TECHNICAL UNIVERSITY OF MOLDOVA

JOURNAL OF ENGINEERING
SCIENCE
Technical and applied scientific publication founded on 9 February 1995
Alternative title: Meridian ingineresc

2022
Vol. XXIX (3)

ISSN 2587-3474
eISSN 2587-3482

TECHNICAL UNIVERSITY OF MOLDOVA (PUBLISHING HOUSE)

„TEHNICA UTM” (PRINTING HOUSE)
According to the Decision of the NAQAER No. 19 from 06.12.2019, JES is classified as
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Main subjects areas of the Journal of Engineering Science:
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• Mechanical Engineering and Technologies
• Applied Engineering Sciences and Management
• Materials Science and New Technologies
• Electrical Engineering and Power Electronics
• Energy systems
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• Industrial and Applied Mathematics
• Vehicle and Transport Engineering

B. Electronics and Computer Science

• Electronics and Communication
• Microelectronics and Nanotechnologies
• Biomedical Engineering
• Computers and Information Technology
• Automation

C. Architecture, Civil and Environmental Engineering

• Architecture, Urbanism and Cadaster
• Civil Engineering and Management
• Energy Efficiency and New Building Materials
• Environmental Engineering

D. Food Engineering
• Food Technologies and Food Processes
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• Equipment for Food Industries

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Technical University of Moldova
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 Editorial Board
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Ion Bostan, Dr.hab., Acad. Academy of Science, Republic of Moldova
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Ion Rusu, Dr. hab. Professor, Technical University of Moldova
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Ion Vișa, PhD, Professor University Transilvania of Brașov, Romania
Jorj Ciumac, Dr., Professor, Technical University of Moldova
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Lee Chow, PhD, Professor, University of Central Florida, USA
Leonid Culiuc, Dr.hab., Acad. ASM, Institute of Applied Physic
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Moldova
Mardar Maryna, Doctor of Technical Science, Professor, Odessa National Academy of Food
Technologies, Odessa, Ukraine
Mitrofan Ciobanu, academic MAS, Dr.Sc.,PhD, Professor Tiraspol State University, Chișinău,
Republic of Moldova
Natalia Tislinschi, Dr., Ass. Professor, Technical University of Moldova
Oleg Lupan Dr.hab. Professor, Technical University of Moldova
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Moldova
Peter Lorenz, PhD, Professor University of Applied Science Saar, Saarbrucken, Germania
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Petru Stoicev, Dr.Sc., PhD, Professor, Technical University of Moldova, Chișinău, Republic of
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Polidor Bratu, PhD, academic RATS, president ICECON S.A. București, Romania
Radu Munteanu, PhD, Professor Technical University of Cluj Napoca, Romania
Radu Sorin Văcăreanu, Dr. hab. Professor, Technical University of Civil Engineering Bucharest,
Romania
Sergiu Zaporojan Dr., Professor, Technical University of Moldova
Spiridon Crețu, PhD, Professor Technical University „Gh. Asachi”, Iași, Romania
Eden Mamut, PhD, Professor University „Ovidius” Constanța, România
Stanislav Legutko, PhD, Professor Poznan University of Technology, Poland
Rafał Gołębski, Dr., Ass. Professor, Częstochowa University of Technology, Poland
Stefan Tvetanov, Dr., Professor, University of Food Technologies, Bulgaria
Ștefan-Gheorghe Pentiuc, Dr., Professor, University “Stefan cel Mare” of Suceava, Romania
Svetlana Albu, Dr. hab. Professor, Technical University of Moldova
Thomas Luhmann, Dr-Ing. habil. Dr. h.c. Professor, Jade University of Applied Sciences, Germany
Tudor Ambros, Dr.Sc., PhD, Professor, Technical University of Moldova, Chișinău, Republic of
Moldova
Valentin Arion, Dr.Sc., PhD, Professor, Technical University of Moldova, Chișinău, Republic of
Moldova
Valentina Bulgaru, PhD, Assoc. professor, Technical University of Moldova, Chișinău, Republic
of Moldova
Valeriu Dulgheru, Dr.Sc., PhD, Professor, Technical University of Moldova, Chișinău, Republic
of Moldova
Vasile Tronciu Dr.hab. Professor, Technical University of Moldova
Victor Ababii, Dr. Professor, Technical University of Moldova
Victor Șontea Dr. Professor, Technical University of Moldova
Vilhelm Kappel, PhD, Institute of Research INCDIE ICPE-CA, Bucharest, Romania
Vladimir Zavialov, Dr. hab., Professor, National University of Food Technology, Ucraine
Vladislav Resitca, Dr., Ass. Professor, Technical University of Moldova
Yogendra Kumar Mishra, Dr. habil., Kiel University, Germany
Yuri Dekhtyar, Professor, Riga Technical University, Riga, Latvia

Responsible Editor
Dr. hab. Rodica STURZA
Editorial Board address: [email protected]
Editorial Production:
Dr. hab. Aliona Ghendov-Moșanu
Dr. Nicolae Trifan
Dr. Țurcan Iuliu
Dr. Svetlana Caterinciuc
Dr. Rodica Cujba
 CONTENT

A. Industrial Engineering

Vasile Plămădeală Driving tiredness – the end enemy of the driver ................................... 9

Adinife Patrick Azodo,

Olasunkanmi Salami
Objective approach in investigating implication of road vehicle tyre
Ismaila,
safety knowledge on compliance ............................................................... 23
Titus Y. Jibatswen,
Owoeye Femi Timothy

B. Electronics and Computer Science

Stefan Schröder,
Nicolae Magariu,
Thomas Strunskus, New vapor deposited dielectric polymer thin films for electronic
Nicolai Ababii, applications ..................................................................................................... 34
Oleg Lupan,
Franz Faupel

Dumitru Tsiulyanu,
Olga Mocreac, Gas sensitive films based on Te-SnO2 nanocomposite on flexible
Andrei Afanasiev, substrate .......................................................................................................... 45
Eduard Monaico

Anas Shehu,
Application of privacy-preserving data publishing in tertiary
Alhassan Salihu,
institutions of Kebbi State using generalization and suppression .... 59
Abubakar Sani

Victor Moraru,
Interest based adaptive billboard content management ..................... 70
Viorel Cărbune

Ana Turcan,
Victor Ababii,
Viorica Sudacevschi,
Radu Melnic, Smart City Services based on Spatial-Temporal Logic......................... 78
Victoria Alexei,
Silvia Munteanu,
Constantin Ababii

Arun B. Mathews, A novel classification with deep convolutional neural networks on

Krishna Prasad K. pulmonary nodule.......................................................................................... 86

Artur Buzdugan Nanotechnology: reflections on health benefits and risks .................. 93

C. Architecture, Civil and Environmental Engineering

Photovoltaics solutions and energy communities in a clean energy

Cristina Efremov
roadmap ........................................................................................................... 110
 Chukwuka Ezemenike,
Olugbenga Oyedepo,
Olufikayo Aderinlewo, Rheological characterization of industrial waste modified bitumen 126
Isiaka Oladele,
Omoniyi Olukanni
Aremanda Ramesh
Babu, Tekle Arsiema ,
Daniel Heaven , Physicochemical characterization of Asmara Brewery effluents........ 136
Berhane Filmon,
Mehari Abiel

D. Food Engineering

Buhari U. Umar,
Olayemi M. Olaniyi,
Recent advances in smart kitchen automation technologies:
Idris A. Dauda,
principles, approaches, and challenges.................................................... 150
Danlami Maliki,
Cindy P. Okoro

Rodica Siminiuc, Evaluation of gluten contamination of gluten-free products in the

Dinu Țurcanu Republic of Moldova ..................................................................................... 166

Gheorghe Duca,
Olga Covaliova,
Effect of bioactive additives on biomass fermentation from
Ecaterina Covaci,
winemaking sector ........................................................................................ 176
Lidia Romanciuc,
Corina Tașca

Spectral and chromatographic characterisation of the Yellow Food

Alexandra Savcenco
Dye from Safflower ........................................................................................ 189
 CONȚINUT

A. Industrial Engineering

Vasile Plămădeală Oboseala de conducere – dușmanul șoferului ...................................... 9

Adinife Patrick Azodo,

Olasunkanmi Salami
Abordarea obiectivă în investigarea implicației cunoștințelor de
Ismaila,
siguranță a pneurilor de vehicule privind conformitatea.................... 23
Titus Y. Jibatswen,
Owoeye Femi Timothy

B. Electronics and Computer Science

Stefan Schröder,
Nicolae Magariu,
Thomas Strunskus, Noi filme subțiri de polimeri dielectrici obținuți cu vapori pentru
Nicolai Ababii, aplicații electronice ...................................................................................... 34
Oleg Lupan,
Franz Faupel

Dumitru Tsiulyanu,
Olga Mocreac, Filme sensibile la gaze pe bază de nanocompozit Te-SnO2 pe
Andrei Afanasiev, substrat flexibil.............................................................................................. 45
Eduard Monaico

Anas Shehu, Aplicarea publicării datelor pentru conservarea confidentialării în

Alhassan Salihu, instituțiile terțare ale statului Kebbi folosind generalizarea și
Abubakar Sani supresia............................................................................................................ 59

Victor Moraru, Gestionare adaptativă a conținutului panoului publicitar bazat pe

Viorel Cărbune interese ............................................................................................................ 70

Ana Turcan,
Victor Ababii,
Viorica Sudacevschi,
Radu Melnic, Servicii Smart City bazate pe Logica Spațial-Temporală .................... 78
Victoria Alexei,
Silvia Munteanu,
Constantin Ababii

Arun B. Mathews, O nouă clasificare cu rețele neuronale convoluționale profunde pe

Krishna Prasad K. nodul pulmonar ............................................................................................. 86

Nanotehnologie: reflecții asupra beneficiilor și riscurilor pentru

Artur Buzdugan
sănătate ........................................................................................................... 93

C. Architecture, Civil and Environmental Engineering

Centrale fotovoltaice si comunități energetice în cadrul unei foi de
Cristina Efremov
parcurs pentru o energie curată ................................................................ 110
 Chukwuka Ezemenike,
Olugbenga Oyedepo,
Caracterizarea reologică a deșeurilor industriale de bitum
Olufikayo Aderinlewo,
modificat.......................................................................................................... 126
Isiaka Oladele,
Omoniyi Olukanni
Aremanda Ramesh
Babu, Tekle Arsiema,
Daniel Heaven, Caracterizarea fizico-chimică a efluenților berăriei Asmara .............. 136
Berhane Filmon,
Mehari Abiel

D. Food Engineering

Buhari U. Umar,
Olayemi M. Olaniyi,
Progrese recente în tehnologiile inteligente de automatizare a
Idris A. Dauda,
bucătăriei: principii, abordări și provocări .............................................. 150
Danlami Maliki,
Cindy P. Okoro

Rodica Siminiuc, Evaluarea contaminării cu gluten a produselor aglutenice în

Dinu Țurcanu Republica Moldova ....................................................................................... 166

Gheorghe Duca,
Olga Covaliova,
Efectul aditivilor bioactivi asupra fermentării biomasei din sectorul
Ecaterina Covaci,
vitivinicol......................................................................................................... 176
Lidia Romanciuc,
Corina Tașca

Caracteristica spectrală și cromatografică a colorantului alimentar

Alexandra Savcenco
galben din șofrănel ....................................................................................... 189
Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 9 - 22
Fascicle Industrial Engineering ISSN 2587-3474
Topic Applied Engineering Sciences and Management eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).01
UDC 159.944.4:656.086

DRIVING TIREDNESS – THE END ENEMY OF THE DRIVER

Vasile Plămădeală*, ORCID: 0000-0003-1722-2649

Technical University of Moldova, 168 Stefan cel Mare Blvd., Chisinau, Republic of Moldova
*Corresponding author: Vasile Plămădeală, [email protected]

Received: 07. 01. 2022

Accepted: 08. 10. 2022

Abstract. In modern society, little or no sleep at all has become a habit, almost a good
tradition. Fulfilled sleep is one of the key factors of a healthy lifestyle and longevity, along
with proper nutrition, physical activity and that one is fighting stress. Driver fatigue reduces
the level of traffic safety, having a negative impact on all psychophysical qualities. Fatigue
at the wheel, like driving under the influence of alcohol, is a major factor in road accidents
and should not be neglected, regardless of the experience of the driver, the car driven or, the
road he travels. A moment of inattention at the wheel can turn the driver, passengers or other
innocent people into a simple statistics of road accidents. The article describes the signs and
causes of fatigue, measures to prevent and restore the driver's work capacity, as well as
warning systems introduced by several manufacturers on keeping the car on the lane,
monitoring the driver's fatigue etc.

Keywords: driving fatigue, fatigue, road accidents, traffic accidents, drowsiness, car safety systems.

Rezumat: În societatea modernă, a dormi puțin sau a dormi insuficient a devenit un obicei,
aproape o tradiție bună. Somnul împlinit este unul dintre factorii cheie ai unui stil de viață
sănătos și longevitate de trai, împreună cu o alimentație adecvată, activitate fizică și luptă cu
stresul. Oboseala conducătorului auto reduce nivelul de siguranță a traficului, având un
impact negativ asupra tuturor calităților psihofizice. Oboseala la volan, ca și conducerea sub
influența alcoolului, este un factor major în producerea accidentelor rutiere și nu trebuie
neglijată, indiferent de experiența pe care o are conducătorul auto, de automobilul condus
sau de drumul pe care se deplasează. O clipă de neatenție la volan îl poate transforma pe
conducător, pe pasageri sau pe alți oameni nevinovați într-o simplă statistică a accidentelor
rutiere. În articol sunt descrise semnele și cauzele stării de oboseală, măsurile de prevenire
și restabilire a capacității de muncă a conducătorului, precum și sistemele de avertizare
introduse de mai mulți constructori privind menținerea automobilului pe banda de circulație,
de monitorizare a stării de oboseală a conducătorului etc.

Cuvinte cheie: oboseala la volan, stare de oboseală, accidente rutiere, accidente de circulație,
stare de somnolență, sisteme de siguranță a automobilului.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

10 V. Plămădeală

1. Introduction
There is no clear definition of the term „fatigue”. The term defines different meanings:
physical – the result of hard physical or mental work, neurobiological – determined by the
rhythm of sleep-wake cycles and mental/psychological – lack of energy needed to do
something alternatively, demotivating the continuation of an action.
Fatigue also has many direct and indirect causes [1]. It is often directly associated with
the period of time in which a person performs certain activities. Fatigue is also due to lack of
sleep, which can be chronic or acute. Fatigue or drowsiness can occur without sleep. This
type of fatigue is usually related to the daily cycle of sleep, or biorhythm, meaning that within
24 hours, the human body needs sleep several times. It takes place in the prolonged
mornings, approximately between midnight and four o'clock in the morning or after 12 hours
later, between 1400-1600.
Among the factors with indirect influence on fatigue can be considered the following:
age, physical condition, habit of consuming alcohol, drugs, medications or external factors,
such as: temperature, noise, vibration, routine of work. For example, driving alone on a boring
road for a long time does not cause fatigue or drowsiness, but can lead to the rapid
manifestation of their effects. Fatigue [2, 3] is the natural process of temporary reduction of
work capacity, which occurs as a result of human activity. The work capacity of the driver
depends on the condition of the central nervous system. As a result of overwork of the brain,
disorders occur in the evolution of mental processes, perception, attention, thinking and
memory are affected. Moreover, it reduces the acuity of vision, narrows the visual field,
worsens stereoscopic vision, confuses the precision of movement coordination, reduces the
degree of automatism, intensifies the pulse, increases blood pressure and reaction time,
disappears the sensation of speed, apathy and asthenia appear, so that the ability to react
quickly to unexpected and unusual changes in traffic situations is lost.
Vision fatigue is directly dependent on the duration of the driver's work. It was found
that, after eight hours of uninterrupted work, the driver can visually perceive the road sign
not from a distance of 100 m, but only from 80 m [2]. Visual fatigue has a negative effect on
the driver's activity. Even experienced drivers, being tired, reduce the radius of visibility;
direct the view in front of the vehicle and on the side of the road, which makes it difficult to
forecast traffic situations. Only simple skills chiseled to the level of automatism are
maintained in a state of fatigue, which gives possibilities to act only in known, standard
situations. All these mentioned considerably reduce the reliability of the driver; contribute to
the commission of errors and road accidents.
The tired driver involuntarily changes his working position: an improper seat is
noticed, that makes it difficult to use the steering wheel, pedals and on-board devices, as
well as worsens visibility. The driver with obvious signs of fatigue often loses the accuracy of
driving actions, more often than usual he turns the steering wheel from side to side. Fatigue
worsens with increasing energy consumption, as a result, serious errors begin to occur.
Signs of characteristic fatigue are noticed at drivers after 4...5 hours of driving, become
clearly visible after 6…8 hours of driving, and after 9 hours, strong efforts must be made to
drive the vehicle safely [4]. After 9 hours, the risk of a car accident increases. Sad practice
shows that more than half of road accidents are caused by tired drivers. The tired driver may
not feel tired under the influence of strong psycho-emotional arousal or danger.
The driver, who is beginning to feel tired, may initially drive the vehicle safely, but not
for long. Falling asleep or drowsiness usually occurs instantly and unexpectedly, creating a

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Driving tiredness – the end enemy of the driver 11

very dangerous situation on the road. Therefore, you do not have to fight drowsiness, but it
is recommended to stop and sleep, or to do some exercise. The most effective way is to get
out of the car for a few minutes and relax your muscles.
It is known that the aromas of coffee, lemon, mint and cinnamon remove fatigue, have
a beneficial effect on the brain and bring the human body into an active state. Air flavors and
lollipops with such flavors are beneficial. It also helps remove drowsiness, music, audio books
and conversations with passengers. The open window of the cab allows fresh and cold air to
enter, which invigorates the driver.
Every driver should know that driving a tired vehicle is one of the main causes, leading
to road accidents from simple bumps to serious and particularly serious ones. Statistics show
[2] that drivers who drive a vehicle without breaks for 7…12 hours as a result of drowsiness,
are involved in road accidents approximately twice as often, and if the duration of driving
exceeds 12 hours, the frequency of driving in road accidents increases 9 times. The driver
must rest at least 8 hours before the working day, as drivers who sleep only 6 hours at the
end of the working day have less than 2,5 times less attention. Also, according to statistics,
60% of overworked drivers are already asleep at the wheel after 3…4 hours of work.

2. Statistical data on the driver's fatigue

In order to better assess the effects of drowsy driving, some statistical data are
presented below [5]:
• if the duration of sleep for 24 hours is less than 6 hours, the risk of drowsiness,
which can lead to a car accident, increases 3 times;
• 18 hours of wakefulness in a row leads to a condition comparable to alcohol
intoxication;
• $ 12,5 billion – this is the annual loss of US money due to road accidents, caused
by drowsiness while driving;
• 37% of drivers said that they fell asleep at least once while driving;
• it is estimated that 1550 deaths each year are caused by road accidents caused by
drowsy drivers;
• 15% of serious road accidents involving trucks are attributed to driver fatigue;
• 55% of road accidents resulted of fatigue are caused by drivers up to the age of 25.
The mentioned figures refer to the USA, but they can also be successfully included in
the sad statistics of road accidents in the Republic of Moldova.
Driver fatigue leads to a much higher number of road accidents than it previously was
believed. The risk group included young people aged 18-20: they often go to bed late at night,
but have to wake up early in the morning. In this category of drivers, signs of fatigue are more
common during the day than at night.
According to the study conducted by specialists from the Polytechnic Institute of
Transportation in Virginia, USA [6], the number of road accidents caused by driver fatigue is
close to 20% of the total number, so it does not constitute 2-3%, as previously established
other studies and surveys on similar topics. The study, called the „100-car naturalistic study”,
was conducted over two years with the participation of the State Department of Transportation
and the US National Road Safety Administration. The study allowed close monitoring of leaders
without direct involvement in their lives.
The study involved 100 car owners from Virginia and Washington: five cameras were
installed on their cars, collision warning systems in the front and rear of the car, several

Journal of Engineering Science September, 2022, Vol. XXIX (3)

12 V. Plămădeală

accelerometers, belt traffic monitoring systems and a network sensor. For the research, the
Institute's specialists tried to attract as many drivers up to the age of 25 as possible, as well
as motorists whose annual journey is higher than the national average.
With the help of the study, it was possible for the first time to follow the behavior of
drivers before the accident. In 20% of all road accidents and in 16% of all situations close to
the accident, drivers showed obvious signs of fatigue: closed eyes, „nibbling” with the nose,
„disconnection” of facial muscles, as well as moments of microsleep, when the driver's eyes
close slowly, and open immediately.
During the study, experts analyzed 110000 situations in which drivers were involved.
Of these, 10500 cases were particularly important, when drivers were involved in a car
accident (82 times) or managed to avoid a car accident (761 times), as well as emergencies
(8200 times) and other potentially dangerous situations – for example, the driver did not stop
at the „no-stop crossing” sign (1400 times).
The European Commission, together with the International Road Transport Union (IRU),
has conducted a unique scientific study of the causes of road accidents. The aim of this study
was to identify the main causes of road accidents with the involvement of trucks. To this end,
teams of experts were involved in the study of over 600 road accidents in 7 European
countries (France, Germany, Italy, Hungary, the Netherlands, Slovenia and Spain) [7].
Of the 624 road accidents investigated in 6% of cases, driver fatigue was the main
cause of the road accident. 37% of such road accidents had a fatal end. In 68% of the
situations, in which fatigue is the main cause of the road accident, the truck and another
vehicle were involved in the accident, and in 29% of the cases, only the truck.
Regarding the time of day, when an accident occurred due to the driver's fatigue, two
critical periods of time were identified. Most accidents occurred between 200 and 300 at night
– the time when the driver's biorhythm is at its lowest point, as well as between 1500 and
1600 – almost at the end of the working day. Almost 90% of all road accidents caused by
driver fatigue occurred on highways or roads between localities. In localities, road accidents
due to the driver's fatigue are extremely rare.
Most drivers overestimate themselves when it comes to long driving distances, often
ignoring fatigue. Many fatal accidents occur a few kilometers from the destination, due to the
fact that the driver is confident that he will resist. A study conducted in the UK showed that
many drivers drive tired, but very few of them resort to measures to protect them from that
critical level, which puts them in great danger [8]. The study shows that 70% of drivers prefer
to open a window and drive on, while 69% take short breaks to refresh them. 54% of leaders
listen to music to stay awake and only 21% stop for a few minutes of sleep, 43% resort to
various caffeinated beverages. Of those who stop for refreshment, 39% resort to short walks
and only 21% fall asleep for a few minutes.

3. Signs of driver fatigue and circumstances of accelerated fatigue

One of the most important issues regarding road safety is to reduce and avoid driver
fatigue. Of great practical importance, it is of concern to many renowned scientists around
the world. The more tired the man, the lower his production rates and the higher the
probability of serious road accidents.
In such cases, from the point of view of medicine, the events take place according to
a certain scheme [9]. About halfway through, the driver feels very tired and begins to fall
asleep. Due to the tense pursuit of the road, eye pain occurs, the eyelids become heavy as

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Driving tiredness – the end enemy of the driver 13

lead. Coffee or tea served before departure has no stimulating effect, does not help the sound
of the radio or conversations with passengers. The reaction becomes slowed down to the
rapid changes of the situation, the pulse rate decreases and for a few fractions of a second a
euphoric sleep appears. After the blows, the consciousness clears for a few moments, then
drowsiness reappears, but now for a longer period of time. This is the cause of the tragedy.
The only way to avoid this tragedy is to stop and fall asleep for a while or give up driving.
Recognition of signs of fatigue is manifested by [3, 10]: difficulties in concentrating
attention, keeping eyes open or head up, daydreams and the appearance of random thoughts,
the tendency to have hallucinations, especially at night, the sensation of sand in the eyes,
and their repeated need to rub, the need to blink more often, and the tears of the eyes, the
weakening of coordination between movements, the attenuation of the ability to operate
commands, the sensation of weight in hands, feet and eyelids, prolonged and frequent
yawning, driving in zigzag and omission of road signs or indicators, anxiety or irritation, etc.
Among other manifestations of fatigue: headaches, feeling of lethargy and weakness
throughout the body, yawning, unwillingness to communicate with someone.
Although the movements necessary to drive the vehicle are easily performed as a
result of accumulated skills and physical effort, without difficulty covered by the driver's
energy resources, driving activity, carried out with tension and continuous attention, tires the
nervous system of the subject, the fatigue process being accelerated of a number of
circumstances. Among these are [3, 9-11] external causes: the monotony of some roads and
the landscape, the known character of the itinerary, the intense rhythm of the traffic, the
driving in the evening and especially at night with intense traffic in the opposite direction
way etc.; causes depending on the vehicle: uncomfortable or inadequate seats, awkward
position while driving, uniform engine noise, rocking motion of the vehicle, heat in the cab,
inadequate or incomplete ventilation of the passenger compartment, penetration of harmful
gases by technical ventilation or ventilation etc.; causes that depend on the driver: the activity
submitted before driving, driving under the influence of low alcohol consumption, the
influence of drug use contraindicated for driving, prolonged driving time (every fifth car
accident occurs after eight hours of driving), psychological state before going on the road,
immobility of the driver's position, feeling hungry, excessive smoking while driving, driving
with unjustified low speeds, the existence of diseases etc.
All these circumstances often cause sleep, which is why short stops are recommended
when leaving the driving position and exercising, proper ventilation of the cabin, having a
snack or eating sweets etc., all having an effect disconnecting. Among the signs that precede
sleep may be: a pleasant state of lethargy; drowsiness for a short time, during this time the
eyes are open and the gaze is fixed forward, but does not perceive anything; the waking state
is completely annihilated; the muscles of the hands and feet relax; the trajectory of the
vehicle becomes unpredictable, etc. These signs appear in the early hours of the morning or
at the end of the program, when the state of fatigue reaches maximum values.
Driving fatigue during driving is manifested by dispersed attention, abnormal reactions
to external stimuli, decreased ability to coordinate movements, accuracy and speed of
reactions, increased reaction time. The driver who is tired makes an effort to be careful and
focused. He notices that he no longer clearly observes the signs, the markings, and he
perceives the traffic situations late. To concentrate, the driver consumes the last reserves of
physical and mental energy.
Fatigue is a natural process of temporary decrease in work capacity, caused by long or

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14 V. Plămădeală

great effort, but this condition disappears after a good rest, when work capacity is fully
restored. Dangerous is the state of over fatigue, over fatigue, i.e. the accumulation of fatigue,
which can suddenly manifest itself in a sick state.
Over fatigue is harmful and must be prevented. At the same time, moderate fatigue
increases work capacity. If the man is tired at work to the right extent, then he has a good
appetite and a good night's sleep. Therefore, it is necessary to know and forecast the
functional possibilities, the time of onset of fatigue.
It should be noted that, under road law [12], it is forbidden to drive in an advanced
state of fatigue, which affects the driving ability of the vehicle.
At the same time, it is necessary to take into account the experience of driving, keeping
in mind that if you have not driven for a long time, then the first trips are accompanied by
excessive physical and emotional stress. These emotions are manifested by tightening the
steering wheel, following the road carefully and, as a result, static tension, which leads to
rapid fatigue. These actions are also characteristic to novice drivers. In parallel with physical
tasks, the human information request must be dosed. Lying down all day, doing nothing, for
people with strong, mobile nervous system (blood) can be much harder than intense muscle
activity. Both monotony and excess of information lead to fatigue. The monotony of the task
causes the permanent tension of some and the same centers of the nervous system and this
the nervous fatigue develops. The same legitimacies are noticed when poor information
request. During the movement on the highway and in the conditions of an information deficit,
the situation appears when the driver's eye fulfills one and the same thing – it follows the
road. In this case, the same visual centers of the brain are permanently included in the activity
and the uniformity of visual perception causes the development of fatigue in the centers of
the brain, and the appearance of the inhibition state of some groups of nerve cells causes
drowsiness. The lack of information can also be the cause of falling asleep at the wheel.
Fatigue and psychological stress are more pronounced at night, especially if the driver
is blinded by car lights, moving in the opposite direction. Roads on which there are trees or
poles placed at regular intervals also amplify this aspect. In addition to the feeling of
monotony, the driver may enter a state in which sight and hearing are slightly reduced, or at
least not as effective as normal. At night, fatigue can turn into a state of drowsiness, this
being a very dangerous phase, both for drivers and passengers. This condition can be
exacerbated due to situations where uneven surfaces are present on the road. Driving a car
at night on a less crowded road, where there are no traffic signs, can also have a negative
impact on the driver. A feeling of loneliness may set in, and the driver will be tempted to
accelerate to a seemingly safer place. As a result, with acceleration, there is a high risk of
losing control of the steering wheel or getting involved in a collision with another vehicle.
It is recommended to drive a car with a companion or to share driving hours with
another driver, when it comes to very long roads and especially at night. Of course, the person
on the right does not have to sleep, as this is contagious. Autopilot (Adaptive Cruise Control)
is perhaps the worst choice when the driver is drowsy. It significantly reduces the interaction
with the car, thus further accentuating the state of drowsiness.
Roads covered with snow or ice, water or wet can also cause difficulties, as the driver
is subject to increased energy consumption. The arrhythmic movements of the wipers, the
poor lighting of the headlights can also increase fatigue and reduce the level of attention
while driving. The same weakening effect can be produced by billboards of different colors
arranged on the side of the road.

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 Driving tiredness – the end enemy of the driver 15

4. Measures to prevent and reduce driver fatigue

Fatigue prevention is possible by optimal planning of the race or trip, correct and
proportionate staging of the trip, observing time schedules, ensuring the supply of physical
and mental energy until the end of the trip, taking breaks to relax, ventilating the passenger
compartment of the car, etc. Smoking is not recommended while driving, because polluted
air in the cabin accelerates the onset of fatigue, due to the fixation of carbon monoxide on
hemoglobin, which reduces the oxygenation capacity of the circulatory system.
In order to reduce fatigue [3, 9, 13], it is recommended to pay attention to the work
and rest regime, the duration of the car driving process. Thus, for example, before leaving a
long distance, especially if you are going to drive at night, the driver must rest. Several studies
have shown that sleeping for about an hour, the body regains its energy level and is rested
enough to stay awake all night. The struggle with fatigue and procrastination to save time is
not justified, it is much more important for the driver and his passengers to reach their
destination healthy and sound.
Immediately before departure, it is recommended to consume 30…50 g of lemon or
1–2 ascorbic acid pills [9]. Pay close attention to medications consumed, some of which can
cause severe drowsiness and are not recommended while driving. Even if the driver has eaten
well before setting off, he will take a few healthy snacks with him. The fast foods found along
the way are convenient and comfortable, but are full of fat, salt and sugar that make you feel
tired. Foods that give more energy and provide long-lasting resistance are made up of
complex carbohydrates and proteins. Consumption of energy drinks can help in this case, but
it is not the safest method. They can increase the level of alertness, but not for long, and then
fatigue can occur even more strongly. Sugar-containing drinks are not recommended, as they
can also create a greater state of fatigue later, even if for the moment they make us feel good.
During the trip, every 2 hours until noon and 1,5…2 hours after lunch, interruptions of
10…15 min must be made, during which it is recommended to perform the simplest gymnastic
exercises, also recommended for passengers. During the warm period of the year, it is
recommended to wash your face with cold water. However, when you feel the first signs of
drowsiness, you must refresh yourself with fresh air while driving, opening the side window.
It works very well if it is hot in the car and cold outside. Cold air gives the body a temporary
shock and makes it more alert. The conversation with the passengers also helps, if it does not
distract, and in their absence we can open the radio or the tape recorder, but the music must
be rhythmic, lively, light and not noisy. It is recommended that the leader himself sing. It is
not recommended to listen to radio reports from sports competitions, they distract.
If these easily acceptable measures do not help, then it is necessary to stop the
movement, because it is known that the most effective remedy for fatigue is rest. In case of
pronounced manifestation of fatigue and drowsiness, a short rest of 30…40 min in the places
indicated for this purpose helps to get out of the state of inhibition. Many drivers, fighting
fatigue, drink coffee. It really stimulates the body, but for a very short time, after which there
is an even more pronounced fatigue.
When the body is about to give in to sleep, on the border with reality you can meet
hallucinations (hypnogic). These are practically fragments of dreams, detached from the
immediate reality. Under these conditions you can get to what specialists call microsleep. It
is a state of sleep, which sets in for a period of 2…10 seconds, often followed by a shock on
waking. Then the brain is „overwhelmed” by the situation and involuntary reactions occur,
such as the sudden steering wheel or brake, which leads to destabilization and loss of control

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16 V. Plămădeală

of the car. During this time, the driver has his eyes open, sees the road, but in a state of
blurring of reality. The reflexes are very slowed down, and the driver misses any maneuver
to avoid an obstacle.
5. Car safety systems
This state of microsleep, in which the hesitations of maintaining the tread, are the
basis of the warning and prevention systems introduced by several car manufacturers. They
produce alarm signals, vibrations in the steering wheel and seat, when the driver crosses the
lane marking line without signaling. Lane restraint systems could help to avoid many road
accidents caused by the driver's fatigue.
The lane-keeping assistance system (lane keeping system) helps the driver to keep his
or her chosen lane, thus preventing accidents. The system is efficient when driving on
highways and national roads, because the quality road marking is drawn on them. There are
two types of lane departure assistance systems: passive and active. The passive system warns
the driver about the deviation from the chosen traffic lane, the active system, together with
the warning, corrects the traffic trajectory.
At different car manufacturers the lane keeping system has its trade name, but all the
proposed systems have practically a similar construction [14, 15]:
• Lane Assist from Audi, Volkswagen, Seat (figure 1);
• Lane Departure Warning System from BMW, Citroen, Kia, Ceneral Motors, Opel, Volvo
(figure 2, a);
• Lane Departure Warning from Continental Teves AG (figure 2, b);
• Lane Departure Prevention from Infiniti;
• Lane Keep Assist System from Honda, Fiat;
• Lane Keeping Aid from Ford;
• Lane Keeping Assist from Mercedes-Benz;
• Lane Keeping Support System from Nissan;
• Lane Keeping System from Continental Teves AG (figure 3, a);
• Lane Monitoring System from Toyota.

Figure 1. Lane Assist system LA.

The Lane Assist system is an electronic system and includes the control button, a video
camera, the control unit and the actuators. By means of the control button, the system is
activated. System operation information is displayed on the instrument panel as a control
lamp. The driver's warning is given by the vibration of the steering wheel or seat, as well as
by the visual light and sound signals. The vibrations are generated by a vibrating motor
integrated in the steering wheel or seat.

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 Driving tiredness – the end enemy of the driver 17

a) b)
Figure 2. Lane Departure Warning systems: a) Lane Departure Warning system LDWS;
b) Lane Departure Warning LDW.

Correction of the travel trajectory is achieved by forced steering of the steering system
using an electromechanical amplifier (most systems) or by braking the wheels of a part of the
car (Lane Departure Prevention system). The control unit operation algorithm determines the
position of the lane marking lines, evaluates the quality of the mark recognition, assesses the
width of the lane and its curvature and determines the position of the vehicle on the lane.
Based on the calculations, a control action is taken on the steering system or the braking
system, and if the necessary effect of keeping the car on the lane is not achieved, the driver
is warned by the vibration of the steering wheel, seat, audible and light signals.
It should be noted that the value of the torque, applied to the steering mechanism or
the braking force on two wheels of a part of the car, is small and can be exceeded by the
driver at any time.
When the traffic lane is premeditated, the turn signal must be switched on, otherwise
the system opposes the maneuver. In case of unfavorable conditions (lack of one of the lines
or the entire road marking, dirty or snow-covered roadway, narrow traffic lane, non-standard
marking on the road sections under repair, short-radius curve), the system is deactivated, thus
with no help for the driver.

a) b)
Figure 3. Lane Keep systems: a) Lane Keeping system LKS; b) Opel Eye system.

The Opel Eye system (figure 3, b) is designed to prevent the car from leaving the lane
automatically. The effectiveness of the system on narrow roads with local destination is
especially emphasized: it helps to prevent accidents related to the exit on the opposite lane.
If this system were installed on all European cars, it would help save 5000 lives and avoid
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18 V. Plămădeală

serious trauma for 20000 people. The doubling of road speed limit signs makes it possible to
avoid overtaking it in dangerous areas.
A similar system [15, 16] is also Alerte de Franchissement Involontaire de Ligne (warning
system for involuntary intersection of road markings), which starts operating at speeds of
80 km/h and determines with the help of transducers the intersection of road markings
without connecting turn signal. The system (figure 4) prevents the tired or careless driver from
vibrating in the seat cushion on one side, which corresponds to the intersecting road marking,
so that he can react in time.

Figure 4. Warning at unintentional intersection of road markings AFIL.

Road accident statistics show that the cause of a large number of accidents is the
physical condition of the driver. A large number of car manufacturers are actively working on
the creation of various driver monitoring systems, designed at least to announce the
occurrence of a dangerous condition of the driver and, at most, to intervene in driving and
prevent accidents. The work is carried out in several directions, including monitoring fatigue,
assessing physical stress, establishing the state of tension of the driver [15, 17].
Volkswagen is installing the emergency system on cars, which is an extension of the
lane keeping assistance system. If the driver is unable to drive the car (loses consciousness,
falls asleep), the Emergency Assist system takes control and stops the car, also warns other
road users of a dangerous situation. If the driver does not use the steering system for a certain
period of time, the Emergency Assist system warns him with visual and audible signals, brakes
the car. If there is no reaction from the driver, the system determines that he is not able to
drive the car. The lane-keeping assistance system ensures the car's movement within the
boundaries of the busy lane, and the adaptive cruising speed system prevents collisions with
the car in front. To warn other drivers, the damage signal is triggered, the car starts to move
sinusoidally within the lane and finally stops.
Another direction in the development of driver status monitoring systems is the
equipment of cars with biometric sensors, with the help of which important health indicators
(pulse, respiration rate, skin conductance etc.) can be monitored. These systems are promising
and must be installed on mass-produced cars. The closest to solving the problem is Ford,
which proposes a system for assessing the driver's load (strain), designed to reduce
distractions and excessive stress. The physical stress of the driver is estimated by processing
several parameters:
• vehicle traffic (speed, longitudinal and transverse acceleration, speed of rotation);
• driver actions (steering wheel rotation angle, accelerator pedal position and brake pedal);

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Driving tiredness – the end enemy of the driver 19

• road conditions (traffic density, character of road pavement);

• biometric indicators (heart rate, respiratory rate, skin temperature).
If the load on the driver is large enough, the system takes steps to reduce the tention,
including automatically connecting the mobile phone lock function to incoming calls („do not
disturb” function).
The following biometric sensors are used for the operation of the driver load
assessment system:
• piezoelectric sensor in the seat belt for monitoring the respiratory rate;
• conductive conductors on the steering wheel for measuring the pulse;
• infrared sensors on the steering wheel for measuring the temperature of the
palms;
• infrared sensor behind the wheel, which monitors the face temperature.

a) b)
Figure 5. Driver Status Monitoring systems:
a) Driver Wellness Monitoring DWM; b) Mind Sense systems MSS.
The Jaguar Land Rover company proposes to monitor the driver's condition with the
help of biometric sensors, built into the driver's seat. The Driver Wellness Monitoring system
(figure 5, a) uses breath and pulse rate sensors. If the system identifies serious health problems
or excessive driver agitation, measures shall be taken to ensure traffic safety. In case of stress,
internal cooling, audio system and air conditioning control are adjusted. In the event of a
sudden and serious illness, an emergency call is made and the car stops automatically.
In 2016, Audi presented the FitDriver project (figure 6) under the motto „My Audi takes
care of me”. Vital parameters of the leader, such as pulse and temperature, are monitored
using mobile devices (training bracelet or SmartSatch). These data are supplemented by
information on driving style, breathing frequency, weather and road conditions, provided by
various car sensors. Taken together, the data obtained allow to determine the current state
of the driver, including high fatigue or stress.
Ferrari has patented the technology, which assesses the driver's tention level after
changing brain waves. The bioelectrical activity of the brain is measured using wireless
sensors, built into the driver's headrest. Depending on the condition of the driver, there is a
reduction in the fuel supply of the engine and automatic stabilization of the car.
The Jaguar Land Rover is also working in this direction. The Mind Sense system (figure
5, b) determines when the driver is distracted or falls asleep while driving through brain
activity. It has been found that the human brain generates several brain impulses of different
frequencies. By constantly measuring the impulses, one can estimate how focused the driver

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20 V. Plămădeală

is (hesitated, drowsy or distracted). The monitoring of brain waves is done with the help of
sensors, built into the steering wheel.

Figure 6. The system FitDriver.

If the activity of the brain indicates drowsiness or low concentration of the driver, then
the steering wheel or accelerator pedal begins to vibrate, drawing attention to driving. If the
driver does not show any reaction, a visual and audible signal is given.
The fatigue monitoring system [15, 17] monitors the driver's physical condition and, if
it detects certain deviations, warns the driver about the need to stop and rest. The system
suggests a rest pause by means of a warning beep or a signal on the instrument panel „coffee
cup” (figure 7, a). Depending on the method of assessing the driver's fatigue, there are three
types of systems. The first are built on the control of the driver's actions, the second – the
control of the car's movement, and the third – the control of the driver's eyes. Currently, the
driver fatigue monitoring system is implemented on Mercedes-Benz, Volvo, Lexus cars.
Since 2011, Mercedes-Benz has been installing the Attention Assist system on its cars
[15, 18], in which the control of the driver's actions is based on many factors: driving style,
driving behavior, use of driving organs, character and driving conditions. and so on The
control unit processes the input signals and determines:
• driving style (analysis of speed, longitudinal and transverse acceleration for 30 minutes
after starting the movement);
• driving conditions (analysis of the time of day, duration of the trip);
• use of controls (analysis of the use of brakes, switches under the steering column,
buttons on the control panel);
• the character of the steering wheel rotation (speed, acceleration analysis);
• road condition (lateral acceleration analysis);
• the character of the car's circulation (analysis of longitudinal and transverse
acceleration).
As a result of the calculations, the deviations in the driver's actions and the driving
trajectory of the car are established. A warning signal about the need for a pause is displayed
on the control panel screen and an audible signal sounds. If, after signals, the driver does not
stop and continues driving in a state of drowsiness, the system repeats the signals at intervals
of 15 min. The system activates at a speed of 80 km/h.
Unlike the Attention Assist system, Volvo's Driver Alert Control system (figure 7, b) only
sets the character of the car's movement on the road. The camcorder facing forward fixes the
car's position on the lane. Deviation from the established traffic parameters is considered by
the system as the beginning of the driver's fatigue. Depending on the driver's condition, the
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Driving tiredness – the end enemy of the driver 21

system performs two levels of warning – „soft” and „hard”. The levels differ according to the
intensity and tone of the sound signal. The Driver Alert Control system works together with
the Lane Departure Warning system and is based on its constructive elements. The system
activates at a speed of 60 km/h.
Eye control for driver fatigue assessment is introduced by General Motors. Based on the
existing technique Seeing Machines (figure 7, c), which used in air, rail, quarry, commercial
freight. A special unit controls the degree of opening of the eyes and the direction of the
driver's gaze. When recognizing the driver's lack of attention, fatigue or drowsiness, the
system warns of the need to stop.

a) b) c)
Figure 7. Driver Fatigue Monitoring systems: a) Attention Assist system AA; b) Driver Alert
Control system DAC; c) Seeing Machines systems SM.

The presence of resonant bands in the longitudinal direction is a measure that warns
both audibly and sensitively the driver, if the car tends to go off the road or enter the opposite
direction of traffic. The positive experience of using resonator tapes in different countries
demonstrates the high efficiency of this technology for raising road safety. In the US,
resonator tapes are used in 85% of countries [19], significantly reducing the number of
deaths. On highways in Japan, the construction of roadside resonant lanes and the line
separating opposite transport flows has reduced the number of collisions with oncoming
traffic by up to 55%. In Finland, Denmark and Sweden, the use of resonator tapes has also led
to a significant reduction in the frequency of accidents and is mandatory for new road
construction.
Other safety features related to road infrastructure are sidewalks and off-road parking
lots, that limit the consequences of a fatigue accident.
6. Conclusions
1. Based on what is described in the article, it can be concluded that fatigue has a negative
effect on car driving skills and road safety, being the cause of many road accidents.
2. The problem of driving a car in an advanced state of fatigue will not lose its relevance as
long as each driver will not be aware of the danger to which he is subjected.
3. Traffic fatigue is a problem not only for countries with well-developed road infrastructure
or professional drivers, but for all drivers.
4. Driving in an advanced state of fatigue, which affects the driving ability of the vehicle is
prohibited in most countries, including the Republic of Moldova. But statistics show that
this restriction does not reduce the number of road accidents caused by driving fatigue.
5. There are many recommendations on how to reduce fatigue, but the most effective
remedy is rest.

Conflicts of Interest: The author declares no conflict of interest.

Journal of Engineering Science September, 2022, Vol. XXIX (3)
22 V. Plămădeală
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Citation: Plămădeală, V. Driving tiredness – the end enemy of the driver. Journal of Engineering
Science 2022, 29 (3), pp. 9-22. https://doi.org/10.52326/jes.utm.2022.29(3).01.

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Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
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Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 23 - 33
Fascicle Industrial Engineering ISSN 2587-3474
Topic Applied Engineering Sciences and Management eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).02
UDC 629.067(669)

OBJECTIVE APPROACH IN INVESTIGATING IMPLICATION OF ROAD VEHICLE

TYRE SAFETY KNOWLEDGE ON COMPLIANCE

Adinife Patrick Azodo1*, ORCID: 0000-0002-2373-1477,

Olasunkanmi Salami Ismaila1, ORCID: 0000-0002-9875-8594,
Titus Y. Jibatswen2, ORCID: 0000-0002-1392-3264,
Owoeye Femi Timothy3, ORCID: 0000-0003-4535-1459

Department of Mechanical Engineering, Federal University of Agriculture Abeokuta, Nigeria

1

2
Department of Mechanical Engineering, Federal University Wukari, Taraba state, Nigeria
3
Department of Metallurgy and Material Engineering, Yaba College of Technology, Yaba, Lagos Nigeria
*Corresponding author: Adinife Azodo, [email protected]

Received: 06. 17. 2022

Accepted: 08. 25. 2022

Abstract. Standard effectual directive on tyre safety management operations on its own is
nothing without appropriate compliance and application. Deliberate oversight and neglect of
safety precautionary measures may result in an accident and eventually be classified as an
unforeseen event. This study on safety knowledge and its implication for on-road vehicle tyre
safety compliance was conducted among one hundred and thirteen private vehicle owners in
Abeokuta, Nigeria. Data collection for this study was done using subjective and physical
measurement procedures. The analysis of data obtained showed that sixty-eight participants
(60.2%) of the participants had a fair knowledge of road vehicle tyre safety, followed by those
that had good knowledge 39 (34.5%). No participant had poor or excellent knowledge.
Overall operational tyre safety and compliance with the specifics for tyre standard condition
showed that 1 (0.9%) of the assessed vehicles were of very high safe and appropriate
compliance status. Forty-three (38.1%) of the assessed vehicles owned and used by the
participants were of very low operational tyre safety and practices. This was followed by
average safe and appropriate practice 39 (34.5%). Pearson's chi-square test analysis was used
to check if there is an association between tyre safety knowledge and safe and appropriate
compliance status variables gave χ2 = 1.135 and p = 0.769. This implies that there is no
statistically significant association between the two variables.

Keywords: tyre, safety, knowledge, vehicle, compliance, on-road.

Rezumat. Directiva standard privind operațiunile de management al siguranței anvelopelor

nu valorează nimic fără respectarea și aplicarea corespunzătoare. Supravegherea deliberată
și neglijarea măsurilor de precauție de siguranță pot duce la accident și, în cele din urmă, pot
fi clasificate ca un eveniment neprevăzut. Acest studiu analizează cunoștințele privind
siguranța și implicațiile sale pentru conformitatea anvelopelor vehiculelor rutiere. Studiul a
fost realizat în rândul a o sută treisprezece proprietari de vehicule private din Abeokuta,
Nigeria. Pentru colectarea datelor s-au folosit proceduri de măsurare subiective și fizice.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
24 A. P. Azodo, O. S. Ismaila, T. Y. Jibatswen, O. F. Timothy
Analiza datelor obținute a arătat că șaizeci și opt (60,2%) dintre participanți aveau cunoștințe
corecte despre siguranța anvelopelor vehiculelor rutiere, urmați de cei care aveau cunoștințe
bune 39 (34,5%). Niciun participant nu avea cunoștințe slabe sau excelente. Siguranța
operațională generală a anvelopelor și conformitatea cu specificațiile pentru starea standard
a anvelopelor au arătat că 1 (0,9%) dintre vehiculele evaluate avea o stare de conformitate
foarte sigură și adecvată. Patruzeci și trei (38,1%) dintre vehiculele evaluate utilizate de
participanți au avut o siguranță și practici operaționale foarte scăzute pentru anvelope.
Aceasta a fost urmată de o practică medie sigură și adecvată – 39 participanți (34,5%). Testul
Pearson a fost utilizată pentru a verifica dacă există o asociere între cunoștințele
privind siguranța anvelopelor și variabilele de stare de conformitate sigure și adecvate -
χ2 = 1,135 și p = 0,769. S-a constatat, că nu există o asociere semnificativă statistic între
cele două variabile.

