Applsci 11 05642 v2

applied
sciences
Article
Research on Testing Method of Oil Characteristic Based on
Quartz Tuning Fork Sensor
Hao Sun 1 , Yingshuai Liu 1,2,3, * and Jianwei Tan 3
1 School of Intelligent Manufacturing, Weifang University of Science and Technology, Weifang 262700, China;
sunhao21@126.com
2 School of Mechanical Engineering, Shandong University, Jinan 250061, China
3 National Lab of Auto Performance and Emission Test, School of Mechanical and Vehicular Engineering,
Beijing Institute of Technology, Beijing 100081, China; tanjianwei@bit.edu.cn
* Correspondence: liuyingshuai1983@163.com
Abstract: There is increasing demand for the on-board diagnosis of lubricating oils. In this research,
we consider various sensor principles for on-board diagnosis of the thermal aging of engine oils. One
of the parameters investigated is the viscosity of the lubricating oil, which can be efficiently measured
using a microacoustic sensor. Compared with conventional viscometers, these sensors probe a
different rheological domain, which needs to be considered in the interpretation of measurement
results. This specific behavior is examined by systematically investigating engine oils, with and
without additive packages, that were subjected to a defined artificial aging process. This paper
presents design strategies for the algorithm developed and applied for direct on-board diagnosis
of engine oil conditions with a fluid property sensor; this enables prediction of remaining oil life
and optimization of oil change intervals, thereby minimizing the likelihood of dramatic engine
failure and reducing maintenance costs. After a general description of the principles of sensor
measurement, different engine oil contaminants, aging phenomena, and associated sensor detection
Citation: Sun, H.; Liu, Y.; Tan, J. and measurement capabilities are discussed.
Research on Testing Method of Oil
Characteristic Based on Quartz Keywords: heavy-duty engines; property sensor; lubricating oil; fluid property
Tuning Fork Sensor. Appl. Sci. 2021,
11, 5642. https://doi.org/10.3390/
app11125642
1. Introduction
Academic Editor: Guangdong Tian
Lubricating oil in an internal diesel engine is exposed to various strains that depend
on operating conditions, fuel quality, ambient conditions, and operating parameters. The
Received: 24 May 2021
rate of deterioration strongly depends on these influences. To avoid engine failure, the
Accepted: 16 June 2021
Published: 18 June 2021
oil must be changed before it loses its protective properties. However, an unnecessary oil
change should be avoided for environmental and economic reasons. To reliably determine
Publisher’s Note: MDPI stays neutral
the optimum oil change interval, it is necessary to monitor the actual physical and chemical
with regard to jurisdictional claims in
conditions of the oil [1,2].
published maps and institutional affil- The aging process of the oil is very much influenced by, among other things, fuel
iations. quality, because of the blow-by gases of the combustion process [3,4]. Therefore, especially
for gas engines fueled with biogas of a priori unknown and fluctuating fuel quality, direct
monitoring of the oil condition is essential [5].
According to the current state-of-the-art for automotive applications, the condition
of engine oil is estimated by means of indirect methods that mainly rely on operating
Copyright: © 2021 by the authors.
Licensee MDPI, Basel, Switzerland.
parameters, such as engine speed, performance, and temperature [6].
This article is an open access article
For large-scale stationary engines, a more reliable, but also more elaborate approach
distributed under the terms and
is currently used, in which oil samples are taken at regular intervals for off-line labora-
conditions of the Creative Commons tory analysis to determine the optimal oil change interval [7,8]. The disadvantages of
Attribution (CC BY) license (https:// this method are high fixed costs and the delay between sample drawing and return of
creativecommons.org/licenses/by/ analysis results.
4.0/).
Appl. Sci. 2021, 11, 5642. https://doi.org/10.3390/app11125642 https://www.mdpi.com/journal/applsci

Currently developed alternative approaches are aimed at utilizing sensors to
Appl. Sci. 2021, 11, 5642
input for on-board diagnosis systems that determine the current oil 2condition of 29
i
engine. The sensor signals should provide information on the actual physical an
cal oil quality to provide the information needed for the prediction algorithms, a
Currently developed alternative approaches are aimed at utilizing sensors to provide
ininput
Figure 1. Moreover,
for on-board thesystems
diagnosis sensorsthatshould
determine exhibit a long
the current lifetime,inside
oil condition evenanthough
continuously exposed
engine. The sensor signalsto an aggressive
should environment
provide information inside
on the actual an operating
physical and chemicalcombu
oil quality
gine [9,10].toThe
provide thesystem
entire information needed
should givefor athe prediction
reliable algorithms,
indication ofasthe
shown in oil c
current
Figure 1. Moreover, the sensors should exhibit a long lifetime, even though they are contin-
and estimate when the oil will reach the end of its lifetime and an oil change wil
uously exposed to an aggressive environment inside an operating combustion engine [9,10].
essary.
The entire system should give a reliable indication of the current oil condition and estimate
when the oil will reach the end of its lifetime and an oil change will be necessary.
Figure 1. Structure of a sensor-assisted algorithm for a lubrication-monitoring system. The indirect

Figure 1. Structure
data provided of a sensor-assisted
by the engine algorithm
management system for a lubrication-monitoring
and its relationship to oil wear will depend onsystem.
the Th
data provided
actual by the used,
engine platform engine management
whereas system
the data provided byand its relationship
the sensors to oil to
are directly linked wear will depe
the oil
actual engine
condition and platform used, whereas the data provided by the sensors are directly linked
are thus platform-independent.
condition and are thus platform-independent.
Previous attempts in the automotive field were based on measuring the permittivity
or conductivity of the oil [11].
Previous
Although attempts in theare
these parameters automotive field were
measured directly based
in the oil, theyon are measuring
of limited usethe per
orbecause
conductivity of the oilby[11].
they are influenced many different oil wear mechanisms; this results in a signal
thatAlthough
is of only limited
these utility. There have
parameters also been attempts
are measured directly to sense
in the a representative
oil, they are of lim
chemical parameter directly, but chemical sensors commonly exhibit a limited lifetime and
because they are influenced by many different oil wear mechanisms; this results in
show adverse properties with respect to aging and drift [12–14].
that isMonitoring
of only limited
of internalutility. There
engine oil have
condition also
with been
a fluid attempts
property sensorto sense a repres
definitively
chemical
simplifiesparameter directly, but
oil quality management chemicala higher
by providing sensors commonly
capacity exhibit
for detection a limited
of slow
and rapid changes in oil contamination or quality levels,
and show adverse properties with respect to aging and drift [12–14].thereby enabling economical and
environmentally friendly optimization of oil change intervals [15,16].
Monitoring of internal engine oil condition with a fluid property sensor def
Waszczuk et al. [17] adopted the low frequency commercial piezoelectric tuning forks
simplifies oilmeasurement
(QTFs) to the quality management by providing
of physicochemical properties of aliquids,
higher andcapacity for detection
the result showed
and rapid
that changes
the applied in oil contamination
measurement technique based or quality levels,ofthereby
on the analysis the QTFenabling
equivalenteconom
environmentally friendly optimization of oil change intervals [15,16]. up to
electric circuit proved its usefulness for determining liquid viscosity in the range
16 cP. Gonzalez et al. [18] researched a novel sensor system for downhole measurements
Waszczuk
of viscosity, et and
density, al. other
[17] fluid
adopted the low
properties. frequency
Gonzalez et al. [19] commercial
demonstrated the piezoelectri
use
forks
of a (QTFs)
tuning forkto sensor
the measurement ofand
for fast viscosity physicochemical
density measurements properties
that wouldof liquids,
enable and t
the characterization
showed of transient
that the applied fluid properties,
measurement such as in
technique multiphase
based on the flows of liquids.
analysis of the QT
The result showed that by monitoring the frequency and the decay rate during ring-down,
alent electric circuit proved its usefulness for determining liquid viscosity in the r
to 16 cP. Gonzalez et al. [18] researched a novel sensor system for downhole m
ments of viscosity, density, and other fluid properties. Gonzalez et al. [19] demo
the use of a tuning fork sensor for fast viscosity and density measurements tha
the smart probe. Finite element analysis was conducted with COMS
theoretical calculation and lab tests were carried out to verify and eva
results. Ghader et al. [21] studied a novel microelectromechanical sen
Appl. Sci. 2021, 11, 5642 measurement of fluids viscosity and density. 3 of 29
Although this paper demonstrates the feasibility of an oil cond
models and analyses are highly dependent on oil type and applica
transient changes in density and viscosity could be obtained within milliseconds in liquids.
Specific studies should be performed with each application before im
Zhang et al. [20] presented a smart sensing system for viscosity and density measurement of
to adapt
viscous and
fluids. optimize
Using the PMN-PTthe described
transducer, models
the measured [22].and density of fluids
viscosity
were extracted by analyzing the vibrational properties of the smart probe. Finite element
analysis was conducted with COMSOL Multiphysics for theoretical calculation and lab
2. Fluid
tests Property
were carried out toSensing
verify and evaluate the simulation results. Ghader et al. [21]
studied a novel microelectromechanical sensor for simultaneous measurement of fluids
2.1. Fluid Property Sensor
viscosity and density.
Although
A physicalthis paper demonstrates
diagram the feasibility
of the of an oil condition
fluid property sensoralgorithm,
is shown the in Fig
models and analyses are highly dependent on oil type and application characteristics.
ment parameters
Specific studies should beof the fluid
performed property
with each sensor
application are shownsoinas Table
before implementation to 1
sensor directly and simultaneously measures the viscosity, density
adapt and optimize the described models [22].
and temperature
2. Fluid Property Sensing of nonconductive fluids. Relying on patented tuni
2.1. Fluid Property Sensor
the sensor monitors the direct and dynamic relationship between mu
A physical diagram of the fluid property sensor is shown in Figure 2. The measure-
erties to determine the quality, condition and contaminant loading of f
ment parameters of the fluid property sensor are shown in Table 1. The fluid property
oil,
sensorfuel, transmission
directly andmeasures
and simultaneously brakethe fluids, hydraulic
viscosity, and constant,
density, dielectric gear oils,
and refrig
temperature
The capacityof nonconductive fluids. Relyinganalysis
for multiparametric on patented tuning fork fluid
improves technology, the
characteriza
sensor monitors the direct and dynamic relationship between multiple physical properties
fluid property
to determine sensor
the quality, provides
condition in-lineloading
and contaminant monitoring of fluids
of fluids such for
as engine oil,a wid
fuel, transmissioninstallations,
aftermarket and brake fluids, including
hydraulic andfluid
gear oils, refrigerants, process
reservoirs, and solvents.
lines an
The capacity for multiparametric analysis improves fluid characterization algorithms. The
flow conduits
fluid property sensor(e.g., engine
provides oil gallery)
in-line monitoring andforfor
of fluids applications
a wide range of OEM that
and inclu
vehicles, compressors,
aftermarket installations, industrial
including equipment
fluid reservoirs, process linesand
andturbines. This pap
pressurized high
flow conduits (e.g., engine oil gallery) and for applications that include on- and off-road
pally
vehicles,on engine industrial
compressors, oil applications,
equipment andbut most
turbines. Thisofpaper
these
will analyses can be a
focus principally
for otheroilapplications
on engine applications, but[23,24].
most of these analyses can be adapted or replicated for
other applications [23,24].
Figure 2. Physical view of quartz tuning fork sensor.

