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Metamaterial-Based Sensor Integrating Microwave Dielectric and Near-Infrared

Spectroscopy Techniques for Substance Evaluation

Article in IEEE Sensors Journal · October 2022

DOI: 10.1109/JSEN.2022.3202708

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19308 IEEE SENSORS JOURNAL, VOL. 22, NO. 20, 15 OCTOBER 2022

Metamaterial-Based Sensor Integrating

Microwave Dielectric and Near-Infrared
Spectroscopy Techniques for
Substance Evaluation
Euclides Lourenço Chuma , Senior Member, IEEE, and Thomas Rasmussen

Abstract —A novel era of “smart” sensors is emerging,

in which they are being used in combination with artificial
intelligence (AI) to achieve a better understanding of the
world. Such sensors need to be ubiquitous. Accordingly,
they should have miniaturized dimensions and low costs.
However, there is a tradeoff between cost and accuracy of the
sensors, which should be overcome with the use of new types
of sensors and techniques. In this article, a metamaterial-
based sensor that performs simultaneous microwave dielec-
tric spectroscopy and near-infrared (NIR) spectroscopy
measurements is presented. It uses a planar circular com-
plementary split-ring resonator for dielectric measurement
with an optical path, and NIR spectroscopy is performed
in the same physical structure. A greater diversity of data
can be achieved from the electromagnetic spectrum using
the data from microwave dielectric spectroscopy and NIR
spectroscopy; thus, it becomes possible to enhance the accuracy of substance identification with fewer samples. The
proposed sensor was evaluated for the identification of olive oil adulteration and achieved an accuracy of 100% using
only 14 training samples. To achieve this same accuracy, other techniques used for the detection of adulteration in olive
oil need more than 50 training samples. Therefore, the proposed sensor needs 72% fewer samples for training classifier
algorithms used in olive oil adulteration identification. This implies the reduction of computing requirements and wall
clock time. The proposed sensor opens new avenues to perform material characterization and identification using a
combination of microwave dielectric and NIR spectroscopies in the same structure.
Index Terms — Metamaterial, microwave, near-infrared (NIR), sensor, spectroscopy.

I. I NTRODUCTION Sensors combined with ML have enabled the development

S ENSORS are essential components of modern electronic
devices. All modern equipment with even the slightest
complexity rely on at least one sensor, and complex equipment
have dozens of sensors [1], [2], [3].
Recent advancements and major breakthroughs in artificial
intelligence (AI) and machine-learning (ML) technologies over
the past decade have enabled the collection, analysis, and
interpretation of a large amount of sensory data.
Manuscript received 24 August 2022; accepted 26 August 2022. Date
of publication 5 September 2022; date of current version 14 October
2022. The associate editor coordinating the review of this article and
approving it for publication was Prof. Carlos Marques. (Corresponding
author: Euclides Lourenço Chuma.)
Euclides Lourenço Chuma is with the Department of Communications,
School of Electrical and Computer Engineering, University of Campinas
(UNICAMP), Campinas 13083-970, Brazil (e-mail: euclides.chuma@
ieee.org).
Thomas Rasmussen is with the Department of Photonics Engineer,
Technical University of Denmark, 2800 Kongens Lyngby, Denmark
(e-mail: thomas.rasmussen@ibsen.com).
Digital Object Identifier 10.1109/JSEN.2022.3202708
of “smart” sensors [4], [5] for several sensing applications and
diverse sensing modalities to gain a more holistic understand-
ing of objects and scenarios being monitored.
Different types of sensors are used in diverse practi-
cal applications, such as the industry [6], [7], medical
diagnostics [8], [9], [10], energy solutions [11], infrastruc-
ture [12], [13], [14], and agriculture [15]. It is important to
mention that sensor manufacturing technology is constantly
improving mainly through miniaturization techniques and new
materials [16], [17], [18], [19].
A case that can be analyzed involves the demand for
improved food safety and quality, which has been accompa-
nied by advancements in technology. Sensors and methods for
food quality evaluation are critical for ensuring food safety
and avoiding malpractices such as adulteration [20].
Near-infrared (NIR) spectroscopy is based on the absorption
of electromagnetic radiation at wavelengths in the range of
780–2500 nm [21], [22]. It has attracted increasing atten-
tion in the food processing industry because of its low
operational costs and because it does not require sample