Cuvinte cheie: anvelopă, siguranță, cunoștințe, vehicul, conformitate, pe drum.

1. Introduction
The road accident phenomenon is apparently a complicated and remarkable
development due to its diverse resultant effects on lives and property. The associated
physical, economic and social problem calls for concern. The frequency and intensity of road
traffic crashes are better explained in the witnessed 1.2 million lives it claims yearly and an
additional 20 - 50 million non-fatal injury cases [1]. Nigeria alone records 10,050 road
accident death cases yearly, with an average of 27 death cases per day [2, 3]. Afolabi and
Gbadamosi [4] traced the significance of morbidity and mortality cases from road traffic
crashes to population growth flight as well as an increased level of motorization. However,
the record of road traffic accidents in the developing countries where vehicles are relatively
few is proportionately upsurging but surprising declining in the industrialized nations [5].
From this perspective, Iteke et al. [6] linked the continued amplifying morbidity and mortality
cases in road traffic accident records in most developing countries especially in the sub-
Saharan Africa region to inconsequential and avoidable causation root factors. That is to say,
most road traffic crashes are predictable and perhaps preventable [7].
Road vehicles and their operations play a significant role in road traffic accidents [4].
The features representing road vehicles in road traffic crashes includes defective tyres, faulty
braking system, dysfunctional steering system, etc. these factors are directly or indirectly
connected to the functions tyres offer in an on-road vehicle which includes acceleration,
cornering, braking, and steerability. However, defective operation of any of these systems or
components arising from poor maintenance of the vehicle influences the ride comfort and
safety [8]. Safe vehicle actions and activities are very crucial in road traffic crashes morbidity
and mortality reduction. Vehicle maintenance for safety and ride comfort involves
assiduousness management of every component or system involved in vehicle controlling
and maneuvering function. This involves compliance with the equipped tire pressure
monitoring system specifics for vehicle tyre air pressure, plying speed on different road
surfaces whether wet or dry as well as an electronic stability control system [8].
The necessity for accuracy in tyre pressure inflation and wheel alignment is a ride
comfort and safety necessity to tyres flexing and heat during wheel rotation [8]. Most
assuredly maintenance of appropriate tyre contact patch pattern and effective function in
accelerating, steering, braking or cornering is only within its service life and proper inflation.
Accordingly, the service life of vehicle tyres should effectively deal with tyre/road interface
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Objective approach in investigating implication of road vehicle tyre safety knowledge on compliance 25

interactions at the molecular level as well as the loading and unloading energy absorption
of the vehicles [9, 10]. To maintain good tyre road grip, avoid aquaplaning on a wet road,
vehicle instability, tyre blowout, and long braking distance, the specifics for tyre condition
standard which includes tread depth, tyre age, and inflation pressure must be observed.
Understanding of the accident preventive measures as regards effectual and
appropriate tyre safety management operations on its own is nothing without application.
Deliberate oversight and neglect of safety precautionary measures may result in an accident
and eventually be classified as an unforeseen event [11]. Subjective factors or variables are
perchance independent of their actual performance [12]. Azodo and Ismaila [13] observed
that awareness depending on its level may or may not translate to appropriate practices.
Though subjective procedures for data collection from record raise bias response issues,
conscious perception explanations vulnerability and publicly verifiable as a major concern
[12, 14, 15]. However, individuals' inner states, potential knowledge and introspective reports
about conscious experiences are reliable on the subjects and can only be assessed using a
subjective approach [16]. On the other hand, utilizing objective design measures only because
of its valid evidence relevant facts, logical implications and viewpoints, and humanitarian
purposes in data collection precludes the existence of oblivious perception [17, 18]. That is
to say, the adoption of an objective research technique in a study deal with an accepted
standard which includes valid evidence relevant facts, logical implications and viewpoints
and human purposes of that issue. If relevant valid evidence is denied, an objective approach
is impossible. This study, therefore, adopted subjective and objective procedures in
investigating the implication of road vehicle tyre safety knowledge on compliance among
Nigerians.
2. Materials and Methods
This was a cross-sectional study of safety knowledge and its implication for on-road
vehicle tyre safety compliance conducted among private vehicle owners in Abeokuta, Nigeria.
Purposive multi-stage random sampling was used in the selection of participants. Subjective
and physical measurement approaches were used for data collection in this study. The
questionnaire (subjective approach) comprises demographic information (highest educational
qualification, occupation and driving experience) whereas the categories of information
assessed for knowledge of established operational road traffic safety standards were
appropriate size of vehicle tyres, specified tyre inflation pressure, tyres expiry date and
roadworthiness tread depth (Table 1). The variables on correct tyre safety rules developed
based on the conceptual basis of the study after due consultation with related works of
literature and established operational road traffic safety standards were assessed using a self-
administered questionnaire. The same formed the guide for the evaluation of operational tyre
safety and compliance among the participants. The responses of the participants to the
variable were classified as either correct or incorrect. The scaling mean-point of each
participant’s responses was computed to 100% and presented as 70 – 100 for “Excellence”
60 – 69 for “Very Good”, 50 – 59 for “Good”, 40 – 49 for “Fair”, and 0 – 39 for “Poor”
knowledge.
Analysis of the operational tyre safety and compliance with the specifics for tyre
standard condition which includes tread depth, tyre age, and inflation pressure was carried
out on each participant’s vehicle. The physical measurement was conducted before sunrise
and also before the owners used the vehicle with regards to the arrangement priory made
with the vehicle owners.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
26 A. P. Azodo, O. S. Ismaila, T. Y. Jibatswen, O. F. Timothy

Table 1
Applicable road vehicle operational tyre safety standards [19-23]
Road vehicle tyre safety Road vehicle operational tyre safety
specifics
Appropriate tyre inflation pressure 25% below and above the manufacturer's
recommended inflation pressure
Inflation pressure specifications guide and Driver's door ledge, the fuel tank cover, the
size designation recommended by the manufacturers’ car manual or online search
tyre/vehicle manufacturer. using the vehicles model for specified
standard inflation pressure.
Shelf life of tyre from date of manufacture Four years
(DOM)
Legal minimum tread depth 1.6 mm
Instructed guide to tyre purchase Tread depth, DOM and cracks or damage
Factors necessitating change of vehicle tyre Worn out, expired, bad cut,bulges,
punctures, impacts, cracks, and failing often
The scoring scheme associated with systematic observations made through physical
measurement was analyzed as appropriate and inappropriate compliance status. This was
conducted for the four tyres in each of the assessed vehicles. The level of safe and appropriate
practice compliance for each of the assessed vehicles was computed to 100% and evaluated
using the scaling range as follows “Very high safe and appropriate practice” = 70 – 100, “High
safe and appropriate practice” = 60 – 69, “Average safe and appropriate practice” = 50 – 59,
“Low safe and appropriate practice” = 40 – 49 and “Very low safe and appropriate practice” =
0 – 39. The data obtained were subjected to descriptive statistics in the form of frequencies
and percentages.
Statistical Package for the Social Sciences (SPSS) software version 16.0 (Chicago, IL,
USA) was used for descriptive statistical analysis on the data collected. The measure of the
safety knowledge and its implication on operation compliance level regarding the tyre safety
was conducted using the Pearson chi-square test at a p-value of 0.05 for significance level.
3. Results and Discussions
The response rate for the one hundred and twenty questionnaires distributed to the
private vehicle owners in Abeokuta, Nigeria, was (113/120) 94%. Participants’ distribution
according to gender showed 60 (53.1%) female and 53 (46.9%) male. The highest
educational training among the participants was tertiary education 93 (82.3%) probably
owing to the presence of three institutions of higher learning in the study area,
Federal College of Education, Oselle, Moshood Abiola Polytechnic, Ojere and Federal
University of Agriculture, Abeokuta (Figure 1). The distribution of the participants by
occupation showed that most of the participants were civil servants 33 (29.2%), followed
by entrepreneurs 22 (19.47%) with the applicants having the minimum number of
participants as 4 (3.54%) (Figure 2). Participants’ years of present vehicle ownership and
driving experience with it are presented in figure 3.
Accidents are a naturally unforeseen event or occurrence that results in death, injury,
or property damage but when they happen one can’t really say they are unanticipated [24].
However, caution can only be effectively taken and acted upon if appropriate
awareness of associated danger is in place [11].
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Objective approach in investigating implication of road vehicle tyre safety knowledge on compliance 27

1.80% 7.10%

16.80% No formal education

Primary education
74.30% Secondary education
Tertiary education

Figure 1. Highest educational training of participants.

35 31.0%
30
25 23.0%
Percentage

20 16.8%
15.0%
15
10 6.2%
5.3%
5 2.7%
0

Participants

Figure 2. Occupation of participants.

14.20% Less than 1 year

21.20% 1-2 years
8.80%
3-4 years
8.80% 5-6 years
11.50%
7-8 years
20.40% 9-10 years
15.00%

Figure 3. Participants years of driving experience.

Lack of awareness can result in a number of unsafe acts towards tyre safety practices.
The safety knowledge and its implication on on-road vehicle tyre safety compliance
conducted in this study cut across the lifespan of tyres, tyre pressure, tyre tread wear, and
tyre sizes. Table 2 gives the response of the study participants for various levels of knowledge
on on-road vehicle tyre safety. Considering that the shelf life of a tyre whether used or not is

Journal of Engineering Science September, 2022, Vol. XXIX (3)

28 A. P. Azodo, O. S. Ismaila, T. Y. Jibatswen, O. F. Timothy
four years from the DOM [22]. Sixty-two (54.9%) of the participants had correct knowledge
on tyre DOM for expiry date check out of which thirteen (11.5%) of the participants had
correct knowledge about the shelf life of tyre from DOM with ninety-three (82.29%) having
incorrect knowledge.
Every vehicle has its own tyre inflation pressure specification according to the vehicle
manufacturer. It is important to note here that two different models of vehicles may have the
same tyre inflation pressure values but this should not be taken for general value. The
structural damage scope covered in this study includes tyre inflation pressure (used for under-
inflation, over-inflation, and appropriate inflation determination) and tyre wear. Sixty-eight
(60.2%) of the participants had correct appropriate tyre inflation pressure knowledge for their
vehicle nonetheless the 74 (65.5%) that had correct knowledge of the location where inflation
pressure specifications guide for their vehicle by the manufacturers of the vehicles is found
(Table 2). Ten (8.85%) of the participants’ informed knowledge of appropriate tyre pressure
was from the right source (Table 2). Knowledge of the designation location for
the recommended tyre size by vehicle manufacturer had 74 (65.5%) correct responses from
the participants. The knowledge eight-seven (77.0%) of the participants had about
the appropriate size of their vehicle tyre was correct. Fifty-one (45.1%) had correct
knowledge instructed guide to tyre purchase whereas on factors necessitating a change of
vehicle tyre 74 (65.49%) had correct knowledge (Table 2).
Table 2
Appropriate knowledge on on-road vehicle tyre safety
Participants responses for road
Assessed variables on knowledge of road vehicle tyre safety vehicle operational tyre safety
Correct n (%) Incorrect n (%)
Appropriate tyre inflation pressure for owner’s vehicle 68 (60.2) 44 (38.9)
The location where inflation pressure specifications guide for 74 (65.5) 38 (33.6)
the vehicles manufacturers is found
Shelf life of tyre from DOM 13 (11.5) 93 (82.29)
Legal minimum road worthiness tread depth 50 (44.2) 63 (55.8)
The designation location for the recommended tyre size by 74 (65.5) 38 (33.6)
vehicle manufacturer.
Instructed guide to tyre purchase 51 (45.1) 62 (54.9)
Factors necessitating change of vehicle tyre 74 (65.49) 39 (34.51)
Informed knowledge of correct tyre pressure 10 (8.85) 98 (86.73)
Tyre DOM for expiry date check 62 (54.9) 51 (45.1)
Appropriate size of tyre for owner’s vehicle 87 (77.0) 26 (23.0)

Overall safety knowledge of on-road vehicle tyre safety on the various variables
assessed in the questionnaire by the participants showed that no participant had poor and
excellent knowledge of road vehicle tyre safety. Sixty-eight (60.2%) of the participants had a
fair knowledge of on-road vehicle tyre safety, followed by those that had good knowledge 39
(34.5%). Only 6 (5.3%) of the participants had very good knowledge (Table 3).
In a normal and appropriate operation condition, tyres smooth roll and durable
functions are imperative for acceleration, cornering, braking, and stability owing to the high-
quality composite and expertly-engineered chassis component that is specifically adapted to
vehicles to match a variety of different suspension systems and respond accurately for proper
traction needed.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Objective approach in investigating implication of road vehicle tyre safety knowledge on compliance 29

Table 3
Overall knowledge road vehicle tyre safety per participant vehicle owner
Frequency Percentage
Levels of road vehicle tyre safety
(n) (%)
Poor knowledge 0 0.0
Fair knowledge 68 60.2
Good knowledge 39 34.5
Very good knowledge 6 5.3
Excellent knowledge 0 0.0
Total 113 100.0

Table-4 shows the analysis of the operational tyre safety and compliance with the
specifics of the tyre condition standard which includes tyre size, tread depth, tyre age, and
inflation pressure carried out on each participant’s vehicle. The assessment was carried out
on each of the four tyres; the front right, front left, back right, and back left as well as for the
vehicle as a unit. From the standard for tyre roadworthiness in Nigeria [22], tyres have a 4-
year validity period from their DOM which means that beyond a four years duration of from
its DOM used or not, the such tyre has high accident risk potential, therefore should be
avoided. Purchase of new expired tyres is susceptible to road accident risk. The shelf life of
tyres in the vehicles showed that only 33 (29.20) of the participant vehicles were road worthy.
Tyre inflation pressure measured when compared with the specification stipulated by
the manufacturers either driver's door ledge, the fuel tank cover, the manufacturers' car
manual or online search using the model of the vehicle for specified standard inflation
pressure with considered accuracy of ±0.05 observed 6 (4.42%) of the participant vehicles had
appropriate tyre inflation pressure. In practice, the road contact patch pattern of tyres needs
to be maintained through appropriate operational safety standards for it to uphold its shape
and perform effectively in load carrying function and stability. In addition, incorrect tyre
pressure also increases the potential for hydroplaning (aquaplaning) and much longer
stopping distances.
Reithmaier and Salzinger [25] opined that excessive wear of tyres significantly
contributes to road traffic accident due to the rolling resistance and friction between the road
and tyre. The tyres of the assessed vehicles witnessed a much uneven wear due to
inappropriate inflation pressure 33 (29.20%) of the participant vehicles recorded even tyre
pressure.
The rolling resistance of tyres mainly depends on how the tread of the tyres touch the
road surface. Tread depth is very important in maintaining straight line headway of the loaded
tyre, especially at a constant speed. On the basis of hydroplaning potential and stopping
distances, it is expected that tyre replacement for safe driving of used vehicle tyre should be
at the tread depth of 1.6 mm as the chance of worn out tyre to cause an accident is high
especially on the wet road [22, 26]. ROSPA [26] added that increases in stopping distance
become significant when the tyre is worn past 3mm. The legal minimum tread depth of 1.6
mm notwithstanding, Hardy and Fenner (2015) reported that tyre tread depth of 3 mm
performs 25% better than those at 1.6mm. In this study, the roadworthiness of road vehicle
tyres (total compliance of the four tyres) was analyzed on the basis of legal minimum tread
depth of 1.6 mm and 3.0 mm for dry and wet road conditions respectively (across 75% of the

Journal of Engineering Science September, 2022, Vol. XXIX (3)

30 A. P. Azodo, O. S. Ismaila, T. Y. Jibatswen, O. F. Timothy

tyre). Legal minimum roadworthiness tread depth for wet road conditions analyzed at the
depth of 3.0 mm showed that 55 (48.7%) of the assessed vehicles were roadworthy as they
had appropriate depth cut. When the legal minimum roadworthiness tread depth for dry road
conditions was assessed at the depth of 1.6 mm, it showed that 85 (75.2%) participants’
vehicles were of appropriate tread depth.
All the four tyres in a vehicle should be of appropriate sizes, speed rating and
construction (radial or cross ply). Of the factors assessed, the same tyre size recommended by
the tyre/vehicle manufacturer had the most appropriate safety compliance with a proportion
of 105 (92.9%) of the assessed vehicle owned by the participants. This observation is in line
with Reithmaier and Salzinger’s [25] study.

Table 4
Analysis of the operational tyre safety and compliance with the specifics for
tyre condition standard
Appropriate operational status of tyre from physical measurement data
analysis
The
Assessed variables
Front right Front left Back right Back left assessed
n (%) n (%) n (%) n (%) vehicle n
(%)
Tyre inflation pressure 26 (23.01) 25 (22.12) 25 (22.12) 17 (15.04) 6 (4.42)
Shelf life of tyre 44 (38.9) 46 (40.7) 63 (55.8) 53 (46.9) 33 (29.20)
Even wear of tyre tread 31 (27.4) 33 (29.2) 29 (25.7) 23 (20.4) 13 (11.50)
Legal minimum road 89 (78.8) 88 (77.9) 86 (76.1) 78 (69.0) 55 (48.7)
worthiness tread depth
for wet road condition
Legal minimum road 98 (86.7) 104 (92.0) 101 (89.4) 103 (91.2) 85 (75.2)
worthiness tread depth
for dry road condition
The same tyre size 113 (100) 109 (96.46) 112 (99.12) 111 (98.23) 105 (92.9)
recommended by the
tyre/vehicle
manufacturer.

A vehicle is made up of many component parts and systems. A default of any of the
component parts and systems, a tyre, for example, may affect the proper functioning of the
vehicle. Overall operational tyre safety and compliance with the specifics of the tyre condition
standard for each assessed vehicle showed that no assessed vehicle was of very high safe
and appropriate compliance status. Forty-three (38.1%) of the assessed vehicles owned and
used by the participants' were of very low safe and appropriate operational tyre safety and
practices. This was followed by high safe and appropriate practices 39 (34.5%) (Table 5).
Pearson's chi-square test used to analyse data obtained to check if there is an
association between tyre safety knowledge and safe and appropriate compliance status
variables giving χ2 = 1.135 and p = 0.769 which is greater than 0.05.
This implies that statistically there is no significant association between knowledge
of road vehicle tyre safety and operational tyre safety and compliance with the specifics for
tyre condition standard among the participants (Table 6).

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 Objective approach in investigating implication of road vehicle tyre safety knowledge on compliance 31

Table 5
Operational tyre safety and compliance with the specifics for tyre condition standard per
assessed vehicle
Levels of safe and appropriate practice compliance Frequency (n) Percentage (%)
Very low safe and appropriate practice 43 38.1
Low safe and appropriate practice 30 26.5
Average safe and appropriate practice 39 34.5
High safe and appropriate practice 0 0.0
Very high safe and appropriate practice 1 0.9
Total 113 100.0

Phi and Cramer’s used to test the level of association of knowledge of road vehicle
tyre safety and operational tyre safety and compliance with the specifics for tyre condition
standards showed that the level of association between the two variables was weak (Table 7).

Table 6
Chi-Square tests
Asymp. Sig.
Value df
(2-sided)
Pearson Chi-Square 1.135a 3 0.769
Likelihood Ratio 1.130 3 0.770
Linear-by-Linear
0.096 1 0.756
Association
No of Valid Cases 113
a. 0 cells (0.0%) have expected count less than 5. The minimum expected count is 7.43.

Table 7
The table of symmetric measures
Value Approx. Sig.
Nominal by Phi 0.100 0.769
Nominal Cramer's V 0.100 0.769
Contingency Coefficient 0.100 0.769
No of Valid Cases 113

Conclusions
For a vehicle to serve its intended purpose which is to convey materials, goods, and
people safely to their intended destinations, precautionary action must be judiciously
observed and implemented. The safety aspect of road transportation and its operation is very
important as it is closely related to human lives. This experimental research that assessed
the effect of awareness and cautionary information on safe and appropriate tyre safety
management operations among private vehicle owners in Abeokuta, metropolis, Nigeria on
the established operational road traffic safety standards which includes vehicle tyres sizes,
specified tyre inflation pressure, tyres expiry date and roadworthiness tread depth observed
Journal of Engineering Science September, 2022, Vol. XXIX (3)
32 A. P. Azodo, O. S. Ismaila, T. Y. Jibatswen, O. F. Timothy

that there was an association between the safety knowledge and its implication on-road
vehicle tyre safety but it is not statistically significant. This calls for proactive awareness of
tyre safety among vehicle owners.

Conflicts of Interest: The authors declare no conflict of interest.

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Citation: Azodo, A. P.; Ismaila, O. S.; Jibatswen, T. Y.; Owoeye, F. T Objective approach in investigating
implication of road vehicle tyre safety knowledge on compliance. Journal of Engineering Science
2022, 29 (3), pp. 23-33. https://doi.org/10.52326/jes.utm.2022.29(3).02.

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Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 34 - 44
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Microelectronics and Nanotechnologies eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).03
UDC 539.234:621.38

NEW VAPOR DEPOSITED DIELECTRIC POLYMER THIN FILMS FOR ELECTRONIC

APPLICATIONS

Stefan Schröder1, ORCID: 0000-0001-9996-2637,

Nicolae Magariu2,3, ORCID: 0000-0001-7006-3443,
Thomas Strunskus1, ORCID: 0000-0003-3931-5635,
Nicolai Ababii2,3, ORCID: 0000-0001-5046-8611,
Oleg Lupan2,3,4*, ORCID: 0000-0002-7913-9712,
Franz Faupel1, ORCID: 0000-0003-3367-1655

1
Chair for Multicomponent Materials, Institute for Materials Science, Kiel University, Kaiserstr. 2, D-24143, Kiel,
Germany
2
Center for Nanotechnology and Nanosensors, Technical University of Moldova, 168 Stefan cel Mare Av., MD-2004
Chisinau, Republic of Moldova
3
Department of Microelectronics and Biomedical Engineering Technical University of Moldova, 168 Stefan cel Mare
Av., MD-2004 Chisinau, Republic of Moldova
4
Department of Physics, University of Central Florida, Orlando, FL 32816-2385, USA
*Corresponding author: Oleg Lupan, [email protected]

Received: 05. 28. 2022

Accepted: 06. 30. 2022

Abstract. Dielectric materials are of great interest in a vast amount of applications ranging
from cable insulation to advanced electronic devices. The emerging trend of device
miniaturization is creating an increased demand for dielectric thin films that can be produced
precisely on the nanometer scale. In addition, special mechanical properties are often
required, for example in the field of flexible organic electronics. Polymers are first-choice
materials for this purpose. However, it is extremely difficult to produce precise nanoscale
thin films, which have a low defect density and are free of e.g. residual solvent, by wet
chemistry approaches. Initiated chemical vapor deposition (iCVD) is a solvent-free polymer
thin film deposition process which can be used to produce high quality dielectric thin films
with nanoscale control and circumvents thus these problems. This work demonstrates the
versatility of the iCVD process in the field of electrical applications by some new application
examples of iCVD. By adding e.g. a hydrophobic organosiloxane thin film on columnar zinc
oxide (ZnO:Fe) gas sensing structures there was a change in the selectivity from ethanol to
hydrogen, as well as improved performance at high humidity level. The modified sensors can
thus be used in humid ambient, especially for breathing tests, which can lead to the diagnosis
of some diseases by cutting edge non-invasive approaches.

Keywords: Polymers, Initiated Chemical Vapor Deposition, Electronic Materials, Dielectrics,

Electrets, Gas Sensors.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 S. Schröder, N. Magariu, T. Strunskus, N. Ababii, O. Lupan, F. Faupe 35

Rezumat. Materialele dielectrice prezintă interes pentru numeroase aplicații, de la izolarea

cablurilor până la dispozitive electronice avansate. Tendința emergentă de miniaturizare a
dispozitivelor creează o cerere crescută pentru pelicule subțiri dielectrice care pot fi produse
exact la scara nanometrică. În plus, sunt adesea necesare proprietăți mecanice speciale, de
exemplu în domeniul electronicii organice flexibile. Polimerii sunt materiale de primă alegere
în acest scop. Cu toate acestea, este extrem de dificil să se producă filme subțiri precise la
scară nanometrică, care au o densitate scăzută a defectelor și sunt lipsite de solvent rezidual,
prin abordări ale chimiei umede. Depunerea chimică de vapori inițiată (iCVD) este un proces
de formare a peliculei subțiri de polimer fără solvenți care poate fi utilizat pentru a produce
pelicule dielectrice de înaltă calitate cu control la scară nanometrică și eludează astfel aceste
probleme. Această lucrare demonstrează versatilitatea procesului iCVD în domeniul
aplicațiilor electrice prin câteva exemple noi de aplicare a iCVD. Prin adăugarea, spre
exemplu, a peliculei subțiri de organosiloxan hidrofob pe structurile de detectare a gazului
de oxid de zinc columnar (ZnO:Fe), se atestă o schimbare a selectivității de la etanol la
hidrogen, precum și o performanță îmbunătățită la un nivel ridicat de umiditate. Senzorii
modificați pot fi astfel utilizați în mediu umed, în special pentru teste de respirație, care pot
duce la diagnosticarea unor boli prin abordări non-invazive de ultimă oră.

Cuvinte cheie: polimeri, depunere chimică inițiată de vapori, materiale electronice, dielectrice,
electreți, senzori de gaz.

1. Introduction
The current advent of polymer thin films enabled by the combination of chemical
vapor deposition (CVD) with organic chemistry provides a variety of new pathways in the field
of organic electronics and electronic applications. In particular, oxidative chemical vapor
deposition (oCVD) and initiated chemical vapor deposition (iCVD) developed by Gleason et al.
facilitate the precise deposition of new electronic materials from a few nanometers to several
micrometers in film thickness [1]. While in oCVD a step growth reaction allows the
preparation of conjugated polymers such as PEDOT or PANI [2], iCVD usually results in
insulating films due to the underlying free radical polymerization. In the latter, the polymer
backbone is sp3-hybridized and the polymer films can be used as dielectrics. Due to the
solvent-free nature of iCVD, the dielectric thin films are of very high quality and have no
defects that accelerate e.g dielectric breakdown [3]. Thanks to the CVD-typical growth
character, the iCVD process can easily be scaled up and integrated into modern
microelectronic process lines. A schematic illustration of the iCVD process is shown in Figure
1(a). The respective monomer (M) and initiator (I) are introduced to the reactor. The reactor
is equipped with a heatable filament array, located above a sample stage, which is cooled to
room temperature. The monomer molecules adsorb at the substrate stage and once the
filaments are heated the initiator molecules are decomposed into free radicals (R). These
radicals meet e.g. a vinyl groups of the adsorbed monomer molecules. They start a free radical
polymerization, which follows similar kinetics like the well-known kinetics for wet chemistry
free radical polymerization [4] in order to produce high quality polymer thin films at the
substrate surface.
Figure 1(a) shows schematic design of the iCVD process. It is shown that monomer (M)
vapor and initiator (I) vapor are introduced to a hot wire CVD (HWCVD) reactor at the same
time. Afterwards, thermally decomposed I results in free radicals (R), which initiate a free
radical polymerization with adsorbed M. Figure 1(b) shows possible monomers and initiators
Journal of Engineering Science September, 2022, Vol. XXIX (3)
36 New vapor deposited dielectric polymer thin films for electronic applications

for dielectric thin films. In this work, some application examples of different tailored
dielectric iCVD films are shown to demonstrate the versatility of the process in the field of
electrical applications.

Figure 1. (a) Schematical illustration of the iCVD process. Monomer (M) vapor and
Initiator (I) vapor are introduced to a hot wire CVD (HWCVD) reactor. Thermally
decomposed I results in free radicals (R), which initiate a free radical polymerization with
adsorbed M. (b) Possible monomers and initiators for dielectric thin films.
2. Experimental details
All polymer thin films reported in this study are deposited via iCVD. A home-made
ring-inlet iCVD reactor explained in our previous works has been used for this purpose [3, 7,
8]. The hydophobic PV3D3 thin films have been obtained by the combination of the monomer
V3D3 with the initiator PFBSF. The electrostatic potential maps have been illustrated using
Jmol. The V3D3 and V4D4 molecules have been geometry-optimized employing density
functional theory (DFT) at the B3LYP/ccPVDZ level for this purpose. The reported gas sensing
structures have been obtained initially by the chemical deposition of solutions (SCS) method,
which yields a nanostructured ZnO:Fe film. The film was deposited on a glass substrate (75
mm × 25 mm × 1 mm). The obtained ZnO, ZnO:Fe nanostructured films have been thermal
annealed (TA) in furnace for 2 hours at 650 oC in normal ambient. A more detailed description
is given in our previous works [5, 6]. An ultra-thin deposition of CuO/Cu2O with a thickness
of 18 nm was grown on the ZnO:Fe film with a custom setup with DC and RF magnetron. After
this step a heat treatment was applied to the samples in a furnace at 420 °C for 30 minutes.
In the next fabrication step 25 nm of the hydrophobic PV3D3 thin film was deposited on top
of the sensors. Finally, Au contacts were sputtered on top of the samples through a
meandering mask [9]. For the sensor performance measurements, a computer-controlled
Keithley 2400 sourcemeter at 0.2 V applied bias voltage was used. The details on the sensing
experiments can be found in our previous works on gas sensing studies [10, 11].
3. Results and Discussion
The application of iCVD thin films as dielectric layer is reported by many authors,
especially organocyclosiloxanes, like PV3D3, PV4D4 and fluoropolymers, have demonstrated
excellent performance [12-14]. The chemical structure of possible monomers and initiators
which yield excellent dielectric properties are presented in Figure 1(b). The polymer films can
also be deposited on flexible substrates, as shown in the digital photograph in Figure 2(a),
were we use a dielectric iCVD thin film as part of a flexible electronic device. Figure 2(b)
shows a schematic representation of trap states, which are positioned between the highest
occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) bands
of the polymer. Figure 2(c) illustrates calculated electrostatic potential maps of geometry-
optimized V3D3 and V4D4.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 S. Schröder, N. Magariu, T. Strunskus, N. Ababii, O. Lupan, F. Faupe 37

Figure 2. Photograph of the application of an iCVD thin film as part of a flexible

electronic device, produced in our lab (a). Schematic illustration of trap states, which are
located between the HOMO and LUMO bands of the polymer (b). Calculated electrostatic
potential maps of geometry-optimized V3D3 and V4D4 (c).

The iCVD coatings are thus also highly attractive as dielectric thin films for flexible
organic electronics. One further argument for using iCVD is the high film quality, because no
organic solvents are used during the fabrication of the polymer thin films. Residual solvent
and defects can cause e.g. conductive paths and this lowers the dielectric breakdown strength
of the material. For dielectric iCVD films the breakdown strength has been found to be
extremely high, because of the low defect density and high film quality without residual
solvent molecules [3]. Since dielectric iCVD films exhibit such high breakdown strength and
film quality, we demonstrated the use of iCVD grown PTFE thin films as electret materials in
a previous work [3]. Electrets are dielectric materials with a quasi-permanent surface charge.
They can be produced by exposing the dielectric materials e.g. to a corona discharge in order
to transfer excess charge to the material. The charge carriers are stored in trap states, which
are located in the gap between the HOMO and LUMO of the polymer, as illustrated in Figure
2(b). Typically deep level traps provide enough depth to store the charge carriers over a long
period of time. The result is a surface potential which can be applied for many different
application fields like portable electret condenser microphones, energy harvesting, air filters
or magnetic field sensors [15, 16]. However, the charged film is in a metastable state and at
some point the charge will decay. A good electret is thus characterized by the fact that its
charge decay is negligible compared to the device lifetime in which it is used. Fluoropolymers
like polytetrafluoroethylene (PTFE) typically exhibit the best charge storage properties [3].
The unique adjustability of the functional groups in the iCVD process allows the electrical
properties to be specifically tailored. These can also be correlated with theoretical
calculations. In Figure 2(c), the calculated electrostatic potential maps of the above-
mentioned V3D3 and V4D4 monomers are shown as an example.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
38 New vapor deposited dielectric polymer thin films for electronic applications

In addition to the production of such new tailored polymer thin films for electronic
applications by iCVD, it is also possible to functionalize existing electronic devices. As an
example, we recently demonstrated the functionalization of metal-oxide gas sensors with an
ultra-thin hydrophobic cyclosiloxane-type of polymer [5]. In this previous work we have
reported data for CuO/Cu2O/ZnO:Fe heterostructures, which were as-grown and Rapid
Thermal Annealed (RTA) for 60 s at 650°C. After the deposition of the ultra-thin hydrophobic
thin film via iCVD using the monomer V3D3 and the hydrophobic initiator PFBSF we were
able to tune the selectivity of the gas sensors to hydrogen gas. Furthermore, we were able to
operate the sensors at high humidity level, which has been a major problem for metal-oxide
gas sensors before. Also, new metal-oxide CuO/Cu2O/ZnO:Fe heterostructures, which have
been thermally annealed (TA) at 650°C for 2h in a furnace in air, can be applied as gas sensors.
Scanning electron microscopy (SEM) images of these new structures are shown in Figure 3.

Figure 3. SEM images of CuO/Cu2O/ZnO:Fe heterostructures after thermal annealing at

650 °C for 2 h at low (a) and high magnifications (b).

From Figure 3 can be concluded that the samples are composed of highly packed
columnar-type grains of ZnO:Fe with the CuO/Cu2O layer on the surface. The structures cover
the glass substrate completely. The increasing surface/volume ratio is beneficial for sensor
applications.
The gas sensors shown in Figure 3 are coated with 25 nm hydrophobic PV3D3, similar
like in our previously reported study [5]. PV3D3 layer was deposited on top of such sensor
structure to protect it from the effect of environment and especially from the high relative
humidity, which affect the sensor performances seriously. Figure 4 shows the XRD patterns
of the samples.
The formation of hetero-junctions is evidenced by the coexistence of the phases of
CuO, Cu2O and ZnO, so that at the values 2θ of 32.45°, 35.3°, 46.15°, 65.4° and 68.05°. The
reflections hkl were found for the copper oxide CuO (Tenorite) with the Miller planes of (-
110), (-111)/(002), (-112), (022) and (113), respectively. These results clearly prove crystal
quality and no changes due to iCVD process. Furthermore, the diffractions from the gold layer,
Au (111) and Au (220), can be observed, which was deposited on top of the sensor structure
as an electrical contact.
Reflections at 2θ of 34.35°, 34.35°, 47.95°, 56.75°, 62.2° and 66.45° with the Miller
planes of (002), (102), (110), (103) and (200), respectively, are attributed to zinc oxide ZnO,
according to the card (pdf # 36-1451) Zincite syn. In addition, reflections of iron oxide Fe2O3
are observed in Figure 4, which indicate the doping of zinc oxide with iron impurities. After
thermal treatment Fe2O3 is found according to the card (pdf # 89-0599) Hematite syn with
Miller indexes (104), (202), (024) and (125) at the 2θ angle of 33.45°, 43.45°, 49.05° and 67.1°,
respectively.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 S. Schröder, N. Magariu, T. Strunskus, N. Ababii, O. Lupan, F. Faupe 39

Figure 4. XRD pattern of CuO/Cu2O/ZnO:Fe heterostructures thermally annealed at 650 oC

and contacted with Au on top as electrical contacts.

Figure 5. The dependence of the gas response (hydrogen, acetone, 2-propanol, n-butanol,
ethanol and ammonia) versus working temperature for (a) uncoated heterostructured
samples and for (b) hydrophobic PV3D3 coated samples.
As mentioned above, reflections at 2θ of 37,25 ° and 63,75 ° in Figure 4 are assigned
to metallic Au, which originate from the sputtered contacts during device fabrication.
In order to test the final sensor performance with and without the polymer coating we
performed gas response measurements with respect to various gas and volatile organic
compounds in normal ambient. The results of the measurements of the gas response versus
operating temperature are shown in Figure 5.
The sensors have been tested with hydrogen gas, acetone, 2-propanol, n-butanol,
ethanol and ammonia vapor at different working temperatures. The results for thermally
Journal of Engineering Science September, 2022, Vol. XXIX (3)
40 New vapor deposited dielectric polymer thin films for electronic applications

annealed CuO/Cu2O/ZnO:Fe heterostructures without the PV3D3 are shown in Figure 5(a).
Results from the sample set of thermally annealed CuO/Cu2O/ZnO:Fe hetero-structures with
additional PV3D3 coating are shown in Figure 5(b) for comparison. Figure 5(a) reveals that
the highest gas response can be observed for ethanol vapors. The growth of the hydrophobic
PV3D3 on top of the sensor surface shows a shift of the selectivity to hydrogen gas, similar
like our observations for the samples from our previous work [5]. The highest response can
be obtained at an operating temperature (OPT) of 350 oC with a response value of ~165%.
Figure 6(a) illustrates the dynamic response of the uncoated CuO/Cu2O/ZnO:Fe
heterostructures to ethanol vapors in normal ambient. The dynamic response for hydrogen of
the PV3D3 coated heterostructures is shown in Figure 6(b), which proves that selectivity was
changed from ethanol vapor to hydrogen gas and pulses are reproducible during all experiments.

Figure 6. Dynamic response of the CuO/Cu2O/ZnO:Fe heterostructures thermally annealed

at 650 oC for 2 h in air: (a) to ethanol vapors (sample set without PV3D3) and (b) to
hydrogen gas (sample set with PV3D3 layer on top of the sensor) at optimal operating
temperature of 350 oC measured in normal ambient.

Both measurements have been performed at an OPT of 350 oC and data recorded in
normal ambient. The results in Figure 6 demonstrate that uncoated as well as coated
heterostructures show quite high response values, when they are exposed to the respective
gas. Furthermore, a very good repeatability can be observed in Figure 6(b). The sensors show
a complete restoration of the response after each gas pulse.
The current-voltage (I-V) curves of the uncoated as well as coated heterostructures are
shown in Figures 7(a) and 7(b), respectively. Figure 7a shows the electrical measurements for
an uncoated heterostructure CuO/Cu2O/ZnO:Fe and Figure 7b shows the measurements for a

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 S. Schröder, N. Magariu, T. Strunskus, N. Ababii, O. Lupan, F. Faupe 41

PV3D3-coated heterostructure on glass substrates. The measurements have each been

performed at different OPT as indicated in the graphs and numbered accordingly. The
electrical measurements reveal that the I-V curves for all heterostructures show Ohmic
behavior at each of the targeted operating temperatures. This demonstrates that the sensors
work correctly even with the additional 25 nm polymer coating on top of the heterostructure.
As observed in the measurements above, the selectivity of the covered sensors has shifted
towards hydrogen gas due to the additional PV3D3 coating, similar like in our previous study.

Figure 7. Current-voltage characteristics of the CuO/Cu2O/ZnO:Fe heterostructures

thermally annealed at 650 oC: (a) without PV3D3; and (b) covered with PV3D3 layers.

Dynamic response measurements at different humidity levels have been performed in

order to investigate the influence of moisture or value of relative humidity RH on the sensor
performance and to identify if it is suitable for breath test, as an example. The obtained
results are shown in Figure 8. Figure 8(a) illustrates the dynamic response to ethanol vapor
for the uncoated heterostructures. The dynamic response for the PV3D3-coated
heterostructures are presented in Figure 8(b) for hydrogen. The gas concentration was in both
measurements 100 ppm and the measurements have been performed at 20 % and 65 %
relative humidity each. Figure 8(a) shows that the response of the uncoated heterostructure
to ethanol vapor decreases drastically by about 88 % at relative humidity of 65 % compared
to the response at relative humidity of only 20 %. As expected, this indicates that the gas
sensors no longer work reasonably in a high humid environment and can’t be used for
example in non-invasive breath tests. The dynamic response measurement for the PV3D3-
coated heterostructure, which is shown in Figure 8(b), reveals that the response to hydrogen

Journal of Engineering Science September, 2022, Vol. XXIX (3)

42 New vapor deposited dielectric polymer thin films for electronic applications

decreases to about 1/3 of the original response in the high humidity environment. In addition,
it is evident that pulses are still repeatable at higher humidity. This clearly proves the effect
of the coverage with a PV3D3 thin film to protect the gas sensing samples from moisture.
The performed experiments thus show, that the additional hydrophobic PV3D3 coating can
also increase the stability of the heterostructure with regard to a high relative humidity,
similar like in our previous study. Furthermore, it can also protect the sensing structures from
the environment conditions.

Figure 8. Dynamic response at operating temperature of 350 oC at different

concentrations of relative humidity: (a) to ethanol vapors (samples without PV3D3 layer)
and (b) to hydrogen gas (samples covered with PV3D3 layer on top).

4. Conclusions
Dielectric thin films deposited by iCVD can be used in a vast amount of electrical and
electronic applications. We presented potential applications in organic electronics or as thin
film electrets as examples. The individual tunability of the functional groups makes it
possible to specifically adjust the electrical properties of the polymer thin films. Furthermore,
in addition to creating new polymer thin film materials, existing devices can also be
improved. The films can be used e.g. to protect electronic circuits or electronic devices.
Following our previous study, we show as a real example, the use of hydrophobic coatings to
protect semiconducting oxide-based gas sensors from moisture or high relative humidity.
According to the presented results, CuO/Cu2O/ZnO:Fe heterostructures after thermal
treatment at 650 oC for 2 h were successfully obtained in this current work. The structural
results were confirmed by XRD data, with a granular morphology of columnar type confirmed
by SEM. The heterostructures of CuO/Cu2O/ZnO:Fe with a thermal annealing regime in the

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 S. Schröder, N. Magariu, T. Strunskus, N. Ababii, O. Lupan, F. Faupe 43

electrical furnace at 650 oC for 2 h in ambient air are selective for ethanol vapors. After the
deposition of a 25 nm hydrophobic PV3D3 thin film on the heterostructure, the selectivity
changes from ethanol vapor to hydrogen gas. At the same time, the deposition of the PV3D3
thin film increases the stability at high relative humidity values, namely 65% RH in our
experiments. A possible application field for the modified gas sensors in the future are
biomedical applications. The sensors can here be applied for e.g. breath tests in non-invasive
diagnosis, due to the fact that humidity does not significantly influence the response value
to hydrogen gas in a high humid environment.

Acknowledgments. This research was partially sponsored by the NATO Science for
Peace and Security Programme (SPS) [grant number G5634 „Advanced Electro-Optical
Chemical Sensors”]. In addition, it was partially funded by the Deutsche
Forschungsgemeinschaft (DFG, German Research Foundation) [grant number Project-ID
434434223-SFB 1461, Project-ID 286471992-SFB1261 project A2, GRK 2154 project P4].
Furthermore, the authors would like to thank the WTSH and the EUSH for partially funding
this project BAEW [grant number LPW-E/1.1.2/1486].

Conflicts of Interest. The authors declare no conflict of interest.

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14. Lau, K. S.; Caulfield, J. A.; Gleason, K. K. Structure and morphology of fluorocarbon films grown by hot filament
chemical vapor deposition. Chemistry of Materials 2000, 12 (10), pp. 3032-3037.
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Citation: Schröder, S.; Magariu, N.; Strunskus, T.; Ababii, N.; Lupan, O.; Faupel, F. New Vapor Deposited
Dielectric Polymer Thin Films for Electronic Applications. Journal of Engineering Science 2022, 29 (3),
pp. 34-44. https://doi.org/10.52326/jes.utm.2022.29(3).03.

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Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 45 - 58
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Microelectronics and Nanotechnologies eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).04
UDC 539.23:681.586

GAS SENSITIVE FILMS BASED ON Te-SnO2 NANOCOMPOSITE ON FLEXIBLE

SUBSTRATE

Dumitru Tsiulyanu1, ORCID: 0000-0003-3711-4434,

Olga Mocreac1*, ORCID: 0000-0002-4362-4556,
Andrei Afanasiev1, ORCID: 0000-0003-1523-5542,
Eduard Monaico2 ORCID: 0000-0003-3293-8645

1
CIMAN Research Centre, Department of Physics, Technical University of Moldova, 41 Dacia Blvd,
MD-2060, Chisinau, Republic of Moldova
2
NCMST Research Centre, Technical University of Moldova, 168 Stefan cel Mare Blvd, MD-2004, Chisinau,
Republic of Moldova
*Corresponding author: Olga Mocreac, [email protected]

Received: 04. 27. 2022

Accepted: 06. 12. 2022

Abstract. Flexible films based on novel Te-SnO2 nanocomposites were fabricated for
detection of toxic gases at room temperature. The Te-SnO2 nanocomposites were obtained
via solvohermal recrystallization of pure crystalline tellurium in nitric acid in the presence of
tin chloride. The energy-dispersive X-ray spectroscopy (EDX) and XRD analyses have shown
that the Te-SnO2 films consists of fluffy structures of tiny agglomerates of the
nanodimensional irregular blocks of hexagonal Te and polycrystalline SnO2. Both current /
voltage and transient characteristics of the flexible Te-SnO2 films were investigated at room
temperature in ambiance comprising different toxic gases. The maximum selectivity was
revealed toward NO2, for which in the dynamic range of 0.5 - 5.0 ppm of NO2, the response
and recovery times are about 30 s and 150 s respectively. Analysis of the response kinetics
meets the Langmuir theory of adsorption. This study revealed a simple route of fabrication of
the printable Te-SnO2 nanocomposites that can be used in electronics, inclusive for
development of flexible and compostable gas sensors, operating at room temperature.

Keywords: Nanocomposites, Te-SnO2, Conductometric sensors, NO2.

Rezumat. Filme flexibile bazate pe noi nanocompozite Te-SnO2 au fost fabricate pentru
detectarea gazelor toxice la temperatura camerei. Nanocompozitele Te-SnO2 au fost obținute
prin recristalizarea solvotermală a telurului cristalin pur în acid azotic în prezență de clorură
de staniu. Spectroscopia cu raze X cu dispersie energetică (EDX) și analizele XRD au arătat că
filmele de Te-SnO2 constau din structuri pufoase de aglomerate mici ale blocurilor neregulate
nanodimensionale de Te hexagonal și SnO2 policristalin. Atât caracteristicile curent/tensiune,
cât și tranzitorii ale filmelor flexibile de Te-SnO2 au fost investigate la temperatura camerei
într-o ambianță cuprinzând diferite gaze toxice. Selectivitatea maximă a fost evidențiată față
de NO2, pentru care în intervalul dinamic este de 0,5 - 5,0 ppm de NO2, timpii de răspuns și
de recuperare sunt de aproximativ 30 s și, respectiv, 150 s. Analiza cineticii răspunsului

Journal of Engineering Science September, 2022, Vol. XXIX (3)

46 D. Tsiulyanu, O. Mocreac, A. Afanasiev, Ed. Monaico

corespunde teoriei Langmuir a adsorbției. Acest studiu a dezvăluit o cale simplă de fabricare
a nanocompozitelor imprimabile Te- SnO2 care pot fi utilizate în electronică, inclusiv pentru
dezvoltarea senzorilor de gaz flexibili și compostabili, care funcționează la temperatura
camerei.

Cuvinte cheie: Nanocompozite, Te-SnO2, Senzori conductometrici, NO2.

1. Introduction
In the last years, printed electronics becomes very attractive due to the ability of using
sustainable, compostable and recyclable materials including biobased plastics and paper in
the elaboration of different flexible devices, such as photodetectors, light-emitting diodes,
transistors, piezo-resistive transducers, circuit boards etc. [1-5]. Many reports are available
on development of flexible gas sensors (see extensive reviews [6-7]), based on plastic,
polyimide, polypyrrole or polytetrafluoroethylene and paper platforms, using active layers
from two-dimensional chalcogenides SnSe(S)2 [8-10], nanostructured spinel ferrite Zn(x)Fe(1-
x)2O4 [11], carbon nanotubes graphene [12-15] and others. The flexible gas sensors on paper

substrates are of particular interest as they are cheap, ecological and recyclable. Besides, the
paper is lighter and exhibits a lower thermal expansion coefficient (2–16 ppm/C) compared
to plastic substrates (20–80 ppm/C) [16]. Were reported flexible gas sensors on paper
substrates designated to detect hydrogen sulfide [17, 18] ammonia [19-21] and nitrogen
dioxide [22, 23]. Hydrogen sulfide gas sensors have been fabricated via printing of polyaniline
(PANI)-metal salt (CuCl2) composite on a paper substrate. The resistance of the sensor drops
by several orders of magnitude within exposure to H2S and behaves irreversibly due to gas
induced transformation of metal salt into resulting metal sulfide [17]. Ammonia sensors were
developed using carbon nanotubes (CNT) and graphite abraded on the fibers of cellulose [19],
cellulose –TiO2 – multiwall carbon nanotube hybrid nanocomposite [20] or multilayered
graphene deposited on a filter paper [21]. In all cases the effect of NH3 consists in reversible
increasing of the resistance by gas adsorption, although the sensing parameters are rather
different. Thin films based on single walled carbon nanotubes and graphene were also used
for the development of flexible nitrogen dioxide gas sensors [21-24]. Single walled CNTs
carbon nanotube ink on a cellulosic paper was shown to detect low (~ 0.25 ppm)
concentrations of nitrogen dioxide at room temperature [22]. Exposing to NO2 vapors
diminishes the resistance of the sensor. The relative change of resistance nonlinearly
decreases with NO2 concentration increase. No significant change of the baseline was
observed but the recovery time is in the range of 7 min. Graphene-based, flexible NO2 sensors
on paper substrates were reported to exhibit a fast (~ 50 s) response once exposed to 200
ppm NO2 gas, but when the supply of NO2 is stopped the current drops by ~ 20% at 360 s and
slowly decreases thereafter during a long time without reaching the initial value [24]. The
overall process of fabrication of such flexible chemical sensors on paper substrates appears
to be rather sophisticated. Alongside, in the last decades, the remarkable performances for
the NO2 detection have been achieved via using the thin films based on elemental tellurium
and its alloys (extended reviews [25-27]). Although such films exhibit high sensitivity toward
nitrogen dioxide at room temperature, their morphology, electrical properties and gas
sensing properties strongly depend on fabrication technology, material composition,
temperature, geometry and post fabrication treatment [28-30]. The main methods of the
fabrication of gas sensitive Te based films implies the thermal vacuum evaporation of either
pure polycrystalline Te or its alloys, pulsed laser deposition [31], the rf sputtering [32] or
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Gas sensitive films based on Te-SnO2 nanocomposite on flexible substrate 47

direct vapor phase process [33] in an argon atmosphere. The films usually were grown onto
hard substrates of glass Pyrex, quartz, sintered or porous alumina [34], Si / SiO2 wafers and
others.
In all cases, the growing technology of Te thin films consisted of a number of physical,
chemical and electrochemical procedures, including photolithography, electrochemical
pickling, thermal vacuum evaporation etc.
The present work is devoted to avoiding the mentioned above complex and costly
technology of tellurium based thin films fabrication, maintaining their good gas sensitivity
and room temperature operating ability. A simple technology of Te-SnO2 nanocomposite
preparation was developed via thermal dissolution of polycrystalline tellurium powder in
nitric acid, followed by Te reduction in the presence of tin chloride. We also demonstrated a
facile method of fabrication of thin films based on Te-SnO2 nanocomposite paste via its
painting on standard paper substrates. Being supplied with contacting electrodes these films
exhibit sensitivity to toxic and dangerous chemical gasses (NO2, H2S, and SO2) at
concentrations of 0.5–10 ppm or higher. The highest sensing performance was revealed with
respect to nitrogen dioxide within a dynamic range 0.5 – 5.0 ppm with fast, reversible and
reproducible response time ~30 s and recovery time ~ 150 s.