Figure 2. Physical view of quartz tuning fork sensor.
Table 1. Measurement parameters of the sensor.
Measurement Parameter Measurement Range Precision

Viscosity 0.5–50 cP ±2%
Density 0.65–1.5 g/cm3 ±1%
Appl. Sci. 2021, 11, 5642 4 of 29
Table 1. Measurement parameters of the sensor.
. Sci. 2021, 11, x FOR PEER REVIEW Measurement Parameter Measurement Range Precision Resolution Ratio 4
Viscosity 0.5–50 cP ±2% 0.015625 cP
Density 0.65–1.5 g/cm3 ±1% 0.00003052 g/cm3
Dielectric constant 1.0–6.0 ±1% 0.00012207
◦C ◦C
The Temperature
hardware circuit − 40–150
design of this paper 0.1
consists of parts,◦an
two 0.03125 C STM32F10
crocontroller system control circuit and impedance measurement circuit based on AD

impedance Themeasurement
hardware circuit design
chip. ofThethishardware
paper consists of two parts,
structure an STM32F103
of the system ismicro-
shown in F
controller system control circuit and impedance measurement circuit based on AD5933
3. The AD5933measurement
impedance chip is integrated
chip. Thewith a DDS
hardware frequency
structure generator,
of the system I–V
is shown amplifier,
in Figure 3. low
filterThe
circuit,
AD5933A/D conversion
chip is integratedcircuit, andfrequency
with a DDS FFT module, which
generator, I–V can realize
amplifier, impedance
low-pass
urements based on the vector current–voltage method in a high integration
filter circuit, A/D conversion circuit, and FFT module, which can realize impedance mea-environ
surements based on the vector current–voltage method in a high integration environment
with certain accuracy. The chip realizes data communication through the I2C interfac
with certain accuracy. The chip realizes data communication through the I2 C interface.The
hardware
hardware structure
structureofof the system
the system is designed
is designed as follows:
as follows:
Figure
Figure 3. Design
3. Design of ofhardware
hardware circuit
circuitof of
thethe
measurement system.system.
measurement
The peripheral circuit design of AD5933 is shown in Figure 4. The chip is powered
The
by peripheral
a 5-V circuit
power supply. Thedesign
SCL and ofSDA
AD5933
pins ofisthe
shown in Figure
microcontroller are4.used
Theaschip
I2 C is pow
by a communication
5-V power supply.pins and areThe connected
SCL and to the 15 and
SDA 16 pins
pins of of
thethemicrocontroller
AD5933 chip through area used
pull resistance of 10 kΩ. The AVDD and AGND of the analog circuit are directly connected
communication pins and are connected to the 15 and 16 pins of the AD5933 chip thr
with the VCC and GND, while the AVDD and DGND of the digital circuit are connected
a pull resistance
with the VCC andof GND
10 kΩ. by aThe
10-uHAVDD and AGND
chip inductor, of the
respectively, analog
to realize thecircuit
separationareofdirectly
nectedthe with
analogthe
and VCC
digital and GND,
circuits. while
The input andthe AVDD
output ends ofand DGND
the quartz of the
tuning digital circu
fork sensor
are, respectively, connected to the VOUT, RFB and VINT pins of
connected with the VCC and GND by a 10-uH chip inductor, respectively, to realiz the AD5933 chip through
the connectors; VOUT is the excitation voltage signal output, RFB is the external feedback
separation of the analog and digital circuits. The input and output ends of the quart
resistance, and VINT is the transconductance amplifier input. Because the component to be
ing fork
testedsensor are,
is a quartz respectively,
crystal oscillator, its connected
impedance is to theso VOUT,
large, RFB and
it is not necessary VINT pins o
to increase
AD5933 chip through
the external the connectors;
amplifier circuit to improve theVOUT is theand
load capacity, excitation
the outputvoltage
end of thesignal
chip is output
directly connected to the crystal oscillator, the measurement can be
is the external feedback resistance, and VINT is the transconductance amplifier inpu realized.
cause the component to be tested is a quartz crystal oscillator, its impedance is large
is not necessary to increase the external amplifier circuit to improve the load capacity
the output end of the chip is directly connected to the crystal oscillator, the measure
can be realized.
is the external feedback resistance, and VINT is the transconductance amplifier input. Be-
cause the component to be tested is a quartz crystal oscillator, its impedance is large, so it
is not necessary to increase the external amplifier circuit to improve the load capacity, and
the2021,
Appl. Sci. output
11, 5642 end of the chip is directly connected to the crystal oscillator, the measurement
5 of 29
can be realized.
Appl. Sci. 2021, 11, x FOR PEER REVIEW 5 of 28
Figure 4. AD5933 peripheral circuit

Figure diagram.
4. AD5933 peripheral circuit diagram.
The fluid property sensor measurement is based on a tuning fork flexural resonator.
2.2. resonator
This Measurement Principle of quartz, a piezoelectric material capable of being deformed
is composed
2.2. Measurement Principle
upon The fluid property
the application of asensor
voltagemeasurement is based
and reciprocally on a tuning
electrically fork flexural
polarized under resonator.
the action
This resonator is composed of quartz, a piezoelectric material capable of
of mechanical stress. The two tines of the fork oscillate and generate a response indicative being deformed
ofupon
the the application of aand
physicochemical voltage and reciprocally
electrical properties electrically
of the fluid polarized
in which under the action
the sensor of
is im-
mechanical
mersed. stress. The two tines of the fork oscillate and generate a response indicative of
the physicochemical and electrical
A sinusoidal excitation voltageproperties
applied of tothe
thefluid in which
tuning fork’sthe sensor
thin is immersed.
electrodes causes
A sinusoidal
mechanical excitation
stress and voltage
periodic elasticapplied to the tuning
deformation. fork’s thin
This vibration electrodes
produces causes me-
a correspond-
chanical stress and periodic elastic deformation. This vibration produces a corresponding
ing current through the electrodes. The ratio of the excitation voltage to the induced cur-
current through the electrodes. The ratio of the excitation voltage to the induced current
rent allows measurement of the impedance of the system, and this process will be depend-
allows measurement of the impedance of the system, and this process will be dependent
ent on the excitation frequency, the elastic properties of the piezoelectric material, and the
on the excitation frequency, the elastic properties of the piezoelectric material, and the
properties of the fluid. The quartz tuning fork impedance response in air has a sharp res-
properties of the fluid. The quartz tuning fork impedance response in air has a sharp
onance at approximately 31 kHz. In a fluid, the resonance frequency and amplitude are
resonance at approximately 31 kHz. In a fluid, the resonance frequency and amplitude are
reduced
reducedduedueto tothe
theincreased
increased mass
mass load and frictional
load and frictional forces
forcesininthe
thesystem
system[25,26].
[25,26].
As
Asdescribed
described in Figure5,5,the
in Figure thecalculation
calculationofof thethe fluid
fluid properties
properties is allowed
is allowed through
through the
the use of a tuning fork equivalent electrical
use of a tuning fork equivalent electrical model. model.
Figure
Figure5.5.Tuning
Tuningfork
fork equivalent
equivalent electrical model.
The tuning fork complex impedance in air is modeled using the following formula:
1
Z ω = R ∕∕ C ∕∕ R + iωL + (1)
iωC
Serial capacitance (Cs), resistance (R0) and inductance (L0) depend only on geomet-
Appl. Sci. 2021, 11, 5642 6 of 29
The tuning fork complex impedance in air is modeled using the following formula:

1
ZTF (ω) = RP //CP // R0 + iωL0 + (1)
iωCs
Serial capacitance (Cs ), resistance (R0 ) and inductance (L0 ) depend only on geometrical
tuning fork parameters. Fluid impact is described by an additional term:
√
Z(ω) = A i ω ρ + B ω ρ η ( 1 + i ) (2)
where ω is the excitation frequency, η is the dynamic viscosity, ρ is the density, and A and
B are constants that depend on the resonator geometry [27].
The dielectric constant ε and the electrical resistivity P are measured with the parallel
capacitance (Cp ) and resistance (Rp ) [28,29]:
∂CP
CP ( ε ) = ( ε − 1 ) + CP yaccum (3)
∂ε
∂(RP )
RP (P) = P (4)
∂P
After a calibration step required to calculate each parameter, the fluid property sensor
is used to measure the dynamic viscosity, density, dielectric constant, and Rp, an indication
of resistivity, of the unknown fluid in which it is immersed.
For measuring the density “ρ”, the principle is that when the quartz tuning fork is
immersed in the oil medium, its surface that is attached to the oil medium experiences
effective mass changes, resulting in a reduction in resonance frequency; the use of density
and effective mass of the relationship can be realized to measure the density of the oil
medium. The principle of measuring viscosity (η) is that when the quartz tuning fork
is used as the sensitive element, the impedance characteristics of its equivalent circuit
will change due to the influence of viscosity. The purpose of online viscosity monitoring
can be achieved by real-time monitoring of impedance. The measured temperature (T)
is measured using a resistance temperature detector (RTD). The dielectric constant (ε) is
calculated from the temperature measured by the RTD and the oil-related constant. The
resistivity of a medium, P, refers to the resistance encountered by free carriers when moving
in the medium under the action of an electric field. The resistivity of the oil depends on
the viscosity of the fluid, the density of free charge carriers, and the specific chemical
composition of the oil. Resistivity (P) can be modeled in a simple linear form: P = H + I.T,
where T is the temperature measured by the RTD, and H and I are constants related to oil.
2.3. Engine Oil