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CHUMA AND RASMUSSEN: METAMATERIAL-BASED SENSOR INTEGRATING MICROWAVE DIELECTRIC AND NIR SPECTROSCOPY
preparation. Moreover, it is used in the food processing
industry for the compositional, functional, and sensory analy-
ses of food ingredients, process intermediates, and final
products [23], [24], [25]. It is also used in petrochemical
and refinery [26], pharmaceutical [27], and agricultural [28]
industries.
Recently, microwave dielectric spectroscopy has attracted
attention for several applications. It measures the dielectric
properties of a material as a function of microwave frequency
(1–100 GHz) [29]. Applications of microwave dielectric spec-
troscopy are commonly found in the food [30], fuel [31], and
agricultural [32] industries.
This article presents a novel metamaterial-based sensor that
integrates NIR spectroscopy and microwave dielectric spec-
troscopy in the same physical structure and simultaneously
performs measurements in different regions of the electromag-
netic spectrum.
The diversity of the electromagnetic spectra analyzed
(NIR and microwave regions) by the proposed sensor leads to
better accuracy in the identification of substances with fewer
samples for training ML classification algorithms.
In addition, NIR spectroscopy and microwave dielectric
spectroscopy have been considered solutions for identifying
olive oil adulteration [33], [34]. Therefore, the proposed sensor
was evaluated to identify pure olive oil from other oils and
olive oil adulterants.
Other techniques for identifying adulteration in olive oil are
already well known and used, as in the case of UV/Vis spec-
troscopy [35] and FTIR spectroscopy [36]. Other techniques,
such as the use of a “colorimetric sensor array,” are being
proposed [37] with good results.
Adulteration in olive oil was chosen to evaluate the proposed
sensors because olive oil production is a costly process that
increases the cost of the final product. Consequently, olive oil
is widely adulterated with other cheap edible oils, such as
sunflower and canola oils.
II. T HEORY AND S ENSOR D ESIGN
A. Adulteration of Extra Virgin Olive Oil
Owing to its high added value, the olive oil industry has
been subject to fraudulent activity. Extra virgin olive oil,
which is the highest quality olive oil, is the most adulterated.
Most consumers may not be able to detect whether a product
that is labeled as extra virgin is authentic, or whether it is
refined or mixed to some degree with other lower-quality
oils.
Typically, the adulteration of extra virgin olive oil consists
of the addition of and/or substitution with other types of edible
oils or lower-quality olive oils [37].
Edible vegetable oils are primarily composed of different
proportions of the same or similar fatty acids [38]. When
extra virgin olive oil and edible oil are mixed, the resulting
oil consists of the fatty acids and other compounds from both
oils [39].
The NIR spectrum of olive oil has previously been described
in the literature [40]. One is the absorption peaks at 1660 nm,
which is related to the C-H vibration-related and contains
information about fatty acid composition [41]. A broad
absorbance band can be observed at 1210 nm as a result of
second overtones of C–H and CH=CH– stretching vibrations.
These spectral regions show spectral features characteristic of
vegetable species. Broadband at 1400 nm has been related to
the presence of water.
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19309
B. Operating Principle of the Sensor
The operating principle of the proposed sensor is as follows.
The substance to be analyzed is inserted into a quartz cuvette
that passes through the CSRR of the sensor and determines
a specific resonance frequency in S21 . In the same sensor,
an optical path passes through the substance to be analyzed
in the cuvette. A broadband NIR light source is inserted into
a hole in the optical path, and the light passes through the
substance. At the other end of the optical path, the light passing
through the sample is measured using an NIR spectrometer.
The resonance frequency S21 and the data from the
NIR spectrometer were joined and processed by a trained
ML classification algorithm that determined whether the sub-
stance in the cuvette was extra virgin olive oil with high
accuracy.
In this study, classification algorithms, such as the neural
network classifier, naive Bayes Gaussian, k-nearest neighbors
(KNNs), and support vector machines (SVMs) were used.
C. Near-Infrared Spectroscopy
NIR spectroscopy is based on the absorption of electromag-
netic radiation at wavelengths in the range of 750–2500 nm
(13 333 to 4000 cm−1 ) [21], [22].
The NIR spectra comprise broadbands arising from overlap-
ping absorptions that primarily correspond to overtones and
combinations of vibrational modes involving C-H, O-H, and
N-H chemical bonds [42], [43]. Therefore, in principle, the
concentrations of constituents, such as water, protein, fat, and
carbohydrates, can be determined using NIR spectroscopy with
chemometric techniques [44].
NIR spectroscopy has a highly complex theoretical descrip-
tion of anharmonic effects that are inherent to it and thus
necessarily involves complex approaches [21] since the anhar-
monic model considers some nonideal behaviors of the oscilla-
tor which account for the repulsion between electronic clouds
when the atomic nucleus approaches and variable behavior
of the bond force when the atoms move apart from one
another.
The O-H and C-H bonds have stretching modes that can be
approximated using anharmonic vibration modes.
A theoretical approach useful for NIR spectroscopy requires
an anharmonic approach. These can be obtained by solving the
vibrational Schrödinger equation, as reported recently [45],
which employed the numerical solution of the 1-D vibrational
Schrödinger equation for selected vibrational modes [46]
 