2. Materials and Methods

All reagents used in the experiments were of analytical grade and used as received
without further purification. HNO3 (55%) and H2SO4 (57 %) were purchased from Centro –
Chem but SnCl2 (99.95%) from Brenntag (both Poland). The procedure of the fabrication of
Te-SnO2 nanocomposites can conventionally be divided in four steps:
1) Obtaining the tellurous acid via reaction of the pure Te powder and dilute nitric
acid.
2) Obtaining of a solution of the tin chloride SnCl2 via dissolving the SnCl2 salt into
diluted sulfuric acid.
3) Obtaining a suspension of Te and SnO2 via mixing the solutions of tin chloride SnCl2
and tellurous acid.
4) Obtaining of Te-SnO2 paste via filtering the obtained suspension and washing the
filtrate under a vacuum.
In a typical experimental procedure, the tellurium powder (purity 99.999 %) was
dissolved via the hydrothermal reaction in diluted nitric acid to form the tellurous acid
(H2TeO3) accompanied with emission of the gaseous nitric oxides (NO, NO2).
In parallel the aqua solution of tin chloride (SnCl2) has been prepared via following
procedure: 1.6 g of stannous chloride was placed in a container and a solution of 4 g of H2SO4
diluted in 150 g of distilled water was added with continuous stirring. As a result, a
transparent aqua solution of SnCl2 was obtained, which further has been added to aqua
solution of the tellurous acid under a strong stirring. A chemical reaction occurred that
resulted in formation of a black colored suspension. The resulting solid product was collected
from solution through filtering and repeatedly washing with distilled water. Finally, a viscous
paste has been obtained, which then was painted by Doctor Blade coating technique onto a
paper substrate forming a large flexible film (Fig.1 a), which after drying at room temperature
for 24 h had a thickness of around 35 µm.
Fabricated solid films were cut using scissors for further characterization and gas
sensors fabrication. The gas sensor design is schematically shown in Fig. 1b.

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48 D. Tsiulyanu, O. Mocreac, A. Afanasiev, Ed. Monaico

Figure 1. The view of flexible thin film based on Te-SnO2 nanocomposite on paper
substrate (a); schematic of the gas sensor design (b): 1- paper substrate; 2- active
sensing Te-SnO2 layer; 3 - metallic electrodes.
It consists of a paper substrate on which a layer of Te-SnO2 nanocomposite is printed,
above which two (or a series) of metallic (Ag, In, etc.) electrodes in a planar arrangement are
deposited or painted. The sensors were encapsulated in sockets, and their contacts were
thermally bonded to socket pins by means of copper wires.
Both the surface morphology and thickness of the dried films were investigated with
VEGA TESCAN TS 5130 MM scanning electron microscopy (SEM). The film’s elemental analysis
was performed by the energy-dispersive X-ray spectroscopy (EDX) using INCA Energy 200
EDX equipment coupled with SEM. X-ray diffraction (XRD) was carried out to identify the
structural phases in the grown films with a DRONE –YM1 diffractometer using Fe Kα
radiations. The scattering angle was between 18 and 80 but the rotation velocity of the
scintillation counter was 2 (or / and 4) angle degrees /min.
The description and detailed parameters of the gas sensing testing system, as well as
of methodology of the current - voltage (I-U) and current – transient (I-t) characteristics
measurement can be found in our recent publication [35]. Gaseous media with different
concentration of NO2 H2S, NH3, SO2, ethanol (C2H5OH), acetone (CH3)2CO and toluene C7H8
were obtained by using the calibrated permeation or diffusion tubes (Vici Metronics, USA),
which were introduced into the experimental set-up described elsewhere [36, 37].
The sensor sensitivity was defined as the relative resistance variation expressed in
percent [35]:
𝑆𝑆 = 100��𝑅𝑅𝑎𝑎 − 𝑅𝑅𝑔𝑔 ��/𝑅𝑅𝑥𝑥 (1)

where: 𝑅𝑅𝑎𝑎 and 𝑅𝑅𝑔𝑔 are the electrical resistances of the sensor in the air and in the presence of
target gas respectively and 𝑅𝑅𝑥𝑥 is the highest from either 𝑅𝑅𝑎𝑎 or 𝑅𝑅𝑔𝑔 .
The response and recovery time were estimated as the times taken to reach or to lose
the 90% of steady-state values of the current respectively.

3. Results
3.1 Morphology, elemental composition and structural analysis
Figure 2 shows the typical SEM image of films fabricated in this study. The SEM reveals
that Te-SnO2 films consist of fluffy structures of tiny agglomerates of the nanodimensional
irregular blocks of about 100 nm.

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 Gas sensitive films based on Te-SnO2 nanocomposite on flexible substrate 49

Figure 2. Typical SEM image of Te-SnO2 based film on paper substrate.

The nanodimensional blocks were identified by energy - dispersive X-ray spectroscopy

(EDX) as a composite consisting of several chemical elements. Results of EDX study of the
fabricated nanocomposites are depicted in Fig. 3. As can be seen the EDX spectrum revealed
the presence of about 39 at. % Te, 52 at. % O, 5.5 at. % Sn and 3.5 at % remnants of Cl.
Compositional and phase state analysis of the fabricated nanocomposite thin films
have been examined by XRD, which appeared to be consistent with EDX analysis. Figure 4
displays a typical XRD pattern of the sample obtained via above-described technology along
with expected location of the diffraction peaks from standard data for pure Sn [38] and TeO2
[39] shown by colored dotted lines.

Figure 3. EDX analysis of Te-SnO2 based film.

As it is seen, all of the diffraction peaks in this pattern can be readily indexed to the
hexagonal phase of tellurium with lattice constants of a = 4.46 Å and c =5.94 Å [40, 41] (JCPDS
Card No.: 36-1452), along with polycrystalline tin dioxide, with predominant orientation of
the crystals (110) and (002) [42, 43] (JCPDS 41-1445).

Journal of Engineering Science September, 2022, Vol. XXIX (3)

50 D. Tsiulyanu, O. Mocreac, A. Afanasiev, Ed. Monaico

Figure 4. X-ray diffraction pattern of Te-SnO2 nanocomposite obtained via hydrothermal

reaction of tellurium powder, nitric acid and tin chloride.

3.2 Electrical conductivity at interaction with NO2

3.2.1 Current – voltage characteristics. Effect of bending
Fig. 5 a shows the typical current /voltage characteristic of Ag/Te-SnO2/Ag functional
structures, which was measured at room temperature in ambient air and 1.0 ppm NO2 gas,
respectively. The linearly increased current, independently of the direction of the bias
voltage, reflect the absence of depletion regions at the Ag contacts, i.e., they are ohmic in the
entire range of applied bias voltage.

Figure 5. Current / voltage characteristic of Ag / Te-SnO2 /Ag functional structure in air

and in the presence of 1.0 ppm of NO2 in linear (a) and semi-logarithmic scale (b).

The last is clearly confirmed by representation of I-U characteristic in a semi

logarithmic scale (Fig.5 b). The influence of NO2 gas consists in increasing of the current flow
through the specimen, boosting the I-U characteristic slope. To study the effect of bending
(stress) on electrical conductivity of Ag / Te-SnO2 / Ag functional structure, its resistance has
successively been measured for many times before and after bending by ~ 90 degrees. Fig. 6
shows the electrical resistance evolution of both straight and bent Ag / Te-SnO2 / Ag
functional structure grown on paper substrate in function of number of bending by ~ 90 degrees.

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 Gas sensitive films based on Te-SnO2 nanocomposite on flexible substrate 51

Figure 6. Evolution of electrical resistance of the straight {R(o)} and bent by 90 degrees
{R(b)} Ag / Te-SnO2 /Ag functional structure grown on paper substrate dependent of
number of bending.

As can be seen, initially the resistance of both straight and bent devices increases but
after approximately one dozen of bends, it tends to saturate. Moreover, for each number of
bending the resistance of the straight and bended device does not differ much that confirms
its flexibility.

3.2.2 Transient characteristics

Figure 7 shows the dynamic response of a Te – SnO2 sample towards different
concentrations (0.5 - 5.0 ppm) of nitrogen dioxide at room temperature and constant bias
voltage, for gas pulses of similar or falling concentration (Fig 7a) as well as at increasing
concentration (Fig. 7 b).

Figure 7. Transient characteristics of gas - induced current by exposure to different

concentrations of NO2 for: a) gas pulses of similar or falling concentration; b) increasing
concentration. Dotted lines of the bottom show the schedule of the gas pulses.

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52 D. Tsiulyanu, O. Mocreac, A. Afanasiev, Ed. Monaico

It is seen that the sensor shows the reversible and reproducible response following
the schedule of the gas application (dotted line on the bottom), without noticeable drift of
the baseline. The response time is about 30 s but the recovery time is about 150 s.

Figure 8. Sensitivity (a) and sensitivity per unit concentration (b) versus NO2
concentration (calibration curve) at room temperature. C – is gas concentration in ppm.
Fig. 8a shows the calibration curve, that is the relative resistance variation versus gas
concentrations. This curve is non-linear: the sensitivity sharply increases but tends to saturate
at high NO2 concentrations. As far as the sensitivity per ppm unit is concerned (Fig. 8 b), it
oppositely sharply increases at low gas concentrations. Thus, the sensor is able to effectively
to detect the low concentrations of NO2, including the sub ppm range.

3.2.3 Effect of other gases and humidity

The selectivity, i.e. the effect of other gases towards Te – SnO2 based gas sensitive device
has been assessed via direct measurement of the relative variation of the resistance under
exposure to H2S, NH3, SO2, ethanol (C2H5OH), acetone (CH3)2CO and toluene C7H8. It was
established that ethanol, acetone, toluene and ammonia do not interact with these films as
no response signal has been detected. The comparison of sensitivities to the other tested
gases can be only qualitative because of very different dynamic ranges. Figure 9 shows the
response of Te – SnO2 based sensor to rectangular pulses of NO2, H2S and SO2. As the
ambience usually contains water vapor, we have checked the interfering effect of water
vapors with NO2 sensing at room temperature.
Fig.10 shows the sensor response toward rectangular pulses of humid air with 58% RH
(shown by arrows) and 1.0 ppm NO2 successively applied. The schedule of the NO2 pulse
application is shown by dotted line. It is seen that the effect of both H2O and NO2 vapors is to
increase the current. Such behavior of the Te –SnO2 based gas sensitive thin films cordially
differs from behavior of the pure Te based ones, in which it was definitely pointed out that
the humidification of ambiance diminishes the current flow through the sample [25].
Comparison of Figs. 7 and 10 shows that increasing RH from 20 to 58 % shifts the baseline,
but the sensitivity remains nearly the same, around 30% toward 1.0 ppm NO2.

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 Gas sensitive films based on Te-SnO2 nanocomposite on flexible substrate 53

Figure 9. Transient response of a film based on Te – SnO2 nanocomposite to

rectangular pulses of NO2, H2S and SO2 of different concentration and duration, shown by
dotted line on the bottom. Inset shows the relative resistance change of sensor under
exposure to different gases of indicated concentrations at 22 oC.

Nevertheless, it is evident that the effect of humidity is quite large and requires finding
the reason, explanation and ways for its avoidance. This needs additional investigations,
which are outside of the present study but are in progress.

Figure 10. Effect of water vapor on the Te – SnO2 based film by NO2 detection at 22 °C.

4. Discussion
The chemical reactions for the synthesis of tellurium-based nanocomposites can be
formulated as following: During the hydrothermal reaction, initially, tellurium powder was
dissolved in dilute nitric acid to form the tellurous acid (H2TeO3) accompanied with emission
of the gaseous nitric oxide:
𝑇𝑇𝑇𝑇 + 4𝐻𝐻𝐻𝐻𝑂𝑂3 + 𝐻𝐻2 𝑂𝑂 ⇌ 3𝐻𝐻2 𝑇𝑇𝑇𝑇𝑂𝑂3 + 4𝑁𝑁𝑁𝑁 (2)

Journal of Engineering Science September, 2022, Vol. XXIX (3)

54 D. Tsiulyanu, O. Mocreac, A. Afanasiev, Ed. Monaico

Alongside, the synthesis of tellurium dioxide occurs via the reactions:

2𝑇𝑇𝑇𝑇 + 9𝐻𝐻𝐻𝐻𝑂𝑂3 ⇌ 𝑇𝑇𝑇𝑇2 𝑂𝑂3 (𝑂𝑂𝑂𝑂 )𝑁𝑁𝑁𝑁3 + 8𝑁𝑁𝑂𝑂2 + 4𝐻𝐻2 𝑂𝑂 (3)
𝑇𝑇𝑇𝑇2 𝑂𝑂3 (𝑂𝑂𝑂𝑂 )𝑁𝑁𝑁𝑁3 ⇌ 2𝑇𝑇𝑇𝑇𝑂𝑂2 + 𝐻𝐻𝑁𝑁𝑁𝑁3 (4)
When the aqua solution of SnCl2 has been added to the solution obtained via reactions
(2-4) under a continuous stirring, the tin chloride acts as a reducing agent and the followed
reaction occurs:
𝐻𝐻2 𝑇𝑇𝑇𝑇𝑂𝑂3 + 2𝑆𝑆𝑆𝑆𝐶𝐶𝐶𝐶2 ⟶ 𝑆𝑆𝑛𝑛𝑂𝑂2 + 𝑆𝑆𝑆𝑆𝐶𝐶𝐶𝐶4 + 𝑇𝑇𝑇𝑇 ↓ +𝐻𝐻2 𝑂𝑂 (5)
Thus, the resulting solid products, collected via filtering of black colored resulted
suspension followed by multiple washing in distillate water, have to contain pure tellurium,
tin oxide and perhaps some leftovers of SnCl4. Meanwhile the XRD analysis of fabricated thin
films based on synthesized via above shown reactions black solid paste (Fig.4), has confirmed
the presence of hexagonal phase of tellurium alongside with polycrystalline tin dioxide but
did not reveal the remainders of SnCl4. Perhaps, the last is due to low amount of SnCl4 in the
synthesized nanocomposite that is consistent with EDX analysis. The elemental analysis of
fabricated thin films performed via EDX spectroscopy (Fig.3) has identified the presence of
only about 3.5 at. % remnants of Cl, alongside with about 39 at. % of the nanostructured Te.
Thus, the compositional and structural analyses of synthetized nanocomposite in
conjunction with above shown experimental results related to gas sensing characterization
of developed films, provides evidence that the gas sensitivity of films in question is due solely
to the tellurium component that change its conductivity proportional to surface coverage [35]
given by classical Langmuir’s theory of adsorption [44]. The Langmuir’s kinetics can be
expressed in the form [45]:
𝑑𝑑𝑑𝑑
= 𝛼𝛼𝛼𝛼 (1 − 𝜃𝜃 ) − 𝛽𝛽𝛽𝛽 (6)
𝑑𝑑𝑑𝑑

where θ is the surface coverage that is a quantity proportional to surface concentration

of adsorbed particles, C is the NO2 concentration, 𝛼𝛼 and 𝛽𝛽 is the direct and inverse reaction
constant respectively. According to this equation, while the surface coverage and the
desorption are small, 𝑑𝑑𝑑𝑑/𝑑𝑑𝑑𝑑~(1 − 𝜃𝜃). In such case, as the gas induced current in Te film is
caused by releasing of majority carriers (holes) at chemical adsorption of gaseous (NO2)
species [46], the time derivative of this current, under constant bias voltage, has
proportionally to decrease with ∆𝐼𝐼increase.
Fig. 11 shows the response current from data of Fig.7 (b) plotted, as 𝑑𝑑𝑑𝑑/𝑑𝑑𝑑𝑑, a function
of ∆ I for several concentrations of the NO2 applied at 22 0C. The data in this picture were
averaged by 5-point smoothing. It is seen that in principle the response toward NO2 of Te–
SnO2 based films is consistent with the Langmuir’s model of surface coverage. The time
derivative of the gas induced current linearly diminishes with change current increase, at that
these derivative increases with gas concentration increase and even the slope change of line
𝑑𝑑𝑑𝑑/𝑑𝑑𝑑𝑑 = 𝑓𝑓 (𝐶𝐶 )can be observed.
Finally, it is worth noting that the SnO2 nanoparticles of nanocomposite in question
were not observed to participate in the gas sensing process, that obviously is caused by sensor
low operation temperature (~ 22 °C). Tin oxide becomes gas (NO2) sensitive only at operation
temperature higher than 200 °C [47, 48]. At that, SnO2 does not disturb the gas sensing
properties of Te nanoparticles from nanocomposite but can be the reason for large influence
of the humidity.

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 Gas sensitive films based on Te-SnO2 nanocomposite on flexible substrate 55

Figure 11. The Langmuir plot of the sensor response toward a rectangular pulse of
NO2 drawn using the data shown in Fig.6 for the Ag / Te - SnO2 / Ag device.
5. Conclusions
Nano-composites of Te-SnO2 were synthesized via a simple thermal dissolution of
polycrystalline tellurium powder in nitric acid, followed by its chemical reduction in the
presence of tin chloride solution. Showed by SEM, EDX and XRD analyses the composites
consists of nanoparticles of around 100 nanometers, comprising about 40 at. % Te and 6.0 at.
% of tin oxide. The synthesized nanocomposites can be used for fabrication of thin flexible
gas sensors via screen printing technology, onto paper sheets. Such sensors exhibit selective
and rapid (~30 s) response to nitrogen dioxide and operate at room temperature.
Acknowledgments. This work was supported by National Agency for Research and
Development of Moldova, project PS 20.80009.5007.21. Author expresses his gratitude to Dr.
G. F. Volodina at Institute of Applied Physics of MER RM for XRD analysis.
Conflicts of Interest. The authors declare no conflict of interest.
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58 D. Tsiulyanu, O. Mocreac, A. Afanasiev, Ed. Monaico
Citation: Tsiulyanu, D.; Mocreac, O.; Afanasiev, A.; Monaico, E. Gas sensitive films based on Te-SnO2
nanocomposite on flexible substrate. Journal of Engineering Science 2022, 29 (3), pp. 45-58.
https://doi.org/10.52326/jes.utm.2022.29(3).04.

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Submission of manuscripts: [email protected]

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Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 59 - 69
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Computers and Information Technology eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).05
UDC 004.056(669)

APPLICATION OF PRIVACY-PRESERVING DATA PUBLISHING IN TERTIARY

INSTITUTIONS OF KEBBI STATE USING GENERALIZATION AND SUPPRESSION

Anas Shehu1*, ORCID: 0000-0002-5307-1457,

Alhassan Salihu1, ORCID: 0000-0003-1926-6813,
Abubakar Sani2, ORCID: 0000-0001-9616-0647

1
Department of Computer Science Kebbi State Polytechnic Dakin-gari, Dakin-gari, 862106, Nigeria.
2
Department of Computer Science Yusuf Maitama Sule University, Kano, 700214, Nigeria.
*Corresponding author: Anas Shehu, [email protected]

Received: 06. 14. 2022

Accepted: 08. 02. 2022

Abstract. The research was conducted in the field of publishing data to preserve
confidentiality. Several educational datasets have been used to address privacy and utility.
The sample questionnaires served to investigate the level of privacy awareness and
enforcement in the records of students in tertiary institutions in Kebbi State, Nigeria. The
benchmark datasets were obtained from Kebbi State Polytechnic Dakin-gari. K-anonymity
and l-diversity models were used with k configurations and suppression limits of 10 and 50%
in the ARX 3.9.0 de-anonymization environment. The work evaluates data privacy, quality,
and execution time for each k value and suppressions limit. Experimental results demonstrate
that the higher the suppression the more balanced exists between privacy and utility. It was
observed that suppression of 50% provides less anonymization time irrespective of k
compared to k values in suppression = 10%. This was proved to be due to less time it takes
anonymization to be completed Also, from respondents, 92% of students’ records were kept
permanently in plain and, issued to third parties like that—with no privacy guarantee. This
poses privacy threats to datasets.

Keywords: Arx de-anonymization tool, Dakin-gari, k-anonymity, privacy, quality, utility.

Rezumat. Cercetarea a fost efectuată în domeniul publicării datelor pentru păstrarea

confidențialității. Au fost folosite câteva seturi de date educaționale pentru a aborda
confidențialitatea și utilitatea. Chestionarele eșantion au servit pentru a investiga gradul de
conștientizare a confidențialității și aplicarea acesteia în dosarele studenților din instituțiile
terțiare din statul Kebbi, Nigeria. Seturile de date care au servit drept reper au fost obținute
de la Kebbi State Polytechnic Dakin-gari. Modelele de K-anonimitate și l-diversitate au fost
utilizate cu configurații k și limite de suprimare de 10 și 50% în mediul de de-anonimizare
ARX 3.9.0. Lucrarea evaluează confidențialitatea datelor, calitatea și timpul de execuție
pentru fiecare valoare k și limită de suprimare. Rezultatele experimentale demonstrează, că
o suprimare este mai mare induce echilibru între intimitate și utilitate. S-a observat, că
suprimarea de 50% oferă mai puțin timp de anonimizare indiferent de k comparativ cu valorile
Journal of Engineering Science September, 2022, Vol. XXIX (3)
60 A. Shehu, A. Salihu, A. Sani

k în suprimare = 10%. Acest lucru se datorează faptului că anonimizarea durează mai puțin
pentru a fi finalizată. De asemenea, din partea respondenților, 92% din dosarele studenților
au fost păstrate în mod permanent neconfidențial, fiind eliberate astfel unor terți, fără
garanție de confidențialitate. Acest lucru reprezintă amenințări de confidențialitate a
seturilor de date.

Cuvinte cheie: instrument de dezanonimizare, Arx, Dakin-gari, k-anonimitate, confidențialitate,

calitate, utilitate.

1. Introduction
In Computer Science & Information Technology, privacy could be seen as control over
the disclosure of Personally Identifiable Information (PII), or quasi-identifiers (QI). This PII or
QI helps in establishing a user profile when combined with a publically available dataset that
leads to personality being watched, profiled, and make unwanted revelations that resulted in
physical and economic harm. Privacy ought to be guaranteed when sensitive biomedical data
is shared for any reason [1], though the most common datasets use are biomedical and
demographic data [2]. Notwithstanding, that did not limit other datasets to be used as
individuals and industries carry out research from multiple and disparate domains day in and
day out where attributes of individual should be protected using industry acceptable
techniques. With the current growth of information technologies, various organizations such
as hospitals, financial houses, educational institutions are constantly collecting information
about individuals and keep it in their databases for future use. These volumes of data increase
exponentially [3] as a result of this, privacy becomes the subject of hot debate as it requires
models, privacy risks for protecting it as well as providing utility [2]. On this note, this work
intends to explore the available resources to apply privacy to student datasets before sharing
them with researchers. To protect privacy, recommended data transformation models should
be used in the process. Examples of such models are Global recoding, full-domain
generalization Plus record suppression [1], user defines hierarchy is always useful for
generalization as it dictates transformation rules that minimize attributes precision in a
hierarchical pattern. While full domain generalization makes an attribute generalized on an
equal level of associated hierarchy. Refer to figure 1 for generalization hierarchy level 0 of
gender and LGA are more specific compared to level 1 and of course level 2 presents the
B/Kebbi highest level that cannot be recognized.
As for suppression, the original attribute value is replaced by a symbol such as ‘*’, ‘#’
and so on to detach meaning from it [3].

Figure 1. Generalization hierarchy adopted from [4].

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Application of privacy-preserving data publishing in tertiary institutions of Kebbi state using generalization… 61

1.1. Privacy Models

Privacy models were developed aimed at mitigating the risk of linkage attacks taking
quasi identifier (QI) as a target [2], that QI cannot be eliminated from the dataset as they are
important and needed for analyses. We formally defined QI as attributes A1…… Ad in table T
that can be joined with external public data to re-identify individual records such as student
matric no., application no., gender, zip code, date of birth, age, etc. K-anonymity is a
commonplace model used in preserving QI privacy. For more detail about k-anonymity, refer to [2].
Also, attributes are sensitive if an individual may not want to be linked with it, for
example in our case, student registration fee, student department, occupation, salary, and
disease in the biomedical domain. To protect sensitive attributes, l-diversity, and t-closeness
as prevalent models are being utilized [5]. Figure 2 below shows the taxonomy of the privacy model.

Figure 2. Taxonomy of Privacy Models.

1.2. Contributions
In summary, this work will present the following contributions: 1. Presentation of
questionnaire and its response 2. Presentation and analyses of survey results concerning
privacy in the educational domain. 3. Application of Student datasets in the field of PPDP
using the ARX tool. 4. Extensive evaluation of the anonymized dataset concerning different
values and two different suppression limits. And finally, we present the experimental setup
used in the work.

1.3. Survey Results

The questionnaire was designed for the survey work to ascertain the level of data
privacy, information awareness, and its application in all tertiary institutions in Kebbi State.
Each institution was administered 30 questionnaires with the targeted respondents of Level
Coordinators, Management and information Units, Bursary and Registry among others, and
below are the name of the institutions:
1. Waziri Umaru Federal Polytechnic Birnin Kebbi (WUFP),
2. Kebbi State Polytechnic Dakingari (K/S Pol. Dakingari),
3. Collage of Education Argungu (COE Argungu),
4. Health Technology Jega (Health Tech.Jega),
5. Aleiro University of Science and Technology (AUST),
6. Federal University Birnin Kebbi (FUBK).
The table below provides samples of questionnaires administered and the associated
responses per each institution.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
62 A. Shehu, A. Salihu, A. Sani

Table 1
Sample of questionnaire responses
K/S Pol. COE. Health Tech.
Question WUFP l AUST FUBK
Dakingari Argungu Jega
What is the Above 5000- 1000-2000- 4000-5000- Above 5000- Above 5000- Above 5000-
total number of (66.66%) (66.66%) (46.66%)
(63.66%) (60.66%) (60.66%)
students in
your
institution?
Does your Yes – (80%) Yes – (100%) Yes – (100%) Yes – Yes – (100%) Yes – (100%)
institution keep (73.33%)
student
records?
How long does Forever- Forever- Forever- Forever- Forever- Forever-
your institution (68.96%) (73.33%) (100%)
(90%) (20%) (100%)
keep the
student’s
record?
Which of the Account No.- Account No.- Account No.- Account No.- Account No.- Account No.-
student’s (36.66%) (93.33%) (50%) (50%) (20%) (20%)
details do you
consider
sensitive?
Does your Yes.-(100%) Yes.-(86.66%) Yes.-(86.66%) Yes.-(86.66%) Yes.-(93.33%) Yes.-(100%)
institution use
a computing
platform in
keeping
student
records?
Does the Yes.-(56.66%) Yes.-(60%) Yes.-(56.66%) Yes.-(76.66%) Yes.-(80%) Yes.-(80%)
student’s
record keep in
plain text?
How simple it Very Simple.- Very Simple.- Very Simple.- Very Simple.- Very Simple.- Very Simple.-
is to identify (63.33%) (66.66%) (53.33%) (66.66%) (96.66%) (96.66%)
individual
records?
Does your Yes.-(23.33%) Yes.-(66.66%) Yes.-(56.66%) Yes.-(56.66%) Yes.-(26.66%) Yes.-(26.66%)
institution give
out student
data to a third
party?
Are you aware Yes.-(46.66%) Yes.-(86.66%) Yes.-(36.66%) Yes.-(53.33%) Yes.-(80%) Yes.-(80%)
of information
privacy and
data protection
law?

Does the No.-(100%) No.-(100%) No.-(100%) No.-(100%) No.-(100%) No.-(100%)

institution
prevent
students’ data
from any
attack?

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Application of privacy-preserving data publishing in tertiary institutions of Kebbi state using generalization… 63

From Table 1 above, the results provided are consolidated for the whole six (6) higher
institutions of learning in the state. We chose to use a one-sided response as it is the majority
and provides insight into what the research wants. The most interesting things to note from
the table are: (1). 92.22% of the student records were collected for the entire institution only,
and 75.38% were kept for eternity. Though 92% of the record were stored in computing
platforms used by various institutions, 68.33% of the total record were kept as plain text-(as
is collected). This shows the extent of privacy threats faced by the record. (3). Also as
indicated in the table above, 73.88% of all student records in the entire school are prone to
internal attack due to the simplicity of identifying individual records with less effort. For
these, we can attest to the fact that the entire records for the whole institutions of Kebbi
state are being faced with privacy threats as figures shown in table 1 due to the absence of
any privacy protection techniques applied to the information. Even though respondents
claimed to be aware of information privacy and data protection law.

2. Methodology
In this section, we will present the methodology used in the conduct of this work such
as the experiment framework, the dataset used, the Experiment setup, the toolbox used, and
the results in discussion. Figure 3 below is the entire work activity diagram.

Begin

Anonymization Operations

Models Taxonomy

Datasets

ARX De-identification Toolbox

Results Discussion

End

Figure 3. Activity Diagram.

Anonymization operations and taxonomy tree has been explained in the previous
section above.

2.1. Experiment Framework

Figure 4 below shows the framework for experimenting. The first process involved in
the framework is New Project where a user must provide the name of the newly created project
before the ARX environment becomes enabled. Importing data is a process also where ARX

Journal of Engineering Science September, 2022, Vol. XXIX (3)

64 A. Shehu, A. Salihu, A. Sani

user brings in .csv datasets for the anonymization process and will only be enabled if a project
is created. The configuration enables the user to create and edit rules, define privacy
guarantees, parameterize the coding model and configure utility measures. While
anonymizing is a process of performing data transformation. Filtering, analyzing the solution
space, and organizing transformations are done through Explore results. The user keeps doing
this process until the anonymized data suits his needs. If the final results are acceptable then,
Analyze Results process is used where the main analysis takes place to compare and analyze
the input and output such as attribute analysis, equivalence class analysis, performing local
recoding, and final results summary. Lastly, the final results are stored for further use and analysis.

Analyze
New Results
Project

Configure Anonymize

Explore
Data Results
Import

Figure 4. Experiment Framework.

2.2. Dataset
To the best of our knowledge, no dataset benchmark is set for the educational domain
and since the ARX anonymization toolbox works with any dataset we chose to use a dataset
collected from one of the institutes of higher learning in Kebbi State, Nigeria, known as
Polytechnic Dakingari. Initially, the dataset contained 260 records which after data cleanup
became 180 records only. Tables 2 and 3 show the overview of the datasets.

Table 2
Overview of the datasets
Dataset Quasi-Identifier Records Highest Transformation Size (KB)
Student 8 180 1,223,040 2

Table 3
Overview of the attributes in the datasets
SA (Distinct
Dataset Quasi-Identifier (height of Hierarchy)
Values)
Student Sex (2), Matric Number (13), invoice (11), Application Department
number (9), State (7), local govt. (12), session (1), status (1) (23)

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 Application of privacy-preserving data publishing in tertiary institutions of Kebbi state using generalization… 65

2.3. Experimental Settings

In this work, the experiments were conducted on a laptop computer running 64-bit
Windows 8 (6.2, Build 9200) with AMD E-300 APU with Radeon (TM) processor at 1.3GHZ
clock speed with 4 GB RAM. As for the five models, this work uses the ARX anonymization
toolbox, to be explained next. Moreover, all the five models and the metrics are implemented
in the toolbox. The research did not perform any pre-computation in the toolbox that can
give an advantage to some models over others.
2.4. Parameter Value
Parameter values of k used in the experiment were recommended as the best
configurations in[5]. As for parameter L values also cannot exceed the distinct values of SA
for a good result, refer to [5] and [2], thus, this research takes care of that. Our work use
recursive (c, l) diversity, where c stands to be constant and l “well represented” sensitive value.
Table 4 below summarizes the configurations used in the experiments carried out.
Table 4
Experimental Configurations
Experiment Parameter Settings Datasets (Size)
Varied Parameter values [ k-value = 3, c =4, l=3 Student (180)
k-value = 5, c =4, l=3
Suppression limit = 10% k-value =7, c =4, l=3
k-value = 9, c =4, l=3
k-value = 11, c =4, l=3]

Varied Parameter values [ k-value = 3, c =4, l=3

k-value = 5, c =4, l=3
Suppression limit =50% k-value =7, c =4, l=3
k-value = 9, c =4, l=3
k-value = 11, c =4, l=3]
2.5. ARX Anonymization Toolbox
ARX - Powerful Anonymization Toolbox is a comprehensive open-source software for
anonymizing sensitive personal data. It supports full-domain generalization, record
suppression, local recoding, and microaggregation [6]. It was developed within three years
by five computer scientists in Germany, refer [7]. For ARX graphical interface refer to [2].

3. Results and Discussion

In this section, the results obtained during the experiments using the configuration
and student dataset above are going to be analyzed and explained about certain quality
metrics such as Granularity, Non-uniform entropy, and Discernibility. Also, some
transformations and anonymization time per run will be presented. The best score is the one
with the lowest score [8].
Granularity. This model collects and presents the granularity of the output dataset.
From the first set of four bars in figure 5 we can see how this model displays two different
sets of results as the suppression limit is 10%. As k = 3 and 5, almost 90% of the output
dataset cannot be identified due to a high level of anonymization. This indicates that when
this data is shared for research purposes, it will provide little utility and hardly achieve
Journal of Engineering Science September, 2022, Vol. XXIX (3)
66 A. Shehu, A. Salihu, A. Sani

research purposes due to high privacy. Similarly, as the k value increased from 3 to 5, the
same results were obtained with no effect. On the other hand, when the k value moved to 7,
9, and 11, we can observe the slightest increase from 91.11% to 95% all through. This no
doubt affects the attribute quality more and made it unworkable by researchers, though
privacy became higher than 3 and 5. But, the effect of the k value became constant as
observed.
In figure 6 below displays results as suppression limit = 50%, indicating attributes level
details are clearer than when suppression was 10%. All the returned results indicate 61%
down. That proves that privacy and quality were balanced.
Non-uniform entropy. This model measures information loss based on common
information in a dataset that measures the amount of information that can be obtained about
the original values of variables in the input dataset by observing the values of variables in
the output dataset. However, the metric makes this quantification for an individual attribute
in the dataset. In the second four bars of figure 5 below, as suppression limit = 10%, we can
also see that as the k value keep increasing from 3 through 7, information loss for the datasets
keeps decreasing, though, with different values of 16.58%, 8.88% and 6.03 % respectively.
However, 6.03% remains constant from k = 7 through 11. Meaning that the datasets cannot
be de-anonymized more than k = 7 and, these values provides minimum loss.
On the other hand, figure 6 presents results as a suppression limit = 50%. It is evident
that as k = 3 and 5, distortion was not much compared to the same values as suppression =
10%. When k = 9, loss of information is almost the same as its counterpart in 10% above. On
the other hand, in the 10% limit, k = 7 and 11 outperformed their counterparts in the 50%
limit.
Discernibility. This measures how identical a record is to others within each
equivalence class by assigning an additional penalty to it equal to the size of the equivalence
class it belongs. For detail refer to [9]. As indicated in the third group of bars in figure 5 as
suppression = 10%, the best scores are when k = 7, 9, and 11 which showed the highest
identicality of the records in the output dataset. And that indicates higher privacy than
quality. But in figure 6 where suppression = 50%, we can also observe the third group of bars
with different scores all less than in figure 5. This indicates not much additional penalty as
there are fewer equivalence classes.
Anonymization Time. This quantifies the time taken to complete transformation per run
and, it measures in seconds. From the last group of four bars in figure 5, we can observe that
as the suppression limit is 10%, the last time was when k=9, followed by k=5. That should not
be unconnected with search space until a global optimum solution was returned. And in these
two values, the time to return was small. We can also see that as k=11, anonymization time
was the longest, because of the time taken to return the global optimum.
In figure 6, when the suppression limit was 50 % we can deduce that k=3 returned the
least anonymization time compared to its counterpart in suppression limit 0f 10 %. This
happened because the privacy has been relaxed the more and returning to global optimum
will not take much time. Also, the rest of the k values here outperformed their counterparts
above with the increase of values even though they maintain consistent values among
themselves. That could be understood that as the suppression limit is relaxed to 50, the
increase of k values has little or no effect on anonymization time unlike when suppression is
tight to 10% which showed different timing due to stricter privacy and suppression.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Application of privacy-preserving data publishing in tertiary institutions of Kebbi state using generalization… 67

100
90
80
70

Percentage[%]
60
50
40
30
20
10
0
Granularity N-U. Entropy Discernability Anonimzation
Time

K=3 K=5 K=7 K=9 K=11

Figure 5. Suppression limit of 10%.

70

60

50
Percentage [%]

40

30

20

10

0
Granularity N-U. Entropy Discernability Anonimzation
Time

K=3 K=5 K=7 K=9 K=11

Figure 6. Suppression limit of 50%.

In [10] three privacy models were compared based on information loss metrics. The
experiment was conducted using three datasets of which the largest among them contains
16, 422 tuples. In their work, it was concluded that t-closeness has better utility compared to
k-anonymity and l-diversity. Yadav compared only two models and the dataset was unknown
[11]. Execution time was measured, and it was concluded that k-anonymity outperformed l-
diversity. In the work of [8], five privacy models were compared out of which one of them-
slicing is the anonymization technique and not the privacy model [12]. Furthermore, only one
benchmark dataset was used in the work but with a larger size (640,000 records). It was
reported that k-anonymity outperformed the rest in terms of execution time. On the other
hand, slicing was the worst performer. Prasser et al. present a comprehensive theoretical
review of the three most prominent privacy models in big data. The advantages and
limitations of these models were stated therein. Though, their proposed solutions can only
work where there is only one sensitive attribute in the dataset.
In a model proposed by [13] that data utility can be increased and maintain significant
privacy based on the outlier equivalence class. K-anonymity and l-diversity were used but,

Journal of Engineering Science September, 2022, Vol. XXIX (3)

68 A. Shehu, A. Salihu, A. Sani

with the single configuration of 5 and 2 respectively. In their work, two datasets were used
with a suppression limit of 100%. However, their work was conducted using ARX 3.5.1
environment. Also [14], proposed a model based on superclass substitution for utility
improvement on k-anonymity. Their model proved better quality than the other two.
Furthermore, a student admission dataset was used. In a similar research effort by [15], four
privacy models were used made in a single framework-ARX. The beauty of this work is that
various parameter values were used to ascertain the correctness and validity of the result.
Though the metric used during the analysis was also four, the dataset is non-educational, and
the factor of study is information loss as parameter values changes. The authors in [16] used
adult dataset from UCI machine learning repository which was partitioned into five groups
from 40000 to 640000 records. On each set of group, five different privacy models were run
against execution time and data utility. Though from their work non-of the model
outperformed others from all angles.
Based on this literature, we can confirm that none of the work mentioned above has
categorically used a dataset from the educational domain, and none used the quality model
of Granularity, Non-uniform Entropy, and Discernibility. Also, none of them used this set of
configurations in the ARX environment based on suppression limits of 10 and 50%
respectively.

4. Conclusions
In this research, it could be concluded that the higher the suppression limit the more
balance exists between privacy and utility. Also, it was observed that the suppression limit of
50% provides less anonymization time in respective k values compared to k values in
suppression = 10%. This was proved to be due to less time it takes anonymization to search
and return a globally optimum solution. Conclusively, we can say that the suppression limit
of 10% does not provide a balance between privacy and quality. However, the work observed
that 92% of the students, records faced privacy threats as there was no privacy policy
implemented on data at rest or during sharing with a third party in all Kebbi State educational
institutions. Additionally, none of the respondents has a clear view of what privacy is all
about. We note also that all the respondents misunderstood data privacy with data
confidentiality. Therefore, there is a need for stakeholders in all the institutions to educate
data holders about privacy and privacy-enhancing technologies.

Conflict of interest. The authors declare no conflict of interest.

References
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identification. BMC Medical Informatics and Decision Making 2016, pp. 1 - 14.
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Dimensional Data. Transactions on data privacy 2016, 9, pp. 161 - 185.
3. Narula, D.; Kumar, P.; Upadhayaya, S. Performance Evaluation of K-Anonymization Algorithms for Generalized
Information Loss. IJCTA 2016, pp. 227 - 235.
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Institutions of Kebbi State Using K-Anonymity. International Journal of Innovative Science and Research
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5. Kohlmayer, F.; Prasser, F.; Kuhn, K.A. The cost of quality : Implementing Generalization and Suppression for
Anonymizing Biomedical Data With Minimal Information Loss. Journal of Biomedical Informatics 2015, 58, pp.
37 - 48.

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Citation: Shehu, A.; Salihu, A.; Sani, A. Application of privacy-preserving data publishing in
tertiary institutions of Kebbi state using generalization and suppression. Journal of Engineering
Science 2022, 29 (3), pp. 59-69. https://doi.org/10.52326/jes.utm.2022.29(3).05.

Publisher’s Note: JES stays neutral with regard to jurisdictional claims in published maps and
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Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
and conditions of the Creative Commons Attribution (CC BY) license
(https://creativecommons.org/licenses/by/4.0/).

Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 70 - 77
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Computers and Information Technology eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).06
UDC 659.133:004.353.254.5

INTEREST BASED ADAPTIVE BILLBOARD CONTENT MANAGEMENT

Victor Moraru*, ORCID: 0000-0002-5454-8341,

Viorel Cărbune, ORCID: 0000-0002-1556-4453

Technical University of Moldova, 9/7 Studenţilor street, MD-2045, Chisinau, Republic of Moldova
*Corresponding author: Victor Moraru, [email protected]

Received: 05. 28. 2022

Accepted: 06. 30. 2022

Abstract. The street advertising has undergone some significant changes in recent years:
traditional billboards are gradually being replaced by electronic display devices (LED screens)
that are able to change in real-time the broadcast advertising, thus allows the dynamic
content management. This paper aims to develop an adaptive advertising strategy based on
the preferences of the people in front of the screen. Each of them has a special application
installed on their personal smartphone through which they can configure their interests
regarding the broadcast advertising. These interest profiles are then collected by billboards
which, based on them, select the most appropriate type of ad to run at that time. The
proposed method focus on transformation of a simple display equipment into an intelligent
one, capable of adapting the broadcast content to the requirements of the nearby audience
and aims to maximize the efficiency of the billboard operation and at the same time bring
maximum satisfaction to the target audience. The performance of the method was evaluated
using agent based computer simulation.

Keywords: adaptive content management, digital advertising screens, street advertising.

Rezumat. Publicitatea stradală a suferit câteva schimbări semnificative în ultimii ani:

panourile tradiționale sunt înlocuite treptat cu dispozitive electronice de afișare (ecrane LED)
care sunt capabile să modifice în timp real publicitatea difuzată, permițând astfel gestionarea
dinamică a conținutului. Această lucrare își propune să dezvolte o strategie de publicitate
adaptativă bazată pe preferințele oamenilor din fața ecranului. Fiecare dintre ei are instalată
pe smartphone-ul personal o aplicație specială prin care își pot configura interesele cu privire
la publicitatea difuzată. Aceste profiluri de interes sunt apoi colectate de panouri publicitare
care, pe baza lor, selectează cel mai potrivit tip de anunț pentru a rula în acel moment. Metoda
propusă se concentrează pe transformarea unui echipament simplu de afișare într-unul
inteligent, capabil să adapteze conținutul difuzat la cerințele publicului din apropiere și are
ca scop maximizarea eficienței operațiunii panoului publicitar și, în același timp, să aducă
satisfacție maximă țintei public. Performanța metodei a fost evaluată folosind simularea
computerizată bazată pe agenți.

Cuvinte cheie: management adaptiv al conținutului, ecrane de publicitate digitală, publicitate

stradală.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 V. Moraru, V. Cărbune 71

1. Introduction
Street or outdoor advertising, called more recently out of home (OOH) advertising is
one of the oldest and simplest methods of promoting products and services. Street
advertising is usually represented by billboards designed to display information about
products, manufacturers, sellers, services, locations, etc. [1]. They are managed by specialized
companies which display that information for a certain period of time. The advertising
companies are interested in implementation of new display strategies in order to reach as
wide audience as possible and to increase in this way their profits.
In the Republic of Moldova, OOH accounts for approximately 20% of the advertising market
volume. The street advertising market in Moldova offers more than 10 formats (billboard, big-
board, city-light, LED screens, cubes, clocks, panels, banners, light-boxes at public transport
stations, etc.). Also, the street advertising market in the Republic of Moldova has more than
10 operators with a total of over 6000 different advertising billboards.
Advantages of the street advertising:
● More than 70% of people spend most of their time outside their homes.
● Street advertising is the best cost-effective advertising method.
● It has a high visual impact on the people compared to other advertising sources:
print media, online press, shops, telephone.
● Continuous display of the message 24/24 hours for all nearby pedestrians and all
cars in traffic in the area with the possibility to reach busy, active, and moving
people. Statistics show that we spend an average of 1.3 hours per day on the street.
● It is free and doesn't require specific technical means to access it.
● It reaches a lot of nearness people without requiring significant investments.
A more detailed analysis of this topic can be found in [1, 2].
The main disadvantages of the traditional street advertising are the inability to select the
target audience and the extremely low volume of disseminated information (laconic text of
up to 2-3 sentences, some images, etc.) without the possibility to provide details [3].
Among the factors influencing the efficiency of the billboard are its location, the quality of
the content presentation, and, last but not least, the coherence between the broadcasted
content and the existing at that time audience near the billboard. As the everyday audience
is very heterogeneous, it is practically impossible for traditional billboards to adapt the
broadcasted content to present people. More recently, one of the most important factors for
increasing efficiency is the use of digital display equipment, its impact on the audience being
about 2.5 times higher compared to traditional display. These equipments have marked a new
era in the development of the street advertising known as Digital Out Of Home advertising
(DOOH) and which offer great possibilities compared to the classic methods. The DOOH was
stormy developed in recent years [4, 5].
A lot of new approaches for advertising management based on DOOH technologies
have been proposed aiming to improve the effectiveness and to touch better the targeted
audience [6-9]
This article proposes an innovative person-centric adaptive method (according to
classification proposed in [10]) of organizing street advertising which, been based on modern
technological displaying equipment and smart technologies, is able to collect the information
about the composition of the people in front of the billboard and adapts in real time the
broadcasted content to the interest of as many as possible people.

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72 Interest based adaptive billboard content management

2. Description of the proposed method

In this article we will analyze the operation of a billboard with digital display (LED
screen, plasma screen, projector, etc.) on which are displayed advertising information that is
perceived by pedestrians passing in front of the billboard (Figure 1).

Figure 1. Traditional billboard.