Engine oils are composed of paraffinic, naphthenic, and aromatic hydrocarbons mixed
with different additives and elaborated to fulfill several functions: lubrication, sealing,
power transmission, engine part cooling, cleaning, and neutralization of acid components.
The objective of lubrication is to reduce the friction between sliding surfaces and
minimize wear. Insufficient lubrication leads to engine heating, oil degradation, and
acceleration and higher risk of engine failures. Sealing between cylinders and piston rings
is necessary to avoid blow-by fuel contamination and nitrogen oxide contamination from
the combustion gas [30]. Sealing is also required between the valve and valve stem guides
to prevent unburned fuel from reaching the oil. Power transmission increases engine
efficiency and ensures tappet clearance and camshaft adjustment.
Appl. Sci. 2021, 11, 5642 7 of 29
Proper lubrication, sealing, and power transmission are ensured by appropriate

oil viscosity.
The viscosity of a fluid is a measure of its resistance to gradual deformation by shear
stress. Dynamic viscosity can be defined by considering a fluid trapped between a fixed
plate and a second plate moving at a velocity (u).
The friction between each fluid layer of area A leads to a force (F) resisting the
relative motion.
∂u
F = η.A. (5)
∂y
Dynamic viscosity η is the proportionality factor relating F and the local shear velocity
∂u
∂y .Viscosity can also be expressed in other forms such as through kinematic viscosity
µ (cSt), which is the ratio of dynamic viscosity η (cP) to density ρ (gm/cc) of the fluid.
Viscosity is closely linked to the fluid temperature.
Kinematic viscosity µ (T) can be modeled with the following expression:
log(log µ + 0.7) = B − C. log(T + 273.15) (6)
where T is the temperature in ◦ C, log is the base 10 log, and B and C are oil-dependent constants.
Density (ρ) can be modeled in a simple linear form:
ρ = D + E.T (7)
where D and E are oil dependent constants. Dynamic viscosity η (T) can be deduced from
kinematic viscosity µ (T) and density ρ (T).
Base oil viscosity has a naturally high temperature dependence and is characteristically
low [31]. To ensure efficient engine performance, oil viscosity should be sufficiently high at
high temperature but not thick enough at low temperature to prevent easy engine start-up.
To increase the viscosity index (VI), engine oils contain additives designed to improve
the VI and these are composed of long–chained hydrocarbon polymers tightly folded
at low temperatures and unfolded at high temperatures. Lubrication is also improved
by anti-wear additives, which prevent friction between metallic surfaces during extreme
operating conditions. Zinc dithiophosphate (ZDP) is an example of an anti-wear agent.
Incorrect sealing can lead to functional deficiency or foam formation. Foam inhibitor
additives containing silicon compounds prevent formation of stable oil foams and improve
air removal ability [32–34].
Oil cleaning is ensured by two types of additives: dispersants and detergents.
A dispersant is composed of a long, nonpolar oleophilic tail and a polar head. The
function of the dispersant is to maintain solid or liquid contamination particles suspended
in the oil and thus avoid any agglomeration that could lead to sludge formation. The two
phenomena involved in this process are peptization and solubilization. Peptization consists
of wrapping solid oil contamination particles (diameters of 50–150 nm), such as dust and
soot, and keeping them in suspension. Solubilization uses the same mechanism, but it is
related to liquid contaminants, such as acids or condensates (less than 20 nm).
A detergent is a colloidal metal-based additive and has a structure similar to that of the
dispersant, but its tail is shorter and the polarity of its head is greater. Detergents are used
to remove, or avoid formation of, carbon, varnish, or lacquer deposits and to neutralize
acids created from combustion, oxidation, and nitration processes. Indeed, contaminating
acids are dangerous because they can cause corrosion and accelerate oil degradation.
Appl. Sci. 2021, 11, 5642 8 of 29
Engine oil also provides alkaline reserves to prevent acidification. The alkaline reserve
can be determined by the value of the total base number (TBN). In the same way, acidity can
be determined by the total acid number (TAN). The pH value is not suited for measurement
in oil because the medium is not aqueous. The unit for TAN and TBN measurement is
mg KOH/g, which corresponds to the equivalent mass of potassium hydroxide required
to neutralize one gram of solution. Neutralization is ensured by the use of detergents.
Some over-based detergents composed of calcium carbonate or magnesium carbonate
achieve a high level of protection against acidity. However, they can lead to ash formation,
which is problematic for diesel particulate filters. Manufacturers tend to use engine oils
with a relatively low ash content, meaning lower TBN and alkaline reserves; this reduces
resistance to chemical degradation.
During oil aging, polar compounds and charge carrier degradation products are
created. In parallel, base additive compounds are depleted, decreasing protection against
acidification. The electrical and chemical behaviors of these substances have a direct impact
on the oil dielectric constant (ε) and resistivity (P).
The dielectric constant (ε) or relative permittivity is the ratio of media permittivity
to vacuum permittivity. The dielectric constant represents the capacity of the medium
to be polarized under the application of an electric field. Concretely, polarization is the
consequence of the reorientation of molecular dipoles in the lubricant. During oil aging,
dipole moments change because of microscopic chemical reactions, such as oxidation or
nitration, or because of the addition of polar contaminants, such as water (ε water = 80) or
soot. The dielectric constant (ε) is defined according to the following equation:
ε = F + G.T (8)
where T is the temperature in ◦ C and F and G are oil-dependent constants.

Indeed, the dielectric constant (ε) can be linked with the density (ρ) using the following
relationship (9):
ε−1 α
= 4.π.ρ .Na. (9)
ε+2 3.M
where Na is Avogadro’s number, α is the molecular polarizability volume, and M is the
molar mass of the substance.
The resistivity (P) of a medium measures the drag force encountered by free charge
carriers moving through the medium under the application of an electric field. Oil resistivity
is dependent on fluid viscosity, the density of free charge carriers and the specific chemical
composition of the oil. To a first approximation, resistivity (P) can be modeled in a simple
linear form:
P = H + I.T (10)
where T is the temperature in ◦ C and H and I are oil-dependent constants.
General measurements of oil temperature are presented in Figure 6. Two engine
oil samples (new 15W40 and 1000 h aged) were measured in the standard engine oil
application temperature range. Temperature homogeneity was ensured by mechanical
stirring. The results demonstrate the ability of the fluid property sensor to measure oil
viscosity (η), density (ρ), dielectric (ε) and Rp as an indicator of resistivity (P) over the
entire range of application temperatures.
Viscosity, density, and dielectric constants are increased during aging. Without any
contamination, increases in the three parameter can be considered normal, even if we also
observe viscosity decreases due to oil shear. The increase in resistivity at high temperatures
is due to depletion of free charge carrier additives [35]. The gradients of variations will
depend on oil type and application characteristics, such as temperature or contamination.
samples (new 15W40 and 1000 h aged) were measured in the standard engine oil applica-
tion temperature range. Temperature homogeneity was ensured by mechanical stirring.
The results demonstrate the ability of the fluid property sensor to measure oil viscosity
(η), density (ρ), dielectric (ε) and Rp as an indicator of resistivity (Ρ) over the entire range
Appl. Sci. 2021, 11, 5642 9 of 29
of application temperatures.
50 0.85
15W40 new 15W40 new
15W40 1000h aged 0.84 15W40 1000h aged
40
0.83
Density (gm/cc)
Viscosity (cP)
30 0.82
0.81
20
0.80
10
0.79
0.78
60 70 80 90 100 110 120 60 70 80 90 100 110 120
o
Temperature ( C) Temperature (oC)
(a) (b)
2.6 2.1x107
15W40 new 15W40 new
15W40 1000h aged 2.0x107 15W40 1000h aged
2.5
1.9x107
2.4 1.8x107
Rp (Ohms)
Dielectric
1.7x107
2.3
1.6x107
2.2
1.5x107
2.1 1.4x107
60 70 80 90 100 110 120 60 70 80 90 100 110 120
Temperature (oC) Temperature °(o°C)
(c) (d)
Figure 6. New and6.aged
Figure Newengine oilengine
and aged (15W40): (a) viscosity;
oil (15W40): (b) density;
(a) viscosity; (c) dielectric;
(b) density; andand
(c) dielectric; (d)(d)
Rp.Rp.
3. Oil Ageing Processes and Sensors for Fluid Property Detection

During its whole lifespan, engine oil experiences different degradation and contam-
ination processes resulting from high temperatures and exposure to chemically reactive
combustion byproducts and various contaminants. The following sections describe these
processes and how each process is detectable with a fluid property sensor.
3.1. Oxidation
When exposed to high temperature, engine oil reacts with oxygen and this reaction
is called oxidation. Oil molecules chemically combine with oxygen to form carbonyl
compounds (C=O), such as aldehydes, ketones, esters, and carboxylic acids, in different
concentrations. The process actually corresponds to two degradations: the evaporation
of minor oil components and the incorporation of oxygen elements in oil components.
This oxidation induces the polymerization of oil molecules and the formation of insoluble
products that lead to an increase in viscosity. Oxidation also induces the formation and
depletion of various polar and conductive compounds, which will impact the oil dielectric
constant and resistivity [36].
centrations. The process actually corresponds to two degradations: the evaporation of mi-
nor oil components and the incorporation of oxygen elements in oil components. This ox-
idation induces the polymerization of oil molecules and the formation of insoluble prod-
ucts that lead to an increase in viscosity. Oxidation also induces the formation and deple-
Appl. Sci. 2021, 11, 5642 10 of 29
tion of various polar and conductive compounds, which will impact the oil dielectric con-
stant and resistivity [36].
The oxidation process is accelerated by heat, light, and metal catalysts, such as copper
or iron, andThethe presence
oxidation of water,
process acids, orbysolid
is accelerated heat,contaminants
light, and metalthat could such
catalysts, causeasdeposit
copper
or iron,Oxidation
formation. and the presence of water,by
is also favored acids, or solid
oil shear. contaminants
Hydrocarbon that could cause
compounds deposit
and polymer
formation.
viscosity additives Oxidation is also favored
are degraded by oilcreating
by shearing, shear. Hydrocarbon
carboxylic acids compounds andactive
and carbon poly-
mer viscosity additives are degraded by shearing, creating carboxylic
sites that can be oxidized to induce a new polymerization. Eventually, oxidation is accel- acids and carbon
eratedactive sites that or
by biodiesel canethanol
be oxidized
fuelsto induce
due a new
to their polymerization.
hygroscopic Eventually, oxidation is
properties.
accelerated by biodiesel or ethanol fuels due to their hygroscopic properties.
Oxidation was measured in the laboratory using Fourier transform infrared (FTIR)
Oxidation was measured in the laboratory using Fourier transform infrared (FTIR)
spectroscopy as specified by the standard test methods ASTM D7418 or ASTM D7214. The
spectroscopy as specified by the standard test methods ASTM D7418 or ASTM D7214. The
measurement
measurement is based on quantification
is based on quantificationof the
of carbonyl functional
the carbonyl group
functional (C=O),
group using
(C=O), the
using
1700 the
cm1700
−1 frequency
cm frequency peak in the absorbance spectrum. Oxidation measurementex-
− 1 peak in the absorbance spectrum. Oxidation measurement is is
pressed in A/cm.
expressed in A/cm.
The measurement
The measurement of fluid oxidation
of fluid oxidationwith
withthetheproperty
property sensor ispresented
sensor is presentedininFigure
Figure 7.
7. Engine oil (15W40) was stored in the laboratory at 120◦ °C for 3000
Engine oil (15W40) was stored the laboratory at 120 C for 3000 h and regularly sampledh and regularly sam-
pled and
andanalyzed
analyzeduntil untilthethe point
point of complete
of complete degradation.
degradation. The results
The results demonstrate
demonstrate the
the ability
of of
ability thethe
fluid property
fluid property sensor
sensorto detect andand
to detect measure
measureoil oxidation, mainly
oil oxidation, with with
mainly viscosity,
vis-
dielectric,
cosity, dielectric,andandresistivity measurements.
resistivity measurements.
40 400 0.86 3
Viscosity Relative Evolution % (∗)
Density Relative Evolution % (*)

0.84 2
Density gm/cc 120°C (o)
Viscosity cP 120°C (0)
30 300
0.82 1
20 200 0.80 0
0.78 -1
10 100
0.76 -2
0.74 -3
Appl. Sci. 2021, 011,
0
x FOR
5
PEER
10
REVIEW
15 20 25 30 35 40
0
0 5 10 15 20 25 30 35 40
10 of 28
Oxidation A/cm Oxidation A/cm
(a) (b)
2.30 6 2.6x107 15
Dielectric Relative Evolution % (*)
2.5x107 10 Rp Relative Evolution % (*)

