edge type SMA connector [29] was used to connect
the sensor via coaxial cable to the VNA. The sensor and associated
equipment were all specied for 50  impedance.
The data (60,000 points for each measurement) was captured in
the frequency range of 115 GHz for the reected (S11 ) signals. All
the measurements were performed at a constant temperature of
Fig. 2. Measurement setup showing VNA and a microwave sensor connected via
coaxial cable.
51
Fig. 3. S11 signal distribution of microwave sensor response in 015 GHz frequency
range when in contact with COD and NO3 solutions of 54.7 mg/l and 56.6 mg/l con-
centrations, respectively.
18 C, with all the samples being 30 l in volume for consistency.
Each solution sample was measured at least seven times to ensure
repeatability and reproducibility or the results, and the average
spectra were plotted on the graphs and analysed. The discrepancy
between each sample measurement was within 5%, and could be
due to imperfection of manual sample loading process, as it was
shown that the system is sensitive to water volume changes [30].
Since each spectrum contains 60,000 points, the recorded signal is
of superior accuracy and resolution.
The average spectra from each measured analyte solution are
plotted on common graphs to illustrate that each sample has a
unique response to the microwave signal resulting in resonant
peaks occurring at different frequencies. This particular feature
makes the developed sensor an attractive option for real-time
monitoring of analyte solution type and concentration brought in
contact with it.
4. Results and discussion
The spectra for the microwave sensor were recorded in the
015 GHz frequency range when in contact with 30 l of NO3 and
COD analyte solutions in various concentrations. The ability of this
sensor to distinguish the presence and type of these solutions is
evident in Fig. 3, which depicts the reected microwave spectra for
54.7 mg/l COD and 56.6 mg/l NO3 solutions.
Further experiments conrmed the microwave sensor potential
to produce different responses depending on the NO3 solution con-
centration in the 3072 mg/l range, as shown in Fig. 4. The distinct
feature is the change in the resonant peak amplitude at a frequency
just below 9 GHz, with the amplitude modulus decreasing with the
increasing NO3 concentration. The resonant peak value alone can
be used as an indicator of the NO3 concentration, as illustrated in
Fig. 5.
Similarly to NO3 measurements, the ability of the sensor to mea-
sure various COD solutions was tested. The shape of the microwave
spectra produced by the sensor when in contact with COD solutions
is different, and there is a change in both the amplitude of the res-
onant peaks and their frequencies, as shown in Fig. 6. A number of
resonant peaks can be focused upon to serve as an indicator of the
COD level in a solution, which is brought in contact with the elec-
tromagnetic eld of the sensor. One can see that the whole spectra
experienced change in the amplitude depending on COD concen-
tration, with the resonant peak at around 4.6 GHz being particularly
sensitive to the change, as highlighted in Fig. 7. Also, there are
52 O. Korostynska et al. / Sensors and Actuators B 198 (2014) 4954

Fig. 4. S11 signal distribution of microwave sensor when in contact with NO3 solu- Fig. 7. Change in the resonance peak amplitude depending on COD level: 16 GHz
tions of various concentrations, in mg/l. The response is shown in 7.011.0 GHz range.
range.

-14
Amplitude of the resonant peak S11, dBm

-16

-18

-20

-22

-24

-26

-28
40 60 80
NO3 concentration, mg/l
Fig. 8. Change in the reected microwave spectra depending on COD level:
711 GHz range.
Fig. 5. Dependence of the resonant peak amplitude on the concentrations of NO3
solution placed in contact with the sensor.

The change in the resonant peak amplitude with COD can be

two overlapping resonant modes at 9.19.8 GHz range, with both used as a calibration curve to reveal the COD concentration in the
peaks experiencing the shift to lower frequencies and decreasing analyte solution, as for example shown in Fig. 9 for 4.6 GHz reso-
amplitude module with increasing COD concentration, as shown in nant peak.
Fig. 8.