The efficiency of this approach is relatively low for the simple reason that the same
information is disseminated for a long time (weeks or even months) and the public passing
on the street tends to be largely the same (people leaving and returning home from service,
those walking through the street near the house, etc.). The proportion of these people can be
considerable, reaching in some cases 80-90%. Which means that the informative value of the
display decreases day after day, hence the low efficiency of this approach. It depends largely
on the location of the billboard and can be quite high in places where the public varies a lot
every day (near stations, markets, shopping malls, etc.).
Equipping the billboard with a digital display screen greatly reduces these problems
because the information displayed can be changed more often, thus maintaining pedestrians'
interest in it. The advertising company can run advertising for several products for the same
duration, which leads to a considerable increase if the revenue.
The proposed method aims to increase the efficiency of the billboard by adapting in
real time the strategy of the content dissemination to the surrounding public. Assuming that
the most part of pedestrians have a smartphone capable to connect to WiFi wireless network
(IEEE 802.11), this equipment can be used, in addition to all, as a source of information about
the preferences of its owner. In order to define his preferences, the user will be asked to
install on his phone a mobile application available in the store (Google Play for Android
operating system and iTunes for Apple products). That proposal should be attractive in order
to interest the user to accept it (a smart marketing solution is required here). It could also
include other useful services (eg weather forecast display, exchange rate, etc.). When
installing the application, a questionnaire will be launched. By answering the asked questions
(checking the answers in a proposed list) the user will create his profile that will specify his
preferences and interests. This mobile profile that doesn't contain any personal information
(name, phone number, address, email, etc.) may be broadcasted on-demand if requested by
another application on the network or may be continuously broadcasted by the application
in order to discover certain services in the proximity network (for example, to search in the
network some people with similar preferences). It is very important to establish the structure
of the questionnaire, which should be neither too voluminous with the risk of boring the user

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 V. Moraru, V. Cărbune 73

when completing it, nor too short to avoid an incomplete and uninformative profile. In order
to simplify the structure of the questionnaire, users' preferences will be divided into
categories (e.g. sports products, mobile phones, women's clothing, footwear, household
appliances, etc.). The user profile will be specified through a list of selected categories in the
questionnaire. It will start with the most favorite categories followed by others arranged in
descending order according to the degree of the preference. It may also be proposed to set
the weights for each category in the list. The definition of the content and of the optimal
structure of the questionnaire requires a more rigorous analysis and will not be discussed
further in this article. The simplest strategy for running advertising is to use a circular
algorithm (Round Robin type) displaying the advertising one by one for a certain duration for
each of the categories on the server. The same policy can be applied to products that fall into
the same category. This method is a traditional one and ensures an equal display time for
each product in the long run. It is not adaptive and does not take into account the audience
composition next to the billboard. Its only advantage is the simplicity and the fairness of the
display resources sharing between the promoted products.
One way to improve the efficiency of this system would be to adapt the broadcasted
content to the preferences of the audience near the billboard. For this purpose, it is proposed
to equip the advertising screen with a WiFi access point that will be open (unsecured) and
that will support the connection without security key of any equipment in the radio sensitivity
area with a radius that can reach up to 100 meters. Given the omnidirectional nature of radio
coverage for traditional access points, the billboard should be installed at the side of the road
so that pedestrians pass only in front of it and not have the rear access. Another solution
would be to use a directed broadcast access point (which transmits and receives radio waves
only in a certain direction or which uses shielding elements to limit emissions/receptions
in/from unwanted directions). The panel will also contain a server with some installed
applications for ensuring the logic of the system work, including a video streaming server
and the information to be broadcasted. The advertised content may be modified in real time
through the network. The information about the promoted products is classified in the same
categories that were specified in the questionnaire. When it is decided to launch the display
of a certain category, a product in this category will be selected according to a predefined
algorithm and that information will be displayed on the screen.
When the pedestrian enter into the radio sensitivity area near the panel he will
automatically connect to the access point and the server will receive his profile. The
appearance of the pedestrian will be counted by entering his profile in a list and by increment
a variable that corresponds to the number of present users in front of the billboard. From this
moment the server will start monitoring the presence of the respective equipment in the
sensitivity area, this being possible because its IP address is known being assigned to it by
the DHCP server on the access point. Presence monitoring is done by transmitting through
the network at regular intervals of short messages (pings) to which the mobile equipment
will respond confirming its presence. From the moment when no confirmations are received
from the respective mobile phone, it is removed from the list and the presence variable is
decremented. The proposed system is shown in Figure 2. Pedestrians move in the billboard
direction, reach the sensitivity area and then leave it continuing their way.
Given that we have N categories of advertising, we expect to have near the panel up
to N groups of pedestrians, each of which will correspond to one of the categories defined
above.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

74 Interest based adaptive billboard content management

Figure 2. Billboard with adaptive content management.

The groups are monitored separately to know in real time the number of pedestrians
in each of them. The application that manages the advertising display performs the following
functions: receives user profiles with their preferences and interests, continuously monitors
their presence, counts the audience in the area of radio sensitivity, makes decisions about
real-time content be displayed on the advertising screen, etc. For simplicity, we'll assume
that the ad delivery time for all products in all categories is the same (for example, 30
seconds). That means the information displayed on the screen must change every 30 seconds
regardless of the evolution of other factors.
The decision on the content been broadcasted in the next time interval is based on
the data collected in the previous interval. Advertising will be broadcasted for the category
that has the largest presence in front of the panel and at the same time information will be
collected about the composition of the audience that will be used in the next time slot.
3. Effectiveness estimating of the method
The methods of advertising effectiveness estimation are very different: from
conducting a survey on its quality [11] to assessing its impact on the sales volume of the
advertised products [12]. In this article we will use a specific evaluation method based on
results obtained by simulation, that would show us the efficiency of our method in relation
to other methods. We aimed to use an agent-oriented approach for simulation [13] and to
implement our model using a specialized software: GAMA platform [14,15], a modeling and
simulation development environment for building spatially explicit agent-based simulations.
This approach makes possible to describe each agent and its spatial movement through its
attributes and behavior. In this case, each pedestrian and the ads screen are represented by
specific agents that interact with each other, thus realizing the logic of the system operation.
We have to define some technical parameters of the analyzed system before the
simulation. We will simplify the initial model described in the previous chapter by reducing
the number of advised product categories to 4 assuming that a user can request only one
category (the simplest case). Consequently, we will have only 4 groups of pedestrians who
will move in both directions in front of the billboard. The sensitivity area will be a square
with the size 50x50 meters, the speed of pedestrians will be from 0.5 m/s (slow pedestrians)
to 1.5 m/s (fast pedestrians). The pedestrian speed and his moving direction will be chosen
randomly. Pedestrian arrivals are independent, there are 4 types of pedestrians (one for each
category). Pedestrians can move in any direction, they are counted at the entrance on the
sensitivity area and at the exit of this area.
In Figure 2 the product categories are coded by color: we have pedestrians belonging
to each of the 4 categories (so 4 different colors or gray degrees in our case) and the screen
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 V. Moraru, V. Cărbune 75

can also broadcast 4 categories of advertising that correspond to those colors (the color of
the light on the screen in Figure 2 corresponds to the color of the broadcast category at a
certain time). We will set the duration of a time slot equal to 30 seconds (it corresponds to
the duration of the advertisement for a product belonging to one of the categories), and the
simulation time in the example analyzed below is 700 minutes. The simulation environment
and the respective process are shown in Figure 3: pedestrians cross the sensitivity area of the
billboard moving in arbitrary directions. The system monitors and counts these movements
and establishes the category of advertising currently broadcasted taking into account the
largest group (the color of the square that corresponds to the ads screen in Figure 3).

Figure 3. Simulation environment and the system simulation (pedestrian movement,

dynamic content changing) in GAMA platform.
In Figure 4 are shown the evolution of the groups and the state of the screen: at the
top is the number of pedestrians in the 4 groups (4 different colors), and at the bottom are
presented the timers for each time slot, their color indicates the category advertising
displayed on the screen in that time slot.

Figure 4. The evolution of the groups and of the screen status over the time.
During the simulation for each pedestrian we will calculate the satisfaction index
defined by the ratio between the display time of his favorite advertisement and the total
duration of his presence in the sensitivity area in front of the screen. The range of variation
of this index: [0,1]. The average of these values will be used to estimate the overall system
performance index: the overall average satisfaction. The index allows us to compare different
system configurations: the larger it is, the more efficient is the system.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

76 Interest based adaptive billboard content management

Following the long-term similar simulation of the system described above and the one with
circular screen allocation, it turned out that the first one is on average 15-20 percent more
efficient than the Round Robin system.
4. Conclusions
The main purpose of the article is to propose a solution that would allow an adaptive
management of the content broadcast through billboards based on digital display equipment
using information collected in real time about the preferences and the interests of the people
in front of the screen. The obtained results are encouraging, they demonstrate the feasibility
of the proposed method and its adaptability in real time. The new proposed performance
index allows the comparison of results for different configurations of the analyzed system.
In the future, a more detailed and realistic simulation of the proposed method is foreseen:
several product categories and profiles with multiple weighted preferences, more complex
pedestrian flows with grouped arrivals, studying the possibility of integrating the method at
the level of billboard network.
The paper was presented at the works of the conference ECCO 2021.
Conflicts of Interest. The authors declare no conflict of interest.
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10.05.2022]. Disponibil: https://repositorium.sdum.uminho.pt/handle/1822/18875
10. Bauer, C.; Lasinger, P. Adaptation strategies to increase advertisement effectiveness in digital media.
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11. Mehta, A. Advertising Attitudes and Advertising Effectiveness. Journal of advertising research 2000, 40(3),
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13. Ioretti, G. Agent-based simulation models in organization science. Organizational research methods 2013,
16(2), pp. 227-242.
14. Drogoul, A.; Amouroux E.; Caillou P.; Gaudou B; Grignard A.; Marilleau N.; Taillandier P.; Vavasseur M.; Duc-
An V.; Zucker J-D. GAMA: A Spatially Explicit, Multi-level, Agent-Based Modeling and Simulation Platform. In:
International Conference on Practical Applications of Agents and Multi-Agent Systems. Springer, Berlin,
Heidelberg, 2013. pp. 271-274.
15. GAMA platform [on-line]. [accesat 20/11/2021], Disponibil: https://gama-platform.github.io/.

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 V. Moraru, V. Cărbune 77
Citation: Moraru, V.; Cărbune, V. Interest based adaptive billboard content management. Journal of
Engineering Science 2022, 29 (3), pp. 70-77. https://doi.org/10.52326/jes.utm.2022.29(3).06.

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Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 78 - 85
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Computers and Information Technology eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).07
UDC 004.89:338.49:711

SMART CITY SERVICES BASED ON SPATIAL-TEMPORAL LOGIC

Ana Turcan1, ORCID: 0000-0002-9334-7606,

Victor Ababii1*, ORCID: 0000-0002-0769-8144,
Viorica Sudacevschi1, ORCID: 0000-0003-0125-3491,
Radu Melnic1, ORCID: 0000-0002-3709-4739,
Victoria Alexei1, ORCID: 0000-0003-4560-3131,
Silvia Munteanu1, ORCID: 0000-0003-0749-8457,
Constantin Ababii1,2, ORCID: 0000-0002-6599-3811
1
Technical University of Moldova, 168 Stefan cel Mare blvd., Chișinău, Republic of Moldova
2
IAW Internationale Akademie, Brigachtal, Germany
*Corresponding author: Victor Ababii, [email protected]

Received: 06. 22. 2022

Accepted: 09. 05. 2022

Abstract. The development and research of Smart City Service Systems is a very important
area for the future of mankind. The urbanization process imposes new criteria for qualitative
and quantitative assessment of population well-being, which will involve processing a very
large volume of information, organizing the data exchange and processing. This paper
proposes a Multi-Agent Smart City Services system based on Spatial-Temporal logic. In order
to optimize the criteria for the qualitative and quantitative evaluation of services, the set of
agents is divided into: the subset of agents that deliver services and the subset of service
consumers agents. The system diagram, the synthesis of the agents, the operators of temporal
and spatial logic was elaborated. The relationship between the subset of service delivery
agents and the subset of agents of service consumers is determined by game theory models.
Keywords: Spatial - Temporal Logics, Distributed Computing, Multi-Agent Systems, Swarm
Intelligence, Collective Decision Making, Game Theory, Knowledge Bases.
Rezumat. Dezvoltarea și cercetarea sistemelor Smart City Service prezintă un domeniu foarte
important pentru viitorul omenirii. Procesul de urbanizare impune noi criterii de evaluare
calitativă și cantitativă a bunăstării populației, care va implica procesarea unui volum foarte
mare de informații, organizarea schimbului de date și procesarea acestora. În lucrarea de față
se propune un sistem Multi-Agent Smart City Services bazat pe logica Spațial-Temporală.
Pentru optimizarea criteriilor de evaluare calitativă și cantitativă a serviciilor, mulțimea de
agenți este divizată în: sub-mulțimea de agenți care livrează servicii și sub-mulțimea de
agenți consumatori de servicii. A fost elaborat diagrama sistemului, sinteza agenților,
operatorii de logică temporală și spațială. Relațiile dintre sub-mulțimea de agenți care
livrează servicii și sub-mulțimea de agenți consumatori de servicii este determinată de
modele din teoria jocurilor.
Cuvinte chee: Logica Spațial-Temporală, Calcul Distribuit, Sisteme Multi-Agent, Inteligența
Roiului, Luarea Deciziilor Colective, Teoria Jocurilor, Baze de Cunoștințe.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 A. Turcan, V. Ababii, V. Sudacevschi, R. Melnic, V. Alexei, S. Munteanu, C. Ababii 79

1. Introduction
The smart city can be defined as a set of services offered by a distributed computing
system that explores large volumes of data and applies communication technologies in order
to improve the quality of life of its citizens. The target objectives of the services offered by
the smart city are oriented towards the application of knowledge bases and databases, at the
same time being based on information provided by its citizens online. The paper [1] proposes
a Smart City Service System that is implemented as an ontology-oriented system, which
ensures decision-making based on reasoning and inference, and provides objective
information characteristic of the situation in the city.
Designing a smart city is a long and complex process because it involves human,
financial, technical and technological essential resources. In order to meet the requirements
of the Smart City Service System, a holistic approach on the management process is necessary
[2, 3], where service is the basic concept, or rather the element of interaction between the
actors involved in the decision-making process (citizens, administration, enterprises,
organizations, etc.).
The smart city system, in order to provide the most relevant information, requires the
application of decision-making models’ knowledge based or cognitive. A cognitive system has
a complex structure that has the ability to self-develop by accumulating new information and
knowledge in the process of evolution in space and time [4, 5].
Since the Smart City Service System has a spatially distributed structure, it is obvious
that models based on architectures of distributed computing, parallel or cloud are applied for
data processing [6-8]. At the same time, it can be mentioned that the same performance
features are offered by Multi-Agent systems [9, 10] and collective / collaborative systems for
decision-making [11], based on Artificial Intelligence methods and models [12, 13].
The smart city being a dynamic system that evolves in space and time requires a
special approach to apply decisional models based on spatial-temporal logic in which
geographical position and time to play a decisive role in decision making. In parallel with the
definition of spatial-temporal logic, also appears the notion of event that takes place in space
and time. Temporal logic also plays a very important role in agency theory, a field of science
where the integration between philosophy, computer science and game theory takes place
which provides paradigms for researching Multi-Agent systems that make decisions and gain
new knowledge in real time [14]. The problem of combining and the relationship between
spatial logic and temporal logic is analyzed in paper [15] which addresses how computational
complexity and the expressive power of component logic are related to the complexity and
expressiveness of spatial-temporal logic.
This paper proposes a method of applying spatial-temporal logic for the development
of Smart City Service Systems. The system represents a distributed computing architecture
consisting of a set of Agents working together aiming to solve a common problem. The set
of agents is divided into two subsets: the first is the subset of Agents that deliver services,
the second subset are the agents that request services. These two subsets are always in the
process of concurrency the balance between which is regulated by the Nash Equilibrium [16].

2. Synthesis of the Diagram for Smart City Service System

Nature-based computing provides a designer with the most efficient methods and
models for developing complex systems, especially Smart City Service systems, which can be
considered as multi-dimensional and dynamic systems in space and time. Therefore, solving

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80 Smart City Services based on Spatial-Temporal Logic

the problem of finding the optimal solution in the definition space requires the involvement
of essential resources for processing a very large volume of data coming from a lot of
heterogeneous sensors or stored on distributed systems. Reducing the complexity of these
systems can be achieved by applying computational models based on intelligence agents and
evolutionary algorithms [17-19] with distributed or concurrent data processing.
The Spatial-Temporal Diagram of the Smart City Service System is shown in Figure 1,
where: 𝑆𝑆𝑆𝑆𝑆𝑆 - Service Delivery Agent; 𝑆𝑆𝑆𝑆𝑆𝑆 - Service Consumer Agent; 𝐺𝐺𝐺𝐺𝐺𝐺 - Global Positioning
System; 𝐺𝐺5- Fifth-Generation Technology Standard for Mobile Communications.
Let be in the activity space 𝑆𝑆 ⊂ (𝑅𝑅𝐾𝐾 ∪ 𝑋𝑋 ∪ 𝑌𝑌 ∪ 𝑍𝑍 ∪ 𝑇𝑇) the Multi-Agent decisional
distributed system is defined:
𝐴𝐴𝑆𝑆 = {𝑆𝑆𝑆𝑆𝑆𝑆, 𝑆𝑆𝑆𝑆𝑆𝑆, 𝐺𝐺𝐺𝐺𝐺𝐺, 𝐺𝐺5}, (1)
where: 𝐾𝐾 are the total set of services and parameters defined for the Smart City activity;
𝑋𝑋, 𝑌𝑌, 𝑍𝑍 are the spatial coordinates of the agent; 𝑇𝑇 is the time coordinate; 𝑆𝑆𝑆𝑆𝑆𝑆 =
{𝑆𝑆𝑆𝑆𝐴𝐴𝑛𝑛 , 𝑛𝑛 = �����
1, 𝑁𝑁} is the set of Agents that deliver services; 𝑆𝑆𝑆𝑆𝑆𝑆 = {𝑆𝑆𝑆𝑆𝐴𝐴𝑚𝑚 , 𝑚𝑚 = ������
1, 𝑀𝑀} is the set
of mobile or stationary agents of services consumers; 𝐺𝐺𝐺𝐺𝐺𝐺 is global positioning system that
provides information for the spatial positioning of agents; 𝐺𝐺5 is the communication system
that ensures the transfer of data between the set of agents and the temporal synchronization.

- SDA Module

- SCA Module

- SCA Mobile
U N I V E R S I T Y
Module

Cloud
Service
SCA G5

SDA
SCA
Cartier

G5
SDA

SDA

G5

Cathedral
SDA

SCA G5

G5

Figure 1. Spatial-Temporal Diagram of the Smart City Service System.

3. Agent Synthesis
The Smart City Service System includes two types of Agents: 𝑆𝑆𝑆𝑆𝑆𝑆 - Service Delivery
Agents and - Service Consumer Agents.

3.1. Service Delivery Agent Synthesis

The functional model [22,24] of the Service Delivery Agent is defined by the
expression (2):

𝐴𝐴𝑆𝑆𝑆𝑆𝑆𝑆 = �𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] , 𝐾𝐾𝐾𝐾[𝑇𝑇], 𝑆𝑆𝑆𝑆: (𝐸𝐸𝐸𝐸 [𝑇𝑇], 𝑇𝑇𝑇𝑇𝑇𝑇[𝑇𝑇], 𝑆𝑆𝑆𝑆𝑆𝑆[𝑇𝑇], 𝑆𝑆𝑆𝑆[𝑇𝑇])�, (2)

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. Turcan, V. Ababii, V. Sudacevschi, R. Melnic, V. Alexei, S. Munteanu, C. Ababii 81

where: 𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] - the request coefficient for the services offered by SDA for SCA; 𝐾𝐾𝐾𝐾[𝑇𝑇] - the
knowledge [20,23] base available to the SDA agent at the time 𝑇𝑇; 𝑆𝑆𝑆𝑆 - data processing logic
applied by the SDA agent; 𝐸𝐸𝐸𝐸 [𝑇𝑇] - the set of events used by the SDA agent for data processing
for the purpose of delivering quality services to SCA agents; 𝑇𝑇𝑇𝑇𝑇𝑇[𝑇𝑇] - temporal logic operators
used for data processing; 𝑆𝑆𝑆𝑆𝑆𝑆[𝑇𝑇] - spatial logic operators used for data processing; 𝑆𝑆𝑆𝑆[𝑇𝑇] -
the multitude of services offered by the SDA agent at the time 𝑇𝑇.
3.2. Service Consumer Agent Synthesis
The functional model of the Service Consumer Agent is defined by the expression (3):
𝐴𝐴𝑆𝑆𝑆𝑆𝑆𝑆 = �𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] , 𝐾𝐾𝐾𝐾[𝑇𝑇], 𝑆𝑆𝑆𝑆: (𝑆𝑆𝑆𝑆[𝑇𝑇], 𝑇𝑇𝑇𝑇𝑇𝑇[𝑇𝑇], 𝑆𝑆𝑆𝑆𝑆𝑆[𝑇𝑇], 𝑆𝑆𝑆𝑆[𝑇𝑇])�, (3)
where: 𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] - the quality coefficient of the services used by SCA provided by SDA; 𝐾𝐾𝐾𝐾[𝑇𝑇] -
the knowledge [20,23] base available to the SCA agent at the time 𝑇𝑇; 𝑆𝑆𝑆𝑆 - data processing
logic applied by the SCA agent; 𝑆𝑆𝑆𝑆[𝑇𝑇] - the set of services provided by SDA agents used by
the SCA agent for data processing; 𝑇𝑇𝑇𝑇𝑇𝑇[𝑇𝑇] - temporal logic operators used by the SCA agent
for data processing; 𝑆𝑆𝑆𝑆𝑆𝑆[𝑇𝑇] - spatial logic operators used by the SCA agent for data
processing; 𝑆𝑆𝑆𝑆[𝑇𝑇] - the result of the evaluation of the quality of the services used by the SCA
agent.

4. Temporal Logics Operators

Temporal logic operators [21] present mathematical models for events
processing 𝐸𝐸𝐸𝐸 [𝑇𝑇]. The model and basic components of an operator are specified in the
expression (4):
𝑂𝑂(𝜏𝜏): {𝑂𝑂𝑝𝑝1 (𝜏𝜏), 𝑂𝑂𝑝𝑝2 (𝜏𝜏), . . . , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝜏𝜏)}, (4)
where: 𝑂𝑂𝑝𝑝𝑖𝑖 (𝜏𝜏), 𝑖𝑖 = �����
1, 𝐼𝐼 is the set of operands involved in the operator 𝑂𝑂 (𝜏𝜏).
The operand model is defined by the expression (5):
𝑂𝑂𝑝𝑝𝑖𝑖 (𝜏𝜏) = {𝐸𝐸𝑣𝑣𝑖𝑖 [𝑇𝑇], 𝑝𝑝𝑖𝑖 (𝑡𝑡)}, 𝑖𝑖 = �����
1, 𝐼𝐼 , (5)
where: 𝑝𝑝𝑖𝑖 (𝑡𝑡) is the coefficient of decisional influence of the event 𝐸𝐸𝑣𝑣𝑖𝑖 [𝑇𝑇] within the
operand 𝑂𝑂𝑝𝑝𝑖𝑖 (𝜏𝜏).
For the evaluation of the coefficients 𝑝𝑝𝑖𝑖 (𝑡𝑡) three models of temporal evolution are
defined: events in the past, events in the present and events in the future.
The mathematical model for calculating the coefficients of decisional influence for
past events 𝑝𝑝𝑖𝑖𝑡𝑡 (𝑡𝑡) is performed based on the formula (6):
��������
𝑝𝑝𝑖𝑖𝑡𝑡 (𝑡𝑡) = 𝐸𝐸𝑣𝑣𝑖𝑖 [𝑇𝑇]⁄(𝑘𝑘 + 𝑡𝑡 2 ⁄𝛽𝛽 ) , 𝑡𝑡 = 𝑇𝑇, +∞. (6)
The mathematical model for calculating the coefficients of decisional influence for
present events 𝑝𝑝𝑖𝑖𝑝𝑝 (𝑡𝑡) is performed based on the formula (7):
𝑝𝑝𝑖𝑖𝑝𝑝 (𝑡𝑡) = 𝐸𝐸𝑣𝑣𝑖𝑖 [𝑇𝑇]⁄(𝑘𝑘 + 𝑡𝑡 2 ⁄𝛽𝛽) , 𝑡𝑡 = −∞,
�����������
+∞. (7)
The mathematical model for calculating the coefficients of decisional influence for
future events 𝑝𝑝𝑖𝑖𝑣𝑣 (𝑡𝑡) is performed based on the formula (8):
𝑝𝑝𝑖𝑖𝑣𝑣 (𝑡𝑡) = 𝐸𝐸𝑣𝑣𝑖𝑖 [𝑇𝑇]⁄(𝑘𝑘 + 𝑡𝑡 2⁄𝛽𝛽 ) , 𝑡𝑡 = ��������
−∞, 𝑇𝑇. (8)
In formulas (6), (7) and (8) are mentioned: 𝐸𝐸𝑣𝑣𝑖𝑖 [𝑇𝑇] the event underlying that operand;
𝑘𝑘 is the coefficient of credibility; 𝑡𝑡 is the time interval in which the coefficient of decisional
influence is evaluated; 𝛽𝛽 is the coefficient of decision stability.
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82 Smart City Services based on Spatial-Temporal Logic

The list of temporal logical operators is defined according to the functionality of the
Smart City System. The following are some examples of temporal logic operators present in
the most Smart City Systems:
1) 𝑂𝑂(∨𝜏𝜏 ) = max{𝑂𝑂𝑝𝑝1 (𝜏𝜏), 𝑂𝑂𝑝𝑝2 (𝜏𝜏), . . . , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝜏𝜏)};
2) 𝑂𝑂(∧𝜏𝜏 ) = min{𝑂𝑂𝑝𝑝1 (𝜏𝜏), 𝑂𝑂𝑝𝑝2 (𝜏𝜏), . . . , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝜏𝜏)};
3) 𝑂𝑂(∪𝜏𝜏 ) =∪ {𝑂𝑂𝑝𝑝1 (𝜏𝜏), 𝑂𝑂𝑝𝑝2 (𝜏𝜏), … , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝜏𝜏)};
4) 𝑂𝑂(∩𝜏𝜏 ) =∩ {𝑂𝑂𝑝𝑝1 (𝜏𝜏), 𝑂𝑂𝑝𝑝2 (𝜏𝜏), … , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝜏𝜏)};
5. Spatial Logics Operators
Spatial logic operators present mathematical models for event processing 𝐸𝐸𝐸𝐸 [𝑠𝑠],
where 𝑠𝑠 ⊂ (𝑋𝑋 ∪ 𝑌𝑌 ∪ 𝑍𝑍). The model and basic components of an operator are specified in the
expression (9):
𝑂𝑂(𝑠𝑠): �𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), . . . , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠)�, (9)
where: 𝑂𝑂𝑝𝑝𝑗𝑗 (𝑠𝑠), 𝑗𝑗 = ����
1, 𝐽𝐽 is the set of operands involved in the operator 𝑂𝑂(𝑠𝑠) and 𝑠𝑠 =
�(𝛥𝛥𝛥𝛥 )2 + (𝛥𝛥𝛥𝛥)2 + (𝛥𝛥𝛥𝛥)2 .
The operand model is defined by the expression (10):
𝑂𝑂𝑝𝑝𝑗𝑗 (𝑠𝑠) = �𝐸𝐸𝑣𝑣𝑗𝑗 [𝑠𝑠], 𝑝𝑝𝑗𝑗 (𝑠𝑠)�, 𝑗𝑗 = ����
1, 𝐽𝐽,(10)
where: 𝑝𝑝𝑗𝑗 (𝑠𝑠) is the coefficient of decisional influence of the event 𝐸𝐸𝑣𝑣𝑗𝑗 [𝑠𝑠] within the
operand 𝑂𝑂𝑝𝑝𝑗𝑗 (𝑠𝑠).
For the evaluation of the coefficients 𝑝𝑝𝑗𝑗 (𝑠𝑠) the formula is applied (11):
𝑝𝑝𝑗𝑗 (𝑠𝑠) = 1⁄(𝑘𝑘 + 𝑠𝑠 2 ) , 𝑠𝑠 ∈ 𝑆𝑆, (11)
where: 𝑘𝑘 is the credibility coefficient of the event 𝐸𝐸𝑣𝑣𝑗𝑗 [𝑠𝑠].
The following is a list of the most common space logic operators in the Smart City
System:
1) 𝑂𝑂(∨𝑠𝑠 ) = max�𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), . . . , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠)�;
2) 𝑂𝑂(∧𝑠𝑠 ) = min�𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), . . . , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠)�;
3) 𝑂𝑂(∪𝑠𝑠 ) =∪ �𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), … , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠)�;
4) 𝑂𝑂(∩𝑠𝑠 ) =∩ �𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), … , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠)�;
For the functional extension of the list of operators is possible a combination of
temporal logic operands and spatial logic operands. The list of spatial-temporal logical
operators is presented below:
1) 𝑂𝑂(∨𝑠𝑠𝑠𝑠 ) = max�𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), . . . , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠), 𝑂𝑂𝑝𝑝1 (𝑡𝑡), 𝑂𝑂𝑝𝑝2 (𝑡𝑡), . . . , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝑡𝑡)�;
2) 𝑂𝑂(∧𝑠𝑠𝑠𝑠 ) = min�𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), . . . , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠), 𝑂𝑂𝑝𝑝1 (𝑡𝑡), 𝑂𝑂𝑝𝑝2 (𝑡𝑡), . . . , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝑡𝑡)�;
2) 𝑂𝑂(∪𝑠𝑠𝑠𝑠 ) =∪ �𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), . . . , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠), 𝑂𝑂𝑝𝑝1 (𝑡𝑡), 𝑂𝑂𝑝𝑝2 (𝑡𝑡), . . . , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝑡𝑡)�;
2) 𝑂𝑂(∩𝑠𝑠𝑠𝑠 ) =∩ �𝑂𝑂𝑝𝑝1 (𝑠𝑠), 𝑂𝑂𝑝𝑝2 (𝑠𝑠), … , 𝑂𝑂𝑝𝑝𝐽𝐽 (𝑠𝑠), 𝑂𝑂𝑝𝑝1 (𝑡𝑡), 𝑂𝑂𝑝𝑝2 (𝑡𝑡), … , 𝑂𝑂𝑝𝑝𝐼𝐼 (𝑡𝑡)�;
The list of operators for data processing based on spatial-temporal logic can be
extended in relation to the complexity of the developed Smart City System.

6. Economic Model of the Smart City Service System

The economic model of the Smart City Service System can be interpreted as a model
of economic relations defined by game theory (Nash equilibrium) [16, 24, 25], in which two
sets of agents are involved: SDA and SCA.
The profit Ρ obtained by the set of SDA agents as a result of providing services for the
set of SCA agents is calculated in relation to 𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] and 𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] from the expression (12):
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 A. Turcan, V. Ababii, V. Sudacevschi, R. Melnic, V. Alexei, S. Munteanu, C. Ababii 83

𝛲𝛲 = 𝜌𝜌�𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] , 𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] �, (12)

where 𝜌𝜌 is the calculation function.
The target objectives of the set of SDA agents are defined by the expression (13):

𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] = max �𝜈𝜈�𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] , 𝑆𝑆𝑆𝑆 [𝑇𝑇], 𝑠𝑠, 𝑡𝑡��, (13)

𝑠𝑠∈𝑆𝑆

where 𝜈𝜈 is the calculation function.

Whereas the target objectives of the set of SCA agents are defined by the expression
(14):

𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] = max �𝜐𝜐�𝑘𝑘𝑆𝑆𝑆𝑆[𝑇𝑇] , 𝑆𝑆𝑆𝑆 [𝑇𝑇], 𝑠𝑠, 𝑡𝑡��, (14)

𝑠𝑠∈𝑆𝑆

where 𝜐𝜐 is the calculation function.

Expressions (13) and (14) determine that the set of SDA agents will strive to provide
with as many services as possible for the set of SCA agents, but the set of SCA agents will
look for the solution to use the highest quality services offered by the set of SDA agents.

7. Conclusions
The research led in this paper is part of the development of distributed computing
systems for Smart City Services. The functional logic of the system is based on spatial-
temporal logic models in which the decision-making capacity of an event depends on its
spatial position and its evolution over time.
The synthesis of the diagram for the Smart City Service System was performed. The
decision-making functionality of the system is based on the presence of two subset of agents:
Service Delivery Agents and Service Consumer Agents. Mathematical models of agents have
been developed that include qualitative and quantitative parameters of decisional influence.
The functional logic of the Smart City Service system is based on the application of a
set of temporal, spatial or spatial-temporal logic operators. An operator includes a lot of
operands for which mathematical models of spatial-temporal evolution have been developed.
An operand characterizes an event.
The economic model of the system is presented as a relationship between the subset
of agents that provide as many services as possible and the subset of agents that consume
high quality services.
There are planned researches in the development of the system at the level of
hardware and software architecture for the future.

Acknowledgments. The results presented in this paper are part of the research led at
the Department of Computer Science and Systems Engineering. Functional testing of
developed ideas was performed with the technical and technological support provided by the
Embedded Systems Laboratory.

Conflicts of Interest. The authors declare no conflict of interest.

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 A. Turcan, V. Ababii, V. Sudacevschi, R. Melnic, V. Alexei, S. Munteanu, C. Ababii 85
Citation: Turcan, A.; Ababii, V.; Sudacevshi,V.; Melnic, R.; Alexei, A.; Munteanu, C.; Ababii, C. Smart City
Services based on Spatial – Temporal Logic. Journal of Engineering Science 2022, 29 (3), pp.
78-85. https://doi.org/10.52326/jes.utm.2022.29(3).07.

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Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 86 - 92
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Biomedical Engineering eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).08
UDC 004.032.26:616.24-006

A NOVEL CLASSIFICATION WITH DEEP CONVOLUTIONAL NEURAL NETWORKS

ON PULMONARY NODULE

Arun B. Mathews1*, ORCID: 0000-0002-2173-5415,

Krishna K. Prasad2, ORCID: 0000-0001-5282-9038

1
Srinivas University, Pandeshwar, Mangaluru, Karnataka 575001, India
2
College of Computer Science and Information Science, Srinivas University, Mangalore, India
*Corresponding author: Arun B. Mathews, email: [email protected]

Received: 05. 24. 2022

Accepted: 07. 08. 2022

Abstract. Medical images are an important part of a patient's health record, and they need
data manipulation, processing, and handling by computers. As a result, medical data is a type
of bigdata, and its analysis has become complex. Because manual disease diagnosis takes
longer and produces less accurate results, it may result in incorrect treatment. Three DCNN
architectures have been exploited and evaluated for tumor detection and classification. The
sample image for the experimentation is chosen from Lung Image Database Consortium
(LIDC) with Image Database Resource Initiative (IDRI) and Kaggle dataset which consists of
normal and abnormal image. The experimental results of proposed DCNN classifier achieved
best accuracy than the GoogleNet, AlexNet, Artificial neural network and support vector
machine.

Keywords: Lung cancer, DCNN, LIDC and GoogleNet, AlexNet.

Rezumat. Imaginile medicale sunt o parte importantă a dosarului de sănătate al pacientului

și necesită manipularea, procesarea și manipularea datelor de către computere. Drept urmare,
datele medicale sunt un tip de bigdata, iar analiza lor a devenit complexă. Deoarece
diagnosticarea manuală a bolii durează mult și produce rezultate mai puțin precise, aceasta
poate duce la un tratament incorect. Trei arhitecturi DCNN au fost exploatate și evaluate
pentru detectarea și clasificarea tumorilor. Imaginea eșantion pentru experimentare este
aleasă din Lung Image Database Consortium (LIDC) cu Image Database Resource Initiative (IDRI)
și setul de date Kaggle care constă dintr-o imagine normală și anormală. Rezultatele
experimentale ale clasificatorului DCNN propus au obținut mai bună acuratețe decât
GoogleNet, AlexNet, rețeaua neuronală artificială și mașina de suport vector.

Cuvinte cheie: cancer pulmonar, DCNN, LIDC și GoogleNet, AlexNet.

1. Introduction
The Lung tumor detection and classification is one of the most difficult tasks in
medical image processing due to the wide variation in tumor density, size, and location, as
well as the low contrast of the scanned image. Because it directly affects human mortality,

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. B. Mathews, K. K. Prasad 87

the accuracy of such a classification system should be high. When the volume of input is
large, the existing classifier performs poorly. As a result, there is a need to develop an
algorithm that provides greater accuracy in lung tumor detection and classification.
Tumors' unpredictable appearance makes detecting their presence, as well as determining
shape and size, difficult tasks in medical image analysis. Medical images are prone to contrast
and luminance issues, resulting in very low image quality and degraded image features. As a
result, it is critical to develop an algorithm that combines image enhancement and
segmentation to solve the segmentation problem.

2. Survey of the work

SVM classifier for predicting lung tumors. Image denoising was performed using
variation-based denoising, followed by optimal thresholding and morphological-based
segmentation. SVM classifier was used to classify lung tumors. Pixels within the very dense
body and chest wall structures have a different density distribution than low-density pixels
[1]. The region of interest is a lung nodule, and a labelling algorithm is used to extract the
region. Correlation, homogeneity, energy, contrast, and area were extracted as texture and
region features.
A hyper plane represents the largest separation or margin between the two classes in
an SVM linear classifier used for tumor classification. When tested on a large image database,
this classification algorithm performs less well [2].
Eigengene extraction via Independent Component Analysis (ICA) is one method for
tumor classification feature extraction. A novel approach for tumor classification based on
eigengene and SVM-based Classifier Committee Learning (CCL) algorithm. The algorithm
must still investigate the design of an effective approach for optimal results [3].
SVM classifier for classifying cancer stages. Image features are extracted after
preprocessing. Then, for classifying medical images, the support vector machine algorithm is
used. When the input data became large, processing time was required, and it was suspected
to be notoriously redundant [4].
By applying the kernel trick to maximum margin hyper planes, a nonlinear classifier
was created. Kernel functions of various types were used, including polynomial, quadratic,
and Multi-Layer Perceptron (MLP). SVM produces better classification results [5-7].
They combine generalization control with a method for dealing with the curse of
dimensionality. The kernel mapping provides a unifying framework for the majority of the
model architectures that are commonly used. When the number of images used in the
testing process increases, the accuracy of image enhancement must improve [8-10].
A two-stage CAD system for automatically detecting and classifying MRI brain tumors.
The system classified brain tumor images as normal or abnormal. The abnormal MRI is then
used to determine whether the tumor is benign or malignant [11-14]. K-means clustering is
used for image segmentation, DWT is used for feature extraction, and PCA is used for feature
reduction. The feature reduction method is used after feature extraction to select the relevant
features. Classification was used to determine whether an image was normal or abnormal [6].
This system was tested for brain image classification, which had not previously been done
for the other modalities. ANN is used to create a system for detecting and classifying brain
cancer. The main issue in detecting the edge of a tumor is that the tumor appears very dark
on the image. Histogram equalization was used to solve this problem [15-16]. Segmentation
is the process of dividing an image into its constituent parts or objects.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

88 A novel classification with deep convolutional neural networks on pulmonary nodule

Deep learning architecture for classifying medical images of anatomy objects in a

modified CNN architecture with different convolutional and pooling layers used for feature
learning in the modified CNN architecture [7]. The outcomes were compared to existing
architectures such as LeNet, AlexNet, and GoogLeNet. a pulmonary CT image classification
using a hybrid 3D-DCNN architecture. This CNN architecture was implemented with various
layers, and the results were compared to 3D-AlexNet and 3D-GoogleNet.

3. Layout of Proposed Work

DCNN architecture 2 is made up of thirteen layers: seven convolutional layers, four
pooling layers, a fully connected layer, and a SoftMax classifier. All convolutional layers have
a filter size of 5 5 and pooling layers have a filter size of 2 2. In convolutional layers, the
number of filters on feature maps is 64, 96, 128, 192, and 256, respectively. Similarly, DCNN
architecture 3 has seven convolutional layers, four pooling layers, two fully connected layers,
and a SoftMax classifier. In the first convolutional layer, 64 filters with 5 5 filter size are
applied to 256 256 patch size input images. By applying 2 2 filters, the max pooling layer
reduces the output size of the previous convolutional layer. The first pooling layer's output
image size is 126126; this image is passed to the second and third convolutional layers, which
apply 98 and 128 filters to the image, respectively. Following that, max pooling is used,
resulting in an output image size of 5959. Initially, DCNN architecture 1 was implemented
with a small number of layers, yielding good results up to a thousand images. Accuracy
decreases as the number of images in the dataset grows. As a result, two additional DCNN
architectures are implemented in this work that shows in Figure 1.
To improve accuracy, the number of convolutional and pooling layers is increased in
this architecture compared to architecture 1. Approximately ten thousand images were tested
with these classifiers and yielded better results. Similarly, the fourth and fifth convolutional
layers with 128 and 192 filters are applied to the down sampled images with the third max
pooling layer, yielding a 2525 feature map. The model progresses through the remaining
layers until it reaches fully connected layers, where all neurons are connected to all neurons
of the previous layer.

Figure 1. Proposed system flow.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. B. Mathews, K. K. Prasad 89

DEEP CONVOLUTIONAL NEURAL NETWORKS

DCNN consists of two important layers:

1. Input layer
2. Classification layer

Figure 2. Proposed DCNN Architecture 3.

Finally, the SoftMax classifier is used to determine whether the images are normal,
benign, or malignant. The accuracy of the second architecture is higher than that of the first.
In addition, one fully connected layer with the same layer descriptions and hyperparameters
is included in architecture 3 shows in Figure 2.
4. Results and Discussion
From the result, 85.02% accuracy rate obtained in the proposed architecture 3 which
is higher than other two architectures. The second-best accuracy rate is 84.34% and the next
better accuracy rate achieved by 83.53% of the proposed architecture 2. By considering of all
three architectures, the architecture 3 used a greater number of convolutional and fully
connected layers it leads to extract more features and resulted in received higher accuracy
rate. Graphical representation of accuracy comparison is presented in the Figure 3.

Figure 3. Accuracy of three proposed DCNN Architectures.

Journal of Engineering Science September, 2022, Vol. XXIX (3)
90 A novel classification with deep convolutional neural networks on pulmonary nodule

Precision is calculated for all three architectures using 9696, 128 128, 192192, and
256 256 patches, in that order. The results show that architecture 1 had a higher true positive
prediction rate in 128 128 patches, but this rate gradually decreased as patch size increased.
The architecture 2 received better results in 128 128 and 256 256 patches, but the true
positive rate gradually increased in architecture 3, which also produced better results when
compared to the other two architectures, as shown in Figure 4.

Figure 4. Precision Comparison for proposed architectures.

The results show that the GoogleNet achieved higher precision of 82.43%, recall of
83.55% and Specificity of 84.77% compared to AlexNet architecture, but the proposed
architecture is obtained higher precision, recall and specificity than the GoogleNet
architecture shown in Figure 5.

Figure 5. Performance of proposed DCNN architecture with existing algorithm.

5. Conclusions
Deep learning-based algorithms are currently emerging in the field of medical image
classification. Deep learning-based DCNN architectures for CT lung image detection and
classification were presented in this section. The layers of deep learning architecture were
discussed in detail, along with the proposed three types of DCNN architectures. This section
describes the hyperparameters used in the proposed architectures, as well as the input and
output feature sizes. The proposed DCNN architectures take a CT lung image as input and

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. B. Mathews, K. K. Prasad 91

classify it as normal, benign, or malignant. The experimental results show that the proposed
architecture 3 outperforms other existing architectures in terms of accuracy, precision, recall,
and specificity for CT lung image classification. In the future, the proposed HPSO algorithm
can be tweaked to produce higher accuracy with a shorter execution time. HPSO parameters
such as the number of iterations and particles can be optimized to produce better image
quality

Conflicts of Interest. The authors declare no conflict of interest.

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92 A novel classification with deep convolutional neural networks on pulmonary nodule
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Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 93 - 109
Fascicle Electronics and Computer Science ISSN 2587-3474
Topic Biomedical Engineering eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).09
UDC 620.3:61

NANOTECHNOLOGY: REFLECTIONS ON HEALTH BENEFITS AND RISKS

Artur Buzdugan, ORCID: 0000-0002-9226-004X

National Nuclear Security Support Center, Technical University of Moldova

168 Stefan cel Mare Blvd, Chisinau, MD-2004, Republic of Moldova
Corresponding author: Artur Buzdugan, [email protected]

Received: 06. 18. 2022

Accepted: 08. 17. 2022

Abstract. There is a constant increase in the demand for engineers who can transform
nanotechnology from a scientific result into a commercial solution. However, new
technologies often caused conflicts between those who want to exploit them as soon as
possible and those who are waiting to receive absolute proof of safety. Certain types of
nanoparticles are well studied and recommended for use in medicine, biology, chemistry,
cosmetology, etc. Some nanoparticles are proven to be extremely toxic, with drastically
different properties from the same volume compounds. The risks associated with using
nanotechnologies and products containing nanoparticles cannot be minimized in the absence
of regulations, which would allow adequate control to protect the environment and the
population's health. Companies are also extremely careful in investing in this field as long as
there is no transparent regulation, as the ultimate goal is to protect the surrounding
environment and society. In this paper, we present an overview of the benefits of
nanotechnology in areas that affect human health, as well as the risks that may arise from
the early use or ill-will of nanotechnologies.
Keywords: nanotechnology, applications, biomedical engineering, impact, risk, regulation.
Rezumat. Există o creștere constantă a cererii pentru ingineri care pot transforma
nanotehnologiile din rezultate științifice în soluții comerciale. Dar tehnologiile noi totdeauna
au generat conflicte între cei care doresc să le exploateze cât mai repede posibil și cei ce
sunt în expectativă să primească dovezi absolute de siguranța lor. Anumite tipuri de
nanoparticule sunt bine studiate și utilizate sau recomandate pentru utilizare în medicină,
biologie, chimie, cosmetologie. Multe nanoparticule se dovedesc a fi extrem de toxice, cu
proprietăți radical deosebite de aceiași compuși în starea de volum mai mare. Riscurile legate
de utilizarea nanotehnologiilor si a produselor care conțin nanoparticule nu pot fi minimizate
în lipsa unor reglementări ce ar permite un control pentru a proteja sănătatea populației și
mediului. Companiile sunt extrem de precaute în a investi în domeniul nanotehnologiilor atât
timp cât nu există reglementări transparente deoarece este vorba de protecția oamenilor și
mediului care-l înconjoară. Prezenta lucrare este o trecere succintă în revistă a beneficiilor
nanotehnologiei în domeniile ce influențează sănătatea omului, precum și a riscurilor ce pot
apărea din utilizarea precoce sau din rea-voință a nanotehnologiilor.
Cuvinte cheie: nanotehnologie, aplicații, inginerie biomedicală, impact, risc, reglementare.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

94 A. Buzdugan

1. Introduction
Nanoscience is the convergence of physics, materials science, and biology, which deals
with handling materials on an atomic and molecular scale. Nanotechnology and
nanoengineering represent the ability and process to measure, manipulate, assemble, control,
and manufacture nanoscale matter. This science is relatively new and consists of known
processes, as well as new unknown processes. Therefore, it is not surprising that there is no
clear public perception of this topic: on the one hand there is the fear of the unknown as a
potential source of danger, and on the other hand is the potential for good. The ability to
deal with the matter at the atomic or molecular level allows for a deeper understanding of
physical phenomena and control over the functionality of new devices.
In the paper [1] there is a mention, that time ago M.C. Roco predicted the following
four stages in the development of nanotechnology products:
● passive nanostructures, passive properties of nanomaterials, including nanotubes and
nanolayers, which provide more opportunities to renew products in everyday life;
● active nanostructures, which can change their state during use in a predictable way;
● nanosystems - nanorobotics, nanobiotechnologies, information nanotechnologies;
● molecular nanosystems are the most advanced by the intelligent design of devices at
the molecular, atomic, and quantum effects level.
Nanotechnology, nanoengineering, and their microscopic universe are the
globalization product with large investments for research and development around the world,
already representing a huge industry. The global nanotechnology market was estimated at
$1.76 billion in 2020, increasing to $100 billion in 2030. Nanomaterials offer a wide range of
functionalities due to their physical and chemical properties manifested in their new state.
These offer new methods in diagnosis, therapy, and in healthcare monitoring, with
opportunities to solve unanswered medical problems. The applications of nanotechnology in
energy, agricultural, food, consumer products, transport, logistics, and environmental sectors
are also growing rapidly. The fastest growing domains are expected to be health,
nanoelectronics, energy, aerospace, and defense. The USA, Brazil and Germany are expected
to lead the nanotechnology industry in 2024, with a significant presence in the top countries
such as Japan, China, South Korea and India.
Regarding the rapid development of nanotechnologies, we note that in 2019, over
40% of scientific publications on nanoscience came from China, followed by the USA and
India. When it comes to patents, in 2019 the US had the most active market in the world for
nanotechnology innovations (8900 patents filed), followed by the EU, China and South Korea.
From the dynamics of the infiltration of nanotechnologies in practically all the fields
that influence our life, it is paramount that the regulations are aligned with the evolutions.
The safety assessment of nanomaterials is an important process and we expect this to be safe
by design. For these reasons, researchers, innovative engineers and regulators are best placed
in developing guidelines for toxicological assessments and analytical methods to implement
new definitions and various regulatory requirements.

2. Diversity of nanotechnology application in the vital area

To understand the impact of nanotechnology on human health, we analyze a
predictable roadmap for nanotechnology (Figure 1). We note the usefulness of both phases,
both the initial manufacturing process (obtaining new material, measurements and
characterizations, attempts at technology transfer in various fields) and the final process of

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Nanotechnology: reflections on health benefits and risks 95

developing the architecture of nanodevices and possible applications (operating theories,

modeling, formation of functional biochemical systems, new approaches).
The prospects for nanoscience, nanoengineering and nanotechnology are promising
to the society and at the same time these achievements can be recognized as potential threats
to humans in the lack of knowledge.
There are virtually no areas of activity that are not influenced by advances in
nanotechnology and nanoengineering.
And all of them have an impact on human health, including those in the
telecommunications, chemical, textile, automotive, etc. industries [2-8]. In our analysis we
will refer exclusively to those areas (Figure 2), which we consider having a major impact on
human health.