h̄ 2 d 2
H ψν (q) = − + V (q) ψν (q) = E ν ψν (q) (1)
2μ dq 2
where h̄ 2 denotes Planck’s constant divided by 2π, and q,
μ, V (q), and v (q) denote the normal coordinate, reduced
mass, vibrational potential of the given molecular oscillator,
and wave function, respectively.
The correlation between the NIR profiles and the quality
parameters of olive oil clearly demonstrates that the quality
parameters of oils can be used to detect adulteration in olive
oil [33], [35].
NIR spectral analysis was employed to predict quality
parameters of vegetable oils, primarily olive oils and com-
binations with corn oil, sunflower oil, and raw olive residue
oil adulteration in extra-virgin olive oil [47].
19310
Fig. 1. Example of a CSRR geometry and its equivalent circuit model.
Fig. 2. Dimensions of the proposed sensor in perspective view.
D. Dielectric Spectroscopy
The use of dielectric spectroscopy to determine the quality
of food has been studied for applications in different types of
food [48], including olive oil [49].
When the substance is inserted into the cuvette that passes
through the CSRR of the proposed sensor, the molecules of
the substance lead to the change in the properties of the
electromagnetic field of the CSRR and the S21 resonance
frequency.
The CSRR metamaterial-based structure was coupled with a
microstrip transmission line present on each face of the PCB.
The region near and inside the CSRR is sensitive to dielectric
changes and can be used to measure the complex permittivity
of a material. The equivalent circuit model of the CSRR cell
is illustrated in Fig. 1 [50].
The resonance frequency of the circuit model depicted in
Fig. 2 is given by the following equation [51]:
1 in the electric and magnetic fields, and it is still possible
fr = √ .
2π L r (Cc + Cr )
The Q factor of the resonance is as follows:
 III. FABRICATION AND M EASUREMENT
Cr + C C
Q=R . (3)
Lr
The capacitance, Cr , is affected by the materials placed near
and inside the CSSR
Cr = C0 + εsample Ce
where C0 denotes the capacitive effect of the dielectric sub-
strate of the CSRR, empty glass capillary tube, and near
space, εsample indicates the complex permittivity of the liquid
sample, and Ce corresponds to the capacitance of the quartz
cuvette.
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IEEE SENSORS JOURNAL, VOL. 22, NO. 20, 15 OCTOBER 2022
Fig. 3. Dimensions of the proposed sensor in ground plane (CSRR) and
microstrip line plane.
E. Sensor Design
The sensor proposed in this study was designed to operate
at approximately 1.1 GHz. Therefore, the dimensions of the
CSRR were calculated to resonate at 1.1 GHz. Figs. 2 and 3
present the dimensions of the proposed microwave sensor,
which were calculated using electromagnetic simulations with
ANSYS HFSS software.
To verify the influence of the cuvette on the substance in
the proposed sensor, simulations were performed in an E-field
with and without olive oil, as demonstrated in Figs. 4 and 5,
respectively.
From an analysis based on the simulation vectors of the
electric field (see Figs. 4 and 5), it can be concluded that
the cuvette with olive oil placed in the sensor causes changes
(2) to use the sensor with its CSRR resonance structure and its
transmission line.
To validate the operation of the sensor, it was fabricated
by employing a PCB using lithography, which is commonly
employed in the PCB industry. Fig. 6 presents a microwave
sensor prototype fabricated using an SMA connector.
The substrate used for fabrication is Rogers TMM1 3, which
has ε = 3.27, tan δ = 0.002, and a thickness of 5.08 mm.
(4) The samples were placed in a quartz cuvette with a volume
of 3.5 mL and internal dimensions of 45 × 10 × 10 mm.
To obtain the S21 frequency resonance, a vector network
analyzer (VNA, HP8714B) connected with a 10-MHz external
precision reference clock from Lucent was used to obtain
1 Registered trademark.
CHUMA AND RASMUSSEN: METAMATERIAL-BASED SENSOR INTEGRATING MICROWAVE DIELECTRIC AND NIR SPECTROSCOPY
Fig. 4. Simulations of the proposed sensor with E-field vector with
cuvette without olive oil to analyze the behavior of electric field close
to the cuvette.
Fig. 5. Simulations of the proposed sensor with E-field vector with
cuvette with olive oil to analyze the behavior of electric field close to
the cuvette.
Fig. 6. (a) Ground plane with CSRR. (b) Transmission line plane.
maximum precision and stability in frequency measurements
connected to the sensor. The proposed sensor was connected
to a VNA using coaxial cables.
An Ibsen NIR ultra-compact and cost-efficient spectrometer,
model PBM-400, with 950–1700-nm wavelength range and
12 nm of resolution [52] was used to obtain the NIR spectrum.