2.25 3
Dielectric 120°C (o)
Rp Ohms 120°C (o)
2.4x107 5
2.20 0 2.3x107 0
2.2x107 -5
2.15 -3
2.1x107 -10
Phase 1 Phase 2 Phase 3 Phase 4

2.10 -6
2.0x107 -15
0 5 10 15 20 25 30 35 40
0 5 10 15 20 25 30 35 40
Oxidation A/cm
Oxidation A/cm
(c) (d)
FigureFigure
7. Engine oil (15W40)
7. Engine oxidation
oil (15W40) at 120
oxidation °C:◦(a)
at 120 viscosity;
C: (a) (b)(b)
viscosity; density;
density;(c)(c)dielectric;
dielectric;and
and (d)
(d) Rp.
Rp.
Viscosity is highly increased during all oxidation processes. Resistivity is a very use-
ful parameter because it can be directly linked to the four different phases of the oil oxi-
dation process (see Table 2).
Table 2. Four different phases of oil oxidation process.
Stage Oxidation A/cm

Appl. Sci. 2021, 11, 5642 11 of 29
Viscosity is highly increased during all oxidation processes. Resistivity is a very useful
parameter because it can be directly linked to the four different phases of the oil oxidation
process (see Table 2).
Table 2. Four different phases of oil oxidation process.
Stage Oxidation A/cm

Phase 1 0–3
Phase 2 3–16.5
Phase 3 16.5–31.5
Phase 4 31.5–40
During Phase 1, the tested oil resistivity is increased by up to 10% at 120 ◦ C. This
phenomenon can be explained by the depletion of some free charge carrier additives.
The viscosity starts its continuous increase, and the dielectric shows a very slight drop.
Phase 1 corresponds to the predominance of a fast chemical process involving very
reactive additives.
During Phase 2, the tested oil resistivity is decreased up to −10% at 120 ◦ C, rela-
tive to the initial value, and the dielectric showed a significant increase. Phase 2 corre-
sponds to a predominance of a slow chemical process that releases charge carriers and
polar compounds.
During Phase 3, the resistivity shows a new increase linked to a new depletion of
charge carriers, and the dielectric is stabilized.
Phase 4 corresponds to the dramatic increase in viscosity before complete oil degrada-
tion and potential jelling [37].
Even if the density changes remain relatively slight, they can be linked to the four
different oxidation phases.
The four different oil degradation phases and corresponding viscosity and resistivity
behaviors are described in the literature. Temperature has a relatively low impact on the
four oxidation behaviors, and the relative changes, except those for resistivity, are similar
for each temperature. The phase 1 resistivity increase is amplified at high temperatures
and moderated at lower temperatures.
During Phase 1 and Phase 2, the oil condition is considered good, and the level of
degradation is quite low. Phase 3 corresponds to a consequent level of oil degradation.
Entry into Phase 3 is the appropriate time to perform an oil change. During Phase 4, oil had
already reached a very high level of degradation. There is a high risk of dramatic engine
failure. An oil change has to be performed immediately at this point [38].
The oxidation process depends on engine application characteristics and engine oil
composition. Oxidation measurements for three different 15W40 engine oils are presented
in Figure 8. The three engine oils were stored at 120 ◦ C and regularly measured until the
end of Phase 2 of oil oxidation. The results show different measurement gradients for the
oils, but the general trends described above are confirmed.
Brand C oil shows a consequent resistivity increase during Phase 1 and then relatively
low increases in viscosity and dielectric during Phase 2. Brand A oil shows a lower
resistivity increase during Phase 1 but much higher increases in viscosity and dielectric
during Phase 2. These different gradients could be linked to additive compositions. Indeed,
the type and concentration of additives present in oil will favor or prevent different
reactions yielding oxidation and degradation products [39].
engine failure. An oil change has to be performed immediately at this point [38].
The oxidation process depends on engine application characteristics and engine oil
composition. Oxidation measurements for three different 15W40 engine oils are presented
in Figure 8. The three engine oils were stored at 120 °C and regularly measured until the
Appl. Sci. 2021, 11, 5642
end of Phase 2 of oil oxidation. The results show different measurement gradients12for
of 29
the
oils, but the general trends described above are confirmed.
1.20 0.84
15W40 Brand A 15W40 Brand A
15W40 Brand B 15W40 Brand B
15W40 Brand C 15W40 Brand C
1.17 0.83
Density gm/cc 100°C

1.14 0.82
1.11 0.81
1.08 0.80
1.05
0.79
0 200 400 600 800 1000 1200 1400 1600
0 200 400 600 800 1000 1200 1400 1600
Oxidatio Time hours
Oxidation Time hours
(a) (b)
7
2.6 2.5x10
15W40 Brand A 15W40 Brand A

15W40 Brand B 15W40 Brand B
15W40 Brand C 2.4x10
7
15W40 Brand C
2.5
Dielectric 100C
7
Rp ohms 100C
2.3x10
2.4
7
2.2x10
2.3
7
2.1x10
7
2.2 2.0x10
0 200 400 600 800 1000 1200 1400 1600 0 200 400 600 800 1000 1200 1400 1600
Oxidation Time hours Oxidation Time hours
(c) (d)
FigureFigure
8. Engine oil (15W40
8. Engine brands
oil (15W40 A, BA,and
brands C) oxidation
B and at at
C) oxidation 100100 ◦ C:
°C: (a)(a)viscosity;
viscosity;(b)
(b) density; (c) dielectric;
density; (c) dielectric;and
and(d)
(d)Rp.
Rp.
Since
Brand C oxidation
oil showsis adependent
consequenton oil composition
resistivity and engine
increase during application
Phase 1characteristics,
and then rela-
precise
tively and complete
low increases oxidation
in viscosity modeling
and dielectric seems difficult.
during PhaseHowever,
2. Brand A one
oilcan determine
shows a lower
a typical physical change by focusing on Phase 1 and Phase 2. The solution
resistivity increase during Phase 1 but much higher increases in viscosity and dielectric consists of
modeling Phase 1 and Phase 2 and detecting the entry into Phase 3, which is linked to a
during Phase 2. These different gradients could be linked to additive compositions. In-
consequent level of degradation. For example, the 15W40 engine oils presented in Figure 9
deed, the type and concentration of additives present in oil will favor or prevent different
could be modeled with the following equations at constant temperature:
reactions yielding oxidation and degradation products [39].
Since oxidation is dependent ηthon= oil
ηi . composition
1 + 21 × 10−3and.Ox. engine application characteris-

(11)
tics, precise and complete oxidation modeling seems difficult. However, one can deter-

mine a typical physical change by ρth focusing
= ρi . 1 +on 0.5Phase
× 10−1 3 and Phase 2. The solution consists
.Ox. (12)
of modeling Phase 1 and Phase 2 and detecting the entry into
Phase 3, which is linked to
a consequent level of degradation. −3
εthFor
= εexample,
i . 1 + 0.5 the
× 1015W40
.Ox. engine oils presented in Figure
(13)
9 could be modeled with the following equations at constant temperature:
Rpth = Rpi . 1 − 12 × 10−3 .Ox. (14)
ρ = ρ . 1 + 0.5 × 10 . Ox. (12)
ε = ε . 1 + 0.5 × 10 . Ox. (13)
Appl. Sci. 2021, 11, 5642

Rp = Rp . 1 − 12 × 10 . Ox. 13 of 29
(14)
30 80 0.86 3
Viscosity Relative Evolution % (*)

0.84 2

Viscosity cP 100°C(O)
25 60
0.82 1
20 40 0.80 0
0.78 -1
15 20
0.76 -2
10 0 0.74 -3
0 5 10 15 20 25 0 5 10 15 20 25
(a) (b)
2.40 3 2.6x107 15
2.35 2 2.5x107 10
Rp Relative Evolution % (*)

Rp Ohms 100°C (o)
2.30 1 2.4x107 5
2.25 0 2.3x107 0
2.20 -1 2.2x107 -5
2.15 -2 2.1x107 -10
Phase 1 Phase 2 Phase 3

2.10 -3 2.0x107 -15
0 5 10 15 20 25 0 5 10 15 20 25
(c) (d)
Figure 9. Engine
Figure oil (15W40)
9. Engine oxidation
oil (15W40) at 100
oxidation °C:◦ (a)
at 100 viscosity;
C: (a) (b)(b)density;
viscosity; density;(c)
(c)dielectric;
dielectric; and
and (d) Rp.
(d) Rp.
TheThe models
models are plotted
are plotted in Figure
in Figure 9 with
9 with the related
the related accuracy
accuracy specifications
specifications given
given with
full blue lines. The red circles represent detection of the entry into Phase 3 when η ≥
with full blue lines. The red circles represent detection of the entry into Phase 3 when
1.05.ηη≥ 1.05.η
and thRpand Rp ≥ 1.05Rp
≥ 1.05Rp . th .
3.2. Water Contamination
3.2. Water Contamination
Water contamination comes from the fuel combustion process or from the exterior
Water contamination comes from the fuel combustion process or from the exterior
engine system. Water in oil can be dangerous for an engine because it could induce
engine system.
excessive Water
wear, for in oil can by
example, be cavitation
dangerous orfor an engine
corrosion. because
Water it could induce
also promotes exces-
oil oxidation
sive and
wear,
thefor example,
formation of by cavitation
acid or and
byproducts corrosion.
sludge,Water also
and thus promotes
poor oil oxidation and
engine reliability.
the formation of acid byproducts and sludge, and thus poor engine reliability.
Water has three different states in oil: dissolved water, emulsified water, and free
water. Dissolved water is characterized by dispersed individual water molecules chemically
linked to the oil. Above this level, called solubility, the excess water is saturated and will
not be chemically linked to the oil; free water is formed, leading to a two-phase system.
Because the density of water is higher than that of oil, free water typically accumulates at
the bottom of the oil pan. When the mixing ratio is sufficiently high, or in the presence
of surfactant additives, an emulsion can be formed. Emulsified water is homogeneously
dispersed into the oil [40].
tem. 4000
Because the density of water is higher than that of oil, free water
15W40 of
lates at the bottom newthe oil pan. When the mixing ratio is sufficien
3500
presence of surfactant additives, an emulsion can be formed. Emulsif
Appl. Sci. 2021, 11, 5642
Free and Emulsified Water 14 of 29
geneously
3000 dispersed into the oil [40].
Typical water solubility and associated water states are presented
Solubility ppm
2500 Dissolved Water
Typical water solubility and associated water states are presented in Figure 10.
2000
4000
1500 15W40 new