Figure 1. Predictable phases of nanotechnology development.

Medicine

Agriculture,
Animal
Husbandry Biology
& Food

Nanotechnology &
Vital Security

Water , Waste
& Pharmaceutic
Environment & Cosmetics

Security &
Safety

Figure 2. Nanotechnologies and vital security.

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96 A. Buzdugan

3. Nanotechnology and the environment

Nanoparticles (NPs) have been recommended as extremely useful for the protection
and cleaning of the environment [8, 9]. There are applications of selective membranes that
can filter contaminants or even salt from water, or nanostructured traps to remove pollutants
from industrial effluents. Monitoring and characterization of the environment are performed
using nanosensors, and nanostructured intelligent sensory systems (Figure 3). Nanomaterials
contribute to significant reductions in the consumption of materials and energy, while the
sources of pollution are maintained, and the need for industry maintenance determines
increased opportunities for recycling [9]. Therefore, there is a potential to reduce
environmental pollutants.

Nanotechnology
in the environment

Environmentally friendly Sensors,

(non-polluting or Remediation of sensory networks for
pollution-reducing) contaminated materials monitoring
products environmental factors

Figure 3. Nanotechnology in the environment.

However, we also identify the negative side due to reasons such as insufficient
regulation, drastic growth of the nanotechnology industry, and the use of NPs in various fields
that reside through the uncontrolled release of NPs into the environment. For these reasons,
the assessment of the risk of NPs in the environment must be performed in terms of their
mobility, reactivity, ecotoxicity and persistence. In the absence of rigorous control,
nanoengineering applications increase the concentration of nanopollutants in groundwater
and soil, which are the most common routes of exposure for environmental risk assessment.
Due to the high ratio of surface to mass NP, the distribution of the contaminant in the
solid/water environment will be dictated by the absorption at the natural NP surface, the
aggregation of the NP, or the co-precipitation at NP formation. The interaction of
contaminants with NP is complex depending on the physicochemical characteristics such as
size, chemical composition, morphology, porosity, state of aggregation/disaggregation,
surface reactivity, surface loads, and surface passivation. In addition, environmental
characteristics such as pH, temperature and light intensity affect the toxicities of some
nanostructures. The same nanomaterial, but with different geometry: diameter, length, crystal
structure and different surface modification, will have different toxicities.
The environmental pollution with nanoproducts represents a major problem with
unpredictable consequences. Although many nanoproducts are considered harmless (e.g.
nanoelectronics), their tiny size being scattered volens-nolens in the environment can cause
serious consequences, which we do not know yet. Let's take a simple example, a drug in the
form of nanopowder or nanodrage, useful for a person, but out of hand, or thrown away at
the expiration of the easy time will pollute the atmosphere and cause unpredictable
consequences for a healthy person. As a new source of pollution, nanotechnologies need to
be given additional attention through appropriate regulations, following various research on
ecological toxicity.

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 Nanotechnology: reflections on health benefits and risks 97

4. Nanotechnology, agriculture, and animal husbandry

The focus on sustainable agriculture argues for the implementation of the ecosystem
method, in which abiotic-biotic living beings are in harmony with coordinated stability of
food chains and their energy balances. Nanotechnology is one of the most effective solutions
in achieving this goal by using nano- fertilizers, nanopesticides, nanoherbicides, etc. [13].
Water treated with nanotechnologies used for seed softening, irrigation, dilution of
agrochemicals and fertilizer treatment positively influences the rate and condition of seed
germination, seedling quality and crop yield and quality.
Plant genetic engineering leads to personalized benefits, such as increased crop yields
currently achieved through the scientific application of NP chemicals. Nanotechnology is
widely used in various ways (Figure 4) to improve agricultural production. Nanopesticides and
nano-fertilizers have been shown to have little, or no toxicity due to much smaller and strictly
dosed calculated amounts, while improving the effects [13, 19]. The control efficiency of
biopesticides on a nanoscale is one to three times higher than that of regular pesticides when
the dose was the same, reducing the cost by half.

Food supply chain Food processing

Ensuring safe transit
management automation

Preservation of Improving food

Packaging and waste
processing equipment delivery

3D printing Drone Robots

Figure 4. Nanotechnology in the food industry.

Nanofungicides and nanoinsecticides have considerable potential that was not yet
been sufficiently explored in agriculture and nanotechnology-based delivery systems.
Nanotechnologies have the increased ability to inhibit or kill various types of microbes and
are useful in the environmental disinfecting. Also, NPs are useful for monitoring
microelements in soil and plants, detecting soil toxins, detecting, and diagnosing crop
diseases. The sensitivity of nanodevices can be used for the rapid, economical, and efficient
detection of phytopathogens, thus reducing the chance of large-scale destruction of crops.
Nanotechnology is used in animal husbandry to improve the diagnosis, treatment,
delivery of medicines, food preservation, reproduction, monitoring, and improvement of
animal health, as well as for higher quality production [10, 14]. Nanobiocides are
recommended to be effective in disinfection, disinsection, and rodent control procedures that
contribute to sustainable and ecological agriculture.

5. Nanotechnologies in civil security

There is practically no civilian or military field in which nanotechnologies don’t have
applications. As research is the mainstay of identifying new applications of nanotechnology,
it has become a key research priority since the EU's Sixth Framework Program for RTD (FP6,
2002-2006) containing projects targeting security applications. The applications of
nanotechnology for civil security in FP6 covered four areas: detection, protection,
identification, and assessment of societal consequences.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
98 A. Buzdugan

Direct or indirect detection (including imaging, sensory/sensory networks) of radiation,

pathogens, and chemicals refers to the detection of viruses, bacteria, DNA, RNA, proteins, and
nucleotides to prevent acts of bioterrorism, chemicals, industrial harmful gases, ionizing
radiation, but also to other harmful electromagnetic waves, etc. [15-19, 45].
Detection devices for civil security were progressively influenced by the advances in
nanotechnologies and we classify them arbitrarily into three categories:
● X-ray imaging, IR detection, and the emerging field of imaging at THz wavelengths;
● direct or indirect detection sensors of biological and chemical agents. We assign
nanotubes and nanowires to direct detection sensors and electrical and
electromechanical, colorimetric, quantum dots to sensors with indirect detection.
Biological barcodes, consoles for the detection of biomolecules, and
microorganisms we also assign to this category;
● polyfunctional smart miniature sensor networks (smart dust).
Referring to protection devices we note improved nanomaterials with new physical
properties and functionalities, including higher strength and durability, built-in sensory
capabilities and active materials.

Figure 5. Example of blood purification of radionuclides with intelligent NP

(adaptation from [45]).

In terms of civil security applications, nanodevice protection devices mainly benefit

from the following functional materials:
● the advanced physical-mechanical, thermal, chemical resistance and low specific
weight for flexible anti-ballistic textiles; reactive nanoparticle armor; shock
absorber nanotubes; nanofibers, clothing and nano-coatings for biological products
or chemical decontamination; switchable fabrics or materials to improve thermal
control and fire protection etc.;

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 Nanotechnology: reflections on health benefits and risks 99

● smart, containing integrated nanosensors, reactive elements, intelligent materials

for diffusion control and active transport of mass or electric charge control; smart
NPs that recognize, capture, incorporate, eliminate, or destroy certain toxins or
radionuclides. For example, at intravenous injection, biodegradable nanospheres
circulate through the bloodstream, where surface proteins bind to targeted
radionuclides. Nanospheres with identified and captured toxins are removed from
the bloodstream through a small inserted into an artery shunt. The magnetic field
applied to the shunt (Figure 5) immobilizes the Fe-based particles with
radionuclides allowing the direction of the cleaned blood in the blood flow [45];
● shielding or absorption of electromagnetic interference in electromagnetic
radiation fields, depending on wavelengths.
Nanotechnology is effective in the national security field by introducing smart
weapons and nanosensors. But this also represents a major disadvantage of nanotechnology.
Increasing the functionality or capability of weapons, such as miniaturization, can also
constitute a threat. If this technology falls into the hands of terrorists or malicious actors,
then we should be prepared for it as well, or we need adequate countermeasures and
products that would protect people and the environment.
6. Nanotechnology and biomedicine
Interestingly, the colloidal solutions of iron sucrose NP were already in clinical use in
1949, 10 years before Feynman's (1960) call for the world of nano state. We can now confirm
the realization of the idea of another scientist - Paul Ehrlich, who in his work on the concept
of targeted therapy, stated the need for a "Zauberkugel" (magic bullet) - so a drug that would
be specific and intended exclusively for the target without affecting normal host cells.
If we refer to the diversity of nano states of inorganic materials currently used in
medicine (Figure 6), they all show some therapeutic, diagnostic, or delivery properties and
markers [11-12, 15-20]. For example, antibody-functionalized nanostructured surfaces are
used to detect specific proteins or cells resulting from the increased interaction surface and
adhesion that give increased sensitivity in detection and NPs serve as markers for detecting
biomolecules, pathogens, and MRI contrast agents.
Medical diagnosis with nanopores requires small volumes of evidence for counting
and distinguishing a complex mixture of a variety of biological molecules by accessible
electronic measurements. The simplicity, speed, and versatility of nanopore analyzes are
promising for molecular diagnosis.
Quantum dots are another group of nano states, with a unique potential for clinical
use, especially in diagnosis. The ability of quantum fluorescence points in different spectral
regions would be useful for marking and imaging cells, cell structures, or biological
pathogens, as well as observing processes in dynamics, which take place in cells, tissues, and
the body as a whole.
Dozens of metal oxides in the form of NP are currently used in therapy (Figure 7),
which shows, depending on the oxide, neuroprotective properties, antioxidants, antibacterial,
antimicrobial, anticancer, drug carriers, etc. The most significant advances in nanotechnology
in biomedicine are observed in cancer therapy, offering innovative solutions to overcome the
limitations of chemotherapy and radiotherapy, through the targeted delivery of drugs,
proteins, and polynucleotides. NPs based on micelles, liposomes, and polymers with "capture
molecules" attached [11], along with single-walled nanotubes, are used as carriers of drugs
for target delivery.
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100 A. Buzdugan

Nanocrystal

Nanostruc- Nanoparticles
tured Quantum dots
surfaces

Nanomaterials
in
biomedicine
Nanosheet Nanopores

Nanowires Nanotubes

Figure 6. The diversity of nanostates used in biomedicine.

The unique form of NPs allows them to enter selectively through biological barriers
by delivering drugs to the target in the minimum quantities necessary to obtain and maintain
the therapeutic effect, thus reducing the possible toxicity of drug preparations. This is
especially important in the case of very toxic and short-lived chemo- and radiotherapeutic
agents [21-25].

Figure 7. Nanoparticles types as sensitizers for medical purposes.

Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Nanotechnology: reflections on health benefits and risks 101

Another broad area of use of NPs in biomedicine is the design of biosensors for
monitoring physiological parameters, as well as the detection of specific DNA fragments and
regions or the identification of bacterial cells, etc. Thus, nanowires and Graphene oxide (GO-
nS) are recommended to identify cellular interactions in vivo [26].
The potential of nanopores in the detection of direct sequencing of individual DNA
molecules can provide useful information about an individual's genetic structure and
determine the increased risk for certain diseases such as cancer. This nanopore-based
detection sensor has potential for application in agriculture, security, defense, and evolving
biology, where genomic information is useful.
Carbon nanotubes are being intensively investigated from the perspective of
applications in therapy, especially in the treatment of cancer, but also for the development
of new diagnostic agents and nanosensors. Carbon nanotubes can also be used for the
targeted administration of drugs for the generation of new bone tissue.
The use of drugs in the form of nanocrystals facilitates absorption by the body.
Nanocrystals are also used as markers of areas of interest in biomedicine for further studies,
such as by immunofluorescence microscopy.
A report on the beneficial effects of NPs in thermoradio (immune) therapy, targeted
delivery of pharmaceuticals, contrast agents, local amplification of the exposure dose [27-
29], and the summary spectrum of the exposed benefits are represented in Figures 7 & 8.
Furthermore, NPs containing Ag in addition to antimicrobial and cytostatic effects
useful in medicine serve as preservatives in the cosmetics industry.

Figure 8. Nanoparticles as sensitizers, radioprotectors, or labelling of ionizing

radiation for the treatment, diagnosis, and monitoring of cancer and other diseases
(adaptation from [28]).

Treatment for the purpose of:

Treatment
target delivery,
Detection, diagnosis,
dosing accuracy, control,
Nanoengineering mapping with biomarkers
minimized side effects,
in human genetics patient, organs, tumors...
avoidance of repeated dose,
Bio Barcodes,
increased absorption,
Real-time DNA sequencing
selective permeability

Figure 9. The usefulness of nanotechnologies in human genetics.

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102 A. Buzdugan

When we talk about the interrelationship between nanotechnology and biomedicine,

let's not forget about the achievements [30-33] in the field of human genetic engineering
(Figure 9). Without going into details, Figure 8 shows the benefits of nanotechnologies in
treatment and diagnosis.

7. The nanotechnologies specifics risk

Various applications of nanotechnology expose people to potential dangers, such as
potential toxicity. Uncontrolled exposure to NPs occurs through various pathways in the body:
inhalation, ingestion, skin penetration, and intravenous injection [34, 35]. NPs reaching the
extracellular fluid are conjugated with biomolecules present in the environment, which
allows them to be internalized in cells by penetration directly or indirectly through known
mechanisms, e.g. via phagocytosis, endocytosis or pinocytosis.
As a concern, we note with sufficient reasoning, that the skepticism of the usefulness
of nanotechnologies is based on the lack of knowledge about their toxicity to humans and
the environment. It is already established that we are not entitled to deduce the toxicity of a
nanomaterial guided exclusively by its toxicity in macro form, as it is being a complex
function of many parameters. Because of this, some are convinced that NPs are so risky that
they require stopping research and applications in everyday life.
However, the precautionary principle cannot be used to stop nano-state research. We
need to find a stable balance between the further development of nanotechnology and the
need for research to identify potential dangers for establishing a scientifically susceptible
database for risk assessment, with subsequent justified risk management procedures.
The small size of various shapes NPs gives a high penetration of epithelial and
endothelial barriers in the lymph and bloodstream. This ensures the transport of NPs to all
organs and tissues, including intercellular transport by transcytosis or simple diffusion across
the cell membrane with adverse results in the penetration of cells by nanoparticles [36-39],
such as physical damage to the membrane, structural changes in cytoskeleton components,
disruption of transcription and oxidative DNA damage, mitochondrial damage, lysosome
function disturbance, generation of reactive oxygen species, impaired membrane protein
function and synthesis of inflammatory factors and mediators.
The penetration of NP into the bloodstream opens up to the possible penetration of
the blood-brain barrier with consequences that are difficult to underestimate. Experiments
that model NP toxicity on the body have shown that NP can cause thrombosis, inflammation
of the upper and lower respiratory tract, neurodegenerative disorders, strokes, myocardial
infarction, etc. What is certain is that NP, thanks to its size, can penetrate not only organs,
tissues and cells, but also penetrate the cellular organs themselves (mitochondria and nuclei)
which can drastically alert cellular metabolism and cause DNA damage, mutations and cell
death.
We underline that public concerns about the increased toxicity of nanoparticles have
a legitimate experimental basis for many years (silicosis, asbestosis, "black lung" disease, or
anthracnosis) if we refer to their interaction with cells and tissues. Some scientific studies
show the ability of the human body to clean itself of non-specific nanoparticles in the body,
others - reiterate a tragic end of their action on the body through irreparable consequences
or diseases. The ignorance of the interaction of the human body with the whole spectrum of
nanoparticles does not allow us to say for sure about a total success story of
nanotechnologies, and nanostructures, especially in biomedicine.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Nanotechnology: reflections on health benefits and risks 103

New technologies have always caused conflicts between those who want to exploit
them as soon as possible and those who expect to receive reliable evidence. A particular
concern of many is the likelihood that nanotechnology will spiral out of control to the
detriment of humanity. These concerns relate to some advances in the ability of nanorobots
to self-replicate and self-direct.

8. Risks associated with nanotechnology

Given the wide range of applications of the nanotechnologies mentioned above and
the variety of industrial sectors affected, it is certain that the risks associated with
nanotechnologies will be complex. The focus on the type of risks to be considered depends
on the perspective of the particular entity involved in nanotechnologies. Suffice it to name
just a few of these potential risks:
● political and economic,
● military (proliferation of WMD),
● societal impact,
● proliferation of bio-chemo-terrorism,
● environmental (uncontrolled release of NPs into the environment,
● nanoparticle harm risks/work hazards,
● risks of final ignorance of the interaction of the NPs with the biological environment
or with other NPs,
● futuristic risks such as the nanotechnology of Homo sapiens, and the risk of the
existence of Homo sapiens caused by the self-replication of nanomachines.
As with any new technology, risks can arise that we do not even intuit yet, which
confirms the need for continuous and dynamic risk analysis. We risk saying that virtually all
the safety issues addressed about nanotechnologies are related to the “free” uncontrolled
nano state and less to the built-in, “fixed or immobilized” states of the already designed NPs.
Of course, there are exceptions when products or materials with embedded NPs are thrown
away, burned or destroyed in an uncontrolled manner by humans, thus causing risks that can
be easily avoided.
From the risks outlined above, we draw attention to occupational hazards caused by
the potential harm of nanoparticles. As shown in Figure 10, several conditions can be
expected for potentially hazardous exposure of workers employed in nanotechnology
research and innovation.

Figure 10. Potentially hazardous exposure conditions for research and innovation
workers (inspired from [6]).

Journal of Engineering Science September, 2022, Vol. XXIX (3)

104 A. Buzdugan

Nanomaterials can present significant, often unknown, hazards to researchers,

engineers, laboratory technicians, and support staff. In this regard, an analysis of the risk and
impact of the life cycle of nanomaterials undergoing research on workers' health is needed.
Although during evolution the human body has developed a tolerance to most
elements and molecules in their natural form of existence (dust, microparticles) with which
it comes into contact, it has no natural immunity to new substances, new forms of existence
(e.g. nano state) to identifying them as toxic, causing a reaction of the body's intolerance.
As mentioned, NP toxicity can be dictated by many factors (Figure 11) [34-38].
Moreover, NP size and surface area play an important role, largely determining the unique
mechanism of NP interaction with living systems.

Figure 11. Determinants of nanoparticle toxicity (adaptation from [26]).

NPs are characterized by a very large specific surface area, which determines their
high reaction capacity and catalytic activity. Dimensions from 1 to 100 nm are comparable to
the size of protein cells (2–10 nm), the diameter of the DNA helix (2 nm), and the thickness
of cell membranes (10 nm), which allows them to easily penetrate cells and organs [26]. For
example, it is shown that gold NPs less than 6 nm penetrate easily into the cell nucleus, while
the largest (10-16 nm) penetrate only through the cell membrane and are found only in the
cytoplasm. This suggests that NPs of a few nanometers may be more toxic than NPs of 10 nm
or more that cannot penetrate the nucleus. The toxicity dependence of gold NPs depends on
their size in the range of 0.8 to 15 nm. It has been identified that 15 nm NP is 60 times less
toxic than 1.4 nm NP for fibroblasts, epithelial cells, macrophages and melanoma cells. It is
noteworthy that the 1.4 nm nanoparticles cause cell necrosis, while the 1.2 nm nanoparticles
predominantly cause apoptosis. These data show us not only that NPs can penetrate the
nucleus, but also that the correspondence of the geometric size of NPs (1.4 nm) with that of

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Nanotechnology: reflections on health benefits and risks 105

the major DNA groove allows them to interact effectively with the backbone of DNA. Sugar-
phosphate loaded with negative sac and blocks the transcription.
The results of several studies show that carbon nanotubes, similar in shape to asbestos
fibers, cause mesothelioma in the lungs. Also, inhaled carbon NP can weaken the immune
system by affecting the T-cells responsible for its organization. On the other hand, it is shown
that the harmfulness of nanocarbon is dictated by its durability, so its shape, the more durable
it is, the more the behavior resembles asbestos particles.
The convergence of nanotechnology, synthetic biology and chemistry allows the
creation of new agents and increases the resilience and lethality of existing ones. There is
already talk of the possibility of editing various bacterial DNAs to create complex organisms
and new chemicals.
New horizons of chemical-biological nano-generation delivery methods can create
diagnostic and treatment impediments, reducing the body's immunity and causing ineffective
diagnostic and treatment methods. As an example, carbon nanotubes can be used to supply
only the lethal parts of the anthrax virus - without the imprinted protein that is recognized
by the immune system.

9. Social impact and regulation

Exposure to nanomaterials is versatile and is achieved through production,
transportation, storage, dissemination, use, and final disposal. Nanoparticles may not be
recyclable or environmentally friendly, and when they lose control of their existence
throughout their life, they could form a new category of non-ecological toxins and create a
new threat to health, including through the environment. For these reasons, risk-based
regulation of nanotechnologies is needed. Bowman and Hodge propose a model [40] that
would argue for a complex regulation for nanotechnology (Figure 12).
This model takes into account product safety, civil society awareness, ethical and
social issues, health, intellectual property rights, the international legal framework, including
the environment. The soft and tough legal framework refers to various aspects of the
consequences of nanotechnology and is applied in various fields: innovation research
(through Codes of Professional Ethics) and, health, industry, pharmaceuticals, chemical
industry, textile, automotive, etc.
We note that the governance system required for nanotechnologies does not differ
substantially from the approach applied to other important environmental and public health
issues. However, we mention that nanotechnologies come with specific challenges such as:
● the profound interdisciplinary character not previously encountered;
● high speed of development and enormous impact on industries and social benefits;
● low and delayed public awareness of nanotechnologies;
● the nature of the risks [41] created by some nanotechnologies;
● ethical, legal and social issues associated with some of the nanotechnologies.
The specific challenges and risks associated with some nanomaterials have posed
questions to regulators, politicians, and researchers about the coverage of nanotechnologies
and nanomaterials within the existing regulatory framework. To fill this regulatory gap, for
example, the Commission of the European Communities has adopted a so-called incremental
approach that recommends adapting existing legislation to the regulation of
nanotechnologies and amending them.
This approach has led to some changes in European regulations and directives.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

106 A. Buzdugan

Figure 12. Bowman & Hodge nanotechnology regulatory model [40].

Thus, nanomaterials in the chemical, cosmetics, food, medical devices, plastic
packaging for food, waste, and waste management are somehow indirectly regulated [42-44].
However, regulation by the incremental approach of the existing legal framework is
characterized by several deficiencies.
10. Conclusions
Certainly, nanoelectronics is perhaps the most harmless nanotechnology with minimal
adverse impact on human health. Exceptions may be due to non-compliance with the vital
security in the technological process of obtaining as well as the uncontrolled discharge of
technological waste into the environment.
Nanotechnologies in biomedicine represent dual-use technologies, which are
characterized by both positive and negative impact from the current final ignorance of the
mechanisms of interaction of nanoparticles with the biological environment.
The perspective of nanoparticles in medicine is primarily related to immunotherapy
for diagnosis and clinical therapy depending on the type of nanoparticles. Immunotherapy
combined with the targeted delivery of nanomedicines, characterized by high efficiency due
to penetration, specific retention, and expected and predictable actions (destroying tumor
cells) is under development for the treatment of various types of untreated diseases.
Nanoparticles have been shown to enter the human system in three ways: inhalation,
ingestion, and penetration of the skin. Thus, it becomes extremely important to know the
interaction of nanoparticles with cells, organisms, the biological environment, biomolecules,
and other biosystems, but also the interaction with other nanoparticles parts of biosystems.
These will determine the biocompatibility, toxicity and efficacy of nanoparticles in biological
environments. This will ultimately allow the identification and design of non-toxic and
beneficial nanomaterials in biomedicine.
Partially, in branches of the industry where nanotechnologies are used, nanoparticles
are already regulated. Although nanotechnologies were not regulated by law in the recent
past, their future in some areas must be largely determined by new regulations.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Nanotechnology: reflections on health benefits and risks 107

Acknowledgments. The article is part of a larger study conducted within the STCU
9608 project entitled “Research, Engineering and Non-Proliferation Culture”.
Conflicts of Interest. The author declares no conflict of interest.
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Citation: Buzdugan, A. Nanotechnology: reflections on health benefits and risks. Journal of Engineering
Science 2022, 29 (3), pp. 93-109. https://doi.org/10.52326/jes.utm.2022.29(3).09.

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Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 110 - 125
Fascicle Architecture, Civil and Environmental Engineering ISSN 2587-3474
Topic Energy Efficiency and New Building Materials eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).10
UDC 621.383.51(478)

PHOTOVOLTAICS SOLUTIONS AND ENERGY COMMUNITIES IN A CLEAN

ENERGY ROADMAP

Cristina Efremov*, ORCID: 0000-0002-6370-0878

Technical University of Moldova, 168 Stefan cel Mare Blvd., Chisinau, Republic of Moldova
*Corresponding author: Cristina Efremov, [email protected]

Received: 07. 28. 2022

Accepted: 09. 05. 2022

Abstract. The present paper deals with solutions regarding the development of the Energy
Strategy toward 2050 for a clean and sustainable future. At the national level conceptual
elements are needed to draw a roadmap for the energy transition in the Republic of Moldova.
The paper presents the renewable energy potential of the country with focus on photovoltaic
energy production. A specific PV deployment solution is also analysed, namely the floating
PV, while use cases for using this solution for serving energy communities in the rural area
has been also proposed. The solutions can be considered steps that will foreshadow the
national energy long-term strategy in the energy sector. An efficient transition to
decarbonised energy systems requires the search for innovative solutions to increase the
penetration of renewable energy sources, for changing the future energy system by
promoting and evaluating innovative perspectives.

Keywords: energy transition, roadmap, energy strategy, renewable energy sources, floating PVs,
energy community.

Rezumat. Articolul prezintă soluții privind dezvoltarea strategiei energetice a Republicii

Moldova până în anul 2050, în vederea unui viitor energetic curat și sustenabil. Sunt necesare
în acest sens elemente conceptuale care să traseze o foaie de parcurs pentru tranziția
energetică în Republica Moldova. Articolul prezintă potențialul de energie regenerabilă a țării
cu focalizare pe producția de energie bazată pe centrale fotovoltaice. Se analizează de
asemenea o soluție particulară de implementare a acestora, respectiv centralele fotovoltaice
plutitoare, fiind totodată propuse studii de caz care să deservească comunități energetice din
zona rurală. Soluțiile pot fi considerate exemple de urmat în cadrul strategiei pe termen lung
a sectorului energetic. O tranziție eficientă către diminuarea conținutului de carbon a
sistemelor de energie necesită găsirea de soluții inovatoare care să crească prezența surselor
de energie regenerabilă, pentru a schimba sistemul energetic al viitorului prin promovarea și
evaluarea unor perspective inovative.

Cuvinte cheie: tranziție energetică, foaie de parcurs, strategie energetică, surse de energie
regenerabilă, centrale fotovoltaice plutitoare, comunități energetice.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 C. Efremov 111

1. Introduction
After 2010 the supply of energy from renewable sources in the Republic of Moldova
increased slowly, as first steps in learning and applying the new trend which has been pushed
more strongly in countries such as Germany and some USA states, for example in California.
Consequently, the energy from renewable sources in the primary energy supply increased by
27.2% in 2019 compared to 2010 and represents 22.5% of the primary energy of the country
[1]. To be noted that according to [1], 67.5% of CO2 emissions in Republic of Moldova are
allocated to energy sector in 2019, as a reduction form 70% in 2010, which suggests that
energy sector is a priority for reaching high decarbonisation goals.
With a gradual decarbonisation process, the Republic of Moldova can contribute not
only to the global efforts to mitigate climate change, but also to improving the health and
the quality of life of its citizens. More efficient use of cheap and abundant renewable energy
sources, with the help of digital technologies, will transform cities, transport, industry and
agriculture, reducing greenhouse gas emissions and improving air quality. Thus,
decarbonisation is not just an abstract goal of the European Union or the United Nations, but
a policy with immediate and tangible benefits for all. And the decisive factors that will
generate these benefits will be the digitization and electrification of the usable potential.
In this context, the opportunities of the Republic of Moldova (RM) in the energy sector
are considered in the long-term development. It is especially worth to mention that the
electricity will have to become a strategic tool for the future of transport, air conditioning
and household needs, but the promotion of smart grids will be proved to be the best way to
make this to be possible. Decarbonisation and air quality are also on the list of priorities and
ensuring an adequate access to the energy for the most vulnerable members of the society
continues to be a subject of the maxim importance.
2. PVs as a priority and high potential in the future RES mix
In the study which has been extensively presented in [2], it has been shown that a
small part of the agricultural area of the Republic of Moldova is needed to provide 30% or
even 50% of the annual volume of electricity used in the country. Even so, recent studies
show that such areas can be found in the form of uncultivated land, but the areas where
agricultural activities take place have as well a very high potential, through the application
of the technologies that are particularly promising, namely agricultural activity combined
with photovoltaics.
In this respect, pilot projects in several parts of the world show that there are synergies
between agriculture and the production of renewable energy sources (RES) with
photovoltaics (PV), which may, in fact, change the perception that PV is in competition with
agriculture.
The amount of photovoltaic power plants capacity in the Republic of Moldova can be
determined in a simplified way based on the calculations performed in [2]. The average yearly
energy produced for one kW of installed PV in the Republic of Moldova has been calculated
in [2] by using 11 geographical points with inputs from [3] and gave 1,182 kWh / year for 1
kW of PV installations (also referred as 1 kWp, where p denotes maximum power of the
photovoltaic panels in defined conditions). A revisited and more refined calculation based on
more geographical points (20 points, organised in four zones: North, Middle, South and left
Dniester, as per administrative organisation from [4]) gives a value of 1,191 kWh / year / kW
(Table 1), which is very near to the initial estimation (only 0.7% difference in the more
complex calculation).
Journal of Engineering Science September, 2022, Vol. XXIX (3)
112 Photovoltaics solutions and energy communities in a clean energy roadmap

Table 1
Average yearly energy produced by 1 kWp PV in based on 20 geographical points [3]
Latitude Longitude Yearly energy Y2Y variation
No Location County Zone
(°) (°) (kWh/year) (kWh)
1 Edineț Edineț 48.169 27.298 1,130.78 57.66
2 Briceni Edineț 48.354 27.065 1,141.13 42.08
3 Soroca Soroca North 48.146 28.282 1,144.24 57.76
4 Costesti Rișcani 47.866 27.235 1,174.87 40.84
5 Bălți Bălți 47.781 27.909 1,148.16 55.43
6 Șoldănești Șoldănești 47.812 28.776 1,179.57 51.34
7 Telenesti Telenesti 47.512 28.354 1,182.75 46.95
8 Orhei Orhei 47.396 28.831 1,174.61 51.81
Middle
9 Ungheni Ungheni 47.220 27.815 1,174.53 54.02
10 Chișinău Chișinău 47.039 28.858 1,193.99 58.97
11 Hîncești Lăpușna 46.843 28.596 1,186.33 52.10
12 Leova Leova 46.486 28.243 1,228.96 47.39
13 Căușei Tighina 46.661 29.413 1,194.83 56.03
14 Cahul Cahul 45.929 28.196 1,235.68 37.53
South
15 Palanca Stefan Vodă 46.407 30.078 1,263.10 58.52
16 Comrat Găgăuzia 46.315 28.661 1,213.68 49.74
17 Vulcănești Vulcănești 45.679 28.457 1,267.61 50.59
18 Rîbnița Nistru 47.769 29.060 1,172.62 53.01
Left
19 Dubăsari Nistru 47.272 29.212 1,200.64 52.52
Dniester
20 Tiraspol Nistru 46.866 29.634 1,207.17 60.54
Average energy over a year [kWh/year/kW installed] 1,190.76 51.74
The places considered for the refined average energy production with PVs are
presented in Figure 1, while the average specific energy in each zone is also presented (based
on administrative organisation from [4]), showing a slight improvement of solar energy in the
south region compared with the north part (only 4% more in South). It shows that there are
appropriate conditions for PV installations everywhere across RM, everywhere from North to
South.

Figure 1. Places in the Republic of Moldova used to calculate the annual average
energy with PV power plants.

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 C. Efremov 113

Based on the method described in [2], the energy coverage with PVs of yearly country
consumption is shown in Figure 2, which uses as inputs the following data:
a) the average value of yearly-based specific PV production in RM (1,191
kWh/year/kW) from Table 1.
b) The yearly consumption of RM, based on data from year 2020, which was 5940
GWh (based on processed data obtained from [5]).

Figure 2. The need of PV power for various levels coverage of the consumption on yearly
basis in Republic of Moldova and suggested share with wind, hydro and biomass.
It is observed that for 100% of required consumption the country, the needed capacity
for PV installations is 4.98 GW, while for covering 50% are needed only 2.49 GW.
Wind power plants have the potential to contribute essentially to the second half of
the RES energy production (as suggested in Figure 2). This is already treated in other works.
For instance, in [6] are shown the areas of the Republic of Moldova with wind potential, while
the paper deals extensively with their integration into the national energy system of the
Republic of Moldova.
3. Impact on land use in the scenario of high PV share in the future RES mix
In order to assess if the land needed for PVs if up to 50% of RM yearly consumption is
obtained from PV production, it is needed to estimate the specific area for a power unit of PVs.
Figure 3 shows the relevant geometry of PV rows for deducting the surface needed for
1 kW of PV panels.

Figure 3. PV rows geometry for land-based deployment of Photovoltaic Power Plants.

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114 Photovoltaics solutions and energy communities in a clean energy roadmap

The ideal tilt angle 𝜃𝜃 of the PVs - for a maximum energy obtained over a year, is around
35º for RM, similar for different points, as has been calculated with [3].
The calculation of the power density is based on geometry from Figure 3 (left side) by
applying the following formulas:
𝑆𝑆 = 𝑅𝑅 ∗ 𝐷𝐷 = (𝑊𝑊 + 𝑃𝑃) ∗ 𝐷𝐷 = (𝐿𝐿 cos 𝜃𝜃 + 𝐻𝐻/ tan 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 ) ∗ 𝐷𝐷 (1)
= (𝐿𝐿 cos 𝜃𝜃 + 𝐿𝐿 sin 𝜃𝜃 / tan 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 ) ∗ 𝐷𝐷 (2)
𝑆𝑆1𝑘𝑘𝑘𝑘 = 𝑆𝑆/𝑃𝑃𝑃𝑃𝑃𝑃_𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝 (3)

For 𝜃𝜃 = 35⁰ (best tilt angle for highest energy over a year) and for 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 = 12⁰ (as a
lowest sun angle during winter without shadow) we analyse two types of PV installations:
- Rows of one PV panel of 1000 x 2000 mm (DPV x LPV), having PPV = 420 Wp/panel
(conservative value, higher values may exist) and mounted with DPV side on the
ground (the small side), as per the design V1 in Figure 5 (lower right side). The
length L is therefore equal to LPV = 2 m, while the depth in the row is equal to DPV
= 1 m. The power of the row is PROW = PPV = 420 Wp, as it is only one panel in the
considered DPV depth.
- Rows of 3 x PV panels of the same dimension of 1000 x 2000 mm (DPV x LPV), having
the same output PPV = 420 Wp / panel and mounted with LPV side on the ground
(the large side), as per the design V2 in Figure 5 (upper right side). The length L is
therefore equal to 3 x DPV = 3 m while the depth in the row is equal to DPV = LPV = 2
m. The power of the row is PROW = 3 x PPV = 3 x 420 =1260 Wp.
The total needed surface for one row can be deducted as being:
𝑆𝑆𝑉𝑉1 = (2 cos 350 + 2 sin 350 / tan 12⁰) ∗ 1 = 7.03 𝑚𝑚2 (4)
𝑆𝑆𝑉𝑉2 = (2 cos 350 + 3 sin 350 / tan 12⁰) ∗ 2 = 21.11 𝑚𝑚2 (5)
𝑆𝑆1𝑘𝑘𝑘𝑘_𝑉𝑉1 = 7.03 / 0.420 = 16.7 𝑚𝑚2 /𝑘𝑘𝑘𝑘𝑘𝑘 (6)
𝑆𝑆1𝑘𝑘𝑘𝑘_𝑉𝑉2 = 21.11 / 1.260 = 16.7 𝑚𝑚2 /𝑘𝑘𝑘𝑘𝑘𝑘 (7)
In both situations it is needed the same land area, which shows that they are
equivalent in terms of density. Therefore, both design geometries as used, as per Figure 4
real implementation examples (V1 on the left, as from [7] and V2 on the right, as shown at [8]).

Figure 4. Real PV implementation of design V1 (left) and V2 (right) geometry.

The 16.7 m2/kWp has been calculated at the most difficult situation in winter, when
the sun has a min to max tilt angle which are very low (lowest is expected for 21st of December).
According to [9], in Chisinau area, during the day of 21st of December 2022, we have
𝛼𝛼 ≥ 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 = 12⁰ in the time period between 9h:34m and 14h:32m, which means that there is
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 C. Efremov 115

no shadow for approximate 5 hours. From the same site, it can be deducted that 𝛼𝛼 ≥ 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 =
10⁰ for 5 hours and 40 minutes (13.3% longer period), so the needed land for 1 kW PV is also
calculated for 10⁰.
For 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 = 10⁰ the minimum needed land is:
𝑆𝑆𝑉𝑉1_10𝑔𝑔𝑔𝑔𝑔𝑔 = (2 cos 350 + 2 sin 350 / tan 10⁰) ∗ 1 = 8.15 𝑚𝑚2 (8)

𝑆𝑆1𝑘𝑘𝑘𝑘_𝑉𝑉1 = 8.15 / 0.420 = 19.4 𝑚𝑚2 /𝑘𝑘𝑘𝑘𝑘𝑘 (9)

The calculations show that in usual PV power plants, around 20 m2 can be considered
for each 1 kW installed, based on the ideal tilt angle of the PV (around 35º for Moldova) and
eventually by adding some areas for access roads and other power plant necessities.
With this value 𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 = 20𝑚𝑚2 /𝑘𝑘𝑘𝑘𝑘𝑘, a total power of 2.49 GW in PVs will need only:
𝑆𝑆50% = 𝑃𝑃𝑃𝑃𝑉𝑉50 % ∗ 𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 = 2.49 ∗ 106 ∗ 20 = 49.8 ∗ 106 𝑚𝑚2 = 49.8 𝑘𝑘𝑘𝑘2

Higher densities of PV panels (needing e.g. 12 m2/kWp PV) can be obtained for instance
if 𝛼𝛼𝑀𝑀𝑀𝑀𝑀𝑀 = 15⁰ and 𝜃𝜃 = 25° (lower tilt angle, which brings lower PV specific energy per year).
The need for 4.98 GW in CEF installations (100% coverage of yearly consumption in
RM) uses under 0.8% of the country's agricultural land (based on method used in [2]) to cover
the entire volume on an annual basis, is consistent with similar results for other countries
[10,11]. One conclusion of Greenpeace is that, at the moment, only political will is needed to
achieve such a goal [12]. A World Wildlife Fund study shows that in Germany, 2% of the
country's land area is enough to produce all the energy used annually from renewable sources
alone [13]. The potential for electricity supply from RES alone is also highlighted in [14],
showing that 1% of the EU's surface area can supply the entire usable EU electricity needs.
Moreover, a new field of sustainable development can be addressed, that of the
harmonious interweaving of agriculture with CEF, i.e. an "agro-photovoltaic" development at
the country level [15]. Such a concept is extremely conducive to a country like the Republic
of Moldova, characterized by important activities related to the use of agricultural land, which
can approach new values of their potential to support a society that can keep traditional
activities in a sustainable and competitive way. In [15] are listed explicitly also floating PVs
and their potential is analysed in more depth in the next section.

4. Floating PV solutions for Republic of Moldova

A new field of interest in deploying photovoltaics power plants is the promotion of
floating PVs. There are several reasons why they may become attractive:
a) such installations do not occupy land usable for ordinary human activities
(agriculture, urban areas, etc.).
b) floating PVs ensures a higher conversion yield during the summer, because the PV
panels, whose efficiency decreases with increasing temperature, are better cooled by the
surface of water on which they float;
c) often such water surfaces (e.g. lakes) are located near urban or suburban areas, for
which it can provide energy in an area close to the place where it can be used.
This section will assess the level of installed power which can be reached with PVs
when using floating PV technology. In this respect, Figures 5 [9], 6, 7 and 8 present the
potential of some of these lakes in the Republic of Moldova. The lake areas have been
obtained by using the “Distance” tool of [16].

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116 Photovoltaics solutions and energy communities in a clean energy roadmap

Figure 5. The potential of photovoltaic capacity for two lakes in the Republic of
Moldova: Ghidighici and Kongaz, in the conditions of a low density of photovoltaic
panels: 50 m2/kW installed.
Figure 6 particularly looks in the potential of some lakes placed nearby Prut River,
which can be considered as reservoirs of water related to this river.

Figure 6. The potential of photovoltaic capacity for two lakes in the Republic of
Moldova: Manta and Beleu zones.

Figure 7. The potential of photovoltaic capacity for two lakes in the Republic of
Moldova: Taracilia and Sarata Noua zone.

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 C. Efremov 117

In Figure 8 it is analysed also the potential of using a hydro-power-plant lake (Costești,

on the right side) with dual use: reservoir for the hydro-plant and lake for floating PVs. Such
combination has been also discussed for other lakes around the world [17].

Figure 8. The potential of photovoltaic capacity for two lakes in the Republic of
Moldova: Suruceni and Costești zone.

For the floating PV it is considered a lower density, to allow other lake-based activities,
meaning that the area needed for 1 kW of PV is chosen to be studied in two cases:
- 50 m2/kW (low density), which is 2.5 to 3 times lower than for usual ground-based
implementations.
- 80 m2/kW (even lower density), which is 4 times lower than for usual ground based
implementations.
A brief overview of representative figures related to these locations is presented in the
Table 2, while choosing the low-density PV implementation.
Table 2
Power and yearly energy potential for the selected lakes of RM for low density of
80 m2/kW in PVs
PV power Estimated yearly
Area
Lake denomination potential (MW) energy (GWh)
(km2)
Density V1: 50 m2/kW
1 Ghirghidici 4.7 94 111
2 Kongaz 2.0 40 47
3 Manta 6.7 134 158
4 Beleu 5.7 114 135
5 Taracilia 6.1 122 144
6 Sarata Noua 0.76 15 18
7 Suruceni 1.1 22 26
8 Costesti 4.6 92 109
Total 31.7 633 748
RM consumption coverage 10.7%

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118 Photovoltaics solutions and energy communities in a clean energy roadmap

Table 3 presents the potential of the same lakes by considering an even lower density
(80 m /kW) of the PV panels on the lake surface.
2

It can be seen that the potential of such lakes is not negligible, they also have the
advantage of being close to the cities (e.g. in the case of lakes nearby Chisinau and Kongaz).
Other lakes exist also in other zones of the Republic of Moldova, however even these
locations can bring high contribution of PV based RES:
- 6.7% of yearly consumption in the case of lower PV density of 80 m2 / kW installed,
respectively
- 10.7% of yearly consumption in the case of low PV density of 50 m2 / kW installed.

Table 3
PV Power and yearly energy potential for the selected lakes of RM for lower density
of 80 m2 / kW
PV power Estimated yearly
Lake denomination Area (km ) 2
potential (MW) energy (GWh)
Density V2: 80 m2/kW
1 Ghirghidici 4.7 59 69
2 Kongaz 2.0 25 30
3 Manta 6.7 84 99
4 Beleu 5.7 71 84
5 Taracilia 6.1 76 90
6 Sarata Noua 0.76 10 11
7 Suruceni 1.1 14 16
8 Costesti 4.6 58 68
Total 31.7 396 468
RM consumption coverage 6.7%

To be noted that usual density in fields dedicated to PV panels installations is around

20 m /kW. The lower densities proposed for the floating PVs placed on lakes allow the
2

placement of the panels at least in two ways:

- With larger access lanes between PV lines allowing other activities such as fishery
in between the PV lines.
- With clusters if classic density PVs (e.g. with 20 m2/kW), other activities may be
fully developed in between the clusters.

Figure 9. PV panels setups: a) Large access lanes between PVs; b) Clusters of PVs.

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 C. Efremov 119

Moreover, placing 1 kWp of PVs on 50 or 80 m2, creates a spatiality which practically

avoids shadowing between tow PV rows nearly the whole day even in worst situations in
December.

5. Rural energy communities sustained by local RES production. Examples involving

floating PV solutions
A particularly important added value of encouraging energy production at the local
level is the possibility to grow energy communities around these energy sources. The
following advantages ca be considered:
- local production at traditional users, who thus become active users (prosumers); this
type of distributed production is generally achieved through PV mounted on roofs, especially
in rural areas and in urban neighbourhoods that predominantly have own houses. The power
installed on these roofs, with PVs mounted usually towards south, is usually in the field of 3
to 10 kW;
- local production for the active medium size users, which refers to state institutions
such as schools, hospitals and other public buildings, to industrial buildings and for
commercial use. The PV power of these installations can be from 50 to hundreds of kW. If the
parking lots of the shopping complexes are added, using special carports, the total power can
reach the MW range;
- a third important category represents the energy community. Frequently the users of
a community do not have a functional space to invest each individually in a RES installation,
but are willing to organize themselves in energy "cooperatives", which may be in
collaboration with the mayor's office or other public or private entity from their area. This
aspect of the energy community will be developed further using two cases of small floating-
PV applications.

Figure 10. The potential of photovoltaic capacity for two small lakes and a
potential formation of energy communities.

In can be seen that the small power between 4 to 6 MW in floating PVs can supply
nearby communities, as ca be seen in Figure 11, in areas of 1 up to 7 km radius, while Table
4 estimates installed power in floating PVs and the annual energy for 1191 kWh / kW chosen
in section 1.

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120 Photovoltaics solutions and energy communities in a clean energy roadmap

Figure 11. Energy communities’ formation: a) small community with km range

radius; b) larger community, with up to 7 km radius.

Table 4
PV Power and yearly energy potential for the selected lakes of RM for lower density
of 80 m2/kW of floating PVs
PV power Estimated yearly
Area
Lake denomination potential (MW) energy (GWh)
(km2)
Density V2: 80 m2/kW
1 Cupcici-Chetrosica Veche 0.34 4.25 5.06
2 Tirnova 0.45 5.62 6.70

In order to be a sustainable energy community, the energy from the floating PVs need
to cover an important part of the yearly consumption of the energy community. Table 5
presents an estimated yearly production of the PVs (column 6) which is compared with the
community production over the year (column 5).
The population of the two energy communities is based on [18] and [19]. As shown
also in Figure 11, the energy communities have the following structure:
- Cupcici community: with 7190 inhabitants in Cupcici and 817 inhabitants in
Chetroșica Veche; the total number of inhabitants of the small energy community
(km range radius) is 8007
- Tîrnova community: with the following number of inhabitants: 2050 in Tirnovam
3108 in Trinca, 3265 in Gordinesti and 1921 in Hlinaia; the total number of
inhabitants of the larger energy community (up to 7 km radius) is 10344.

Table 5
Energy community KPIs
E_prod
Energy/ E_cons /
Energy PV / Procent of
Population Houses month year (MWh)
community year consumption
(kWh) community
(MWh)
Cupcici 8007 2669 200 6405.6 5060 79.0%
Tirnova 10344 3448 200 8275.2 6700 81.0%

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 C. Efremov 121

To be noted that the number of houses has been estimated as being an average of one
for each 3 inhabitants, rule which provides the numbers from column 3. In order to estimate
the yearly consumption of the community, a simplified approach is to base these values on
an average monthly consumption per house. The study considers a value of 200
kWh/month/household, while households may consume between a lower energy of around
average 100 kWh and a higher energy of around 300 kWh/month.
Table 5 shows that the yearly consumption is covered in a share of around 80% for
both communities. The assessment suggests that most of the energy is therefore produced
locally and that only a small share of around 20% is needed to be purchased from the public
network. This result shows the potential of such approach, respectively to produce locally, on
a non-agricultural surface (on a lake belonging to the community area), close to entire yearly
need of the community.
This situation allows also to implement aspects of resilience such as:
- Resilience of energy, meaning that short to medium time periods without supply of
energy from main grid can be surpassed by off-grid local supply
- Resilience of local businesses, as most of the energy is supplied based on already
known tariffs deducted from the feasibility study of the local energy investment,
which is not influenced by external factors after the objective is operational.
For the energy resilience it is needed that the PV production is also accompanied by
electrical storage. The need for storage at country level has been already studied in [20] For
local PV production, a usual level of 1 to 2 kWh of energy storage is used already in some
applications for shaving the peak power of 1 kW of PV.
This storage resource allows also a certain resilience (e.g. 1 to two hours or more) if
the main grid fails to supply energy to the community, depending on the adaptation of
consumption to lower values during the power outage.
A priority can be given in this situation only to the most important loads, e.g.:
refrigerators (for keeping food in good conditions), telecommunication means (modems,
routers, switches etc.), low-consumption computers such as laptops or tablets, LED-based
light etc.
For the resilience of the local business, it is targeted finally a sustainable development
of the community, which is less influenced by volatile prices due to external factors, such as
political or proxi-wars situations. This type of resilience is in many cases neglected, despite
the fact that the impact of external factors may be dramatic in some cases.
While the coverage of up to 80% of the consumption over a year looks quite promising,
two additional factors may be also considered:
- Shifting of classic ICE - based cars to electromobility.
- Heating with electricity
The paper is analysing only the first factor.