The complete experimental setup is illustrated in Fig. 7.
The cost of the sensor is relatively low, as it basically
consists of manufacturing a PCB with a quartz or glass
container. The equipment that performs the measurements of
the sensor (NIR spectrometer and the VNA) is still relatively
expensive because it is a laboratory equipment, but it can be
replaced by a simpler and cheaper dedicated device.
We performed 25 measurements of different samples of oil
types and providers: ten samples of olive oil, two samples of
soy oil, two samples of corn oil, two samples of canola oil,
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19311
Fig. 7. Setup used to conduct measurements using the proposed sensor
connected to the VNA and NIR spectrometer.
two samples of sunflower oil, one sample of 10% soya oil
mixed with 90% olive oil, two samples of 75% sunflower
oil mixed with 25% olive oil, two samples of 50% sunflower
oil mixed with 50% olive oil, and two samples of 25% sun-
flower oil mixed with 75% olive oil.
In order to ensure that the olive oils were of high quality,
only olive oils with acidity <0.5% were used.
In summary, ten samples comprised extra virgin olive oil,
whereas 15 did not comprise extra virgin olive oil. The small
number of samples is useful for testing the efficiency of the
proposed sensor, which is one of the distinct features of the
sensor proposed in this work.
The sample measurements were divided into two groups:
the training dataset with 21 samples and the test dataset with
four samples, and the training dataset with 14 samples and
the test dataset with 11 samples. In total, 25 samples were
obtained.
For each oil sample, the S21 (transmission response) curve
was obtained using the VNA, and the transmittance in the NIR
spectrum was obtained using an NIR spectrometer. The mea-
surements were conducted at 25 ◦ C. Fig. 8 shows examples of
S21 measurements of olive oil and mixtures of olive oil with
sunflower oil samples.
IV. R ESULTS
A. Data Pretreatment
First, the raw NIR spectra were subjected to a standard
normal variate (SNV) preprocessing step to eradicate the
offset [53]. The SNV method normalizes the spectra by
subtracting each spectrum by its mean and dividing it by
its standard deviation. The same procedure was adopted for
S21 microwave frequency resonance measurements.
Thus, NIR spectral data and S21 microwave frequency
resonance data were incorporated into the training and test
datasets. The training dataset for ML had 21 rows with
19312
Fig. 8. Example of the S21 measurements of olive oil and mixtures of
olive oil with sunflower oil samples.
TABLE I
ACCURACY OF THE P ROPOSED S ENSOR W ITH AND
W ITHOUT M ICROWAVE D IELECTRIC P ROPERTY
122 columns (features), which were the intensities for each
wavelength/frequency. The test dataset has four rows with
122 columns (features).
The dataset was analyzed using ML classification
algorithms to identify authentic olive oils. ML tests were
performed using the classification learner application imple-
mented in MATLAB R2021a.
B. Results
To study the efficiency of the proposed sensor for identify-
ing olive oil using ML algorithms, four predictive modeling
approaches were used: neural network classifier, naive Bayes
Gaussian, KNN, and SVM linear.
The neural network classifier used had one connected layer
with a size of 10, ReLU activation, and an iteration limit of
1000. To avoid overfitting, we used a k-fold cross-validation
with five cross-validation folds.
To analyze the impact of microwave dielectric property
on test accuracy, 2 approaches were used: NIR spectrum
with (122 characteristics) and without (121 characteristics)
microwave dielectric spectroscopy data.
Table I presents the accuracy of the proposed sensor with
and without microwave dielectric properties. The test accuracy
was obtained with 14 and 21 samples training and using
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IEEE SENSORS JOURNAL, VOL. 22, NO. 20, 15 OCTOBER 2022
Fig. 9. Test ROC curve of positive class for the neural network classifier
using the training dataset with 14 samples and tested with 11 samples.
Fig. 10. Test confusion matrix for TPR (sensitivity) and FNR (specificity)
using neural network classifier.
a neural network classifier, naive Bayes Gaussian, KNN, and
SVM algorithms to identify olive oil adulteration.
From Table I, it can be concluded that the neural network
classifier and naïve Bayes Gaussian algorithms achieved a test
accuracy of 100% when trained with 14 samples and using
microwave dielectric properties. Without microwave dielectric
properties, it was not possible to achieve 100% accuracy using