3500
1000
Free and Emulsified Water
Solubility ppm 3000
500
2500 Dissolved Water
2000 0
20 30 40 50 60 70 80 90 100
1500 Temperature °C
1000
Figure
500 10. Typical water solubility in engine oil and associated water s
0
Solubility
20 30 depends
40 50 60on temperature,
70 80 90 oil additives, contami
100
Temperature °C
Water has low solubility in pure oils and hydraulic oils. Typical
Figure 10. Typical water solubility in engine oil and associated water states.
approximately 2000 ppm at 50 °C.
FigureSolubility
10. Typical water solubilityoil
The solubilities of waterinadditives,
depends on temperature, engine oil
in hydraulic and associated
oil and
contamination, water [9].
fresh
and oxidation states.
and ag
Water has low solubility in pure oils and hydraulic oils. Typical solubility in engine oil is
measured
approximatelyby
Solubility 2000appm
water
depends at 50 ◦ content
C. sensor, are presented in Figure 11.
on temperature, oil additives, contamination,
The solubilities of water in hydraulic oil and fresh and aged 15W40 engine oils, as
Water has
measured bylow solubility
a water in are
content sensor, pure oils and
presented hydraulic
in Figure 11. oils. Typical solubi
approximately
4000 2000 ppm at 50 °C.
15W40 new of water in hydraulic oil and fresh and aged 15W
The solubilities
3500 15W40 1000h aged
measured byHydraulic
a waterOil content sensor, are presented in Figure 11.
3000
Solubility ppm Solubility ppm
2500
4000
15W40 new
2000
3500 15W40 1000h aged
Hydraulic Oil
1500
3000
2500
1000
2000
500
1500
0
20 30 40 50 60 70 80 90 100
1000
Temperature °C
500
Figure 11. Water solubility in hydraulic and engine oil measured by a water content sensor.
0
Figure 2011.
Water Water
in30 40 solubility
oil is typically
50 measured
60 in hydraulic
in the
70 laboratory
80 90 and
with engine
100 Karl oil measured
Fisher titration (ISO12937 by a w
or ASTM D1533). The KarlTemperature °C measures total absolute water in ppm with high
Fisher method
accuracy. However, this method is not totally appropriate with engine oil because the
Watercould
measurement inbeoil is typically
impacted measured
by specific engine in Aqua
oil additives. The the test
laboratory
(ISO/DIS w
Figure
9114 or11.
(ISO12937 Water
ASTM solubility
D7358)
or ASTM in hydraulic
and FTIR spectroscopy
D1533). The and D7418)
(ASTM
Karl engine
Fisherareoil measured
alternative
method by afor
methods
measureswaterto
co
measuring total absolute water down to 100 ppm and with 100 ppm accuracy. These three
with high accuracy. However, this method is not totally appro
Water in oil is typically measured in the laboratory with Ka
cause the measurement could be impacted by specific engine oi
(ISO12937 or ASTM D1533). The Karl Fisher method measures total abs
(ISO/DIS
with 9114 or ASTM
high accuracy. However,D7358) and FTIR
this method is notspectroscopy (ASTM
totally appropriate
Appl. Sci. 2021, 11, 5642 15 of 29
These three methods do not differentiate dissolved or free water. A water content sensor
is methods do not differentiate dissolved or free water. A water content sensor is able to
able to measure water activity and then to deduce solubility, independent of oil aging.
measure water activity and then to deduce solubility, independent of oil aging. Water
Water activity can be defined by the following formula:
activity can be defined by the following formula:
H2 O
aWater = [H2 O] (15)
aWater = H2 O Saturation (15)
[H2 O]Saturation
where 0 < aWater < 1, and H2 O is the concentration of dissolved water in oil (ppm) and
Hwhere 0 < a is the
2 O SaturationWater
< 1, and [H2 O] is of
concentration thedissolved
concentration
waterofindissolved water
oil (ppm) in saturation
at the oil (ppm) andpoint.
[ H
The water
2 O ] is the concentration of dissolved water in oil (ppm) at the saturation
content sensor and its water activity measurements would be the relevant sen-
Saturation point.
sorThe water content
solution sensor and
for measuring its water
water activity
content at themeasurements
saturation pointwould bethe
with the highest
relevantaccuracy.
sensor
solution for measuring water content at the saturation point with the highest accuracy.
The fluid property sensor water dilution measurement is presented in Figure 12. En-
The fluid property sensor water dilution measurement is presented in Figure 12.
gine oil (15W40) was stabilized at 50 °C ◦and diluted with deionized water. Emulsion ho-
Engine oil (15W40) was stabilized at 50 C and diluted with deionized water. Emulsion
mogeneity
homogeneity waswasensured byby
ensured magnetic
magneticstirring.
stirring.The
The results demonstratethe
results demonstrate the ability
ability of fluid
of fluid
property
propertysensorssensorstotodetect
detectand
and measure watercontamination,
measure water contamination,mainly
mainly with
with dielectric
dielectric andand
56 6 0.88 3

54 4 0.86 2
Viscosity cP 50°C (o)
52 2 0.84 1
50 0 0.82 0
48 -2 0.80 -1
46 -4 0.78 -2
44 -6 0.76 -3
0 1000 2000 3000 4000 5000 6000 0 1000 2000 3000 4000 5000 6000
Water dilution ppm Water dilution ppm
(a) (b)
2.6 12 2.6x107 6
2.5x107 4 Rp Relative Evolution % (*)

2.5 9
Rp Ohms 50°C (o)
2.4x107 2
2.4 6 2.3x107 0
2.2x107 -2
2.3 3
2.1x107 -4
2.2 0 2.0x107 -6
0 1000 2000 3000 4000 5000 6000 0 1000 2000 3000 4000 5000 6000
Water dilution ppm Water dilution ppm
(c) (d)
Figure 12. 12.
Figure Water dilution
Water inin
dilution engine
engineoil
oil(15W40)
(15W40)at
at 50 ◦ C: (a) viscosity;
50 °C: viscosity;(b)
(b)density;
dielectric; and
and (d)(d)
Rp.Rp.
Viscosity and density do not show any changes. The dielectric constant is linearly
increased and the resistivity is linearly decreased with water dilution. These noticeable
changes have been described in the literature and can be explained by the high dielectric
constant of water (εWater =80) and the autoionization of water that can release free charge
carriers, e.g., protons, into the oil.
Appl. Sci. 2021, 11, 5642 16 of 29
Viscosity and density do not show any changes. The dielectric constant is linearly
increased and the resistivity is linearly decreased with water dilution. These noticeable
changes have been described in the literature and can be explained by the high dielectric
constant of water (εWater = 80) and the autoionization of water that can release free charge
carriers, e.g., protons, into the oil.
The fluid property sensor measures dissolved and emulsified water, which guarantees
good compatibility with the application. Indeed, engine operation ensures emulsion by
using a sufficiently high mixing ratio. When engine oil reaches a high temperature, water
may evaporate, so the detection has to be performed before evaporation, preferably just
after engine start-up during the oil temperature increase.
Water in engine oil can be modeled using the following equations at a cons-
tant temperature:
ηth = ηi (16)
ρth = ρi (17)

εth = εi . 1 + 20 × 10−6 .WatDil(ppm) (18)

Rpth = RPi . 1 − 6 × 10−6 .WatDil(ppm) (19)
These models are plotted in Figure 12, with the related accuracy specifications given
as full blue lines.
3.3. Coolant Contamination

Engine coolant contamination comes from leakage from the engine cooling system.
Coolant is composed of ethylene glycol or propylene glycol (40 to 60%), water (60 to 40%)
and several additives at relatively low concentrations (approximately 5%). Ethylene glycol
and propylene glycol are miscible with water and with most organic solvents, but are not
miscible with oil. Common coolant additives include sodium silicate, disodium phosphate,
sodium molybdate, and sodium borate, and these function as lubricants, buffers, and
corrosion inhibitors. Coolant contamination in engine oil can be dangerous for an engine,
and have several negative impacts. Low levels of coolant contamination can cause heavy
sludge deposits, the formation of acidic compounds, such as glycolic or methanoic acids,
and acceleration of oil oxidation. When mixed with oil, high coolant contamination could
lead to emulsions or gels and induce occlusions of walls and oil passageways, risks of filter
blocking, reductions in oil flow, and a serious general decrease of lubrication efficiency [41].
Coolants in oil are typically measured in the laboratory using FTIR spectroscopy
(ASTM D7418) or ICP-AES spectrometry (ASTM D7151), mainly through quantification of
the coolant additive elements Na, B, and/or K within the oil.
The fluid property sensor measurement of coolant (50% water) dilution is presented in
Figure 13. Engine oil (15W40) was stabilized at 50 ◦ C and diluted with coolant. Emulsion
homogeneity was ensured by magnetic stirring. The results demonstrate the capability
of the fluid property sensor to detect and measure coolant contamination, mainly with
dielectric and resistivity measurements.
Viscosity and density did not show any changes. The dielectric increased linearly.
With the coolant dilution, when the coolant dilution rate was lower than 2000, the linear
decrease of resistivity was not obvious, but it did decrease linearly at a coolant dilution rate
above 2000. These results are perfectly consistent with the water dilution results described
in the previous section. Indeed, the tested coolant was composed of 50% water, and the
dielectric and resistivity slopes are half as high as those in the water dilution results. The
changes can be explained by the high dielectric constant of water (εWater = 80) and the
autoionization of water, which can release free charge carriers and protons into the oil [42].
Appl. Sci. 2021, 11, 5642 17 of 29
56 6 0.88 3

54 4 0.86 2

52 2 0.84 1
50 0 0.82 0
48 -2 0.80 -1
46 -4 0.78 -2
44 -6 0.76 -3
0 1000 2000 3000 4000 5000 6000 0 1000 2000 3000 4000 5000 6000
Coolant dilution ppm Coolant dilution ppm
(a) (b)
2.6 12 2.6x107 6
2.5x107 4

2.5 9
Rp Ohms 50°C (o)
2.4x107 2
2.4 6 2.3x107 0
2.2x107 -2
2.3 3
2.1x107 -4
2.0x107 -6
2.2 0
0 1000 2000 3000 4000 5000 6000
0 1000 2000 3000 4000 5000 6000
Coolant dilution ppm
Coolant dilution ppm
(c) (d)
FigureFigure
13. Coolant dilution
13. Coolant in engine
dilution oil (15W40)
in engine at 50
oil (15W40) °C:◦ C:
at 50 (a)(a)
viscosity;
viscosity;(b)
(b)density;
density; (c) dielectric;and
(c) dielectric; and(d)
(d)Rp.
Rp.
Viscosity andproperty
The fluid density sensor
did notmeasures
show any changes.
dissolved andThe dielectric
emulsified increased
water cominglinearly.
from
Withthethecoolant
coolantblend, which
dilution, guarantees
when gooddilution
the coolant compatibility withlower
rate was the application. Indeed,
than 2000, the linear
engine
decrease ofoperation ensures
resistivity emulsion
was not obvious,by establishing a sufficiently
but it did decrease high at
linearly mixing ratio. dilution
a coolant When
engine 2000.
rate above oil reaches
Thesea results
high temperature,
are perfectly water may evaporate,
consistent with theso the detection
water dilution has to bede-
results
performed before evaporation, preferably just after the engine start-up during the oil
scribed in the previous section. Indeed, the tested coolant was composed of 50% water,
temperature increase.
and the dielectric and resistivity slopes are half as high as those in the water dilution re-
The coolant in engine oil can be modeled using the following equations at a cons-
sults.tant
Thetemperature:
changes can be explained by the high dielectric constant of water (εWater =80) and
the autoionization of water, which can release ηth =free
ηi charge carriers and protons into the (20)oil
[42].
The fluid property sensor measures dissolvedρth = ρi and emulsified water coming from (21)the
coolant blend, which guarantees good compatibility
with the application. Indeed, engine