6. Impact of electrical vehicles

The ongoing revolution in switching to electrical vehicles plays a key role in its effect
of the energy field. Due to a growing market and a smaller effect of business-as-usual inertia
and the monopolies associated with maintaining this situation, electromobility is the main
driver of the innovation through batteries, power electronics, artificial intelligence and
associated ITC components, having a beneficial effect in the energy field, much more related
to natural and historical monopolies and the fear of changes.

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122 Photovoltaics solutions and energy communities in a clean energy roadmap

Let’s consider that each household has also a light vehicle and that in 2030 we may
have 20% of these cars shifted to EV technology and 50% in year 2040. We consider a scenario
with the following inputs:
a) an EV is driven 10000 km/year, with half of it expected to be covered by local
charging.
b) the average consumption of a light EV is around 15 kWh / 100 km
It means that an EV will need 5000 km supported by local energy production, which means
15 x 50 = 750 kWh / year / EV.
With the data already used in tables 3 and 4, the table 6 shows that additional
consumption energy needed for the 20% and 50% EV fleet. Table 5 shows the impact of EV
charging in the community, compared with the community PV production over a year
(energies shown in MWh).

Table 6
Energy community KPIs related to electrical vehicles introduction
Energy Energy Percentage Percentage
Energy EVs- EVs-
Vehicles for EVs for EVs in 2030 of in 2040 of
community 2030 2040
2030 2040 PV prod. PV prod.
Cupcici 2669 534 1335 400.5 1001.25 7.97% 19.93%
Tirnova 3448 690 1724 517.5 1293 7.78% 19.45%

The table shows that around 8% in 2030 and 20% in 2040 of the energy community
production with floating PVs is needed for covering EV charging due to the rapid expansion
of EVs in the studied energy communities. This means that for the households consumption
presented in table 5 it remains only around 60% of local production for the time horizon of
2040. This situation suggests that the floating PV solution need to be complemented with
additional local sources, such as agri-photovoltaics. By considering also electric heating, the
energy produced locally can be doubled, with a 50% share in floating PVs on the local lake,
while the remaining can be mounted on ground.
The assessment shows however that a local sufficiency is a tangible target and that
each solution need to be treated case by case.

7. Roadmap to 2050 in the Republic of Moldova

In continuation it is presented a roadmap to 2050 in the Republic of Moldova, based
on what has been proposed in [15], with essential elements that can be the basis of the
national policies.
1) It will be facilitated the development of renewable electricity sources distributed in
all regions of the country where there is high consumption in the neighbourhood (cities,
industry, etc.). These must be especially based on photovoltaic and wind-based power plants,
in a proportion that corresponds to the environmental conditions of the Republic of Moldova,
following in-depth, multi-criteria studies. A contribution of at least 50% to the solar proved
to be possible [5]. The paper particularly develops specific solutions for floating PVs and their
potential to help local energy communities. A suitable solar-wind combination requires
further study. It will also be analyzed whether there is still hydropower potential that can be
attracted in the energy mix.

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 C. Efremov 123

2) It will be supported the increase the flexibility of the electrical power system,
especially through important projects, such has the construction of at least one Pumped
Hydro Plant (PHP, with favourite locations being on Dniester river), combined with Battery
Energy Storage Systems (BESS), these one being projected to hold the biggest amount of the
necessary [12].
3) It will be taking into consideration flexibility measures which will reduce the
dependence on technological services system provided by neighbouring countries (especially
Ukraine).
4) It will be electrified in stages the household heating, through various methods
(direct heating through Joule effect, heating with increased efficiency – by using heat pumps,
use of existing thermal power plants combined with heating, adapted for green H2 și CH4
etc.), all these being accompanied by the methods to increase the efficiency of heat
consumption through retrofitting (modernization) at the heating installations level and at the
buildings level.
5) It will be electrified in stages the small vehicles park and then the one with trucks
and busses and it will be promoted EVs with V2G; this process will be accompanied by ITC
charging coordination solutions (solutions equivalent to demand response) and the
promotion of EVs with V2G facilities, whose potential to provide flexibility through the use
of energy in batteries, is extremely high.
6) The introduction of renewable energy sources will be accompanied as much as
possible by agro-photovoltaic solutions which will bring synergistic benefits to both areas,
including accelerated electrification of agriculture; where feasible, floating CEFs on lakes
close to large consumers will also be encouraged.
7) It will be encouraged the digitalisation of the energy activity, including through
smart metering, energy and flexibility services markets, SCADA systems and promotion of
initiatives which contain Smart Grid functionalities.
8) It will be encouraged the creation of resilient energy communities which will reduce
their risk according to the defects in the public network, of large price fluctuations in the
energy field compared to extreme climatic situations. These communities will also be formed
in the perspective of building future smart cities, in which resilience and sustainability play
key roles. In the same context, small RES producers will be encouraged to become active
users.
9) It will be encouraged the realisation of pilots for the emerging technologies, such
as Power-to-Gas, respectively obtaining and transporting green hydrogen, inclusively in
mixture with methane gas; this field is to be developed cautiously by 2030, waiting for the
gradual maturation of technologies at the international level.
10) It will be encouraged new business models, such as Power Purchase Agreements
(PPAs) - which guarantee low prices over known periods of time (helping predictably and
sustainably other activities of the society), but also appropriate approaches for new
technologies, such as financial models Storage as a Service or RES + local storage coupling
models, as unitary solutions.
11) It will be encouraged the high-level education and scientific research to support
new energy revolution with qualified staff and appropriate solutions, in its ambitious path
towards carbon neutrality.
12) Energy policies should be achieved such that they stimulate in an efficient manner
these objectives, through lawmakers, government and regulation agency in the energy field.

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124 Photovoltaics solutions and energy communities in a clean energy roadmap

8. Conclusions
In conclusion, the country's future in the energy field looks pretty good in the long
term perspective. However, in order to ensure that this potential is exploited, the Republic of
Moldova must take courageous decisions to attract investments. There is a fierce global
competition between countries in the world to attract capital, especially between developing
and emerging countries. The Republic of Moldova can be a good participant in this race, if it
presents a solid business plan in the medium and long term development.
The paper presents the potential pf PV-based energy production at national level, with
clear figures for different participations in the total RES, while suggesting a contribution of
up to 50% of total yearly consumption, to be complemented by wind, hydro and biomass-
based RES production. A connection between the power needed to be installed and the
necessary land are is also addressed, while the calculation of needed area for 1 kWp is
presented in detail. Moreover, the potential of floating PVs is assessed for various lakes in
RM and is proven to be of interest in the future. Finally, the local production with floating
PVs has been combined with two local communities needs, by proposing a model for energy
communities, more resilient to power outages and to unpredictable energy prices from
external sources.
The paper makes also a brief presentation of a roadmap of energy developments till
2050 in the Republic of Moldova. These transformations will happen if the energy strategy
planned for decades, state policies and regulations will be put into practice based on specific
projects to be carried out in the energy sector, in order to prepare for the inevitable energy
transition. The Republic of Moldova will face a lot of challenges in the energy sector in the
next ten years, but it is still a process that can be prepared and successfully implemented.

Conflicts of Interest. The authors declare no conflict of interest.

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madhya-pradesh-on-epc-basis (accessed on 20 July 2022).
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bih/ (accessed on 30 March 2022).
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Citation: Efremov, C. Photovoltaics solutions and energy communities in a clean energy roadmap for
Republic of Moldova. Journal of Engineering Science 2022, 29(3), pp.
110-125. https://doi.org/10.52326/jes.utm.2022.29(3).10.

Publisher’s Note: JES stays neutral with regard to jurisdictional claims in published maps and
institutional affiliations.

Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
and conditions of the Creative Commons Attribution (CC BY) license
(https://creativecommons.org/licenses/by/4.0/).

Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 126 - 135
Fascicle Architecture, Civil and Environmental Engineering ISSN 2587-3474
Topic Environmental Engineering eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).11
UDC 625.85:628.4

RHEOLOGICAL CHARACTERIZATION OF INDUSTRIAL WASTE MODIFIED

BITUMEN

Chukwuka Ezemenike 1*, ORCID ID: 0000-0001-5644-0812,

Olugbenga Oyedepo 1, ORCID ID: 0000-0001-6131-0959,
Olufikayo Aderinlewo 1, ORCID ID: 0000-0002-8754-7425,
Isiaka Oladele 2, ORCID ID: 0000-0001-7168-1518,
Omoniyi Olukanni 1, ORCID ID: 0000-0002-6086-5888

Department of Civil Engineering, Federal University of Technology, Akure, Nigeria

1

2
Department of Metallurgical Material Engineering, Federal University of Technology, Akure, Nigeria
*Corresponding author: Chukwuka Ezemenike, [email protected]

Received: 06. 06. 2022

Accepted: 08. 02. 2022

Abstract. The aim of this research is to evaluate the rheological properties of industrial waste
modified bitumen. The varying proportion of polypropylene ranging from 0% to 20% of the
weight of bitumen at 5% interval with 60/70 penetration grade was used. The asphalt binder
modification was prepared by using high-speed mixer at temperature from 150 °C to 190 °C.
The conventional test like softening point, penetration, ductility, flash and fire point test were
carried out to assess the physical characteristics of polypropylene modified and unmodified
bitumen, thereafter dynamic shear rheometer and rotational viscosity test were conducted to
determine the rheological properties of bitumen. The result indicated that polypropylene has
ability to improve the conventional properties of bitumen by increased penetration and
ductility, decrease softening point and flash and fire point. Polypropylene modified bitumen
provides better resistance against permanent deformation due to their increase in complex
modulus and rotational viscosity and decrease in phase angle. It can be concluded that
polypropylene modified bitumen could improve the level of performance and service life of
the road.

Keywords: industrial waste, modified bitumen, performance, polypropylene, rheology.

Rezumat. Scopul acestei cercetări este de a evalua proprietățile reologice ale deșeurilor
industriale de bitum modificat. A fost utilizată proporția variată de polipropilenă, variind de
la 0% la 20% din greutatea bitumului la interval de 5% cu grad de penetrare 60/70.
Modificarea liantului asfaltic a fost preparată utilizând un malaxor de mare viteză la o
temperatură de la 150 °C la 190 °C. Testele convenționale cum ar fi punctul de înmuiere,
penetrarea, ductilitatea, punctul de aprindere și punctul de foc au fost efectuate pentru a
evalua caracteristicile fizice ale bitumului modificat și nemodificat cu polipropilenă, apoi au
fost efectuate reometrul de forfecare dinamică și testul de vâscozitate rotațională pentru a
determina proprietățile reologice ale bitumului. Rezultatul a indicat că polipropilena are
capacitatea de a îmbunătăți proprietățile convenționale ale bitumului prin creșterea
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 C. Ezemenike, O. Oyedepo, O. Aderinlewo, I. Oladele, O. Olukanni 127

pătrunderii și ductilității, scăderea punctului de înmuiere și a punctului de aprindere și de foc.

Bitumul modificat cu polipropilenă oferă o rezistență mai bună împotriva deformării
permanente datorită creșterii modulului complex și a vâscozității de rotație și scăderii
unghiului de fază. Se poate concluziona că bitumul modificat cu polipropilenă ar putea
îmbunătăți nivelul de performanță și durata de viață a drumului.

Cuvinte cheie: deșeuri industriale, bitum modificat, performanță, polipropilenă, reologie.

1. Introduction
The asphalt binders are considered as one of necessary materials of construction in
flexible pavement, and the performance of flexible pavement is related to asphalt binders.
Asphalt pavement with its superior quality has become one of necessary pavement type
demanded in Nigeria. It is achievable to increase the service life of asphalt pavement and
decrease the maintenance activities by using modifies. The bitumen characteristics can be
enhanced using modifies and the toughness of asphalt concrete mixture at high temperature
can be reduced which will help in lay down and compaction during constructions.
Waste plastic have been enormously utilized in different area of their significant
benefit in term of durability, availability, light and cost effectiveness [1]. The worldwide
production of waste plastic attained 368 million metric tons in year 2019 [2], and Nigeria is
one of largest producers, accounting for 25%. The diffused use of waste plastic contributes
outstanding comfort to everyday life and improves social and economic development.
However, large quantity of waste plastic consumed has caused stresses on our environment.
Presently, various nations have different waste management strategies for plastic waste.
Landfill and incineration have been adopted as a simple way of disposing waste in United
State of America, China and other countries. United Stated of America received 27 million
tons of plastic by municipal solid waste (MSW) stream in landfill [2]. Landfill has been the
natural plastic disposal method that demanded high land resource which also becomes
problem facing plastic waste disposal in different countries [2]. The environmental threat
created by chemical leaching from plastic into soils and waters could many decades which
are disadvantage of using landfill method of disposal of waste plastic. But then, incineration
is method of reducing mass and volume of waste in which air pollution results from the high
temperature process in the incinerator producing dioxin, CO2 and other toxic emission [3].
The heavy metals such as lead (Pb) and Cadmium (Cd) released from waste plastic during
incineration process is dangerous to the human health [4]. Additionally, micro plastic gotten
from degradation of plastic waste created intensive worry for waste management sector, as
micro plastic were able to find their way through filtration system and become hard to take
way [5]. Accordingly, plastic pollution is one most urgent environmental threat to the modern
world [6].
Asphalt binder plays an essential role in pavement performance because it
demonstrates the viscoelastic characteristics under pavement operative condition [7]. In
other to enhance the reliability of flexible pavement to satisfy the traffic, climatic and other
requirements, the use of modified binder rather than unmodified binder has been
commended approach [8].
It is established facts that polymer can improve flexible pavement performance in
term of high temperature stability [9]. High costs of construction combined with
environmental problem created by plastic waste have promoted the utilization of plastic
waste in flexible pavement.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
128 Rheological characterization of industrial waste modified bitumen

Many researchers have investigated the suitable application of utilizing waste plastic
in asphalt binder, environmental concern, modified morphology, the properties of waste
plastic modified binder and modified mechanism [10]. The utilization of packaging waste
polymer and organic montmorillonite was researched by [11] studied and they concluded
that waste polymer content resulted increased in viscosity and decrease in penetration while
organic montmorillonite decrease the viscosity and improved cracking resistance. The use
PET as partial replacement for fine aggregate and result indicated the highest resistance to
permanent deformation was recorded at 20 % PET was studied by [12]. The polymer modified
asphalt depend on test temperature, asphalt source and polymer type in a study concluded
by [13]. They further concluded that polypylene-maleic anhydride and oxidized PE required
lower compaction and temperature. A crumb rubber (CR) modified decreased susceptibility to
cracking at low temperature and increased the toughness of asphalt concrete in investigation
carried out by [14]. The use of rubber tire (scrapped) as a replacement to bitumen was studied
by [15] and concluded that scrap rubber modified asphalt binder increased softening point
and had 55% elastic recovery which is higher than 35% of unmodified. The utilization of low
density polyethylene (carry bag waste) in asphalt concrete was studied by [16], they obtained
10% waste content by weight of bitumen as optimum content and concluded that low density
polyethylene improved resistance to fatigue, provide better blending between asphalt binder
and aggregate and as well decreased the permanent deformation. Another studied on
polymer waste aggregate (PCA) modified blended using polypropylene by [17] reported
reduction in water absorption and decrease abrasion of aggregate in asphalt concrete.
Present curiosity in recycling waste plastic indicate substantive gain of utilizing it as
a sustainable polymer in enhancing bituminous characteristics, achieving environmental
stability and advancing economic-industrial growth. Several type of industrial waste such as
modifier were tried globally to improve the rheological characterization of bitumen, such as
nano-materials [18], waste plastic [19], crumb rubbers [20] and geopolymers [21]. Waste
plastic based polypropylene could be used to enhance the rheological characteristics of
bitumen. Polypropylene modified bitumen for road construction can improve the permanent
deformation and thermal cracking resistance at high and lower temperature. These possible
enhancements can improve the pavement life [22].
The main commonly utilized polymer worldwide includes 75% elastomeric modified
binder, 15% plastometric and remaining 10% belongs to either rubber or other modification.
The elastomers often use to increase the bitumen at low and high temperature. Nevertheless
plastomers are well known efficient additive that can increase high service temperature [23].
Polypropylene belongs to plastomers family which provides rigidity to the bitumen and
decrease the deformation under load and effect is more profound when the concentration of
polypropylene is high by weight of the base bitumen. Different researchers have examined
the possibility of using modifiers in polymer form on the bitumen and asphalt concrete
mixture characteristics. The result of these research indicated that modifying using polymers
could alter bitumen properties by increasing viscosity [24], increasing softening point [25],
improving the performance of grade [26] and decreasing the penetration [27].
Polypropylene is one of the most effective polymer modifiers which are generated
from polymer industry. It is semi-crystalline material with excellent chemical resistance,
wears resistance, good fatigue and has wide range of properties. Polypropylene is a simple
structure that has a long chain of carbon atom with hydrogen atoms attached to each carbon
atom. It provides good resistance to organic solvent with low moisture absorption rates.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 C. Ezemenike, O. Oyedepo, O. Aderinlewo, I. Oladele, O. Olukanni 129

Polypropylene is commonly use in sweet wrapping, straws, textile, furniture and automobile
industrial. These qualities have made polypropylene efficient enough to be used as modifier
of bitumen.
2. Materials and Method
2.1. Materials
The bitumen utilized in the present research is 60/70 penetration grade bitumen
obtained from K.K Hassan Construction Company in Akure, Nigeria. As shown (Plate 1 and 2)
local waste plastic in form of polypropylene were collected at dumping site, washed and
grounded to 0.5 to 0.05 mm to be utilized as efficient polypropylene modifier in 60/70
bitumen penetration grade.

Figure 1. Dumping site of waste plastics. Figure 2. Grounded waste plastic.

2.2 Sample preparation

Samples were prepared using melt blending method. The 200 mg of bitumen was
filled inside steel bowel and pre-heated in oven at 130 °C. The grounded polypropylene was
replaced at varying proportion of 5%, 10%, 15% and 20% by weight of bitumen. The modified
bitumen was thoroughly blended at mixing temperature of 185 °C. Mixing was continued for
45 minute to produce homogenous mixtures. Empirical tests such as softening point,
penetration, ductility, flash and fire point were carried out on the samples and thereafter
dynamic shear rheometer and rotational viscosity test were conducted to determine the
rheological properties of modified bitumen.

2.3 Test Method

The physical test performed on the bitumen and modified bitumen to determine its
suitability was flash and fire point test [28], softening point [29], viscosity test [30], ductility
test [31] and penetration test [32]. The rheological test conducted in the bitumen and
modified bitumen were dynamic shear rheometer test [33] at temperature of 60, 70, 80 and
90 °C and rotational viscosity tests [34] at 135 and 165 °C.
3. Results and Discussion
3.1 Conventional test result of modified and unmodified bitumen mixture
The experimental results of conventional physical properties of modified bitumen with
varying percentages of polypropylene are indicated in Figure 3, 4, 5 and 6. It is showed that
penetration values continued to decrease as percentage of polypropylene increased as

Journal of Engineering Science September, 2022, Vol. XXIX (3)

130 Rheological characterization of industrial waste modified bitumen

indicate in Figure 3. They decreased resulted to hardness of modified bitumen because

polypropylene has higher molecular weight thereby increase viscosity of the bitumen [35].

Figure 3. Penetration of Polypropylene.

Figure 4. Softening Point of Polypropylene.

Softening point result increased as percentage of polypropylene increased as shown

in Figure 4, the result clearly indicated that addition of polypropylene to bitumen increased
softening point values. This could be as result of bitumen resistance to the essence of
temperature and this shall decrease asphalt pavement to soften in hot weather, thus
polypropylene modified bitumen will be less affected to temperature changes [35]. Flash and
fire point increased continuously as various proportion of polypropylene increases as
indicated in Figure 5. This can be attributed to the different in temperature of the
polypropylene and bitumen blended together at increase in temperature. This also showed

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 C. Ezemenike, O. Oyedepo, O. Aderinlewo, I. Oladele, O. Olukanni 131

that addition of polypropylene content into asphalt mixture will like to decrease fire hazard
in asphalt pavement [36].
The result of ductility obtained showed that ductility trend to decrease continuously
as proportion of polypropylene increases as shown in Figure 6. As the polypropylene modified
bitumen get harder and stiffer, it could resist anti-cracking performance of asphalt concrete
at low temperature [37].

Figure 5. Flash and Fire Point of Polypropylene.

Figure 6. Ductility of Polypropylene.

3.2 Rheological result of modified and unmodified bitumen

The viscoelastic behavior of asphalt binders was characterized at temperature of 60℃,
70℃, 80 ℃, and 90 ℃ using dynamic shear rheometer (DSR). The test results are shown in
Figures 7 and 8 which illustrate the complex modulus and phase angle respectively against

Journal of Engineering Science September, 2022, Vol. XXIX (3)

132 Rheological characterization of industrial waste modified bitumen

different temperature in the binder. The values of complex modulus obtained at 0% (385.9
kPa, 392.5 kPa, 419.8 kPa, 425.7 kPa, 452.9 kPa); 5% (369.5 kPa, 388 kPa, 418 kPa, 421 kPa,
441.8 kPa); 10% (396 kPa, 407.7 kPa, 411.5 kPa, 431.2 kPa, 435.8 kPa); 15% (379.6 kPa, 385
kPa, 379.6 kPa, 401.5 kPa, 415 kPa), 20% (344 kPa, 368 kPa, 385.3 kPa, 400.5 kPa, 408 kPa)
and the values of phase angle at 0% (89.2 δ, 86.5 δ, 82 δ, 78.2 δ, 75 δ); 5%(80 δ, 79.5 δ, 77.8
δ, 75 δ, 72.5 δ); 10%( 82.5 δ, 77.6 δ, 71.9 δ, 73 δ, 70 δ) δ, 15%( 82 δ, 80 δ, 78.6 δ, 77 δ, 60.4
δ); 20% (70.1 δ, 65.2 δ, 60 δ, 58 δ, 52.6 δ). From the result, it can observe that, all samples
indicated decrease in phase angle and increase in complex modulus values as the
temperature increases. These could be as result of higher shear blending of polypropylene
modified bitumen mixture and its synergistic process, which might resist changes in
polypropylene asphalt binder particle size and arrangement. The engineering properties of
modified was enhanced as seen Figure 7 and 8.

Figure 7. Complex Modulus of Polypropylene.

Figure 8. Phase Angle of Polypropylene.

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 C. Ezemenike, O. Oyedepo, O. Aderinlewo, I. Oladele, O. Olukanni 133

The increase in elasticity is because of the position arrangement of molecule and

bonding system with each other which made it more elastic and tough and therefore more
resistant to rutting and permanent deformation [38]. Moreover when temperature to the
existence to each other increased, it will have higher improvement. The lower phase angle δ
means that asphalt concrete mixture is more elastic than viscous and will recover to its
original condition without break up [39]. Also, at high temperatures, the lower phase angle
is desirable since this will decrease permanent deformation. The addition of Polypropylene
had a significant effect on the rotational viscosity of the asphalt as shown in Figure 9. By
increasing the Polypropylene content, the rotational viscosity of the asphalt increased rapidly.
According to the laboratory test results, Polypropylene contents at 135 °C have high
rotational viscosity values while Polypropylene content at 165 °C has low rotational viscosity
values because polypropylene decrease molecular weight due to higher temperature was
applied [40].

Figure 9. Rotational Viscosity of Polypropylene.

4. Conclusions
The modification of bitumen using polypropylene improves conventional and
rheological properties of the modified bitumen produced. Based on the experimental results,
the asphalt binder containing polypropylene resulted decrease in penetration, increase in
softening point, decrease in ductility and increase in flash and fire point. These results
demonstrated that polypropylene modified bitumen improve resistance against permanent
deformation and also more advantage when compared to unmodified bitumen used in
pavement industry. The rheological property of bitumen was highly affected by addition of
polypropylene as indicated by result of dynamic shear rheometer and rotational viscosity.
This indicated that polypropylene used as a modifier showed better performance in term of
enhancing the rutting deformation and decrease the bitumen susceptibility to crack and
deformation at higher temperature.

Conflicts of Interest. The authors declare no conflict of interest.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

134 Rheological characterization of industrial waste modified bitumen
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Citation: Ezemenike, C.; Oyedepo, O.; Aderinlewo, O.; Oladele, I.; Olukanni, O. Rheological
characterization of industrial waste modified bitumen. Journal of Engineering Science 2022, 29 (3),
pp. 126-135. https://doi.org/10.52326/jes.utm.2022.29(3).11.

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Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
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Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 136 - 149
Fascicle Architecture, Civil and Environmental Engineering ISSN 2587-3474
Topic Environmental Engineering eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).12
UDC 628.3.034.2:663.4(67)

PHYSICOCHEMICAL CHARACTERIZATION OF ASMARA BREWERY EFFLUENTS

Aremanda Ramesh Babu*, ORCID: 0000-0002-6609-8640,

Tekle Arsiema, ORCID: 0000-0003-0239-0834,
Daniel Heaven, ORCID: 0000-0003-4064-038X,
Berhane Filmon, ORCID: 0000-0003-4601-4128,
Mehari Abiel, ORCID: 0000-0002-8891-4805

Department of Chemical Engineering, Mai Nefhi College of Engineering & Technology (MCOETEC), P.O. Box 344,
Asmara, Eritrea.
*Corresponding author: Ramesh Babu Aremanda, [email protected]

Received: 07. 04. 2022

Accepted: 08. 30. 2022

Abstract. Brewing industry is water intensive and consequently generates huge volumes of
wastes. Bottle washing and brewing operations recognized as the major effluent sources of
Asmara Brewery Corporation Share Company (ABCSC), Eritrea. Effluents of bottle cleaning
and brewing sections and their mix of 2:1 characterized on weekly basis for the resemblance
of national and international effluent standards. DO levels of wastes detected as low as 2.14
mg/L, which does not support any life and eventually poses severe environmental issues.
TSS, COD and BOD5 levels have exceeded EU and EPA effluents standards. COD and BOD5
concentrations estimated were higher than other reported breweries and beyond the
benchmarks of Brewer’s Association, USA. Brewery wastewater has a mean COD of 83240
mg/L and BOD5 of 11066 mg/L and highly contaminated than bottle cleaning and mixed
effluents. Therefore, in order to reuse voluminous wastewater and to curb excessive COD
levels, effluents from ABCSC require special attention prior to their discharge into the public
sewer line.

Keywords: Industrial wastewater, characterization, breweries, environmental pollution, chemical

oxygen demand, biological oxygen demand.

Rezumat. Industria berii este consumatoare de apă și, în consecință, generează volume uriașe
de deșeuri. Spălarea sticlelor și operațiunile de fabricare a berii sunt recunoscute ca surse
majore de efluent ale Asmara Brewery Corporation Share Company (ABCSC), Eritreea. Efluenții
secțiilor de curățare a sticlelor și de preparare a berii și amestecul lor de 2:1 sunt caracterizați
săptămânal privitor la corespunderea lor standardelor naționale și internaționale pentru
efluenți. Nivelurile de DO ale deșeurilor detectate variază până la 2,14 mg/L, ceea ce nu
susține nicio formă de viață și în cele din urmă ridică probleme grave de mediu. Nivelurile
TSS, COD și BOD5 au depășit standardele UE și EPA privind efluenții. Concentrațiile de COD
și BOD5 estimate au fost mai mari decât pentru alte fabrici de bere raportate și dincolo de
criteriile de referință ale Asociației Berarii, SUA. Apa uzată a fabricii de bere are un COD mediu
de 83240 mg/L și BOD5 de 11066 mg/L și sunt contaminate la curățarea sticlelor și
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 A. Ramesh Babu, T. Arsiema, D. Heaven, B. Filmon, M. Abiel 137

amestecarea efluenților. Prin urmare, pentru a reutiliza volumele mari de ape uzate și pentru
a reduce nivelurile excesive de COD, efluenții din ABCSC necesită o atenție deosebită înainte
de deversarea lor în canalizarea publică.

Cuvinte cheie: Ape uzate industriale, caracterizare, fabrici de bere, poluare a mediului, necesar
chimic de oxigen, necesar biologic de oxigen.

1. Introduction
Water usage has been increasing globally by 1% every year since 1980’s and is
expected to accelerate at similar rate in future due to continuous growth of population and
socio-economic development activities [1]. Prudent utilization of fresh water resources
accompanied with promising protection of natural ecosystems is one of the most prominent
issues of today’s world. Plenty of research has been done or in progress emphasizing
optimization of fresh water consumption in domestic, agricultural and industrial applications.
Furthermore, there have also been reported the utilization of wastewater with innovative
treatment technologies which, at the same time reduces environmental pollution
significantly. Different types of chemicals discharged into the aquatic systems through
industrial activities pose risk to human health and environment. Some of them are persistent,
toxic and partly biodegradable; hence, they do not easily removed in conventional
wastewater treatment plants and need a special attention to develop an eco-efficient method
for the treatment of a specific pollutant [2].
The brewing industry is water intensive and consequently produces huge volumes of
wastewater despite of the beer is fifth most consuming alcoholic beverage in the world and
brewing is a multibillion-dollar industry that creates jobs, generates taxes, supports
agriculture and attracts tourism [3, 4]. Beer brewing also characterized by the use of high-
quality fresh water due to public perception about the deterioration in quality of beer [3, 5].
It was mentioned in several reports that for every 1 L of beer production, approximately 6 to
10 L of water is used [3, 6, 7]. Water in any brewery used typically for brewing, cleaning and
cooling processes [7]. Usually, wastewater is pre-treated within the brewery before being
discharged into the waterway or municipal sewer system [3]. However, most of them dispose
their effluents without adequate characterization, quantification and pre-treatment due to
economic and technological constraints, which may have adverse effects on the municipal
treatment plant by reducing the efficiency of waste treatment plant and overloading the
system [6]. In recent years, a considerable number of environmental issues includes water
and soil pollution problems such as eutrophication of rivers and dams [6], inhibition of seed
germination, reduction of soil alkalinity and damage of agricultural crops have been reported
due to high inorganic and organic matters from industrial effluents [2].
The quantity and characteristics of brewery wastewater can differ significantly from
time to time and location to location as it depends on several different processes that occur
within a brewery such as malting, mashing, wort processing, fermentation, filtration, bottle
cleaning and packaging. [3, 7]. Commonly, the effluents of the brewery are characterized by
high organic load and high acidic content [3, 6, 7]. It consists of soluble sugar, soluble starch,
carbohydrates, ethanol, volatile fatty acid, suspended solids, yeast etc. [7]. However, the
major component of brewery effluents is organic material, as evidenced by high chemical
oxygen demand (COD) and biological oxygen demand (BOD) [3, 8]. Both of these parameters
(i.e. COD and BOD) are imperative diagnostic parameters for determining the quality of water
in natural waterways and waste streams [3, 9].
Journal of Engineering Science September, 2022, Vol. XXIX (3)
138 Physicochemical characterization of Asmara Brewery effluents

Case Studied
Asmara Brewery Corporation Share Company (ABCSC) originally known as “MELOTTI
BREWERY” established in 1939 and currently it is the only brewery in Eritrea, located in the
southern region of Asmara city in central region of the country. The plant’s water consumption
rates fluctuates from 8.12 to 19.80 L with an average value of 10.76 L for every 1 L of beer
produced against 3.5 L, an average water use by the international best practices. Due to the
poor design of water supply infrastructure with lack of awareness of water management
policies, the water usage rates are very high in the plant [10]. The total average daily available
process water is about 870 m3/day, which is slightly less than the planned water demand of
882.38 m3/day on average, regardless of the status of water quality and water use and
management. Hence, ABCSC system manufacturing operations are vulnerable to the scarcity
of process water and it is essential to adopt the best practices of water use minimization, and
it is mandate to develop wastewater reuse and recycle technologies as early as possible.
Because of voluminous water usage, brewery industry discharges large volumes of highly
polluting effluents the year [11]. Noted that effluents from individual process steps are
variable. For example, bottle-washing results in a large wastewater volume, but it contains
only a minor part of the total organics discharged from the brewery processes. On the other
hand, effluents from fermentation and filtering are high in organics/biochemical oxygen
demand (BOD), but generally low in volume, accounting for about 3% of the total wastewater
volume but 97% of the BOD [11]. Therefore, the present study mainly intensive on
identification of major manufacturing operations of the plant that generates higher volumes
of wastewater and assessment of effluent compositions to facilitate necessary data for further
development of appropriate treatment methods for wastewater recycling. In addition, this
may serve as database for the industry and local authority as well to assess the degree of
compliance by the industries to the legislative guidelines for effluent disposal.

Figure 1. Bottle cleaning and brewing process lines of ABCSC with specified sampling
location.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 A. Ramesh Babu, T. Arsiema, D. Heaven, B. Filmon, M. Abiel 139

2. Materials and Methods

2.1. Wastewater Sample Collection
Effluent water samples collected from the pre-screened independent sewer exit points
of bottle cleaning and brewing sections, two major wastewater-generating units of Asmara
Brewery Corporation Share Company (ABCSC) for every week during April and May months,
2021. Samples also collected for one time from Washer, filler and pasteurizer units of bottle
cleaning section.

2.2. Characterization of wastewater

Wastewater samples analyzed for physicochemical parameters such as pH,
temperature, total alkalinity, salinity, electric conductivity (EC), turbidity, total suspended
solids (TSS), Dissolved Oxygen (DO). They were also tested to know the presence of cations
such as Sodium (𝑁𝑁𝑁𝑁+), Potassium (𝐾𝐾 +), Manganese (𝑀𝑀𝑀𝑀2+ ), Total Iron (Fe) and Chromium
(𝐶𝐶𝐶𝐶 6+). Anions such as Sulphate (𝑆𝑆𝑆𝑆42−), Chlorine (Cl), Nitrate (𝑁𝑁𝑁𝑁3−), Nitrite (𝑁𝑁𝑁𝑁2−), Phosphate
(𝑃𝑃𝑃𝑃43−),) were also measured. Chemical contaminants were determined by quantifying
Chemical Oxygen Demand (COD) and Biological Oxygen Demand for five days (BOD5).

2.3. Conventional and Instrumental Testing Methods

Salinity, Electric Conductivity (EC) and Temperature measured by using calibrated
electrode (WTW Multi 197i, USA). Although pH does not have direct impact, usually it act as
an indicator of the process stability and it was read by using a pH meter (HANNA instruments,
UK), while the conductivity display the presence of total dissolved solids (TDS) and
palatability of water [12]. The dissolved oxygen (DO) content of water determines the
activation of biological processes, measured by using a DO meter in mg/L. Total alkalinity,
Chloride, total hardness and CaCO3 were measured using digital titration procedures followed
by the laboratory of Ministry of Water, Land and Environment of Eritrea.
To measure total alkalinity, 25 mL of a sample titrated with 0.02N H2SO4 in presence
of Bromcresol Green – methyl red pillow powder (BCG) reagent has turned the solution from
green color to pink. Turbidity describes the cloudiness of water caused by suspended
particles, chemical precipitates, organic particles and organisms. Turbidity typically
expressed as nephelometric turbidity units (NTU) and measured by using Eutech TN-100
instrument made by Thermoscientific, UK. The BOD5 measurement accomplished using the
respirometric method for five days (WAGTECH, FTC 90 system, UK). The COD concentration
in the wastewater determined by close refluxing according to the standard method 5220D.
Block heater (Stuart, SBH 200D, UK) was first used to digest the samples at 150°C for 2 h in
COD vials containing the digestion solution (0–15,000 mg COD/L, acquired from HACH,
Germany). Then, COD concentration quantified using a discrete auto-analyzer (HACH,
Germany).
Spectrophotometer applied to know the presence of various chemicals in the sample
of wastewater tested. System was calibrated at corresponding wavelengths to measure
nitrogen in nitrites and nitrates, manganese, iron, sulfates, phosphates and chromium as
shown in Table 1. After calibrating the equipment, a bottle of 25ml filled by the sample and
appropriate reagent was added and mixed for specified reaction time and measured
corresponding absorbance on spectrophotometer. Nitrate and nitrite ions not found from the
spectrophotometer reading directly. Instead, nitrogen in nitrates and nitrites found from the
spectrophotometer reading, later Nitrates and Nitrites are calculated as:

Journal of Engineering Science September, 2022, Vol. XXIX (3)

140 Physicochemical characterization of Asmara Brewery effluents
𝑁𝑁𝑁𝑁3 − = 𝑁𝑁 − 𝑁𝑁𝑁𝑁3 − × 4.429
𝑁𝑁𝑁𝑁2 − = 𝑁𝑁 − 𝑁𝑁𝑁𝑁2 − × 3.286

The amount of sodium and potassium present in the wastewater sample measured
using the flame photometer shown in fig 2B. The function of this instrument is similar to
spectrophotometer except that it uses flame rather than light. Initiation step takes some time
once it turned on, then system calibrated prior to read the values for actual samples. After
that, by taking the sample in a small measuring cup and inserting aspiration tube in to the
cup of the sample, and supplied into the flame photometer to read its absorbance.

Table 1
Characterization methodology using spectrophotometry
Reaction
Wave
Test Code Reagent Mixing method time
length (nm)
(min)
Buffer, citrate
Invert to mix
Manganese(Mn⁺²) 295 525 type Sodium
Invert to mix 2
Periodate
Total Iron (Fe) 265 510 FerroVer Swirl to mix 3
Swirl vigorously to
Sulfates (SO₄²⁻) 680 450 SulfaVer 4 5
mix
1min vigorous
Nitrates (N-NO₃⁻) 355 500 NitraVer 5
shake 5
Nitrites (N-NO₂⁻) 371 507 NitriVer 3 Swirl to mix 15
Phosphates 30sec vigorous
490 890 PhosVer 3
(PO₄³⁻) shake 2
Chromium (Cr⁺6) 90 540 ChromaVer 3 Swirl to mix 5

2.4. Statistical Analysis

Compositions of bottling line wastewater and mixed streams of 2:1 of bottling and
brewery lines wastewater samples are analyzed and the results are verified with analysis of
variance (ANOVA) study using Microsoft Excel®, 2016 software.

Figure 2. a) Spectrophotometer b) Flame Photometer.

Journal of Engineering Science September, 2022, Vol. XXIX (3)
 A. Ramesh Babu, T. Arsiema, D. Heaven, B. Filmon, M. Abiel 141

The variance and mean values of characterized parameters are determined for the
comparison with the reported values for other breweries and other industrial effluents from
the literature and also with national and international industrial effluent standards.

3. Results and Discussion

According to the informants of ABCSC, approximately 8.455 L of wastewater
discharges per every L of beer produced and it is mainly comprised of two major process lines
i.e., bottle cleaning (BC) line and brewing line. Despite of the water consumed in BC line
discharged totally into the sewer a basis for the wastewater treatment set by assuming that
BC line alone contribute 2/3rd of the total wastewater generated from the ABCSC plant and
the remaining by the brewing line. To identify the qualitative nature of the BC wastewater,
samples tested once from each cleaning equipment for physicochemical characteristics as
given in Table 2. Wastewater from filler and pasteurizer units have low pH values whereas in
washer shown significantly higher values and which resulted a further higher value of the BC
line sample collected from a single exit point source just before it discharges into public
sewer line. Filler and pasteurizer wastes have shown greater variation from washer
operations. Higher COD values recorded for filler and pasteurizer discharges.

Table 2
Physicochemical Properties of Wastewater from Bottle Cleaning Operations in ABCSC
Point Sources Wastewater from Bottle Cleaning Section
Parameter Bottle
Filler Pasteurizer Washer 1 Washer 2 Washer 3
Cleaning
Temperature
17.3 17.4 16.9 16.3 17.7 19
(oC)
pH 5.72 5.91 11 10.81 11.04 12.36
EC (µs/cm) 499 566 1696 1350 1290 3840
Turbidity (NTU) 5.85 83.8 94.5 382 1400 112
Salinity (mg/L) 0 0 0.7 0.5 0.4 3.5
Sodium
37.5 38.4 269 209.7 210 526.5
Na⁺(mg/L)
Potassium K⁺
16.1 14.5 3 17.1 3 12.2
(mg/L)
DO (mg/L) 2.43 0.67 5.66 5.85 5.87 3.28
COD (mg/L) 4700 1350 30 42 90 4800
BOD5 (mg/L) 1926.7 806.7 8.9 10 11.1 2310
Note: DO-dissolved oxygen; COD-chemical oxygen demand; BOD5 - biological oxygen demand for five days.

Brewing line has two major discharge streams from wort filtration and clarification
units, hence samples of mixed (50 % of wort filtration waste and 50 % of clarification
wastewater) stream have considered as brewery wastewater. Samples were collected for five
consecutive weeks, from the both BC line (BCWW) and brewery lines (BRWW) and mixed
wastewater (MWW) samples of 2/3rd of BC line discharge and 1/3rd of brewery line discharge
were also prepared. Weekly samples characterized for physicochemical parameters and their
analysis revealed that they possess greater diversity in COD values and the samples collected
during first two weeks have recorded with higher COD values as shown in Figure 3, whereas
BRWW samples have shown higher BOD5 than BCWW and MWW samples in Figure 4.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
142 Physicochemical characterization of Asmara Brewery effluents

BOD5/COD values were higher for BRWW samples; a value of 0.547 was observed as greater
than any other sample and recorded by 4th sample of BRWW as in Figure 5.

Figure 3. Weekly estimated chemical oxygen demands of Asmara brewery waste samples.

Figure 4. Weekly estimated biological oxygen demands of Asmara Brewery waste

samples.

Although pH usually has no direct impact on environment, it is one of the most

important operational water quality parameters and plays key role in controlling
minimization of corrosion of water carrying systems. pH values of all the samples studied
hold relatively higher pH values except for the samples collected during 2nd week. Bottle
washer consumes chemicals such as caustic soda, it caused for higher pH values of BCWW
samples.
However, lower- pH (approximately pH -7 or less) water is more likely to be corrosive.
BRWW samples shown lower pH values than BCWW and MWW samples and a pH of 2.62 was
noted in the sample collected during 1st week as the lower than any other samples as shown
in Figure 5(a).

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. Ramesh Babu, T. Arsiema, D. Heaven, B. Filmon, M. Abiel 143

Figure 5. Weekly estimated pH (a), electric conductivity (b), turbidity (c) and total
suspended solids (d) values of Asmara Brewery effluents.

Dissolved oxygen (DO) levels in the water indicate the potential existence of aquatic
life. Nevertheless, a value of DO less than 4.5 mg/L can’t support any life in water [13]. Figure
6 depicts that BRWW samples has lower DO levels than any other samples and it was also
seen a lowest value of 0.39 mg/L for BRWW sample collected during 2nd week of our study.
Thus, BRWW and MWW samples doesn’t support any aquatic life but BCWW has comparatively
higher DO levels, yet they are far lower than 9.5 mg/L above which a healthy life could be
identified in water bodies [13].
The palatability of water is determined with the presence of total dissolved solids
(TDS) which can be estimated through electric conductivity. Higher levels of TDS, greater
than about 1000 mg/L may objectionable to handle, owing excessive scaling in pipes, heaters,
boilers and household appliances [12]. Higher conductivity has seen for BRWW samples
collected during 1st week and also for the BCWW samples collected in 5th week. MWW samples
have shown less deviation among the conductivity values measured as described by the
Figure 5(b). Turbidity describes the cloudiness of water, increasing turbidity reduces the
clarity of water to transmitted light. Brewery wastewater samples have recorded with higher
turbidity values than BCWW and MWW whilst BCWW has lower turbidity than both MWW and
BRWW for all the samples. Turbidity also indicate the presence of physical, chemical and
biological contaminants. Presence of total suspended solids (TSS) indicate the direct measure
pollutants in the wastewater, and higher TSS values were noticed in the first week samples
of MWW and BRWW. MWW samples have shown higher TSS levels than any other samples

Journal of Engineering Science September, 2022, Vol. XXIX (3)

144 Physicochemical characterization of Asmara Brewery effluents

collected in every week as shown in Figure 5(d) whereas BCWW samples were observed with
lower TSS values.

Figure 6. Weekly estimated dissolved oxygen levels of Asmara Brewery discharges.

Table 3
ANOVA Study of ABCSC Brewery and Bottle Cleaning and Mixed wastewater characteristics
Bottle cleaning
Brewery Wastewater Mixed Wastewater
Parameters wastewater
Range Mean Range Mean Range Mean
Temperature
19-34.4 28.36 26.3-34.4 29.6 24-31.2 27.94
(oC)
pH 2.62-12.36 9.41 2.62-9.03 5.6 4.22-11.59 7.8
1244-
EC (µs/cm) 538-3840 1432.6 1740.2 968-1578 1297.2
2450
Turbidity
5.03-112 83.366 58.9-1400 599.8 51.3-400 218.3
(NTU)
Salinity
0-3.5 1.01 0.4-1.1 0.7 0.3-0.6 0.46
(mg/L)
Sodium Na⁺
29.8-526.5 246 26.7-199.4 108 39.5-185 122.27
(mg/L)
Potassium K⁺
2.1-184.8 52.12 6.7-64.5 24.8 6.3-41.1 17.77
(mg/L)
DO (mg/L) 1.33-6.06 3.84 0.39-3.55 2.14 2.12-5.53 3.98
3500- 10200- 32000-
COD (mg/L) 43560 83240 70000
160000 154000 134000
3133-
BOD5 (mg/L) 357-5633 3594 11066 2856-14667 6641
26667
COD/BOD5 2.57-28.41 13.9 1.83-14.08 8.51 9.17-27.9 15.44
Total
40-400 166.67 400-900 709.33 68-392 273.33
hardness
Note: EC - electric conductivity; DO - dissolved oxygen; COD - chemical oxygen demand; BOD5 - biological
oxygen demand for five days; NTU - nephelometric turbidity units.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. Ramesh Babu, T. Arsiema, D. Heaven, B. Filmon, M. Abiel 145

A single factor analysis of variance (ANOVA) study was performed to determine the
mean and variance values of all characteristic parameters and the results are listed in Table
3. COD and BOD5 values were deviated highly for BCWW, BRWW and MWW samples. The
highest mean of COD has seen as 83240 mg/L for BRWW samples with a range of 10200-
154000mg/L. Although BCWW samples have shown less mean value, a significant range of
COD, 3500-160000 mg/L was noted. The mean COD values of all BRWW, BCWW and MWW
samples were too far from the benchmarks of Brewers Association, USA (Table 4). The
variations in the COD concentrations for each week could be as a result of variation in the
activities and housekeeping practices of the brewery plant, which could cause serious
environmental impact and closure of the production plant by the municipal authority, if not
checked.
Table 4
Comparison of brewery wastewater with Eritrean Effluent standards and Effluent
benchmarks of BA
Industrial Brewers
Bottle Effluent Association
Brewing line Mixed (2:1)
Cleaning standards (USA)
Parameter Effluent Effluent
line Effluent entering Public Benchmarks
Composition Composition
Composition Sewers in for Effluent
Eritrea [15] [14]
Temperature 28.36 29.6 27.94 < 43 NA
( C)
o

pH 9.41 5.6 7.8 6-10 3-12

TDS 1228.67 1166 869 < 3000 < 3000
TSS 98.2 606.8 203 < 600 200-1500
Sulphate 50.5 236.75 95 < 1500 NA
(mg/L)
Fe (mg/L) 0.714 1.466 0.896 < 25 NA
Mn (mg/L) 2.03 7.13 3.325 < 25 NA
COD (mg/L) 43560 83240 70000 NA 1800-5500
BOD5 (mg/L) 3594 11066 6641 NA 600-5000
COD/BOD5 12.12 7.522 10.54 NA NA
Note: TDS - total dissolved solids; TSS - total suspended solids; COD - chemical oxygen demand; BOD5 -
biological oxygen demand for five days.

Physicochemical characteristics of BCWW, BRWW and MWW were analyzed to compare

with industrial effluent quality standards that permit into public sewers of Eritrea as shown
in Table 4. Mean values of Temperature, pH, TDS, TSS, Sulphate, Iron, Manganese were
observed as within permissible limits of national industrial effluent standards, Eritrea.
Average concentration of pH, TDS and TSS were also notified as within the limits of effluent
benchmarks set by the Brewer’s Association, USA. BOD5 is an indicator of organic loading in
the effluent streams, brewery operations have showed 4 times greater BOD5 than bottle
washer line. Mix of 1/3rd of brewery effluent with 2/3rd of BCWW, has doubled the levels of
BOD5. Brewery discharges also shown doubled COD loadings than bottle cleaning wastes.
BOD5 & COD levels of wastewater from bottle cleaning line were comparatively lower and
BOD5 concentration was also dwell within the limitations of Brewer’s Association,
benchmarks. In all other cases, COD and BOD5 levels were very much higher than usual
Journal of Engineering Science September, 2022, Vol. XXIX (3)
146 Physicochemical characterization of Asmara Brewery effluents

brewery effluents which indicates greater chemical and biological contamination of ABCSC
effluents. As COD/BOD5 is 12.12 for BCWW, it has loaded with high levels of chemical
contaminants than BRWW and MWW, whereas COD/BOD5 is 7.522 for BRWW, it contains
higher organic loadings.
Table 5
Comparison of ABCSC wastewater characteristics with other reported parameters in the
literature
Enitan Brito Driessen &
Gemeda et Akunan et
Parameter This work et al. et al. Vereijken,
al. [16] al. [17]
[18] [19] [20]
Temperature
24-31.2 20.9 ND 27.9 30-35 18-40
(oC)
4.22-
pH 6.55 5-11 6.0 6.5-7.9 4.5-12
11.59
EC (µS/cm) 968-1578 5425 ND 1516 ND ND
TSS (mg/L) 154-520 140.15 ND 1826.74 ND 200-1000
0.004-
TN (mg/L) 166.5 20-600 13.29 12-31 25-80
14.7
TP (mg/L) 0-19.45 11.55 4-103 23.71 9-15 10-50
Total COD 32000- 1800- 800-
210.9 5341 2000-6000
(mg/L) 134000 50000 3500
2700- 2700- 520-
BOD5 (mg/L) 209 3215.27 1200-3600
14667 38,000 2300
Note: EC - electric conductivity; TSS - total suspended solids; TN - total nitrogen; TP - total phosphorous; COD
- chemical oxygen demand; BOD5 - biological oxygen demand for five days.