only 14 samples.
The analysis of Table I also shows that all algorithms
achieved a test accuracy of 100% when trained with 21 sam-
ples and using microwave dielectric properties.
Fig. 9 shows the test ROC curve of positive class for
the neural network classifier using the training dataset with
14 samples and the test dataset with 11 samples.
The proposed sensor using the neural network classification
algorithm has an area under the ROC curve (AUC) of 0.91.
The higher the AUC, the better the model is at predicting the
probability of correctly identifying the olive oil adulteration.
Fig. 10 shows the test confusion matrix for true positive
rates (TPRs, also called sensitivity) and false negative rates
(FNRs, also called specificity).
Table II presents a comparison of the performance of the
proposed sensor with other works using other methods to
identify adulteration of olive oil.
CHUMA AND RASMUSSEN: METAMATERIAL-BASED SENSOR INTEGRATING MICROWAVE DIELECTRIC AND NIR SPECTROSCOPY
TABLE II
C OMPARISON B ETWEEN THE P ROPOSED S ENSOR AND O THER W ORKS
FOR I DENTIFICATION OF O LIVE O IL A DULTERATION
Fig. 11. Accuracy and quantity of samples for training for different
spectroscopy methods.
From Table II, it can be concluded that the proposed sensor
achieves the best accuracy (100%) using only 14 samples to
train a neural network classification algorithm, while FTIR
spectroscopy [52] requires 40 samples to reach 85%.
With 14 training samples, the proposed sensor achieved
100% accuracy, and FT-NIR spectroscopy with BOSS-PLS
required 50 samples to achieve the same 100% accuracy. The
UV/Vis spectroscopy [34] (the simplest technique) with SVM
required 342 samples to achieve 98% accuracy.
Fig. 11 shows the accuracy and quantity of samples for
training for different spectroscopy methods. The current work
presents 100% accuracy using only 14 training samples.
Therefore, it is necessary 72% fewer samples for training the
proposed sensor compared with FT-NIR [55] (100% accuracy
using 50 samples for training). This implies a reduction in
computing requirements and wall clock time.
V. C ONCLUSION
The proposed metamaterial-based sensor that integrates
microwave dielectric and NIR spectroscopy techniques for
substance evaluation was tested with success in identifying
olive oil adulteration, with fewer samples, using the training
ML classification algorithms.
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19313
Using data from microwave dielectric spectroscopy com-
bined with NIR spectroscopy, the proposed sensor offers a
greater diversity of data from the electromagnetic spectrum,
thereby improving the accuracy of substance identification
with fewer samples to train ML classification algorithms.
To evaluate the performance of the proposed sensor,
ML classification algorithms were trained and tested with and
without microwave dielectric data. With microwave dielectric
data, it is possible to achieve 100% accuracy with only
14 training samples using the neural network classification
algorithm. Therefore, the proposed sensor needs 72% fewer
samples for training classifier algorithms used in olive oil adul-
teration identification. This implies a reduction in computing
requirements and wall clock time.
The proposed sensor could successfully identify olive oil
adulteration. It can also be used to evaluate other substances.
Therefore, the proposed sensor opens new avenues for material
characterization and identification using a combination of
microwave dielectric measurements and NIR spectroscopy in
the same structure.
ACKNOWLEDGMENT
The authors would like to thank Ibsen Photonics Company
for loaning the compact and cost-efficient NIR spectrometer
used in this study.
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Euclides Lourenço Chuma (Senior Member,
IEEE) received the degree in mathematics
from the University of Campinas (UNICAMP),
Campinas, Brazil, in 2002, the Graduate degree
in network and telecommunications systems
from the Instituto Nacional de Telecomunicações
(INATEL), Santa Rita do Sapucaí, Brazil, in 2016,
and the M.Sc. and Ph.D. degrees in electrical
engineering from UNICAMP in 2017 and 2019,
respectively.
He is currently a Ph.D. Researcher working
with microwave and photonics sensors at UNICAMP. He has experience
in the development of software, sensors, electronics, photonics, telecom-
munications, and information technology.
Dr. Chuma is the Chair of the IEEE Sensors Council Chapter South
Brazil, R9.
Thomas Rasmussen is currently pursuing the
Ph.D. degree with the Technical University of
Denmark, Kongens Lyngby, Denmark.
He is the Director of Product Management with
Ibsen Photonics, Farum, Denmark.