-1.4
Amplitude of the resonant peak S11, dBm

-1.6

-1.8

-2.0

-2.2

-2.4

20 30 40 50 60
COD concentration, mg/l

Fig. 6. S11 signal distribution of microwave sensor when in contact with COD solu- Fig. 9. Change in 4.6 GHz resonance peak amplitude, S11 , with COD concentration
tions of various concentrations, in mg/l. level.
 O. Korostynska et al. / Sensors and Actuators B 198 (2014) 4954
Thus, substantial changes in the microwave spectra caused
by the solutions with varying COD and NO3 concentrations were
recorded and these can be used as an alternative to the traditional
optical method measure of an unknown analyte composition. This
method is non-destructive, it provides real-time responses and the
microwave power used is in the order of 1 mW, which is non-
ionising radiation, less than commonly used even in the mobile
phones, and thus has negligible deleterious effect on the material
being measured. Another advantage of this method is that there
are no additional chemicals required to reveal the concentration of
the analyte solution. The proposed system can potentially be inte-
grated into an industrial production line to automatically assess
the composition of solutions in real time and manage the chemical
processes accordingly.
Notably, the sensors responses returned to their original
benchmark positions, namely air spectra, after each measure-
ment of the analyte solution were performed and the sample was
removed from the sensor surface. This conrms that the developed
microwave sensor is reliable, re-usable and thus a sustainable solu-
tion for precise in-situ method for industrial process monitoring,
where real-time information on solutions composition is essential.
The response of the sensor to other analyte solution types and
concentrations is being explored and a database of these microwave
signature spectra is being compiled, which can later be used for
online process control in a broad range of industrial applications in
the wastewater industry, chemical and pharmaceutical production
lines. Further, the prototype system will be tested in real indus-
trial settings and a challenge of differentiating between multiple
water pollutants possibly present in a sample and determining their
concentrations would emerge.
5. Conclusions
This research was driven by the industrial need for a novel real-
time method of measuring the parameters of aqueous solutions,
in particular the concentrations of NO3 and COD, which are the
standard indicators of water quality, for example in wastewater
treatment monitoring. Microwave sensors were developed for this
purpose and successfully tested in the 015 GHz frequency range. It
was clearly shown that the resonant peaks shift and their amplitude
change depending on the type and the concentration of the ana-
lyte solution in contact with the sensor pattern. Thus, each solution
interacts with the electromagnetic eld of the sensor in a specic
manner, producing unique microwave spectra which are charac-
teristic of the solution type and its concentration and therefore can
be used as a reliable indicator of the analyte composition. Real-time
sensing would provide invaluable information about any changes
in the solution concentration or type during the industrial process,
so that an automated control and management system would take
appropriate actions to remedy the situation instantly.
Acknowledgements
This work is nancially supported by the European Communitys
Seventh Framework Programme through the FP7-PEOPLE-2010-
IEF Marie-Curie Action project 275201, Water-Spotcheck. The
authors would like to express their gratitude to Mike Garner, Gar-
ner Osborne Circuits Limited, UK and to Mabruk Farrah, Mechan
Controls Plc, for manufacturing sensor prototypes.
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Biographies
Dr. Olga Korostynska has a B.Eng. (1998) and M.Sc. (2000) in Biomedical Engi-
neering from National Technical University of Ukraine (KPI) and Ph.D. (2003) in
Electronics and Computer Engineering from the University of Limerick, Ireland.
Currently she is EU Research Fellow in Liverpool John Moores University, UK devel-
oping microwave sensors for real-time water quality monitoring. Before that she
was an engineer in the National Telecommunication Institute in Ukraine; then a
Postdoctoral Researcher in the University of Limerick, working on a number of
projects, including those funded by IRCSET, EI and EU FP7 and also was a Lecturer in
Physics in Dublin Institute of Technology, Ireland. She has published a book, 11 book
chapters and over 200 scientic papers in peer-reviewed journals and conference
proceedings.
Dr. Alex Mason graduated from the University of Liverpool, UK, with a rst class
honours degree in Computer and Multimedia Systems, after which he went on to
complete a Ph.D. in Wireless Sensor Networks and their Industrial Applications at
Liverpool John Moores University, UK. Upon completing his Ph.D. in 2008, he con-
centrated for 2 years solely on research, working on aspects of non-invasive and
non-destructive sensing for the healthcare, automotive and defense sectors. Dr.
Mason is a Reader in Smart Technologies within the School of Built Environment and
has continued research in many areas, developing an interest in Structural Health
Monitoring and Building Performance Analysis, thus utilising his computing and
electronics background and applying it to issues relevant to the Built Environment.
In addition to teaching Materials, Energy Management and Environmental Studies,
he is responsible for a number of Ph.D. students who are working on a wide variety
of topical research projects.
Dr. Montserrat Ortoneda-Pedrola has a B.Sc. in Biological Sciences from the Univer-
sity of Girona (Spain), an M.Sc. in Applied Microbiology and a Ph.D. on the topic on
vitro and in vivo antifungal susceptibility of opportunistic fungi, which she com-
pleted in 2003 at the University Rovirai Virgili in Reus (Spain). After that she has
worked on a number of research projects in Ireland and the UK, including several
funded by EU FP6 and EU FP7. These research projects range from the study of fungal
genomics to microwave applications for the food industry and for the production
ofbioethanol and biogas.
Prof. Ahmed Al-Shammaa is the director of the Built Environment and Sustainable
Technologies (BEST) Research Institute at the School of Built Environment at Liver-
pool John Moores University, UK. He has extensive research interests that cover
a wide range of applied industrial sciences, including advance microwave tech-
nologies for renewable energies from waste including biodiesel, bioethanol and
biobutanol, waste recycling, environmental and sustainable agendas. He has also
extensive experience in the design and construction of wireless sensors for the
construction, healthcare, automotive and aerospace industries as well as bespoke
software solutions to monitor real time energy levels in various industrial applica-
tions and near zero carbon initiatives for the energy sectors. Prof. Al-Shammaa is
one of the EU scientic ofcers on Renewable Energies and has obtained various
supported applied research projects funded nationally and internationally by the
EU, UK and USA Ministry of Defense, Carbon Trust, Technology Strategy Board and
direct funding from industry. He has published over 320 peer reviewed scientic
publications, 15 patents and coordinated over 30 research projects.