Quality of ABCSC mixed wastewater (MWW) composition was comparable with other
reported parameters in the literature as in Table 5.
Table 6
Comparison of brewery wastewater with other industrial and municipal wastewater
Dairy (Milk-
Parameter Brewery cheese) Tannery Textile Mills Municipal
plants
pH 4.22-11.59 5.2-11.3 8-11 4.5-10.1 6-8
Salinity (g/L) 0.3-0.6 0.5 6-40 0.5-0.9 <0.5
TSS (mg/L) 154-520 350-1082 2070-4320 20-210 100-350
TN (mg/L) 0.004-14.7 14-450 250-1000 14-72 20-85
TP (mg/L) 0-19.45 37-78 4-107 1-18 4-15
Total COD 32000-
189-20000 3500-13500 1900-100000 250-1000
(mg/L) 134000
2700-
BOD5 (mg/L) 709-10000 1000-7200 700-1650 110-400
14667
Bielefeldt, Bielefeldt, Bielefeldt, Bielefeldt,
Reference This Work
2017 [21] 2017 [21] 2017 [21] 2017[21]
Note: TSS - total suspended solids, TN - total nitrogen; TP - total phosphorous; COD - chemical oxygen demand;
BOD5 - biological oxygen demand for five days.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 A. Ramesh Babu, T. Arsiema, D. Heaven, B. Filmon, M. Abiel 147

The range of pH was similar with Driessen and Vereijken study in 2003 [20]. Enitan et
al. [18] has reported a conductivity of 1516 µS/cm, which dwell in the range of this study.
TSS concentrations of this report are moderate when it compared with Enitan et al. [18], F.T.
Gemeda et al. [16], and Akunan et al. [17], have reported higher range of total nitrogen (TN)
values, but this study is comparable with Enitan et al. [18], and Brito et al. [19]. Total
Phosphates (TP) are comparable with all the reports with slight deviation. COD
concentrations are too higher than any other reported values, which indicate the presence of
high levels of chemical contaminants in ABCSC wastewater. BOD5 levels also higher than all
reported values except Akunan et al. However, these quantitative comparisons made a clear
conclusion that all the characteristics are case specific and have greater diversity in their
values.
The study also considered brewery industry to compare with other relevant process
industries in Eritrea concerning their effluent compositions. Dairy, tannery, textile mills and
domestic wastewater were comparable with brewery effluents as shown in Table 6. Chemical
loadings of ABCSC effluents are competitive with effluents of textile mills. BOD5
concentrations are approximately in the rage of dairy wastes, pH values are as high as dairy
and tannery wastes and nutrients such as nitrogen and phosphorous are typically in the rage
of textile wastes. Noted that most of the parameters of brewery industry wastes are different
from municipal wastewater. Brewery wastes cannot be treated usually with municipal
wastewater treatment plant, as they require special attention.
Table 7
Assessment of ABCSC effluent quality with EU and EPA effluents standards
Bottle EPA,
Brewing line Mixed (2:1) EU, Effluent
Cleaning line Effluent
Parameter Effluent Effluent Limits
Effluent Standards
Composition Composition [22]
Composition [23]
TSS 98.2 606.8 203 35 50
COD (mg/L) 43560 83240 70000 125 150
BOD5 (mg/L) 3594 11066 6641 25 50
COD/BOD5 12.12 7.522 10.54 5.0 3.0
Note: TSS - total suspended solids; COD - chemical oxygen demand; BOD5 - biological oxygen demand for five
days.

TSS, COD and BOD5 levels of ABCSC discharges are beyond international limits such
as EU discharge limits EPA, USA effluents standards as shown in table 7. Suspended solid are
more in brewery effluent than bottle cleaning wastewater, and it is 17 times and 12 times of
EU and EPA standards. COD concentration of mixed effluent is 560 and 467 times of EU and
EPA effluents limits respectively, which indirectly warns the company to take immediate
action to control such higher chemical contaminants in the effluents. In other words, organic
loadings of mixed effluent exceed 256 and 133 times the permitted values of EU and EPA.
COD/ BOD5 estimated as twice the EU limit and thrice the EPA regulated value that specifies
more presence of chemicals than organics.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

148 Physicochemical characterization of Asmara Brewery effluents

4. Conclusions
According to the informants of ABCSC, approximately 8.455 L of wastewater
discharges per every L of beer produced and it is mainly comprised of two major process lines
i.e., bottle cleaning (BC) line and brewing line. Thus, samples of bottle cleaning and brewery
effluents were collected weekly and their physicochemical characteristics were analyzed.
Mean values of dissolved oxygen (DO) of all wastewater samples were found lower than 4.5
mg/L. Thus, it indicates no life in such effluents and subsequently causes for severe
environmental issues. The results of this study showed that COD and BOD5 concentrations of
wastewater from ABCSC are higher than other brewery industries reported in the literature
and they are also beyond the benchmarks set by Brewer’s Association, USA. TSS, COD and
BOD5 levels have exceeded the international standards such as EU and EPA effluents
standards, which indicate an immediate action by the company to prevent the cost of
penalties. Therefore, there is a need to treat the brewery wastewater in order to protect the
environment and to reduce the use of fresh water sources.
The levels of pH, TSS, COD and BOD5 of brewery effluents are beyond the ranges of
municipal waste water, hence they can’t be treated together. Instead, brewery wastewater
might be treated separately with a special attention to remove higher COD levels. As the
characteristics of bottling and brewery effluents are distinct, treatment technologies can be
developed based on their significant variation in characteristics. As COD/BOD5 is 12.12 for
BCWW, it contains high levels of chemical contaminants than BRWW and MWW, whereas
COD/BOD5 is 7.522 for BRWW, it has higher organic loadings. Characteristics of mixed
wastewater were determined to develop a suitable pretreatment plant for the potential reuse
of water through an existing RO plant in ABCSC.

Acknowledgements. The authors of this report gratefully acknowledge the staff of

Asmara Brewery Corporation Share Company (ABCSC) and the staff of Chemical Laboratory of
Ministry of Land, Water and Environment Eritrea, for their consistent support in sample
collection and characterization. Authors convey the gratefulness to Dr. Sujana Ramesh for her
support in writing this document. Authors would like to extend their thankfulness to Mr.
Abraham Yohannes, Head of Chemical Engineering, and Dr. Kahsay Neguse, Dean of Mai Nefhi
College of Engineering & Technology for their untiring support in providing necessary letters.

Conflicts of Interest. The authors declare no conflict of interest.

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Citation: Ramesh Babu, A.; Arsiema, T.; Heaven, D.; Filmon, B.; Abiel, M. Physicochemical Characterization of
Asmara Brewery Effluents. Journal of Engineering Science 2022, 29 (3), pp. 136-149.
https://doi.org/10.52326/jes.utm.2022.29(3).12.

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Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
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(https://creativecommons.org/licenses/by/4.0/).

Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 150 - 165
Fascicle Food Engineering ISSN 2587-3474
Topic Food Industry and Management eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).13
UDC 643.3:[004.7:621.391]

RECENT ADVANCES IN SMART KITCHEN AUTOMATION TECHNOLOGIES:

PRINCIPLES, APPROACHES, AND CHALLENGES

Buhari U. Umar*, ORCID: 0000-0001-6971-1917,

Olayemi M. Olaniyi, ORCID: 0000-0002-2294-5545,
Idris A. Dauda, ORCID: 0000-0002-2775-6292,
Danlami Maliki, ORCID: 0000-0003-2870-7959,
Cindy P. Okoro, ORCID: 0000-0002-1727-3246

Department of Computer Engineering, Federal University of Technology, Minna, PMB 65, Minna, Niger state Nigeria,
*Corresponding author: Buhari U. Umar, [email protected]

Received: 05. 29. 2022

Accepted: 07. 14. 2022

Abstract. The Internet of Things (IoT) is a growing network of physical devices that are
connected to various types of sensors and can share data with the aid of internet connectivity.
Safety is an important consideration when designing a house, town, smart kitchen, etc., and
it continues to play an important role in today's world. In general, the kitchen is regarded as
one of the most crucial tasks in our everyday lives, making it imperative to equip this vital
element of human life with smart devices to avoid commonplace incidents such as gas leaks,
intense particles in the environment, or fire outbursts. Gas leaks in the kitchen can be
dangerous and deadly, resulting in fires if they go unchecked. For smart kitchens, various
systems have been built to combat gas leaks and fire outbreaks. However, despite their high
precision, these systems each have their own set of flaws that have severely restricted their
implementations. The state-of-the-art in gas leakage, fire, and smoke detection in a smart
kitchen is discussed in this paper. Different methods of gas leakage and fire detection are
also addressed, along with their strengths and weaknesses, as well as products available in
the market today.

Keywords: Internet of things (IoT), smart kitchen, gas leakage, smoke, safety systems.

Rezumat. Internetul lucrurilor (IoT) este o rețea în creștere de dispozitive fizice care sunt
conectate la diferite tipuri de senzori și pot partaja date cu ajutorul conexiunii la internet.
Siguranța este un aspect important atunci când proiectați o casă, un oraș, o bucătărie
inteligentă etc. și continuă să joace un rol important în lumea de astăzi. În general, bucătăria
este considerată una dintre cele mai cruciale sarcini din viața noastră de zi cu zi, ceea ce face
imperativ să echipam acest element vital al vieții umane cu dispozitive inteligente pentru a
evita incidentele obișnuite, cum ar fi scurgerile de gaz, particulele intense în mediu sau
incendiul. izbucniri. Scurgerile de gaz în bucătărie pot fi periculoase și chiar mortale, ducând
la incendii dacă nu sunt controlate. Pentru bucătăriile inteligente, au fost construite diverse
sisteme pentru combaterea scurgerilor de gaze și a focarelor de incendiu. Cu toate acestea,

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 B. U. Umar, O. M. Olaniyi, I. A. Dauda, D. Maliki, C. P. Okoro 151

în ciuda preciziei lor ridicate, aceste sisteme au fiecare propriul set de defecte, care le-au
restricționat sever implementările. Echipamente de ultimă generație în detectarea scurgerilor
de gaze, a incendiilor și a fumului într-o bucătărie inteligentă sunt discutate în această
lucrare. De asemenea, sunt abordate diferite moduri de scurgere de gaze și de detectare a
incendiilor, împreună cu punctele forte și punctele slabe ale acestora, precum și produsele
disponibile pe piață astăzi.

Cuvinte cheie: Internetul lucrurilor (IoT), bucătărie inteligentă, scurgeri de gaz, fum, sisteme de
siguranță.

1. Introduction
Cooking, is often performed in the kitchen and is considered one of the most important
activities in our daily lives and is one of the most important tasks that people do [1]. The use
of the gas cylinder, which is popular in most smart kitchens, is rapidly growing, but it is also
extremely dangerous because it can trigger fires. This work is motivated by the dangers posed
by gas leakage, CO contamination, and fire outbreaks in humans and their resources. Gas
leaks in the home are normally caused by equipment that has been improperly installed,
operated, or damaged [2]. Gas leakage, lit cigarettes, short circuits, and overheating mobile
phones have all been identified as common causes of fire outbreaks at home. While high
temperatures in the frying pan, vegetable oil, and old oil in a deep fryer are all common
sources of smoke in the kitchen, etc. [3]. Since natural gas is odourless, it cannot be detected
by smell alone. As a result, a chemical (Mercaptan) is applied to give it a distinct odour to
warn people in the event of a leak [4]. Some people, on the other hand, have a very weak
sense of smell, which has contributed to the development of gas detection systems. Fire
detection systems are designed to detect fires in their early stages (which includes all types
of fires), giving people precious minutes to flee to safety, saving lives, and reducing property
damage, as well as taking decisive measures to stop the fire from spreading [5]. Figure 1
shows a typical smart kitchen with smart lights, a smart food heater (microwave), intrusion
detectors, a smart electric cooker, a smart kitchen seat, smart cooling appliances, and so on.
Smart systems, smart meters, smart appliances, smart power outlets, and sensing devices are
installed in the smart kitchen to encourage the development of intelligent solutions for the
everyday life of people [6].

Figure 1. A Typical Smart Kitchen [6].

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152 Recent advances in smart kitchen automation technologies: principles, approaches, and challenges

Various studies on gas, smoke, and fire detection have been carried out; however, this
paper aims to explore the state-of-the-art achievement in gas leakage, fire, and smoke
detection technologies in smart kitchen automation, as well as the research gap and open
issues that need to be addressed in the field of smart kitchen automation technologies. The
rest of the paper is organized as follows: an overview of gas leakage, fire, and smoke detection
system in a smart kitchen is presented and discusses gas leakage and detection system in a
smart kitchen. Also, their strength and weakness are discussed. A smoke and smoke detection
system in a smart kitchen is presented, and the fire and fire detection system in a smart
kitchen is discussed as well. Lastly, related works in gas, fire, and smoke detection systems
in a smart kitchen; open issues and challenges in gas leakage, smoke, and fire detection in a
smart kitchen; and the conclusion of the research work.

2. Overview of Gas Leakage, Fire, and Smoke Detection Systems in A Smart Kitchen
Protection systems are also referred to as fire, smoke, and gas detection systems.
System safety is a branch of systems engineering those aids in the management of program
risk. To improve protection, engineers and managers use engineering and management
concepts, requirements, and techniques. The goal of a safety system is to improve safety by
detecting and removing or managing safety risks by designs and/or procedures that are
focused on appropriate system safety priorities [7]. When designing any detection device,
there are a variety of existing systems and techniques to consider, some of which are
discussed in this paper.

3. Gas Leakage and Detection System in a Smart Kitchen

As poisonous gases and vapours build up to unhealthy levels, or when the air is
depleted of oxygen, it can be highly dangerous to people, buildings, and equipment [8]. The
safety and health of a family, machinery, and property must be entrusted to perfectly working
sensors. This is because human sensory organs are often unable to detect airborne threats,
and even when they do, they do so too late.
As a result, hazards must be detected in real-time and consistently, because false
alarms trigger production downtime. As a result, the sensor is the most crucial part of a gas
detection device.

Figure 2. Various Gas Leakage Detection Techniques.

Journal of Engineering Science September, 2022, Vol. XXIX (3)
 B. U. Umar, O. M. Olaniyi, I. A. Dauda, D. Maliki, C. P. Okoro 153

It converts the measured variable into an electrical signal using chemical or physical
processes, depending on the type of sensor. The accuracy with which dangerous substances
suspended in the air can be detected is largely determined by the sensors used to detect
them. As a result, both the gas detector and the sensor must be perfectly balanced [9].
Catalytic Bead Sensor, Thermal Conductivity, Infrared Gas Detection, Electrochemical sensor,
Metal oxide sensors, Colorimetric tape, Optical Gas Detection, Open-path Flammable Infrared
Gas Detection, Open-path Toxic Infrared Gas Detection, Photo Ionization, Flame Ionization,
and light scattering are some of the techniques used to design gas detectors. Figure 2. depicts
the most often used techniques for detecting gas leaks.

3.1. Catalytic Bead Sensors

A heated catalytic bead (usually platinum or palladium) burns at a lower temperature
than combustible gas concentrations (a concept identical to that of a catalytic converter in a
car). The thread in the bead heats up as the gases burn. The resistance of the wire increases
as the temperature rises. This temperature rise is compared to a non-catalytic reference bead
using a Wheatstone bridge to provide a reading of the fuel gas [10].

3.2. Thermal Conductivity

Heat is transported at various rates by different gases. As a result, in the air, the heated
wire can lose heat at a different rate than in gases like helium. This distinction can be used
in the development of a gas detector. Since low-level heat loss is difficult to detect
accurately, this approach is typically used only when the percentage of gas volume is
detected. The detection of the volume percent of combustible gas, helium, and carbon
dioxide is one of the most common applications [10].

3.3. Colorimeter Sensors

If any chemicals are exposed to other chemicals during a chemical reaction, they will
change color. This idea is used to construct a "spot" that can then be seen or sensed
electronically. This approach is used in low-tech detector tubes as well as detection systems
developed specifically for the semiconductor gas detection industry (arsine, phosphine, etc.) [10].

3.4. Metal Oxide Sensors

Some metal oxides (such as tin) have semiconducting properties that make them ideal
for gas detection. Fuel gases and hydrogen sulfide are popular applications, but the device
can also detect a wide range of other chemicals. The electrical resistance of these
semiconductors decreases when they are exposed to certain gases. The decrease in gas
concentration can then be measured and related. These sensors are often used in hostile
environments because they are robust and long-lasting [10].

3.5. Electrochemical Sensors

To oxidize or reduce a chemical, electrochemical sensors use two or more electrodes
in an electrolyte. It is possible to make sensors for a variety of gases by changing the electrode
materials and electrolytes. For the detection of oxygen and poisonous gases, electrochemical
sensors are widely used. They are not usually used for organic compounds [10].

3.6. Infrared Detection

The use of infrared light to detect combustible hydrocarbon gas is known as infrared
gas detection. A source of infrared light, an optical filter to select the correct wavelength, and

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154 Recent advances in smart kitchen automation technologies: principles, approaches, and challenges

an optical infrared receiver make up the detector. Hydrocarbon molecules in the gas absorb
some of the infrared energy as it passes through the vacuum between the source and receiver.
As a measure of the amount of hydrocarbon gas present, the receiver detects a decrease in
receiving energy. The output signal of an Infrared Gas Detector is also compensated for the
effects of temperature, humidity, and the presence of moisture or dirt on the optical filters by
using two wavelengths of infrared radiation, one active wavelength for gas absorption and
the other as a reference wavelength to compensate the output signal of the Infrared Gas
Detection device for the effects of temperature, humidity, and the presence of moisture or
dirt on the optical filters. Open-path detection and close-path (point) detection are two
classifications of infrared gas detection systems [11]:
I. Close-path infrared gas detection (Point devices) measure the amount of gas
present at a fixed location.
II. Open path detectors consist of separate transmitters and receivers that detect the
presence of gas up to 200 meters away. To give the best level of safety, a
combination of open-path and point detectors can be used in most circumstances.

3.7. Flame Ionization

A flame ionization detector (FID) is a scientific device that detects analytes in gas
streams. In gas chromatography, it is commonly used as a detector. This is a mass-sensitive
instrument since it measures ions per unit of time. Standalone FIDs can be used in stationary
or portable instruments for applications such as landfill gas monitoring, fugitive pollution
monitoring, and internal combustion engine emissions measurement [11].

3.8. Photo Ionization

The Photo Ionization Detector (PID) is a vapour and gas detector that can detect a wide
range of organic compounds. When an atom or molecule absorbs enough light to allow an
electron to leave and become a positive ion, this is known as photoionization. An ultraviolet
lamp releases photons that are absorbed by the compound in an ionization chamber, and this
is how the PID works.
Electrodes collect the ions (atoms or molecules that have gained or lost electrons and
thus have a net positive or negative charge) generated during this process. The analyte
concentration is determined by the current produced. This method is considered non-
destructive since only a small fraction of the analyte’s molecules is ionized, allowing it to be
used in combination with another detector to validate analytical findings. PIDs are also
available in a variety of lamp configurations and compact hand-held versions. Results are
almost instantaneous [11].

3.9. Optical Detection

Safety Scan specializes in using optical gas imaging to detect hydrocarbon gas leakage
using infrared thermal imaging. Real-time thermal images of gas leakage are provided by
highly specialized infrared cameras. Optical emission detection is a relatively new technology
that has been developed to identify fugitive gas emissions quickly, accurately, and safely.
This technology allows the user to “see” hydrocarbon gas emissions that would otherwise be
invisible.
Thermal imaging aids in the precise detection of the leak's source, which is critical for
repair efforts. This provides a safer, more effective environment for a variety of industrial
applications, enabling engineers to pinpoint the leak's source and size in real-time [11].

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3.10. Light Scattering

A detector used in high-performance liquid chromatography (HPLC), ultra-high-
performance liquid chromatography (UHPLC), purification liquid chromatography such as
flash or preparative chromatography, countercurrent or centrifugal partition chromatography,
and Supercritical Fluid chromatography is an evaporative light scattering detector (ELSD)
(SFC). It is widely employed for the study of substances that do not easily absorb UV light,
such as sugars, antivirals, antibiotics, fatty acids, lipids, oils, phospholipids, polymers,
surfactants, terpenoids, and triglycerides, where UV detection may be a limitation. The
charged aerosol detector (CAD) is similar to ELSDs, and both come within the destructive
detector family. Both compounds that are less volatile than the mobile phase, i.e., nonvolatile
and semi-volatile compounds, can be detected using an evaporative light scattering detector
(ELSD) [12]. However, these techniques have their strengths and constraints as summarized
in table 1.

Table 1
Summary of gas detection techniques, strengths, and weaknesses
S/N Technique Mode of Operation Strengths Weaknesses
1. Catalytic Makes use of elements Relatively They are non-
Bead sensor (beads) with catalytic sensors inexpensive, specific and
where resistance-change is rugged, and has a the beads are
directly related to the gas long shelf-life. susceptible to
concentration in the poisoning
surroundings and is displayed compounds.
in a meter.
2. Thermal Makes use of varying Simple to design They have
conductivity temperatures and the and have a long limited
difference in transport rate shelf-life. application &
with air as reference. cannot detect
low
concentrations
3. Colourimeter Makes use of the difference in Low cost and Has limited
the chemical reaction of detects varieties of shelf life with a
various gases when exposed gases. It can also low level of
to other chemicals. detect low-level accuracy. Also,
concentrations the “paper
tape” used is
costly to
purchase
4. Metal Oxide Makes use of semiconductors. They are rugged, They are non-
sensor Takes full advantage of the durable, and specific and
properties of some metal resistant to many tend to give
oxides to detect a change in sensor poisons. false alarms.
their electrical resistance. Also, they have
less reliability.

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156 Recent advances in smart kitchen automation technologies: principles, approaches, and challenges

Continuation Table 1
5. Electrochemi Makes use of electrochemical They are portable, The electrolyte
cal sensor sensors and electrodes to durable, and have is prone to
oxidize or reduce a chemical low power leakage. They
to create sensors for various consumption. have a limited
gases. shelf-life and
consume more
power.
6. Infrared The detector consists of a
detection source of infrared light, an
optical filter to select the
proper wavelength, and an
optical infrared receiver.
7. Flame The FID works by detecting It is relatively Inorganic
Ionization ions that are produced during inexpensive to compounds
the burning of organic acquire and and some
molecules in a hydrogen operate and has highly
flame. The number of organic low maintenance oxygenated or
species in the sample gas requirements with functionalized
stream determines how many rugged species are not
of these ions are produced. construction. detectable.
8. Photo When compounds reach the It has a wide range It is not
Ionization detector, they are assaulted of applications due suitable for the
by high-energy UV photons to its linearity; it detection of
and are ionized when they also has low semi-volatile
absorb the UV light, causing maintenance compounds
electrons to be ejected and requirements. and does not
positively charged ions to identify the
form. type of volatile
compounds
present.
9. Optical Uses as well as an optical It has high It is subject to
Detection sensor Lightray are converted sensitivity, environmental
into an electrical signal by an reliability, and a disturbance
optical sensor. This is wide dynamic and is
comparable to the function of range. It is also relatively
a photoresistor. chemically inert pricey.
and is suitable for It's also
remote sensing. vulnerable to
bodily harm.
10. Light It is widely employed for the Good for It has the
Scattering analysis of chemicals where nonvolatile potential for a
UV detection is a limitation, solutes and are high false
such as when the compounds low molecular alarm rate and
do not absorb UV radiation weight polymer. must be
efficiently. cleaned daily.
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 B. U. Umar, O. M. Olaniyi, I. A. Dauda, D. Maliki, C. P. Okoro 157

Most of the time, these detectors are set to detect no more than two separate gases.
When gas is detected, most gas detectors sound a warning buzzer, while others send an SMS
to subscribers. Only a select few make provisions to prevent further gas leakage [2]. While
these systems have flaws, their implementation and installation have so far resulted in the
saving of lives (both plants and animals) and properties.

4. Smoke Detection System in A Smart Kitchen

A smoke detector is a system that detects smoke as a warning sign of a fire. As part of
a fire alarm system, commercial security systems send a signal to a fire alarm control panel,
while household smoke detectors, also known as smoke alarms, typically emit a local audible
or visual alarm from the detector itself [13]. Smoke detectors can detect smoke either
optically (photoelectric) or physically (ionization); they can use either or both methods [14].
Smoking can be detected and therefore discouraged in places where smoking is prohibited
using sensitive alarms. In large commercial, manufacturing, and residential buildings, smoke
alarms are typically operated by a central fire alarm device that is powered by the building's
power with a battery backup [15]. Domestic smoke detectors vary in size from
individual battery-powered devices to multiple interconnected mains-powered units with
battery backup; with these interconnected units, if one detects smoke, they all go off, even if
the power is out in the building. In homes with functioning smoke detectors, the chance of
dying in a house fire is cut in half [13]. Ionization and photoelectric (optical) techniques are
the two main techniques used in smoke detection, as previously described. Figure 4 shows
the various smoke techniques in use. The mode of operation, strength, and constraints of
these techniques are summarized in table 2.

Figure 4. Diagrammatical Representation of Smoke Techniques.

4.1. Ionization Technique

Tiny amounts of radioactive material are present in ionization smoke detectors.
Radiation travels through the ionization chamber, which is an air-filled space between two
electrodes that allows a slight constant current to flow through them. Any smoke that enters
space absorbs alpha particles, reducing ionization and disrupting the current, setting off an
alarm. This form of alarm works best in the event of a fast-moving fire. Optical detectors are
less sensitive to the stage of fire than ionization detectors [16].

4.2. Photoelectric (Optical) Technique

A light source, a collimated light beam device, and a photoelectric sensor are used in
photoelectric smoke detectors. When smoke approaches the optical chamber and travels
along the direction of the light beam, the smoke particles disperse a portion of the light,
pointing it towards the sensor and triggering the detector. Slow smouldering fires respond
better to this sort of warning. Optical detectors are particularly susceptible to fires that are
already in the early stages of combustion [16].

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158 Recent advances in smart kitchen automation technologies: principles, approaches, and challenges

Table 2
Comparisons between smoke detection techniques

A light source, a It works well for It is slow in

collimated light beam detecting fires that are detecting
device, and a swift and blazing. fires with
photoelectric sensor Thanks to its widespread slow
are used in smoke availability, it is still the properties.
detectors. most common method of
smoke prevention.
Makes use of a small Works best in detecting Not reliable
amount of radioactive fires characterized by when
material and their low properties. checking for
electrodes. Also, a reduced number fires with
of false alarms triggered high
by cooking steam. properties.

Using a hybrid solution (ionization and photoelectric) when designing a smoke

detector has proved to be more effective. Regardless of the type of detector technique used,
the proper positioning and management of the instrument must be taken into account for
optimum efficiency.
5. Fire and Fire Detection System in a Smart Kitchen
Fire is one of the most destructive occurrences that can occur; it happens every minute
of the day anywhere on the planet. Although fire is always our ally, it may often be our
greatest enemy when it is unregulated and left to spread within a structure. Of course, fire is
explosive, and smoke from a fire causes a poisonous, hazardous environment [17]. Every year,
early warning and containment of fire will save thousands of lives, thousands of deaths, and
millions of dollars in property damage. Smoke alarms and warning sensors have been
integrated to form life-safety mechanisms in the field of fire detection [5]. An automatic fire
alarm system's goal is to detect a fire, warn the control panel and appropriate authority, and
advise the occupants to take action.

Figure 6. Various Fire Detection Techniques.

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 B. U. Umar, O. M. Olaniyi, I. A. Dauda, D. Maliki, C. P. Okoro 159

A flame detector that uses a sensor to detect and respond to the presence of a flame
or fire is used to detect and respond to the presence of a flame or fire. Sound an alarm,
shutting off a fuel line (such as a propane or natural gas line), and turning on a fire control
device are all possible responses to a perceived blaze, depending on the installation [18].
Figure 6 shows the various techniques for fire detection currently in use.

5.1. Color-Based Fire Detection

The colour of fire pixels is compared to the colour of candidate pixels in colour-based
detection. This is achieved on the basis that the fire pixels would be reddish-yellow in colour.
The methods that employ these features are based on the premise that flames are created by
common materials such as wood, plastic, paper, and other materials. Such that the colour
components in RGB (Red, Green, and Blue), YUV (Luminance, Chrominance), or some other
colour space will accurately characterize the colour to recognize the existence of flames [15].

5.2. Sensor-Based Fire-Detection Method

Fire detection is critical in a variety of settings, including mines and other industrial
settings. As a result, having an alert device capable of detecting fire and sounding an alarm
is critical. Sensor-based fire detection methods use sensors to track fire. In general, the use
of sensors yields high efficiency in all types of detection processes. The sensors detect
features such as fire, light, and other factors to make a decision [15].

5.3. Color and Movement-Based Evaluation

Colour-based assessment will aid in the identification of fire pixels, but it will be less
effective in densely populated environments. This is because these pixels are selected solely
based on their colour. Some aspects go well with the colour of the flames. It would be more
precise if we combine the function of movement with colour-based assessment. This is
founded on the fact that the fire pixels would be in a constant state of motion. As a result, it
would analyze each frame by comparing it to its previous and subsequent frames. As a result,
fire detection will be a little more precise [15].

5.4. Multi-Expert Evaluation

Multi-Expert Evaluation will combine the opinions of many experts and conclude. In
the current scenario, it tests each of the characteristics of fire, such as colour, movement, and
form, as experts and uses them to detect fire. Because of the special colour of flames, colour
is one of the most significant features used. Other elements, such as movement and shape,
may be added to increase efficiency. The flame's movement is assessed based on the fact that
it is constantly moving in nature, and its form is taken into account since the flame's shape
varies every minute seconds. As a result, if we take adjacent pictures, the flame pixels' values
will rapidly change. Multi-Expert Systems usually make use of this property [15].

6. Review of Related Works in Gas, Smoke and Fire Detection in a Smart Kitchen
Automation System
Several analyses of gas, smoke, and fire detection methods have been published
previously, either as academic articles or scientific studies. These efforts have shown to be
beneficial in reducing the risk of dangerous effects. This section presents each of these
research works, as well as their contributions, achievements, and shortcomings.
Research in [19] created a gas leakage detector for protection and protection using an
LPG gas sensor attached to an IoT using an ESP module. The primary controller was an
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160 Recent advances in smart kitchen automation technologies: principles, approaches, and challenges

Arduino. The project's final output was used to detect gas leakage from cylinders and also to
alert the consumer through IoT software. It had three major issues, including energy
efficiency, localization, and routing; however, the proposed solution is less expensive than
currently existing detectors. Research in [20] used the Internet of Things to build a device
that eliminates risks in kitchens (IoT). Multiple sensors, a control unit, an alarm buzzer, and a
GSM module made up this device. To control a gas leak, this mechanism automatically shuts
off (closes) the valve. This machine often controls the cylinder's gas level, and when the
device's weight falls below the "fixed point," it immediately schedules the cylinder for a refill
from the gas agency. This proposed architecture has a wide range of applications that have
proved to be effective and reliable. Research by Adekitan et al. in [21] presented a design
that used a pragmatic protection strategy to track and evacuate gas leaks before they fire. A
control unit, a buzzer bell, a GSM module, and an actuator are all included. This configuration
had the advantage of automatically shutting off the gas supply solenoid valve and evacuating
the gas by turning on the evacuator fans. However, since untreated gas leakage will cause
actual fire outbreaks, there is no actual countermeasure for an actual fire outbreak. Research
by Sharma et al. [17] devised a new approach for detecting fire at an early stage to reduce
risk. A control unit (Arduino UNO), an MQ-5 gas sensor to detect a gas leak, a GSM module
for mobile communications, a buzzer for warnings, an exhaust fan, batteries, LEDs, and other
components are included in the device. The system had safety features such as turning on
the exhaust fan to remove gas from the environment. However, it had no provisions for
dealing with real fires or explosions caused by the use of expired gas cylinders.
Research by in [16] proposed a multi-sensor solution for a fire warning system
prototype. MQ-5 gas sensor, Grove temperature sensor, Grove light sensor, Arduino
microcontroller, GSM module, and GPS shield is included. In the event of fire detection and
outbreak, the device is configured to transmit alerts to registered contacts. Although it is
restricted to residential buildings, this device can identify and distinguish between hazardous
and non-harmful smoke. Research in [22] in their paper, suggests a framework that uses the
Internet of Things (IoT) to connect multiple physical objects that are embedded with
electronics, sensors, and software that can capture data from the environment and transfer it
over the internet. This device can be used for a variety of purposes, including defense,
agriculture, and more. This system necessitates the deployment of a vast number of sensor
clusters for greater reliability. Research in [23] proposed an intelligent smoke detector device
the machine used the Random Forest Algorithm to detect smoke, ZigBee Transmission
Technology to create a wireless network, E-charts for data analysis, and a smoke detector
module to capture environmental data. Temperature, humidity, pressure, and dust sensors
are among the sensors employed. The machine makes use of a low-power optimization
scheme, but there is no safeguard measure put in place. Research in [24], describes the use
of an LPG gas sensor to detect a leak and generate the results in audio and visual formats, as
well as alerting humans via SMS (SMS). The sensors used have excellent sensitivity and a fast
response time, but no countermeasures are provided for the observed leakage.
Research in [25] with the aid of an Arduino, creates a device that can detect a variety
of dangerous gases. This work alters the currently available structures, which are mostly
found in commercial settings but can also be used in homes and at work. The LCD detects
and displays poisonous gases such as butane (also known as LPG), methane, and carbon
monoxide. The percentage concentration of these would be shown on the LCD, but it has a
slow reaction time and does not have countermeasures against the detected gas. [26], the

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 B. U. Umar, O. M. Olaniyi, I. A. Dauda, D. Maliki, C. P. Okoro 161

design of a gas leakage safety device is the subject of this paper. LPG is highly flammable
and can cause a fire even if it is far away from the source of the leak. Most fire accidents are
caused because of a poor-quality rubber tube or when the regulator is not turned off. The
supply of gas from the regulator to the burner is on even after the regulator is switched off.
If the knob is switched on by accident, gas leaks will occur.
The detection, monitoring, and control system for LPG leakage is the subject of the
research. The stove knob is operated automatically by a relay DC motor. Along with safety
features, the mechanism has the added benefit of automatically rebooking the cylinder when
the gas level falls below the cylinder's usual weight. GSM connectivity, on the other hand, is
disabled. While [27], their work focuses on the Internet of Things (IoT) connectivity of every
sensor to create a smart home. Temperature sensors can also monitor high and low
temperatures, allowing the system to identify the temperature and alert the user. The created
android application would allow the user to turn on and off the lights manually. This provides
a significant benefit to the IoT-based smart home system. [28], also, with the assistance of
an Arduino Nano microcontroller, a gas sensor, and an XBee, a gas leakage detection device
was suggested. The sensor node can detect a minute concentration of gas based on the
voltage output of a sensor and will also capture gas leakage data, allowing the sensor node
to be pinpointed to a particular location. A GSM module served as a link between the
microcontroller and the mobile phone unit. It has a wide range of applications, such as in
petrochemical plants and agricultural factories, but it does not provide any safeguards against
detected gases and has a longer response time.
Research in [29], the concept and implementation of an SMS-based Industrial/Homes
Gas Leakage Monitoring and Detection Alarm System were presented in this article. The
device is designed to deter gas leaks from causing damage or deaths. Hardware and software
were designed, developed, configured, and incorporated into the system. When a gas leak is
detected, the time it takes for the customer to receive an SMS from the system control unit
is often reviewed and tested for accuracy to ensure timely transmission of the system's early
warning alert, but it does not have any countermeasure against the detected gas. Research
in [30], in his job, developed and introduced a framework to meet the gas leakage health and
safety requirements. The suggested device is tested, and the findings are checked, by
generating an early warning signal in less extreme conditions and activating a high-pitched
alert during LPG leakage to protect consumers. Even though the device is noisy due to the
lack of a mechanism to switch off the warning buzzer and no precautionary precautions
against detection, the average system cost is smaller and the reaction time is faster. Research
in [31], when the concentration value of toxic gases such as carbon monoxide reaches the
usual value, the paper developed a system that positions gas sensors in the leak points, which
detects the concentration value of toxic gases such as carbon monoxide and imitates to the
mobile unit. The signal is sent to the PIC microcontroller, which uses the ZigBee
communication module to inform the mobile computer. This architecture has a quick
response time, but it is more realistic for large-scale petrochemical applications, so it is
limited to petrochemical industries for optimum efficiency. Research by Saeed et al. in [32],
A GSM-based gas detector system for propane and butane gases was built in this work, and a
GSM module was used to relay messages to the consumer in the event of a leak. The device,
on the other hand, has no safeguards against actual detection. In the work of Saeed, [33],
using multiple sensors, a wireless sensor network was developed and tested for early fire
detection of a house fire. To stop false alarms, GSM was used. Low-cost sensor nodes,

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162 Recent advances in smart kitchen automation technologies: principles, approaches, and challenges

temperature, light, and smoke data are spread out around the forest in this device to gather
information, which is then fed into ANN models and transformed into knowledge. There is a
significant time delay that could endanger human life and property; however, the results
produced are correct.
Research by Kusampudi et al. in [34] Using Fuzzy Logic strategies, proposed a device
architecture for fire-fighting robots that sense the fire and enter the target area without
touching any obstacles, avoiding damage to lives and property. Many ultrasonic sensors
installed on the robot sensed the turn angle between the robot head and the target, the
distance of obstacles around the robot (front, left, and right, including other mobile robots),
and were used as feedback fuzzy members in another contribution. The aim of developing
fire-fighting robots is for them to enter a fire area zone without colliding with any obstacles
to avoid causing harm in an unfamiliar environment. Despite its high reliability and
performance, the net device cost is not cost-effective; therefore, it could be out of reach on
average. Research by Sarwar et al. in [35] with the help of Artificial Intelligence Technology
Fuzzy Logic, created a simple way to detect fire using multiple sensors instead of a single
sensor. In a human way of thought, the built framework was easier to use and was closely
similar to the actual model idea. It needs an accurate dataset for optimum efficiency, which
could be difficult to obtain, and it has no mode of communication (i.e., GSM module), but it is
extremely reliable. Research by Sowah et al. in [36] describes a device for detecting fire in
vehicles using an Arduino microcontroller and Fuzzy Logic Artificial Intelligence Technology
to prevent any harm to the vehicle caused by fire. When a fire is observed, temperature
sensors, flame sensors, and smoke sensors are used. When a fire is detected, a sound detector
is activated, and carbon dioxide is sent to the site, causing both environmental and noise
emissions. A system is installed and tested in a medium-sized physical vehicle, with a 2 kg
cylinder fixed behind the passenger's back seats. Research by Çelik et al. [37] proposed a
model for detecting fire and smoke without the use of any sensors in their work, which is
focused on image processing. The framework is set up in such a way that colour data and
motion analysis are integrated using the derived model. Environmental contamination may
cause this system to fail, resulting in inaccurate readings. This method, on the other hand,
has improved accuracy. In the intelligent house, Suli et al. [38] built an automatic fire alarm
and fire control linkage system. The machine intelligently predicts fire, monitors gas, and has
an automated fire alarm and linkage feature, however, there are no countermeasures in place
to prevent real leaks and fire outbreaks. Finally, Slavkovikj et al. in [39] Social networking
networks are being used to spot fires in the current architecture. According to the author, as
the number of social networks and services grows, so does the volume of knowledge that is
shared on the internet. The author suggested a web design for wildfire social sensors (WSS).
As a result, social media can provide a human-centric sensor network for the early
identification of disasters such as fire; however, the optimum efficiency of this architecture
is solely dependent on the network's stability.

7. Open Issues and Challenges in Gas Leakages, Smoke, and Fire Detection in A Smart
Kitchen Automation System
The critical findings made during the analysis are taken into account. To build an
effective detection system in a smart kitchen, precise knowledge of the application is often
needed. The reviewed papers contain material that can be used as a foundation upon which
a study can begin. It's also important to note that none of these devices can be trusted if their

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 B. U. Umar, O. M. Olaniyi, I. A. Dauda, D. Maliki, C. P. Okoro 163

reactions to external factors including gas, smoke, and fire aren't tested regularly. Available
systems in today's market face problems such as most conventional home systems are
automatic, so they cannot change and respond to the consumers' actual working
environmental conditions. Also, according to the poll, certain devices have a high likelihood
of causing a false alarm because they are vulnerable to noise and minor variations in the
environment's sounds. While these devices sense a fire until it spreads, there is little control
or precautionary measures in place, making property loss almost unavoidable. Also, in some
designs, multiple sensors were used to increase accuracy, however, it requires large numbers
of “clusters” of sensors to be deployed which will inevitably increase overall system cost and
deployment cost.

8. Conclusions
This review paper serves as a basic guide to help researchers choose the right
technology for gas leakage, smoke, and fire detection in a smart kitchen. A comprehensive
survey of several smart kitchen automation systems was performed in this research. Also
included is a description of what has been done in this area to date, as well as the research
gap and open issues that need to be addressed in this research area. A wide range of gas
leakage, fire, and smoke detection systems in a smart kitchen was studied and classified into
three main categories: gas leakage detection, smoke detection, and fire detection in a smart
kitchen. Finally, the research gaps and unsolved challenges in gas leak detection, fire
detection, and smoke detection in a smart kitchen were reviewed. We found that the majority
of existing systems are not dynamic, and as a result, they are unable to adapt and react to
the user's present operating environment. Furthermore, because some of the systems are
sensitive to noise and tiny changes in the environment, they have a high likelihood of
generating a false alert.

Conflicts of Interest. The authors declare no conflict of interest.

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Citation: Umar, B. U.; Olaniyi, O. M.; Dauda, I. A.; Maliki, D.; Okoro, C. P. Recent Advances in Smart Kitchen
Automation Technologies: Principles, Approaches and Challenges. Journal of Engineering Science 2022, 29 (3),
pp. 150-165. https://doi.org/10.52326/jes.utm.2022.29(3).13.

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Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
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Submission of manuscripts: [email protected]

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Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 166 - 175
Fascicle Food Engineering ISSN 2587-3474
Topic Food Industry and Management eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).14
UDC 664:613.2:614.31(478)

EVALUATION OF GLUTEN CONTAMINATION IN GLUTEN-FREE PRODUCTS IN

THE REPUBLIC OF MOLDOVA

Rodica Siminiuc*, ORCID: 0000-0003-4257-1840,

Dinu Țurcanu, ORCID: 0000-0001-5540-4246

Technical University of Moldova, 168 Stefan cel Mare blvd., Chisinau, Republic of Moldova
*Corresponding author: Rodica Siminiuc, [email protected]

Received: 05. 31. 2022

Accepted: 07. 15. 2022

Abstract. Celiac disease (CD) is an autoimmune condition, triggered by gluten ingestion,

which affects the small intestine, destroying the villi. It is considered that in recent years CD
has undergone a real "metamorphosis" due to the constant increase in diagnosed cases. The
only treatment available for BC is to stick to a gluten-free diet throughout your life. Adherence
to a GFD requires strict elimination of gluten-containing products, as patients with CD are
very sensitive to the toxic effect of gluten. The purpose of the research is to evaluate whether
the products marketed on the territory of the Republic of Moldova, labeled as gluten-free
products, are safe for people with celiac disease, from the perspective of their gluten content.
The identification of gluten in GF products sold in supermarkets in the capital was done using
the GlutenToxPro gluten detection kit for food, beverages, and work surfaces (AOAC-RI).
Research has shown that both gluten-free products imported with the Crossed Grain logo and
those just labeled gluten-free (both imported and local), pose no risk to people with gluten-
related disorders: the gluten content of all samples was up to 20 ppm. Local, non-packaged
GF products (developed and made available to consumers by the supermarkets concerned)
pose an increased risk of contamination.

Keywords: celiac disease, certified products, Crossed Grain logo, food safety, food labeling, gluten
free.

Rezumat. Boala celiacă (BC) este o afecțiune autoimună, declanșată de ingestia la gluten,
care afectează intestinul subțire, cu distrugerea vilozităților. Se consideră că în ultimii ani BC
a suferit o adevărată „metamorfoză” din cauza creșterii constante a cazurilor diagnosticate.
Singurul tratament disponibil pentru BC este aderarea pe tot parcursul vieții la o dietă fără
gluten. Aderarea la un GFD impune eliminarea strictă a produselor care conțin gluten,
deoarece pacienții cu BC sunt foarte sensibili la efectul toxic al glutenului. Scopul cercetării
constă a evalua dacă produsele comercializate pe teritoriul Republicii Moldova, etichetate ca
produse fără gluten, sunt sigure pentru persoanele cu maladia celiacă, din perspectiva
conținutului de gluten în ele. Identificarea glutenului în produsele GF comercializate în
supermarketurile din capitală s-a realizat cu ajutorul kitului de detecție a glutenului pentru
alimente, băuturi și suprafețe de lucru GlutenToxPro (AOAC-RI). Cercetările au arătat că atât
produsele fără gluten importate cu sigla Crossed Grain, cât și cele doar etichetate fără gluten
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 R. Siminiuc, D. Țurcanu 167

(atât de import cât și locale), nu prezintă niciun risc pentru persoanele cu tulburări legate de
gluten: conținutul de gluten din toate probele a fost de până la 20 ppm. Produsele GF locale,
neambalate (elaborate și puse la dispoziția consumatorilor de către supermarketurile în
cauză) reprezintă risc sporit de contaminare.

Cuvinte cheie: etichetarea alimentelor, fără gluten, maladia celiacă, produse certificate, siguranța
alimentelor, sigla spicul tăiat.

1. Introduction
Celiac disease (CD) is an autoimmune condition, triggered by gluten ingestion, which
affects the small intestine, destroying the villi. It is considered that in recent years CD has
undergone a real "metamorphosis", largely due to the constant increase in diagnosed cases
[1,2]. Some theories suggest that this is due not only to the high availability of screening
tests, but also to globalization, including the consumption of large amounts of gluten (up to
20 g / day), which has led to the increased prevalence and incidence of MC [3]. It is estimated
that over 70% of people with celiac disease remain undiagnosed, which means that they
become chronic patients who experience a decrease in quality of life associated with various
gluten-related health problems that occur over time [4,5].
The incidence of MC in the world is about 1%. People with MC may experience a wide
variety of gastrointestinal and malabsorption symptoms or extra-intestinal symptoms. The
only treatment available for celiac disease is to stick to a gluten-free diet throughout your
life. Adherence to a GFD refers to the strict elimination of gluten-containing products [6,7].
Gluten is made up of protein fractions, which are found mostly in the endosperm of grains,
such as wheat, barley, rye, and foods that are derived from grains (e.g., semolina, durum,
spelled, triticale, kamut, and malt) [8–11].
Gliadin, a glycoprotein, alcohol-soluble fraction of gluten, is thought to be responsible
for the immune reaction to gluten consumption. In general, gliadin contains both toxic and
immunogenic peptides.
● Toxic peptides can affect tissues, causing damage to the intestinal mucosa,
justifying the activity of T-helper lymphocytes, by activating an innate immune
reaction [12].
● Immunogenic peptides can activate the acquired immune response by specifically
stimulating HLA-DQ2/DQ8 T lymphocytes and B lymphocytes [13].
Due to the chemical complexity, the digestibility of gliadins is quite low. Fragments
obtained from the partial digestion of proline and glutamine cause inflammation and
destruction of intestinal epithelial cells. According to the electrophoretic mobility of
prolamins, 4 fractions were identified: α-, β-, γ- and ω.
The α-gliadin fraction, with 266 amino acids, is considered to be the most toxic,
containing the most active epitopes for the immune system [14, 15].
In people with CD, the sequence 31-34 (A-gliadin) has no immunological activity
against T-helper lymphocytes and is transported across the mucosa of celiac patients in
double amounts compared to healthy individuals (Figure 1).
The main protein fractions are prolamins and glutelins and are responsible for the
development of symptoms in celiac disease [2].
According to European legislation and Codex Alimentarius, a food can only be labeled
“gluten free” if it contains less than 20 ppm gluten (20 mg /kg) in the final product [12–14].

Journal of Engineering Science September, 2022, Vol. XXIX (3)

168 Evaluation of gluten contamination in gluten-free products in the Republic of Moldova

Figure 1. Protein fractions of cereals and subfractions of gliadin.