εth = εi . 1 + 10 × 10−6 .CoolDil(ppm) (22)
operation ensures emulsion by establishing a sufficiently high mixing ratio. When engine

oil reaches a high temperature,Rpth water
= Rpi .may1 −evaporate, so the(ppm
3 × 10−6 .CoolDil detection
)
has to be performed
(23)
before evaporation, preferably just after the engine start-up during the oil temperature
increase.
The coolant in engine oil can be modeled using the following equations at a constant
temperature:
η =η (20)
Appl. Sci. 2021, 11, 5642 18 of 29
These models are plotted in Figure 13 with the related accuracy specifications given
as full blue lines.
3.4. Fuel Contamination

Fuel contamination in engines is caused by imperfect fuel combustion and imperfect
sealing. Unburned fuel reaches the crankcase through the space between the piston and
cylinder and between the piston groove and the ring. Fuel dilution can be enhanced under
particular conditions during the DPF regeneration process.
Internal combustion engines use fuels such as diesel or gasoline, which are mostly
hydrocarbon compounds mixed with a variety of additives. Generally obtained as a specific
fractional distillate of petroleum, they are now increasingly blended with biofuels such as
biodiesel and ethanol. Blended with petroleum diesel, biodiesel is a vegetable oil or animal
fat-based fuel composed of long chain alkyl esters. In the US, fuel standard ASTM D7467
specifies blends from B6 to B20, which corresponds to blends with 6% to 20% biodiesel.
In Europe, fuel standard EN 590 specifies blends up to B7. In gasoline fuels, ethanol is
blended up to 10% (E10) in common markets and can be blended up to 85% (E85) in flexible
fuel vehicle applications (ASTM 5798). In the future, biofuel blending rates are expected to
increase in order to meet environmental protection rules.
Fuel physical properties can be modeled as oil physical properties:
log(log(µ + 0.7)) = B − C. log(T + 273.15) (24)
ρ = D + E.T (25)
ε = F + G.T (26)
RP = H + I.T (27)
where T is the temperature in ◦C and B, C, D, E, F, G, H, and I are fuel-dependent constants.
Dynamic viscosity η (T) is deduced from kinematic viscosity µ (T) and density ρ (T).
Fluid property sensor measurements of different fuels are presented in Figure 14. Fuel
temperature homogeneity was ensured by magnetic stirring. The results demonstrate the
fluid property sensor’s capability to accurately measure fuel properties and allow robust
fuel type differentiation.
B100 biodiesel has a higher viscosity, density, and dielectric value than pure petroleum
fuels. Gasoline shows a much lower viscosity than diesel fluids. The lower resistivity
of biodiesel is explained by its hygroscopic characteristics. Fuel property measurements
allow differentiation between gasoline, B0 and B100 but also with alternative fuels such as
kerosene or hydrotreated vegetable oil (HVO).
Fuel contamination in engine oil can be dangerous for the engine because it can
promote oxidation of oil, formation of acidic compounds and formation of soot. These
degradations are even more prevalent with biofuels because of the hygroscopic characteris-
tics of biodiesel or ethanol. Fuel dilution will also degrade oil lubrication properties and
amplify risks of wear.
Fuel contamination in oil is typically estimated in the laboratory with a method using
flash point (ISO 2719) and viscosity measurements (ASTM D445) or with a more accurate
and more expensive method using gas chromatography measurements [43].
The fluid property sensor fuel dilution measurement is presented in Figure 15. Engine
oil (15W40) was stabilized at 100 ◦ C and diluted with diesel fuel. Blending temperature
homogeneity was ensured by mechanical stirring. The results demonstrate the capabil-
ity of the fluid property sensor to detect and measure fuel contamination, mainly with
viscosity measurements.
Appl. Sci. 2021, 11, 5642 19 of 29
Resistivity does not show any consequent change. Density and dielectric are linearly
related to fuel dilution. Slopes depend directly on the density and dielectric properties
of the two fluids because they are miscible. The most obvious change is measured with
viscosity, which decreases exponentially with fuel dilution.
As engine oil and fuel are miscible fluids, the Refutes method can be used to calculate
the theoretical kinematic viscosity (µ) of the blend. The method consists of determining a
viscosity blending number (VBN) for each component based on their kinematic viscosity
and then calculating the VBN of the blend at a fixed constant temperature [12]:

VBNFuel = 14.534. ln ln µFuelth + 0.8 + 10.975 (28)

VBNOil = 14.534. ln ln µOilth + 0.8 + 10.975 (29)

VBNBlend = VBNOil . 1 − FuelDil(%) /100 + VBNFuel .FuelDil(%) /100 (30)
6 0.95
Gasoline Gasoline
B0 B0
5 B100 0.90
B100
4
Density gm/cc
Viscosity cP
0.85
0.80
2
0.75
1
0 0.70
20 25 30 35 40 20 25 30 35 40
Temperature °C Temperature °C
(a) (b)
3.5 3.5x107
Gasoline Gasoline
B0 B0
B100 B100
3.0x107
3.0
Dielectric
Rp Ohms
2.5x107
2.5
2.0x107
2.0 1.5x107
20 25 30 35 40 20 25 30 35 40
(c) (d)
Figure 14. 14.
Figure Gasoline, diesel
Gasoline, B0,B0,
diesel rapeseed
rapeseedB100
B100biodiesel:
biodiesel: (a)
(a) viscosity; (b)density;
viscosity; (b) density;(c)
(c)dielectric;
dielectric; and
and (d)(d)
Rp.Rp.
B100 biodiesel has a higher viscosity, density, and dielectric value than pure petro-
leum fuels. Gasoline shows a much lower viscosity than diesel fluids. The lower resistivity
of biodiesel is explained by its hygroscopic characteristics. Fuel property measurements
allow differentiation between gasoline, B0 and B100 but also with alternative fuels such
as kerosene or hydrotreated vegetable oil (HVO).
Fuel contamination in engine oil can be dangerous for the engine because it can pro-
mote oxidation of oil, formation of acidic compounds and formation of soot. These degra-
Appl. Sci. 2021, 11, 5642 20 of 29
13 0 0.88 3

12 -5 0.86 2

Density gm/cc 100C (o)

11 -10 0.84 1
10 -15 0.82 0
9 -20 0.80 -1
8 -25 0.78 -2
7 -30 0.76 -3
0 2 4 6 8 10 0 2 4 6 8 10
Fuel dilution % vol Fuel dilution % vol
(a) (b)
2.30 3 2.6x107 6
2.5x107 4

2
2.25
Rp Ohms 100°C (o)
1 2.4x107 2
2.20 0 2.3x107 0
-1 2.2x107 -2
2.15
2.1x107 -4
-2
2.0x107 -6
2.10 -3
0 2 4 6 8 10
0 2 4 6 8 10
Fuel dilution % vol
Fuel dilution % vol
(c) (d)
FigureFigure
15. Fuel
15. dilution in engine
Fuel dilution oil (15W40):
in engine (a) (a)
oil (15W40): viscosity; (b)(b)density;
viscosity; density;(c)
(c)dielectric; and (d)
dielectric; and (d)Rp.
Rp.
Resistivity does not

The kinematic show any
viscosity of theconsequent change.
blend can then Densityusing
be estimated and the
dielectric
VBN ofare
thelinearly
blend
in the following equation:
related to fuel dilution. Slopes depend directly on the density and dielectric properties of
the two fluids because they are miscible. The most obvious change is measured with vis-
VBNBlend − 10.975

Blendth =
cosity, which decreasesµexponentiallyexp with
exp fuel dilution. − 0.8 (31)
14.534
As engine oil and fuel are miscible fluids, the Refutes method can be used to calculate
the theoretical kinematic viscosity
Fuel contamination (µ)oil
in engine ofcanthebeblend.
modeledThe using
methodtheconsists ofequations
following determining
at a a
constant temperature:
viscosity blending number (VBN) for each component based on their kinematic viscosity
and then calculating the VBN of the ηBlend
blendth
=atµBlend
a fixed.ρ constant
th Blendth temperature [12]: (32)

ρBlendVBN
th
= ρOili=
. 114.534. ln (ln
− FuelDil μ
%) /100 ++ρ0.8 + 10.975
Fueli .FuelDil (%) /100 (28)
(33)

= εOili=
εBlendthVBN − FuelDil
. 114.534. ln ln μ
( % ) /100 + 0.8
+ εFueli .FuelDil
+ 10.975(%) /100 (34)
(29)
RpBlendth = RpOili .(1 − FuelDil% /100) + RpFueli .FuelDil(%) /100 (35)
VBN = VBN . 1 − FuelDil % /100 + VBN . FuelDil % /100 (30)
The kinematic viscosity of the blend can then be estimated using the VBN of the blend
in the following equation:
ε =ε . 1 − FuelDil % /100 + ε . FuelDil % /100 (34)
Rp = Rp . 1 − FuelDil% /100 + Rp . FuelDil % /100 (35)

Appl. Sci. 2021, 11, 5642 21 of 29
as full blue lines.
3.5. SootThese models are plotted in Figure 15 with the related accuracy specifications given
Contamination
as full blue lines.
Soot is composed of impure carbon particles resulting from incomplete fuel combus-
tion.
3.5. Soot Contamination
Soot contamination in engine oil can be dangerous for the engine because soot-loaded
Soot is composed of impure carbon particles resulting from incomplete fuel combustion.
oil can cause deposits, inducing further engine problems. Soot particles can be abrasive
Soot contamination in engine oil can be dangerous for the engine because soot-loaded
andoilincrease
can causeengine wear.
deposits, Dispersant
inducing additives
further engine can manage
problems. a certain
Soot level
particles canofbesoot in the
abrasive
oil,and
butincrease
they cannot avoid viscosity increases with excessive soot contamination [44].
engine wear. Dispersant additives can manage a certain level of soot in the oil,
butSoot
theycontamination can be increases
cannot avoid viscosity measured withinexcessive
the laboratory with FTIR [44].
soot contamination spectroscopy
(ASTM SootD7418). Soot contamination
contamination is expressed
can be measured in %.
in the laboratory with FTIR spectroscopy (ASTM
The fluid
D7418). Sootproperty sensorismeasurement
contamination expressed in %. of soot contamination is presented in Figure
16. EngineThe oil
fluid(15W40)
propertywas stabilized
sensor at 100of°C
measurement and
soot contaminated
contamination with standard
is presented diesel
in Figure 16.
Engine oil (15W40) was2975).
stabilized ◦
at 100 C and contaminated with standardstirring.
diesel par-
particulate matter (NIST Oil homogeneity was ensured by magnetic The
ticulate
results matter (NIST
demonstrate the 2975). Oil homogeneity
capability of fluid property was sensors
ensured tobydetect
magnetic
andstirring.
measureThe soot
results demonstrate
contamination, mainly the
withcapability
viscosityofandfluid propertymeasurements.
dielectric sensors to detect and measure soot
contamination, mainly with viscosity and dielectric measurements.
13 9 0.86 10