Also, a food labeled “very low gluten” may be labeled as such if it contains less than
100 ppm gluten (100 mg/kg) in the final product [12,14,15]. There are studies that
have shown that prolonged ingestion of even traces of gluten (10–50 mg/day) can affect
the integrity of the intestinal mucosa, an increased number of IELs being the first
marker of mucosal damage [16].
The most significant long-term risk factor is inadequate adherence to a gluten-free
diet [5,6,17]. A strict gluten-free diet normalizes the levels of antibodies associated with
celiac disease and, respectively, the recovery of the affected tissues takes place, which can
often take several months [4,12,17]. Carefully performed and monitored by a specialist, the
GF diet will positively influence the health of the patient with gluten-related disorders [2].

2. The market for gluten-free products

The size of the global gluten-free market has been estimated at $ 5.9 billion in 2021
and is expected to expand at an annual growth rate (CAGR) of 9.8% from 2022 to 2030 (Figure 2).

Figure 2. The global market for gluten-free products [18].

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 R. Siminiuc, D. Țurcanu 169

The bakery market accounted for the largest share of revenue of almost 29.0% in 2021
and is expected to maintain its dominance over the forecast period. The growing prevalence
of gluten-related disorders stimulates the demand for gluten-free products. The COVID-19
pandemic has also exponentially affected the use of gluten-free products due to growing
concerns about health and well-being among consumers. Inspired by those who encourage
gluten-free diets for better health, many consumers have joined the diet of people for whom
gluten-free consumption is a mandatory medical necessity [18,19]. Studies in the field have
shown that the rate of adherence to a GFD varies from 44 to 90% in patients with MC. Most
often the adherence to a GF diet is restricted by the high cost of these products, compared to
the classic products.
A review of the cost of gluten-free products in the United States found that the total
cost of gluten-free products is 183% higher than their wheat-based counterparts. Gluten-free
biscuits have been found to be 270% more expensive than those made with gluten-
containing flours. Commodities such as bread and pasta were also significantly more
expensive - by 229% and 227%, respectively. In a survey conducted by GIG in 2021, 78% of
respondents - followers of a gluten-free diet said that the cost of gluten-free foods was the
biggest challenge they faced. 38% said access to gluten-free foods in general is a challenge
[20].
The food safety of people following a GF diet is disturbed by other factors such as:
limited availability of gluten-free products, insufficient labeling, risk of cross-contamination,
lack of certification policies for GF products, etc. [6,17,21–24]. Patients with CD are very
sensitive to the toxic effects of gluten.
The purpose of the research is to evaluate whether the products marketed in the
territory of the Republic of Moldova, labeled as gluten-free products, are safe for people with
celiac disease, from the perspective of their gluten content.

3. Materials and methods

During the month of May, this year, the supermarkets and small (corner) stores in the
capital were visited to identify if they have GF products and to evaluate their assortment. List
of supermarkets and subsidiaries under investigation:
1. Nr. 1.
4. Fourchette.
5. Linella.
6. Metro.
7. Kaufland.
A total of 13 supermarkets and 23 small (corner) stores were visited. GF products were
purchased to assess whether they were contaminated with gluten, as well as the degree of
contamination.

3.1. Materials
The gluten-free products (48 products) purchased were classified into 3 categories:
- Imported products, labeled gluten free.
- Imported products, labeled gluten-free, with the logo of the Crossed grain.
- Gluten-free local products (non-certified) - 17 products.
GlutenToxPro Kit (AOAC-RI).

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170 Evaluation of gluten contamination in gluten-free products in the Republic of Moldova

3.2. Methods
In order to achieve this goal, imported and domestic GF packaged products were
purchased from the supermarkets in the capital. A total of 45 products were purchased: bread,
pasta, flour and flour mixes, pastries. Products were tested for gluten using the GlutenToxPro
Kit (AOAC-RI) (Gluten Detection Kit for Food, Beverage, and Workspaces) [25].
GlutenToxPro is an immuno-chromatographic test used to detect gluten in foods with
different levels of processing. The test is used in routine gluten monitoring and to ensure
that products are HACCP compliant and properly labeled. Tests also allow decisions and
corrective action to be taken quickly if there is a risk of contamination along the production
chain. The kit contains the G12 antibody that specifically recognizes the 33-mer peptide of
the α-gliadin protein that induces celiac disease [26], (Figure 3). This recognition sequence is
repeated three times within the gliadin 33-mer peptide. The G12 antibody recognizes
immunotoxic prolamins from wheat, barley, rye and also from some varieties of oat [27]. The
G12 antibody is also capable of reacting to other epitopes that are found in other toxic
prolamins [27,28].

Figure 3. The 33-mer peptide and G12 antibody binding.

The principle of the method. The method consists in the reaction of immunotoxic
peptides, like peptide 33 in the sample, with colored conjugates, previously fixed on the stick.
That complex has capillary spread on the test strip. In the case of a positive result, a red line
appears in the test area of the strip. The result is negative if the red line is missing.
If the test has been performed correctly, a blue line (the control line) will appear on the test
strip, regardless of whether or not there is gluten in the tested sample. The detection
threshold is conditioned by the number of drops (1, 2, 4 or 10 drops) added to the blue cap
dilution bottle (Table 1).
Table 1
Interpretation of results
Detection threshold
10 drops 4 drops 2 drops 1 drop
Test result Positive >5 ppm > 10 ppm > 20 ppm > 40 ppm
negative < 5 ppm < 10 ppm < 20 ppm < 40 ppm

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 R. Siminiuc, D. Țurcanu 171

Warning and limitations. The efficiency of gluten extraction depends on the type of test
samples and in such cases, involves conditions of maximum sensitivity (for a detection limit
of at least 10 ppm, 10 drops of extract are required in the dilution bottle with a blue cap).
This product category includes:
• Food with ingredients (up to 70%) containing polyphenols or tannins in high
concentrations (coffee, black tea, chocolate, wine, berries, legumes, etc.).
• Foods rich in antioxidants (vitamin A, E and C).
• Heat-treated foods with temperatures above 180 °C.
The gluten content could be underestimated in samples subjected to intense
hydrolysis processes (beer, sourdough, syrups) [33].
The tests were performed in May 2022, at the Technical University of Moldova,
Department of Food and Nutrition.

4. Results and Discussion

Complete avoidance of gluten in the diet is difficult to maintain. A "pervasive" nutrient,
gluten can contaminate gluten-free items along the production chain, from the field to the
grinding, storage, and manufacturing stages [16]. Most supermarkets had a (common) section
for special purpose products (diabetic products, vegan products, organic products, gluten-free
products, etc.). Of the 13 supermarkets, only eight had a higher availability of gluten-free
foods during that period. Probably because of the Covid 19 pandemic [29], but also of the war
in Ukraine, the range of GF products was quite limited. Small (corner) stores did not have
gluten-free products.
A total of 48 GF foods were analyzed. The selected products included different brands
of bakery and pastry products, flours and mixes of flour and pasta: 13 imported products,
labeled GF; 18 imported products, with the Crossed Grain logo; 15 local packaged products
and 2 local products for use current (unpackaged). The results of the research are presented
in Table 2.
Table 2
Level of gluten contamination in the products examined
Number Gluten content (GC)
Tested product category (GF) of > 20
products > 10 ppm < 10 ppm
ppm
Imported products, labeled GF n = 13 - 1 (8%) 12 (92%)
Imported products with the n = 18 - - 18 (100%)
Crossed grain logo
Packaged local products n = 15 - 5 (33%) 10 (67%)
Unpackaged local (current) n=2 2 (100%)
products

The European License System (ELS) is the standard by which gluten-free products are
certified. It refers to those products that carry the Crossed Grain logo on the packaging [13].
The products, which had the Crossed Grain on their packaging, have confirmed their safety
and integrity, and continue to be seen as the most effective means of communicating to
consumers that these products are safe for people with MC [12,15,30]. All 18 products tested,
with the Crossed Grain logo on the package, contained less than 10 ppm gluten.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

172 Evaluation of gluten contamination in gluten-free products in the Republic of Moldova

Another 13 imported products, which had the label gluten free but did not have the
Crossed Grain logo, confirmed their safety for consumers with disorders related to gluten
consumption: in 12 of them the gluten content was below 10 ppm and only in one product,
the gluten content was between 10 ppm and 20 ppm. What characterizes these products as
gluten-free products.
The packaged local products under test were products that were naturally gluten-free.
Namely cereal derivatives (sorghum flour, corn, legumes, from different producers). It should
be noted that the list of local products, labeled gluten-free, contained: flour, semolina and
sorghum groats, corn flakes, corn flour, chickpea flour, bean flour, potato flour and flour
mixes. The list did not include any products such as bread, biscuits, pasta, snacks, etc. The
results showed that even local products, labeled as gluten-free products, do not pose risks
for people with disorders related to gluten consumption: in 10 of the 15 local products tested,
the gluten content was below 10 ppm, and in 5, between 10 ppm and 20 ppm.
Only one chain of supermarkets in Chisinau offered consumers gluten-free products
for current consumption, namely bread made from legumes and pseudocereals. These
products were developed in the bakery sections of the supermarkets involved. Those products
had the list of ingredients listed on the label and were marketed as gluten-free products. In
both products, the gluten content exceeded 20 ppm, which constitutes a risk for the safety
of people with celiac disease.
Research has shown that both gluten-free products imported with the Crossed Grain
logo and those just labeled gluten-free pose no risk to people with gluten-related disorders:
the gluten content of all samples was up to 20 ppm.
Local products labeled gluten-free, according to the results obtained, are just as safe.
We just have to keep in mind that when we refer to local GF products, we usually refer to
grains, legumes and their derivatives. In the Republic of Moldova, gluten-free products such
as: bread, pasta, croissants, pizza, puff pastry, etc. are not currently produced.

5. Conclusions
● Gluten-free products are an example of reverse functional foods, in which gluten is
eliminated and not included, like other constituents. These are currently an area in
full swing.
● According to the results obtained, GF products with the Crossed grain logo as well
as those certified GF continue to be seen as the most effective means of
communicating to consumers about their safety for people with MC.
● The assortment of gluten-free foods in the Republic of Moldova is extremely low,
and this makes the food security of these categories of people vulnerable. However,
research results have shown that local products (cereals, legumes, and their
derivatives, etc.) labeled as gluten-free products do not pose risks for coeliacs.
● Unpackaged local GF products (developed and made available to consumers by the
supermarkets concerned) pose an increased risk of contamination.
● The lack of certification policies for this product category reduces confidence in the
safety of local GF products.
● Food education, informatization of the population, especially those in the food
industry, with reference to gluten sources, workplace hygiene, sources, and
consequences of cross-contamination with gluten, would contribute to a better

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 R. Siminiuc, D. Țurcanu 173

safety of these products and increase nutritional security of people with disorders
related to gluten consumption in the Republic of Moldova.
● Launching a systematic gluten-free food sampling program would help to quickly
identify risky products, ensure the safety of available products, and ultimately
improve the long-term well-being of people with CD or other gluten-related
disorders.

Funding: This research was funded by the postdoctoral grant: Contributions regarding
nutritional eradication of gluten consumption diseases, nr. 21.00208.5107.06 / PD and the
state project Personalized nutrition and intelligent technologies for my well-being, nr.
20.80009.5107.10 / PS.

Conflicts of Interest: The authors declare no conflict of interest.

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 R. Siminiuc, D. Țurcanu 175
Citation: Siminiuc, R.; Țurcanu, D. Evaluation of gluten contamination of gluten-free products in
the Republic of Moldova. Journal of Engineering Science 2022, 29 (3), pp. 166-175.
https://doi.org/10.52326/jes.utm.2022.29(3).14.

Publisher’s Note: JES stays neutral with regard to jurisdictional claims in published maps and
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Copyright:© 2022 by the authors. Submitted for possible open access publication under the terms
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Submission of manuscripts: [email protected]

Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 176 - 188
Fascicle Food Engineering ISSN 2587-3474
Topic Biotechnologies, Food Chemistry and Food Safety eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).15
UDC 663.26:579

EFFECT OF BIOACTIVE ADDITIVES ON BIOMASS FERMENTATION FROM AGRO-

INDUSTRIAL SECTOR

Gheorghe Duca1, ORCID : 0000-0001-7265-6293,

Olga Covaliova1, ORCID: 0000-0002-0387-3195,
Ecaterina Covaci2, ORCID: 0000-0002-8108-4810,
Lidia Romanciuc1, ORCID: 0000-0002-4555-1194,
Corina Tașca1,2*, ORCID: 0000-0003-3359-3490

1
Institute of Chemistry, 3 Academiei Str., Chisinau, MD 2028, Republic of Moldova
2
Technical University of Moldova, 168 Stefan cel Mare blvd., Chisinau, MD 2004, Republic of Moldova
*Corresponding author: Corina Zubic, [email protected]

Received: 07. 12. 2022

Accepted: 09. 05. 2022

Abstract. Wastes from the agro-industrial sector, due to their toxic effects with regard to
plants and living organisms, cannot be dumped in the soil. However, they can serve as
renewable source of value-added products, following the specific digestive treatment. This
research was focused on studies of vinasse fermentation processes in the presence of
bioactive substances introduced directly into the digested biomass. The results obtained
testify that the substances of natural origin used as additives, demonstrate the pronounced
effects on alcoholic fermentation of vinasse under the mesophilic conditions. The
comparative assessment of different additives action in the studied processes have
demonstrated that the dihydroxyfumaric acid caused the emission of 266 cm3 CO2 in 76 hours,
aescinum – 251 cm3 in 55 hours, tomatin – 233 cm3 during 78 hours, sclareol – 232 cm3
during 55 hours, vanillin – 229 cm3 during 69 hours, whereas catechin – 180 cm3 during 61
hours of fermentation, until the fermentation process was completed. Thus, the study of the
effects of bioactive substances with possible antioxidant properties on biomass from
winemaking sector with identification of these processes mechanisms can be a perspective
direction, suggesting the new ways of wastes valorisation.

Keywords: Agro-industrial wastes, vinasse, fermentation, bioactive additives.

Rezumat. Deșeurile din sectorul agroindustrial, datorită efectelor toxice asupra plantelor și
organismelor vii, nu pot fi aruncate în sol, dar pot servi drept sursă regenerabilă de produse
cu valoare adăugată. Prezenta cercetare s-a axat pe studiul procesului de fermentare a vinasei
în prezența substanțelor bioactive, introduse în biomasa digerată. Rezultatele obţinute
mărturisesc că substanţele de origine naturală utilizate ca aditivi demonstrează efectele
pronunţate asupra fermentaţiei alcoolice a vinasei în condiţii mezofile. Evaluarea
comparativă a acțiunii aditivilor a demonstrat că acidul dihidroxifumaric a determinat emisia
de 266 cm3 CO2 în 76 ore, aescinum – 251 cm3 în 55 ore, tomatin – 233 cm3 în 78 ore, sclareol
– 232 cm3 în 55 ore, vanilină – 229 cm3 timp de 69 de ore, în timp ce catechina – 180 cm3
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Gh. Duca, O. Covaliova, E. Covaci, L. Romanciuc, C. Tașca 177

pe parcursul a 61 de ore de fermentație, până la finalizarea procesului de fermentație. Astfel,

studiul efectelor substanțelor bioactive cu posibile proprietăți antioxidante asupra biomasei
din sectorul vitivinicol cu identificarea mecanismelor acestor procese poate fi o direcție de
perspectivă, sugerând noi modalități de valorificare a deșeurilor.
Cuvinte cheie: Deșeuri agroindustriale, vinasă, fermentație, aditivi bioactivi.

1. Introduction
The problem of wastes management from agro-industrial sector, to prevent the
environmental pollution with toxic components and at the same time, to obtain the series of
value-added products, is an important issue requiring a smart and complex approach. The
wastes treatment technology is should be selected on the base of the initial wastes nature,
composition and amounts, which, on their turn, are functions on the main production cycle,
raw materials, process technology and conditions applied.
Specifically, in the agricultural regions having the wine, spirit, beer and juice-
producing industries, the specific types of liquid wastes are generated in the state of
continued digestion, which implies the strict prevention of their discharges/dumping directly
into the landfills, natural water bodies or other environmental compartments as they can
destroy the chemical composition of soil, violate the natural balance of microorganisms,
plants, and other living organisms. Existing methods of the solid organic wastes management
involve their application in agriculture, burning (although the rather costly process associated
with air emissions), anaerobic digestion, composting, etc. The liquid wastes from agro-
industrial sector can be treated by sedimentation, decanting in stabilization ponds, anaerobic
fermentation, etc.
To produce ethanol from carbohydrate-containing raw materials, the fermentation
process is applied commercially [1]. Alcohol is obtained by fermentation of the sugars present
in the different raw materials, which are metabolized by microorganisms belonging to the
genera Saccharomyces, Zymomonas, Kluyveromyces, and Zygosaccharomyces [2]. The structural
carbohydrates in biomass componence are broken down into the sugars using enzymes.
Subsequently, the sugars released are transformed by microorganisms into the alcohols,
hydrocarbons or some organic acids during the fermentation process under the atmospheric
pressure and temperature 25-70oC. Intermediate sugars can be also utilized to obtain certain
useful chemicals [3].
Currently, the operation of the most of processing industries in agriculture, including
those dealing with the grain processing into the alcohol, remain unsafe for the environment
[4, 5]. Meanwhile, closed ecologically safe production cycles will make it possible to resolve
fundamental issues such as rational use of natural raw resources, environmental protection
and improving the quality of final product [6]. The alcohol industry affects first of all the
water resources, then air and soil.
Specific consumption of fresh water makes 195-325 m3/t alcohol (10-17 L water/ 1 L
alcohol produced), depending on the raw material type and processing technology, namely,
recycled water supply [7, 8]. Such high amounts of water used trigger the high volumes of
liquid wastes thus formed [9, 10]. The admixtures contained in the waste waters contain
mineral and organic substances of vegetable origin. Such wastes are poorly filtrated, quickly
rotting, releasing unpleasant odors.
Therefore, the indicator of technology efficiency is important, as it determines the
degree of transformation of the initial raw material. Amount of substrate that can be
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178 Effect of bioactive additives on biomass fermentation from agro-industrial sector

transformed in ethanol by microbiological synthesis, depends first of all on the type of raw
material and selected production technology [11]. Basically, from 5 to 60% of substrate, in
average 32-36%, depending on its type and ethanol production method, are transformed into
the production wastes [12]. Thus, conversion degree of glucose in ethanol makes 95-100%,
fructose – 95-100%, xylose – 60-90%, sucrose – 94-100%, hemicellulose – 40-81%,
cellulose – 90-100%. The wastes generated from the alcohol production include yeasts,
vinasse, carbon dioxide, ester-formaldehyde fraction, fuel oils (0.94 kg/t grain). Distilled grain
residue is the main solid waste which contains carbohydrates, proteins, lipids and some
microbial metabolites, which is used as feed, fertilizer or culture substrate for edible
mushrooms [13].
Among these residues, the main type is alcohol vinasse (or post-distillery vinasse),
which is the biomass separated in the distillation process and represents a liquid with
suspended particles, acid pH and high contents in organic matter.
On average, the vinasse production makes about 10-15 L vinasse/L ethanol [14].
Vinasse represents a liquid solution containing the suspended particles, with acid pH The
liquid wastes from food industries have high amounts of organic matter, and, as a
consequence, rather high contents of chemical oxygen demand (COD), biochemical oxygen
demand (BOD) and suspended solids (SS) values: wastes from alcohol production from
grain have on average 130-160 g O2/L BOD, 200-220 g O2/L COD, 340-360 g/L SS and pH=
6.5-8.8, whereas the liquid wastes from sugar industry (sugar beet) have around 2370 g
O2/L BOD, 7540 g O2/L COD, 21320 g/L SS and pH=8.0 [15].
In some cases, vinasse can be discharged to sewerage system, reaching the
wastewater treatment plant, thus significantly impairing its operation. Vinasse discharges
into the environment as a rule, case serious environmental problems. As an alternative, it
could be used as a liquid food additive for cattle or poultry [16-18], biogas production [19-
21] or for fertilization of agricultural fields [22-24]. But the direct suing of vinasse for animals
is not always safe or rational, and cannot resolve the issue of its complete utilization. Some
standardized methods have been developed to evaluate generation of byproducts and
residues in alcohol production cycle, including the entire supply chain, and minimize negative
impacts from crop establishment to consumption of fuel ethanol [25-27].
High water contents in the organic wastes with high fermentable sugar contents and
wet biomass implies their obligatory treatment or recovery which is however rather costly
[28]. Therefore, the development of useful valorization of this waste to obtain the other
value-added products is a perspective approach.
To break down the waste biomass into sugars that can be further converted into the
gas or liquid biofuels, or other useful products, the biochemical conversion by
microorganisms and enzymes is often used [29-31], although the other approaches such as
coagulation and oxidation have been also proposed [32]. Generally, biochemical digestion is
rather slow process that requires some time for biomass transformation into the products.
Among these technologies, anaerobic digestion and fermentation are most popular processes,
resulting in producing the biogas which mainly contains biomethane, carbon dioxide, and in
a smaller amounts biohydrogen, hydrogen sulfide [33-35]. During the anaerobic digestion,
bacteria are applied to hydrolyze carbohydrates into the sugars that are digestible by other,
methanogenic bacteria, which in their turn, produce biogas from the digestible components
of biomass. In dependence on the biochemical digestion conditions, biogas with high
contents in methane [36-38] or hydrogen [39, 40] may be produced under the oxygen-free

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 Gh. Duca, O. Covaliova, E. Covaci, L. Romanciuc, C. Tașca 179

conditions, or under the elevated pressure [41, 42], or using the other approaches such as
adding of bioactive compounds accelerating the biochemical digestion and making it
possible to obtain much higher amounts of biomethane of biohydrogen per shorter time [43-
45]. Biogas can be burnt to produce the heat, or can be converted to energy, or both energy
and heat, using the cogeneration devices [46, 47].
However, not only the biofuels but also a series of value-added products such as sugar
alcohols (xylitol) can be obtained by using the combined technologies such as chemical or
biochemical process combined with the thermochemical method [48, 49].
Production of alcoholic and non-alcoholic beverages generates the wastes and by
products that may be recovered, thus allowing not only to reduce their disposal costs and
minimize the environmental pollution, but also to develop the new useful products, in
addition to the traditional uses of such wastes as animal feed or soil fertilizers. Dumping in
the environment of such residues can provoke the problems such as rotting, higher soil
acidity, phytotoxicity, methane gas production, etc. [50].
Wine-and juice production is a large source of wastes in agriculture [51]. Grape marc
is generated in the grapes processing in rather large amounts in Moldova [52]. Bioactive
compounds are among the potential value-added products than can be extracted from the
organic wastes. They could be isolated and structurally investigated, and subsequently used
for the development of innovative products [53, 54]. Thus, the grape marc along with the
other solid and liquid wine-production residues is used for feeding the cattle and poultry in
agricultural sector, although having a low nutrition value [55, 56], and is also applied as
fertilizer in agricultural fields [57]. But, according to the previous studies, the grape marc is
a prospective raw material for obtaining of series of bioactive substances, specifically, fatty
acids, pectins, phenols, etc. to be further used in the food production, supplements, medical
products, cosmetics, colorants [58-61].
According to numerous works, polyphenols and other components contained in the
grapes, wine or juice have beneficial effects on human health, such as inhibiting the
development of certain cancer cells acting as free radical scavengers [62], antihyperglycemic,
cardioprotective, anti-hyperlipidemic, etc. effects [63, 64]. Apart from the phenolic
compounds, grape marc also contains significant amount of such potentially useful
substances, some of them having the pronounced antioxidant activity as catechin,
epicatechin, hydroxytyrosol, tyrosol, cyaniding glycosides, a series of acids like gallic, caffeic,
procatechinic, syrignic, vanillic, o-coumaric, p-coumaric [65]. A solid-liquid extraction method
[66, 67], hydrothermal treatment [68] and other approaches have been applied to extract the
bioactive components from grape pomace, considering the fluctuating composition of its
solid fraction for further using in food production. As waste biomass from agro-industrial
sector can serve as a raw material for not only the energy production, but also for food and
animal feed production, as a source of bioactive and other substances with useful properties
for industry, its conversion efficiency needs to be improved. For this reason, current research
is focused on increasing the product yields, improving the biochemical conversion
technologies, increasing the conversion degree of biomass, improving the entire biochemical
conversion system. Biochemical digestion of waste biomass using the microorganisms has an
important advantage that no high temperatures are needed. In addition, the wet biomass of
organic wastes has high water contents, making it necessary to apply the effluent treatment.
Our studies are focused on investigation of an original approach in enhancing the
conversion rate and conversion degree of organic wastes biomass, using the small amounts

Journal of Engineering Science September, 2022, Vol. XXIX (3)

180 Effect of bioactive additives on biomass fermentation from agro-industrial sector

of biologically active substances introduced into the fermented mixture, to accelerate the
process rate and obtain the valuable products and, at the same time, to prevent the discharges
of harmful mixtures into the environment. It was of special interest to study the effect of
various additives of natural vegetal origin, introduced into the digested mixture and un type
of biomass used.
2. Materials and Methods
The overall scope of the work was to elaborate processes of liquid wastes treatment
from the agri-food sector, with obtaining the value-added products and avoid discharges into
environment of toxic substances which may provoke unfavorable effects on soil, water, air
and living organisms.
The following instruments and equipment were used for the research: thermostat
PURA, digital pH-meter PH-3CU, refractometer Brix, titration equipment, bench-scale
biochemical reactor. The studies of the effect of biologically active substances (BAS) on the
digestion process have been performed using the vinasse resulted from the grains distillation
at the” Garma Grup” company (Hâncești, Republic of Moldova). Also, the other types of wastes
biomass have been taken for the research, such as wastes biomass from corn distillation.
Bench-scale technological experiments have been performed using the laboratory set-up in
which the nutrition mixture and various types of bioactive additives have been introduced.
The nutrition mixture has been prepared using 30 mL fresh grape juice with 10 % fermentation
yeast 1010 CFU/g), 20 mL inversed sugar (42 %), 150 mL vinasse and 2 mL of BAS (3 g/L).
The biomass mixed with the nutrition mixture was left for alcohol fermentation
under the mesophilic conditions (20-32oC). The digestion process was followed by the
volume of emitted gas (CO2) which replaced NaOH, determined by standard method (titration
with phenolphthalein). Composition and characteristics of initial vinasse used to study the
fermentation process in the presence of bioactive additives, is shown on Table 1 and 2.
Table 1
Composition of initial vinasse* [69, 70]
Corn Grain Barley
Component Rye vinasse
vinasse vinasse vinasse
1. Dry matter, % 8.5 4.2 26.0 8.0
2. Proteins (% of dry 25.5 34.8 31.3 42.4
matter)
3. Lipids (% of dry 11.7 2.2 10.2 3.5
matter)
4. Fibers (% of dry 10.6 3.4 13.7 5.9
matter)
5. Ash (% of dry matter) 4.7 8.6 2.1 3.5
* P≥0,95
Table 2
Physico-chemical indices of media study mediums
Indicator Vinasse Grape juice
1. Sugar content, g/L 26.27 ± 0.91 124. 4 ± 1.6
2. pH 3.91 ± 0.07 3.77± 0.12
3. Titratable acidity, g/L sulfuric acid 3.417± 0.241 2.74± 0.322
4. Contents in amine nitrogen, mg/L 492.2± 0.63 140.8± 1.2

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 Gh. Duca, O. Covaliova, E. Covaci, L. Romanciuc, C. Tașca 181

3. Results
Digestion process was studied with introduction of biologically active substances of
natural origin into the fermented biomass, which included the waste biomass and nutrition
mixture. As can be seen from Figure 1, additives of aecium and betuline suppress the CO2
emission, whereas using of tomatine ensures higher amount of gas evolved, or more
intensive fermentation process, as compared to the witness test.

Figure. 1. Kinetics of carbon dioxide (CO2) emission during the vinasse alcoholic
fermentation in the presence of 0,006 g additives /L.

Practical experiences have shown that introduction of sclareol accelerates the biomass
digestion, whereas addition of aescinum suppresses this process (Figure 2). Unlike these two
bioactive substances, sclareol at the first stages of digestion significantly suppresses the CO2
emission, and after 30 hours of fermentation, it makes this process somewhat more intensive
as compared to the witness test.

Figure. 2. Kinetics of the vinasse fermentation in the presence of additives of aescinum,

menthol and sclareol of 0.006 g /L biomass.

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182 Effect of bioactive additives on biomass fermentation from agro-industrial sector
At the same time, introduction into the alcohol fermentation of sclareol and
menthol in different amounts (0.003-0.012 g/L biomass) have shown that the amount
of additive introduced has no significant effect on the fermentation rate, although the
higher amounts (0.012 g/L) of both additives did not demonstrate higher efficiency; on
the opposite, the fermentation rate was lower as compared to first 3 addition (Figure
3). As compared to menthol, sclareol provokes more intensive fermentation at a much
lower concentration.

Figure. 3. Kinetics of the vinasse fermentation in the presence of sclareol and menthol
additions.
In the presence of dihydroxyfumaric acid the vinasse fermentation proceeds
somewhat more easily as compared to witness test, being approximately similar in case of
introduction of additive in various concentrations (0.1013 ÷ 0.4052∙10-6 mol/L), although
with the lesser amount of addition 0.1013∙10-6 mol/L the fermentation was accelerated
significantly (Figure 4).

Figure. 4. Reaction rate dynamics of the vinasse alcoholic fermentation in the presence
of dihydroxy fumaric acid addiction.

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 Gh. Duca, O. Covaliova, E. Covaci, L. Romanciuc, C. Tașca 183
In case of vanillin introduction into the fermented mixture, likewise, the fermentation
process was suppressed in case of introduction of higher amount of additive (0.19 ÷ 0.39 ∙10-3
mol/L), whereas the insignificant acceleration of carbon dioxide emission, as compared to
the witness test, was observed in case of the using of 0.098 mmol/L amount of vanillin
addition (Figure 5).

Figure. 5. Kinetics of the vinasse fermentation in the presence of vanillin additive.

Different amounts of catechin introduced in biomass have shown a difference in

carbon dioxide gas emission: smaller amounts of additive provoked the lower efficiency of
fermentation, and the higher concentration made the process more intensive as compared to
witness test (Figure 6).

Figure. 6. Kinetics of the vinasse fermentation in the presence of catechin additive.

The results obtained demonstrate that the substances of natural origin with bioactive /
antioxidant properties show the pronounced effects on the alcohol fermentation of vinasse
under the mesophilic conditions. The most efficient concentrations of studied additives are
summarized on Table 3.

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184 Effect of bioactive additives on biomass fermentation from agro-industrial sector

Table 3
Comparative efficiency of different types of additives of bioactive substances in
the vinasse fermentation process at concentration of 0,003 g/L biomass.
Bioactive substance used Total volume
Nr. Fermentation
as an additive to the of CO2 emitted
crt. time, h
fermented biomass gas, cm3
1. Dihydroxy fumaric acid 266.00 76
2. Aescinum 251.01 55
3. Tomatin 233.46 78
4. Sclareol 232.50 55
5. Vanillin 229.00 69
6. Catechin 180.00 61
7. Betuline 250.00 80
8. Menthol 200.00 70

The results demonstrate that introduction of higher compounds of additives into the
fermented biomass is not rational, as generally does not accelerate the fermentation
process. It can be suggested that the ability of studied additives to accelerate the
fermentation of liquid wastes from agro-industrial sector are connected with their molecular
structure and antioxidant, antihypoxant, antimutagen, etc. properties.

4. Conclusions
The study of the influence of additives of biologically active substances on waste
biomass fermentation from agro-industrial sector, along with the revealing of these
processes’ mechanisms can open a new perspective research direction in this area. This would
allow not only to manage the fermentation processes, accelerating or suppressing them for
the specific scopes, but also to obtain a series of value-added products under the more
favorable conditions, as well as to prevent the discharges of harmful wastes into the
environment. It was found that in case of tomatin application, higher amounts of emitted gas
were observed, whereas in case of menthol, dihydroxyfumaric acid, sclareol, vanillin the rate
of the gas emission was lower. At the same time, it became obvious that introduction of 2-4
times higher amounts of additives in many cases makes no sense as it does not provoke
further acceleration of alcoholic fermentation process.
Products of alcohol fermentation can have the added value in agriculture and adjacent
fields. Thus, carbon dioxide emitted during the biomass digestion can be used, for instance,
in the microalgae cultivation basins, which in their turn, could serve as a valuable feed for
poultry/cattle in zootechnical sector, while the water separated from solid fraction can be
used for technical scopes at the industries (cleaning machines and apparatuses, cleaning and
washing up the production halls and territory, etc.), or watering the plants in the city parks,
flower beds, etc. The solid fraction after the fermentation, with the condition of its controlled
composition, can be used as fertilizer for technical crops.
Acknowledgments: This research has been performed under the Moldova National
Research Project Nr. 20.80009.5007.04 “Physical-chemical redox processes with electron
transfer in the vital, technological and environmental processes”, running at Institute of
Chemistry & Technical University of Moldova, Department of Oenology and Chemistry.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Gh. Duca, O. Covaliova, E. Covaci, L. Romanciuc, C. Tașca 185
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Citation: Duca, Gh.; Covaliova, O.; Covaci, E.; Romanciuc, L.; Tașca, C. Effect of bioactive additives on
biomass fermentation from agro-industrial sector. Journal of Engineering Science 2022, 29 (3),
pp. 176-188. https://doi.org/10.52326/jes.utm.2022.29(3).15.

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Journal of Engineering Science September, 2022, Vol. XXIX (3)

Journal of Engineering Science Vol. XXIX, no. 3 (2022), pp. 189 - 195
Fascicle Food Engineering ISSN 2587-3474
Topic Biotechnologies, Food Chemistry and Food Safety eISSN 2587-3482

https://doi.org/10.52326/jes.utm.2022.29(3).16
UDC 667.275

SPECTRAL AND CHROMATOGRAPHIC CHARACTERISATION OF THE YELLOW

FOOD DYE FROM SAFFLOWER

Alexandra Savcenco*, ORCID: 0000-0002-1962-3959

Technical University of Moldova, 168, Stefan cel Mare Bd., MD-2004, Chisinau, Republic of Moldova
*Corresponding author: Alexandra Savcenco, [email protected]

Received: 05.23.2022
Accepted: 07.15.2022

Abstract. Recently, an increasingly trend of public concern for the food safety is observed.
Use of additives in food industry growing steadily. Present study deals with separation and
identification of compounds from Yellow Food Dye from Safflower (YFDS). Spectral and
chromatographic characteristics of YFDS were obtained and discussed. Dry powders and
solutions of YFDS were examined using Thin Layer Chromatography (TLC), UV-Vis
spectroscopy and reversed-phase HPLC. TLC was carried out in three systems I (HCl 0.1 M), II
(aqua 50%, ethanol 45%, citric acid 5%) and III (water, butan-1-ol, acetic acid). Spectral
determinations in the range of 200 to 600 nm were carried out at various pH values. HPLC
method was carried out by the gradient elution technique. Chromatographic method showed
that it is impossible to separate and to identify the components of the YFDS by paper
chromatography. UV-Vis Spectra demonstrated that the most successful interval for the
practical use of YFDS is in the pH range of pH = 4...5, since in this range the coloration activity
of dyes is maximal. HPLC method demonstrated that YFDS-compounds corresponds to the
composition of dry Safflower petals, which confirms its high biological activity. Powdered
yellow pigment from Safflower petals is containing natural chalcones and can be successfully
used in the dairy producing.

Keywords: Anhydrosafflower Yellow B, Chalcones, Hydroxisafflower Yellow A, Izosafflomin C,

Precarthamine, Safflomin C.

Rezumat. Actualmente se observă o creștere din ce în ce mai mare a îngrijorării

consumatorilor față de siguranța alimentelor consumate. Utilizarea aditivilor în industria
alimentară este în continuă creștere. Studiile în acest domeniu demonstrează, că apar noi
aspecte ale toxicității coloranților sintetici. În studiul de față, s-a efectuat separarea și
identificarea compușilor din amestecul de compuși a colorantului galben alimentar din
șofrănel (YFDS). Au fost testate caracteristicile spectrale și cromatografice ale YFDS.
Pulberile uscate și soluțiile de YFDS au fost studiate, utilizând cromatografia în strat subțire
(TLC), spectroscopia UV-Vis și HPLC cu fază inversă. TLC a fost efectuat în trei sisteme I (HCI
0,1 M), II (aqua 50%, etanol 45%, acid citric 5%) și III (apă, butan-1-ol, acid acetic).
Determinările spectrale s-au efectuat în intervalul de la 200 la 600 nm la diferite valori a pH-
ului. Metoda HPLC a fost efectuată prin tehnica de eluare cu gradient. Metoda cromatografică

Journal of Engineering Science September, 2022, Vol. XXIX (3)

190 A. Savcenco

a arătat că este imposibil de separat și de identificat componentele YFDS prin cromatografie

pe hârtie. Spectroscopia UV-Vis a demonstrat că intervalul cel mai de succes pentru utilizarea
practică a YFDS este în intervalul de pH de la 4 la 5, deoarece în acest interval activitatea de
colorare a coloranților este maximă. Metoda HPLC a demonstrat că compușii YFDS corespund
compoziției petalelor uscate de șofrănel, ceea ce confirmă activitatea sa biologică ridicată.
Pigmentul galben sub formă de pulbere din petalele de șofrănel conține chalconi naturali și
poate fi utilizat cu succes în fabricarea produselor lactate.

Cuvinte cheie: Anhidrosafflora Galben B, Chalcone, Hydroxisaflomină Galben A, Izosaflomină C,

Precartamină, Safflomină C.

1. Introduction
Consumers striving for naturalness choose a food product not only in appearance, but
also in composition, rightly considering this factor to be extremely important. The existing
demand for partial or complete abandonment of synthetic dyes in food products is expressed
by a decrease in the growth rate of the production of synthetic dyes, and an increase in the
production of natural ones [1]. At the same time, existing natural sources of food colors are
already actively exploited, and they are clearly insufficient. Therefore, in order to effectively
replace of the synthetic dyes with natural ones, it is necessary to found new and suitable
sources of the latter.
The perspective plant which can be used as a source of food colours is Safflower (Carthamus
tinctorius L.) [2]. Safflower seeds are an important sourse for extracting oil in Asia, North and
Central America [3]. Safflower florets are widely used in cosmetics, modern and popular
medicine [4]. By Safflower petals extraction it can be obtained dyes of two colors: yellow and
red [5]. According to the chimical structure, the dyes represent different chalcones [6].
There are many reasons, which causes confusions in the taxonomy of the sources of
raw materials and/or of the compounds, obtained from these sources. Safflower (Carthamus
tinctorius L., Asteraceae) is often confused in Internet, also in traditional printed scientific
sources, with consonant Saffron (Crocus sativus L., Iridaceae) [7]. Due to this confusion,
Carthamin is considered a dye, extracted from Saffron. But Saffron does not include red
dimeric chalcone Carthamin in composition: red compounds of Saffron are anthocyanins [8].
Instead of correct “Safflower Yellow”, a mistakeous name “Carthamin Yellow” is used in some
research papers [9], but in commerce and Internet especially. So, “Carthamin Yellow” is not a
compound, instead of the correct name, which is not Carthamin (red) but this a yellow dye
derived from Safflower. The Yellow Precarthamin is the biochemical precursor of Red
Carthamin. Precartamin is enzymatically converted to Red Carthamin both in vivo and in vitro
[10]. In the strong acid environment, red Carthamin isomerizes to yellow Izocarthamin [11].
Main goal of this paper is to stable the physico-chemical properties of powered yellow colour
from Safflower petals, growned in Republic of Moldova, in order to its utilisation in food
industry.

2. Materials and Methods

Safflower petals. Safflower was grown in the experimental fields of the Institute of
Genetics and Plant Protection, Chisinau, Moldova. The petals were collected manually. The
green sepals and light gray (almost white) seeds were carefully separated from the petals.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

 Spectral and chromatographic characterisation of the Yellow Food Dye from Safflower 191
Purified petals were dryed in the dark to an absolute humidity of no more than 5% and were
stored in an airtight container.
Solvents. Food grade ethanol 96% (v/v) (“Kvint” distillery, Moldova), freshly prepared
bidistillate, acetic acid purum (“Severodonetsk Azot Association”, Ukraine) and HPLC-grade
acetonitrile, n-butanol and methanol (“Merck KGaA”, Germany) were used for
spectrophotometric and chromatographic analysis.
Separation of the Yellow Food Dye from Safflower (YFDS). Dried safflower petals were
treated with a sodium carbonate solution with a hydromodule of 1:10 at a temperature of
18…20°С. The resulting mixture was pressed in four steps to give a yellow extract. This
solution was centrifuged for 10 minutes at 6000 rpm. Yellow liquid solution, which remained
after the carthamine was removed [12], was purified with activated carbon and cellulose 1
gram per liter for 10 minutes. After filtration, solution was evaporated in a rotary evaporator
at 60-75°C, with speed of 150-210 rpm, under pressure 60-100 mbar. In obtained dark-brown
viscous solution were added 3 volumes of ethyl alcohol and intensely mixed to obtain very
viscous mass, which was dried in vacuum at 65-80 °C and 80-100 mbar. The dry mass of YFDS
constituting 40 % of dry petal mass.
Thin Layer Chromatography (TLC). Chromatograms were obtained in vertical camera on
24×3cm sheets of Whatman Chromatographic Paper, by ascension technique. Three
chromatographic systems with different polarity were used as liquid mobile phases: System I –
acidic medium (HCl 0.10 mol/L); System II – (50% distilled water, 45% ethanol, 5% citric
acid); System III – (4 parts distilled water, 5 parts butan-1-ol, 1 part acetic acid).
UV-Vis spectra. Standard solution of YFDS was prepared by dissolving of 0.2 g of
powder in 200mL distilled water (Solution P1). For farther directly spectroscopic
measurements, Solution P1 was diluted 5.0 times and adjusted to different pH value by
adding crystals of sodium carbonate and citric acid. Distilled water was used as a reference
sample. Spectra of Safflower extracts were recorded at Hach-Lange “DR 5000”
spectrophotometer in the range of 200...600 nm, step of 1 nm, using quartz cell with l = 10mm.
Photodiode Array (PDA) coupled HPLC. Shimadzu “Provinience-i LC-2030C 3D-Plus”,
with integrated Photodiode Array Detector (PDA), on reversed-phase C18 column
“Phenomenex” (4.6x150mm, particle size 4µm, pores 80nm), gradient elution technique by
two mobile phases: Water, containing 0.1% (v) Acetic Acid (Phase A) and Acetonitrile
containing 0.1% (v) Acetic Acid (Phase B) were used. Default flow: Phase B 5% at the constant
rate of 0.8 mL/min. Constant oven and detection cell temperatures of 30 °C. Elution gradient
program: 0...2 min – Phase B 5% (default flow); 2...18 min – Phase B from 5% to 40%; 18...20
min – Phase B from 40% to 90%; 20...24 min – Phase B 90%; 24...25 min - Phase B from 90%
to 5%; 25-40 min – Phase B 5% (default flow). Data acquisitions and interpretations were
performed using Shimadzu LabSolutions software.
3. Results and Discussion
3.1. TLC of red and yellow Safflower dyes
Investigations of the chromatography conditions of the Yellow Food Dye from
Safflower (YFDS) and Cartamine dyes were performed using three chromatography systems,
Table 1. Most acid System I (HCl 0.1 mol/L) confirms the instability of the Carthamin in
the environment with pH = 1.00 [11]. Chromatographic systems II and III demonstrated
the effective separation of Carthamine from yellow dyes. At the same time, we failed to
separate the components of yellow dyes by paper chromatography.

Journal of Engineering Science September, 2022, Vol. XXIX (3)

192 A. Savcenco

Table 1
Thin Layer Chromatography of the Safflower Pigments
System I II III, superior layer
Aqua, 50% (v) Water, 4 parts (v)
HCl
Composition Ethanol, 45% (v) Butan-1-ol, 5 parts (v)
0.1 mol∙L-1
Citric Acid, 5% (m) Acetic Acid, 1 part (v)

View

Rf (Yellow) 0.51 ± 0.05 0.71 ± 0.05 0.35 ± 0.05

Rf (Crt) 0.00 0.03 ± 0.02 0.03± 0.02
*Spotted consecutively: 1 - Safflower extract; 2 - YFDS; 3 - Carthamin

Thus, to obtain a bright yellow (and not orange) YFDS, it is necessary to treat the
extract with a suspension of microcrystalline cellulose.
3.2. UV-Vis Spectroscopy and pH-sensitivity of YFDS
Prepared samples of solutions with different pH values were spectrophotometrically,
and two diagrams were built from the obtained spectra. The spectra were processed using
the Excel program.
The UV-Vis spectra of the yellow dye in Safflower were analysed as a function of pH
(Figure 1). Almost all curves have the same shape with maximum wavelengths between 392
nm and 412 nm and the presence of the left shoulder. The spectra, obtained at acidic (5.10)
and basic (10.95) pH values show an obvious deviation. The maximum absorption of the
yellow pigment solutions takes place in an acid medium (2.12) with a peak wavelength of
405 nm. From the analysis of the spectra of the liquid yellow dye at different pH, it follows
that a change in pH causes a shift in the absorption maxima of the dyes. This is clearly seen
in the graphs λmax = f (pH). The most successful interval for the practical use of dyes is the
pH range = 4...5, since in this range the absorption of dyes is maximum and color of the
solutions is bright yellow.

Figure 1. Spectra of YFDS, Figure 2. YFDS absorbtion maximum,

pH function. pH function.
Journal of Engineering Science September, 2022, Vol. XXIX (3)
 Spectral and chromatographic characterisation of the Yellow Food Dye from Safflower 193
Thus, despite the removal of the Cartamine, highly sensitive to pH, YFDS does not
completely lose sensitivity to the pH value. At the same time, minor changes in the position
of the absorption maximum, 394-405 nm (Figure 2), cannot significantly affect color
perception, which means that YFDS can be successfully used over a wide pH range.

3.3. HPLC profile of Safflower petals extract and YFDS

HPLC profile of Safflower petals and YFDS were analysed using the same method. The
HPLC results (Figure 3) show the five separate peaks were at the retention times of 18.861,
19.589, 20.844, 22.273, 24.398 in YFDS extract, what corresponded to the peaks and
retention time in petals extract. The peaks show the clear separation of yellow compounds
and identification of Safflomin C, Izosafflomin C, HSYA, AHSYB and Precarthamin. This fact
that the composition of the YFDS, obtained from Safflower petals correspond the composition
of the petals, known for its biological activity [13], suggests that the YFDS can be used as a
natural food yellow colorant, which can be successfully in the production of dairy products [14-16].

Figure 3. Multichromatogram UV-Vis = f (Time), and ordinary chromatogram at 404nm.

Table 2
Chromatographic data for yellow compounds from Safflower petals and YFDS
RT Area λmax
Peak No. Area Identification
(min) (%) (nm)
Safflower Petals Extract
1 18.62 263361 2.3 218, 332, 406 Safflomin C
2 19.40 241525 2.2 216, 315, 404 Izosafflomin C
3 223, 335sh,
20.63 8997460 80.1 HSYA
402
4 219, 335sh,
22.32 628858 5.6 AHSYB
410
5 24.67 1098554 9.8 335sh, 407 Precarthamin

Journal of Engineering Science September, 2022, Vol. XXIX (3)

194 A. Savcenco

Continuation Table 2
Yellow Food Dye from Safflower
1 18.86 394512 8.1 215, 332, 408 Safflomin C
2 19.59 313120 6.4 216, 327, 408 Izosafflomin C
3 220, 335sh,
20.84 2410258 49.5 HSYA
402
4 218, 335sh,
22.27 594323 12.2 AHSYB
412
5 24.39 1159907 23.8 335sh, 408 Precarthamin
The UV-Vis spectra clearly seen that the mixture of dyes is yellow in colour (Figure 1),
however, the presence of which yellow components in the mixture are most present, is
impossible to identify using spectroscopy method. Thanks to 3D chromatogram, it was
possible to establish that the largest amount of yellow colour in YFDS is accounted for by
HSYA (RT = 20.84, Figure 4a). Precarthamin (RT = 24.39), AHSYB, Safflomin C and Isosafflomin
C also give yellow colour, in correspondingly decreasing order (Figure 4b).

a) b)
Figure 4. YFDS 3D-chromatogram: a) at 140 mAU resolution; b) at 80 mAU resolution.
4. Conclusions
Five yellow dyes of the chalcone class with a similar chromophore structure were
confirmed in the Safflower petals extract and in the powdered pigment which was obtained
at the concentration of this extract.
Essential condition to obtain bright yelloe colour, is the absence of traces of red
carthamine, which is will achive by treatment of Safflower extract with cellulose.
The separation of yellow substances into individual components is not advisable, since
they have similar UV-Vis absorption spectra, and hence the colour. Therefore, there is no need
to separate the yellow powder into individual components for its further use in the food
industry.
Acknowledgements. This work was funded by the State Project 20.80009.5107.09
“Improving of food quality and safety through biotechnology and food engineering”, running
at Technical University of Moldova.
Conflicts of Interest. The authors declare no conflict of interest.
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Citation: Savcenco, A. Spectral and chromatographic characterisation of the yellow food dye from
safflower. Journal of Engineering Science 2022, 29 (3), pp. 189-195.
https://doi.org/10.52326/jes.utm.2022.29(3).16.

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