0.85
8
12 6 0.84
6
0.83
4
11 3 0.82
2
0.81
10 0 0.80 0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Soot contamination % mass Soot contamination % mass
(a) (b)
7
2.50 16 2.6x10 6
2.45 14
2.5x107 4
2.40 12
Rp Ohms 100°C (o)
2.4x107 2
2.35 10
2.30 8 2.3x107 0
2.25 6
2.2x107 -2
2.20 4
2.1x107 -4
2.15 2
2.10 0 2.0x107 -6
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Soot contamination % mass Soot contamination % mass
(c) (d)
Figure 16. 16.
Figure Soot contamination
Soot in engine
contamination oiloil
in engine (15W40) at at
(15W40) 100 °C:
100 (a)(a)
◦ C: viscosity; (b)
viscosity; (b)density;
dielectric;and
and(d)
(d)Rp.
Rp.
Viscosity and dielectric constant are linearly related to soot contamination. When the
value of soot contaminant is above 0.6, the linear relationship between viscosity and soot
pollution is demonstrated. Since soot persuasion is related to the ratio of carbon content,
the linear relationship is not so obvious in the interval below 0.6. Soot may also induce a
slight increase in density and a slight decrease in resistivity. These noticeable changes
Appl. Sci. 2021, 11, 5642 22 of 29
Viscosity and dielectric constant are linearly related to soot contamination. When the
value of soot contaminant is above 0.6, the linear relationship between viscosity and soot
pollution is demonstrated. Since soot persuasion is related to the ratio of carbon content,
the linear relationship is not so obvious in the interval below 0.6. Soot may also induce a
slight increase in density and a slight decrease in resistivity. These noticeable changes have
been described in the literature and can be explained by the shape, high polarizability, and
charge characteristics of soot particles.
Soot contamination in engine oil can be modeled using the following equations at a

ηth = ηi . 1 + 6 × 10−2 .SootCont(%mass) (36)

ρth = ρi . 1 + 0.5 × 10−2 .SootCont(%mass) (37)

εth = εi 1 + 12 × 10−2 .SootCont(%mass) (38)

Rpth = RPi . 1 − 2 × 10−2 .SootCont(%mass) (39)
as full blue lines.
3.6. Metal Contamination

Metal contamination comes from wear induced by bad lubrication and from corrosion.
The main metals to be monitored are Fe, Cu, or Al, which are components of the main
engine parts.
Metal contamination is dangerous because it can accelerate oil degradation. Metal
contamination is, above all, a sign of abnormal wear.
Metal contamination can be measured in the laboratory with ICP spectrometric analy-
sis (NFT 60 106). Metal contamination is expressed in mg/kg, equivalent to ppm mass [45].
Iron (Fe) contamination measurements are presented in Figure 17. Engine oil (15W40)
was stabilized at 100 ◦ C and contaminated with <10 µm Fe particles up to 105 ppm in
mass. Oil homogeneity was ensured by magnetic stirring. The results demonstrate the
capability of the fluid property sensor to detect and measure extremely high levels of Fe
contamination with viscosity, density and dielectric measurements.
Viscosity, density, and dielectric are strongly and linearly related to Fe contamination
level. Fe contamination also induces a slight decrease in resistivity. These noticeable
changes can be explained by the shape, high polarizability and charge characteristics of
metal particles.
Fe contamination in engine oil can be modeled using the following equations at a

ηth = ηi . 1 + 2 × 10−6 .FeCont(ppm.mass) (40)

ρth = ρi . 1 + 0.4 × 10−6 .FeCont(ppm.mass) (41)

εth = εi . 1 + 0.8 × 10−6 .FeCont(ppm.mass) (42)

Rpth = Rpi . 1 − 0.1 × 10−7 .FeCont(ppm.mass) (43)
Appl. Sci. 2021, 11, 5642 23 of 29
13 24 0.88 6

0.86 3
12 12
0.84 0
11 0
0.82 -3
10 -12 0.80 -6
0 2x104 4x104 6x104 8x104 1x105 0 2x104 4x104 6x104 8x104 1x105
Fe Contamination ppm mass Fe Contamination ppm mass
(a) (b)
2.5 8 2.6x107 6

2.5x107
2.4 6
Rp Ohms 100°C (o)
2
2.4x107
2.3 4 0
2.3x107
-2
2.2 2
2.2x107
-4
2.1 0 2.1x107 -6
0 2x104 4x104 6x104 8x104 1x105 0 2x104 4x104 6x104 8x104 1x105
Fe Contamination ppm mass Fe Contamination ppm mass
(c) (d)
Figure Figure
17. Fe contamination in engine
17. Fe contamination oil (15W40)
in engine at 100
oil (15W40) °C:◦ C:
at 100 (a)(a)viscosity;
viscosity;(b)
(b) density; (c)dielectric;
density; (c) dielectric; and
and (d)(d)
Rp.Rp.
These density,
Viscosity, models are plotted
and in Figure
dielectric 17 with the
are strongly andrelated accuracy
linearly specifications
related given
to Fe contamination
as full blue lines.
level. Fe contamination also induces a slight decrease in resistivity. These noticeable
Similar results can be obtained with copper (Cu) or other metals.
changes can be explained by the shape, high polarizability and charge characteristics of
metal3.7.
particles.
TBN, TAN and Ageing
Fe contamination in engine
Regular, punctual oilTAN
TBN and can measurements
be modeled using theinfollowing
are used equations at a
reference laboratories
to externally monitor oil conditions. Aging and contamination processes induce the
creation of different acidic compounds until oil degradation is complete. These acidic
η = η . 1 + 2×10 . FeCont . (40)
compounds accelerate oil degradation via different chemical reactions. For example,
metal contamination can be increased by corrosion induced by acidic compounds. To
counter the creation of ρ = ρcompounds
acidic . 1 + 0.4×10 . FeCont
and delay .
oil degradation, an alkaline reserve(41)
is added to the chemical composition of the oil. Thus, fresh oil has a high TBN value,
ε == ε8 to
typically ranging from TBN . 1TBN
+ 0.8×10
= 14, and. FeCont
a low TAN value,
. typically ranging from(42)
TAN = 1 to TAN = 4. During oil life, creation of acidic compounds leads to a continuous
decrease in TBN and aRp continuous
= Rp . increase in TAN.
1 − 0.1×10 When alkaline species are completely(43)
. FeCont .
depleted, levels of acidic compounds increase dramatically, and general oil degradation
These
is models
highly are plotted
accelerated in Figure
until the point of17 with thedeterioration
complete related accuracy specifications
and jelling. Dependinggiven
as full blue lines.
Similar results can be obtained with copper (Cu) or other metals.
3.7. TBN, TAN And Ageing

ated until the point of complete deterioration and jelling. Dependi
and application characteristics, limits on TBN and TAN values can
mize oil changes. For example, some manufacturers recommend p
Appl. Sci. 2021, 11, 5642 24 of 29
when TBN = TAN, thereby decreasing the risks of dramatic oil de
failure [46,47].
on oil composition
Typical TBNand and application characteristics,behaviors
TAN dynamic limits on TBNareand TAN values canin Fig
presented
be considered to optimize oil changes. For example, some manufacturers recommend
measurements are plotted
performing oil changes when TBN as= aTAN,
function of oxidation.
thereby decreasing the risks ofEngine oil (15W
dramatic oil
degradation and engine failure [46,47].
°C for 3000 h and regularly sampled and analyzed until complete d
Typical TBN and TAN dynamic behaviors are presented in Figure 18. TBN and TAN
TANmeasurements
were measured are plotted by
as a an external
function reference
of oxidation. Engine oil laboratory. The
(15W40) was stored at oil s
150 ◦ C for 3000 h and regularly sampled and analyzed until complete degradation. TBN
the same
and TAN samples used
were measured toexternal
by an determine the oxidation
reference laboratory. datacorrespond
The oil samples presented in
to the same samples used to determine the oxidation data presented in Figure 7.
TBN
10 TAN
8
TBN TAN mgKOH/g
6
Phase 1 Phase 2 Phase 3 Phase 4
5
2
0 5 10 15 20 25 30 35
Oxidation A/cm
Figure 18. Engine oil (15W40) TBN and TAN were measured in a reference laboratory.
Figure 18.
TheEngine oil a(15W40)
results show continuousTBN and
decrease TAN
in TBN and were measured
a continuous inTAN
increase in a reference
as
oxidation increases. The four different phases of oil degradation described in Figure 18 can
also be considered. During Phase 1 and Phase 2, the TBN value was higher than the TAN
The At
value. results show
the end of Phase 2,athecontinuous
TAN value reached decrease in and
the TBN value TBN and the
surpassed a continuo
TBN
value. TBN and TAN measurements corresponding to the 38 A/cm sample from Figure 18
oxidation
were not increases.
performed becauseThe four
of the different
excessive phases
degree of oil of from
degradation, oil degradation
which the oil d
can also be considered.
was indeed completely jelled. During Phase 1 and Phase 2, the TBN valu
The correlation between the absolute value of the difference |TBN-TAN| and the
TANresistivity
value.measurement
At the end of Phase
is presented in Figure2,18.the TANdemonstrate
The results value reached
the ability ofthe
the TBN
fluid property sensor to measure TBN and TAN values through resistivity measurements.
the TBN value. TBN and TAN measurements corresponding to the
As described in Figure 19, resistivity increased during Phase 1. Phase 1 is relatively
Figure 18 were
short-lived, not
and the levelperformed because
of resistivity increase dependsof on the
the oilexcessive degree of
chemical composition
and application characteristics. Then, the resistivity decreases during Phase 2 until it
which theaoil
reaches wasand
minimum indeed
increasescompletely
again during Phase jelled.
3. |TBN-TAN| has similar behavior,
The correlation between the absolute
starting from a high value (because fresh oil has alkaline reservevalue of concentration)
and low acid the difference
and decreasing during Phase 2 until a minimum is reached, and then increasing during
resistivity
Phase 3 duemeasurement
to creation of acidicis compounds
presented in Figure of18.
and neutralization Thespecies.
alkaline results A dem
2
clear correlation (R = 0.83) is demonstrated between resistivity and |TBN-TAN|. A
the fluid property sensor to measure TBN and TAN values throug
similar correlation has been described in the literature. |TBN-TAN| can be modeled using
ments.
Equation (44) at a constant temperature:
As described in Figure 19, resistivity increased during Phase 1

short-lived, and the level of resistivity increase depends on the oil
and application characteristics. Then, the resistivity decreases du
concentration) and decreasing during Phase 2 until a minimu
creasing during Phase 3 due to creation of acidic compounds
line species. A clear correlation (R2 = 0.83) is demonstrated bet
Appl. Sci. 2021, 11, 5642
TAN|. A similar correlation has been described in the25literatur
of 29
eled using Equation (44) at a constant temperature:

|TBN − TAN|= 1 .224 × 10−6 .RP +25.0778 (44)
7
y=0.000001224*-25.0778
Abs(TBN-TAN) R^2=0.83
6 Model
Phase 3
5
Abs(TBN TAN)
3
Phase 2
2
2.1x107 2.2x107 2.3x107 2.4x107 2.5x107 2.6x107

Rp Ohms
Figure 19. Correlation between Abs (TBN-TAN) and Rp measurements at 100 ◦ C.
Figure 19. Correlation

Simultaneous between do
resistivity measurements Abs
not (TBN-TAN) and
allow a precise direct Rp measureme
measurement of
TBN and TAN values. However, resistivity monitoring allows a prediction of |TBN−TAN|
∂Rp ∂Rp
and detection of Phase 2 (when ∂t < 0, TBN > TAN) and Phase 3 (when ∂t > 0,
TAN > TBN). As stated previously, Phase 3 corresponds to a level of oil degradation for
which an oil change is appropriate. |TBN-TAN|=1.224 × 10 .R + 25.07
-6
P
3.8. Incorrect Fluid Detection
Simultaneous resistivity measurements do not allow a pre
Filling with incorrect fluids can be dangerous for the engine. Indeed, engines are
TBN and TAN values. However, resistivity monitoring allo
designed to operate with determined oil characteristics. Use of the wrong oil may degrade
engine performance and could induce risk of failure.
TAN| and detection of Phase 2 (when < 0, TBN>TAN) a
Fluid property sensor measurements of four different oils are presented in Figure 20:
three engine oils, 0W40, 10W30 and 15W40, and one bio ISO32 hydraulic oil were studied.
TAN>TBN). As stated previously, Phase 3 corresponds to a
Each oil sample was stabilized and tested at different temperatures, ranging from 50 ◦ C
to 120 ◦ C. The results demonstrate the capability of the fluid property sensor to detect the
which an oil change is appropriate.
presence of an incorrect fluid with viscosity, density, dielectric, and resistivity measurements.
A fluid property sensor is capable of differentiating any type of engine oil or hydraulic
oil, mainly with viscosity measurements. Indeed, the viscosity of each sample is clearly
3.8. Incorrect Fluid Detection
identified by fitting with viscosity grade standard SAE J300: 15W40 oil has the highest
viscosity; 0W40 oil has a viscosity lower than those of the other engine oils at low tem-
These models are plotted in Figure 16 with the related ac
perature and has a viscosity similar to that of 15W40 oil at high temperatures; 10W30 oil
as full blue lines.
has lower viscosity at high temperature than the two other engine oils. ISO32 hydraulic
oil has a lower viscosity than the three engine oils. Density depends on oil composition
Filling with incorrect fluids can be dangerous for the eng
and cannot be predicted with the SAE J300 grade standard. Fluid property sensors clearly
differentiate the different oils by using density measurements. The three tested engine oils
signed to operate with determined oil characteristics. Use of
have similar dielectric constants, ε = 2.2 at 100 ◦ C and can easily be differentiated from the
engine performance and could induce risk of failure.
tested biohydraulic oil with ε = 2.7 at 100 ◦ C, although ISO32 hydraulic oils typically have
dielectric constants ranging between ε = 2 and ε = 2.4. Some differences between the fluids
Fluid property sensor measurements of four different oils
can also be observed from resistivity values [48,49].
three engine oils, 0W40, 10W30 and 15W40, and one bio ISO32
Each oil sample was stabilized and tested at different temper
to 120 °C. The results demonstrate the capability of the fluid p
presence of an incorrect fluid with viscosity, density, dielectr
ments.
Appl. Sci. 2021, 11, 5642 26 of 29

Effective detection of incorrect fluid is made possible by modeling the desired fluid
for the considered application and fixing thresholds for each physical parameter. The
threshold levels will depend on the application and the different incorrect fluids that may
be encountered.
40 0.95
0W40 0W40
10W30 10W30
15W40 0.90 15W40
30 Bio Hydraulic Bio Hydraulic
Density gm/cc
Viscosity cP
0.85
20
0.80
10
0.75
0 0.70
50 60 70 80 90 100 110 120 50 60 70 80 90 100 110 120
(a) (b)
3.0 2.8x107
0W40 0W40
10W30 10W30
2.8 15W40 2.6x107 15W40
Bio Hydraulic Bio Hydraulic
Dielectric
2.6 2.4x107
Rp Ohms
2.4 2.2x107
2.2 2.0x107
2.0 1.8x107
50 60 70 80 90 100 110 120 50 60 70 80 90 100 110 120
(c) (d)
Figure 20.Figure
Measurements of 0W40, 10W30, 15W40 oils and biohydraulic oil: (a) viscosity; (b) density; (c) dielectric; and (d)
20. Measurements of 0W40, 10W30, 15W40 oils and biohydraulic oil: (a) viscosity; (b) density; (c) dielectric; and
Rp. (d) Rp.
4. Conclusions
A fluid property sensor is capable of differentiating any type of engine oil or hydrau-
It haswith
lic oil, mainly beenviscosity
shown that the viscosity ofIndeed,
measurements. mineral-based oils canof
the viscosity beeach
reliably measured
sample is clearly
by a microacoustic sensor. However, the influence of particular polymer additives, such
identified by fitting with viscosity grade standard SAE J300: 15W40 oil has the highest
as OCP, on macroscopic viscosity is not detected by the sensor. Specifically, neither the
viscosity; 0W40 effect
thickening oil has a the
nor viscosity lowerof
degradation than those of the
the viscosity otherpolymers
modifier engine oils
are at low temper-
detected by
ature the
andmicroacoustic
has a viscosity similar to that of 15W40 oil at high temperatures; 10W30
sensor used. Accordingly, in the case of engine oil containing viscosity oil has
loweradditives
viscosityof at high
high temperature
molecular weight, thethan the output
sensor two other engine
does not oils.with
correlate ISO32 hydraulic oil
a conventional
viscosity measurement. This behavior was attributed to the fact that
has a lower viscosity than the three engine oils. Density depends on oil composition the sensor probes a and
thin oil film and thus does not detect any changes induced by structures
cannot be predicted with the SAE J300 grade standard. Fluid property sensors clearly dif- or mechanisms
associated
ferentiate with characteristic
the different oils by usinglengths that are
density larger or of the
measurements. Thesame
threemagnitude as the oils
tested engine
have similar dielectric constants, ε = 2.2 at 100 °C and can easily be differentiated from the
tested biohydraulic oil with ε = 2.7 at 100 °C, although ISO32 hydraulic oils typically have
dielectric constants ranging between ε = 2 and ε = 2.4. Some differences between the fluids
Appl. Sci. 2021, 11, 5642 27 of 29
penetration depth of the acoustic wave in the oil. Alternatively, the effect could also be
caused by the high oscillation frequency and/or the small oscillation amplitudes associated
with the microacoustic sensor (in comparison to conventional methods).
At the same time, experiments with artificially deteriorated oils indicate that the
relative increase in the sensor signal provides more direct information on the age of the
oil, using oxidation level rather than the conventionally measured “macroscopic” viscosity.
In particular, it was found that the sensor signal correlates much better with the degree of
oxidation of the oil. This can be explained by the fact that oxidative deterioration causes an
increase in the base oil viscosity. Conventional viscosity measurements do not detect this
increase effectively since deterioration of viscosity modifiers (if present) yields a decrease
in the macroscopic viscosity, which represents an effect trending in the opposite direction.
In experiments with artificially aged oil samples, it has been shown that the sensor
signal correlates with the measured value of the total acid number (TAN) for artificially
aged oil. The acidity of artificially aged oils is caused by the oxidative degradation of the
oil itself, and the presence of oxidized thermal degradation products can be detected by
the microacoustic sensor regardless of the additive content in the oil. Thus, the sensor
is potentially suited for the detection of oxidation-induced viscosity changes caused by
thermal deterioration of the oil.
In association with a specific oil (15W40 grade oil, which is designated for use in
heavy-duty truck engines) condition algorithm with the main strategy described in this
paper, the fluid property sensor is able to directly monitor the heavy-duty truck engine
oil conditions, predict remaining oil life and achieve optimization of oil change intervals,
minimize the risk of dramatic engine failure, and reduce maintenance costs.
Author Contributions: Data curation, H.S., Y.L. and J.T.; form analysis, H.S.; funding acquisition,
J.T.; software, H.S., Y.L. and J.T.; writing—original draft, H.S.; writing—review and editing, H.S. and
Y.L. All authors have read and agreed to the published version of the manuscript.
Funding: This research is financially supported by the Natural Science Foundation of China
(No. 51508304 and No. 41275133).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Data are contained within the article.
Acknowledgments: This work was supported by the National Natural Science Foundation of China
(No. 51508304 and No. 41275133). The authors are grateful to the China Environmental Monitoring
Center for their cooperation. In addition, Hao Sun wants to thank, in particular, the patience, care,
and support from Qi Li.
Conflicts of Interest: The authors declare no conflict of interest.
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Appl. Sci. 2021, 11, 5642. https://doi.org/10.3390/app11125642 https://www.mdpi.com/journal/applsci

Figure 1. Structure of a sensor-assisted algorithm for a lubrication-monitoring system. The indirect

Figure 2. Physical view of quartz tuning fork sensor.

Table 1. Measurement parameters of the sensor.

Measurement Parameter Measurement Range Precision

Table 1. Measurement parameters of the sensor.

crocontroller system control circuit and impedance measurement circuit based on AD

Appl. Sci. 2021, 11, x FOR PEER REVIEW 5 of 28

Figure 4. AD5933 peripheral circuit

2.3. Engine Oil

Proper lubrication, sealing, and power transmission are ensured by appropriate

log(log µ + 0.7) = B − C. log(T + 273.15) (6)

where T is the temperature in ◦ C and F and G are oil-dependent constants.

3. Oil Ageing Processes and Sensors for Fluid Property Detection

Density Relative Evolution % (*)

2.5x107 10 Rp Relative Evolution % (*)

Rp Ohms 120°C (o)

Phase 1 Phase 2 Phase 3 Phase 4

Table 2. Four different phases of oil oxidation process.

Stage Oxidation A/cm

Table 2. Four different phases of oil oxidation process.

Stage Oxidation A/cm

Density gm/cc 100°C

15W40 Brand A 15W40 Brand A

Oxidation Time hours Oxidation Time hours

ε = ε . 1 + 0.5 × 10 . Ox. (13)

Appl. Sci. 2021, 11, 5642

Viscosity Relative Evolution % (*)

Density Relative Evolution % (*)

Density gm/cc 100°C (o)

Rp Relative Evolution % (*)

Rp Ohms 100°C (o)

2.15 -2 2.1x107 -10

Phase 1 Phase 2 Phase 3

1500 15W40 new

Density Relative Evolution % (*)

2.5x107 4 Rp Relative Evolution % (*)

Rp Ohms 50°C (o)

3.3. Coolant Contamination

Viscosity Relative Evolution % (*)

Density Relative Evolution % (*)

Density gm/cc 50°C (o)

Rp Relative Evolution % (*)

Rp Ohms 50°C (o)

3.4. Fuel Contamination

log(log(µ + 0.7)) = B − C. log(T + 273.15) (24)

Appl. Sci. 2021, 11, 5642 20 of 29

Viscosity Relative Evolution % (*)

Density Relative Evolution % (*)

Density gm/cc 100C (o)

Rp Relative Evolution % (*)

Rp Ohms 100°C (o)

Resistivity does not

Rp = Rp . 1 − FuelDil% /100 + Rp . FuelDil % /100 (35)

Density Relative Evolution % (*)

Rp Ohms 100°C (o)

3.6. Metal Contamination

Appl. Sci. 2021, 11, 5642 23 of 29

Viscosity Relative Evolution % (*)

Density Relative Evolution % (*)

Rp Relative Evolution % (*)

Rp Ohms 100°C (o)