Received: 20 March 2017 Revised: 20 June 2017
DOI: 10.1002/ls.1403
RESEARCH ARTICLE
A field test method to quantitatively determine oxidation
stability of gasoline engine oil
Lei Wei1 | Haitao Duan1 | Song Chen1 | Dan Jia1 | Xuzheng Qian1 | Bingxue Cheng1 |
Jianfang Liu1,2 | Jian Li1
1
State Key Laboratory of Special Surface
Protection Materials and Application
Technology, Wuhan Research Institute of
Materials Protection, Wuhan 430030,
China
2
College of Biological and Pharmaceutical
Engineering, Wuhan Polytechnic
University, Wuhan 430023, China
Correspondence
Jian Li, State Key Laboratory of Special
Surface Protection Materials and
Application Technology, Wuhan Research
Institute of Materials Protection, Wuhan
430030, China.
Email: lijianwuhan@tom.com
Funding information
National Natural Science Foundation of
China, Grant/Award Number: 51575402;
National Basic Research Program of China
(973 program), Grant/Award Number:
2013CB632303
1 | INTRODUCTION
Lubricating oils played an important role in machine
system. Lubricating oils served as coolants and corrosion
protectors and helped remove contaminants and debris
from the machine interior. Hence, lubricants may be
considered to be the blood of mechanical system.1,2
Lubricating oil must be changed to counter degradation
and contamination and to maintain the quality necessary
to protect the machine.3,4 Reasonable oil drain interval
can save the energy resource, protect the environment,
and decrease the maintenance cost. Oxidation stability is
one of the most important parameters of lubricating oil
to evaluate the service life in high temperature and
extreme applications. The more resistant a lubricant is
to oxidation, the less tendency it has to form
deposits, sludge, and corrosive by products in industry
Lubrication Science. 2017;1–8.
Accepted: 21 August 2017
Abstract
As oxidation stability of engine oil was hard to evaluate in field, this paper tried
to propose a field test method to determine the oxidation onset temperature
(OOT) of gasoline engine oil. A theoretical model of grey average value of oil
spot image and OOT was established by using spot test method, image
processing, and Pressure Differential Scanning Calorimetery method. The oil
sample unknown OOT was taken to spot test and image processing in field to
obtain the grey average value. The OOT can be calculated by bringing the grey
average value to the established theoretical model. This approach was
successfully used for OOT determination of 4 different kinds of engine oils with
good accuracy and precision. The absolute error of mineral oils was less than
4.52°C, and synthetic oils were less than 1.2°C. This convenient, low‐cost, and
reliable method can achieve OOT of engine oil in field determination and
provide reference for engine oil drain interval evaluation.
KEYWORDS
engine oil, field test, image processing, oxidation stability, spot test
application.5-7 There are some commonly used methods
to evaluate the oxidation stability of lubricating oil, such
as rotary bomb oxidation test (RBOT, ASTM D2272),8,9
oxidation stability test (ASTM D943),10 FTM 791‐3462
coking test, and differential scanning calorimetery
(DSC)/PDSC (ASTM E 2009‐02).11 In RBOT test, a 50‐g
sample plus a 5‐g amount of water and a high‐purity
(99.9%) copper coil are placed in a beaker and loaded into
a pressure chamber, sealed and then filled with 99.5%
pure oxygen gas at a pressure of 0.62 MPa, and the entire
pressurised chamber is rotated in an oil bath at 150°C.
The end of test was considered to be when the oxygen
pressure fell rapidly with oil oxidation. The RBOT test
method has been widely used in testing oxidation stability
of turbine oil. It is hard to maintain the oil bath at 150°C.
It is also very important to ensure the operator's safety
that avoid being splashed by very hot oil.12-14 In procedure
wileyonlinelibrary.com/journal/ls Copyright © 2017 John Wiley & Sons, Ltd. 1
2 WEI ET
of the ASTM D943 method, a mixture of lubricant
(300 mL) and water (60 mL) is exposed to oxygen at a rate
of 3.0 L/h in the presence of solid metal iron‐copper coil
catalyst at 95°C. The total acid number, viscosity, and
residual carbon parameters of the oxidative lubricating
oil was used to characterise the oxidation level. The
ASTM D943 method has widely used in industry to assess
storage and long‐term service oxidation stability of
lubricating oils, steam‐turbine oils, etc. While the method
was time consuming. More than 300 hours were needed
in some determination. FTM 791‐3462 coking test is used
for evaluating the oxidative stability of engine oil by
heating the lubricating oil to contact with the high
temperature (about 320°C) aluminium sheet. The coking
tendency reflects the oxidative stability of the testing
samples. Two hundred fifty–millilitre oil sample and
6 hours are needed for the FTM 791‐3462 method.15 The
DSC technique involves raising or lowing the temperature
of a sample and reference at a constant rate. By measuring
the rate of heat flow extracted or supplied to the sample as
a result of exothermic or endothermic reactions, the
thermal properties of the sample can be determined. The
oxidation onset temperature (OOT) and oxidative induc-
tion time are commonly used to characterise the oxidation
stability of the lubricating oil by DSC. The PDSC is based
on DSC technique bringing pressure to the heating
furnace. The use of a pressurised environment has also
been recognised as essential to suppress the evaporation
of the lubricant.16,17
The trend of engine oil oxidation stability test method
is now to be capable of representing field performance
with a short testing time. It is not usually possible to take
a large number of lubricating oils by running the expen-
sive and time‐consuming apparatus to determine the
oxidation stability in field. All the methods given above
cannot fulfil field test demand. This paper try to propose
a method based on spot test, image processing, and PDSC
for OOT of gasoline engine oil field determination.
2 | EXPERIMENTAL DETAILS
2.1 | Materials and apparatus
Four kinds of gasoline engine oils have been researched in
road test. They were Shell HELIX ULTRA SAE 5W‐30
commercial all‐synthetic engine oil, SAE 5W‐40 commer-
cial semisynthetic oil special for Volkswagen engine, SAE
5W‐20 mineral oil special for Hyundai engine, and SAE
5W‐40 mineral oil special for Citroen engine. The PDSC
was tested by NETZSCH HP204 Differential Scanning
Calorimetery (NETZSCH, Germany). The quantitative
filter paper used in spot test was Shuangquan
AL.
(Shuangquan, China). The oil spot image was taken by
Xiaomi 4C smart phone (Xiaomi, China).
2.2 | Spot test method
Spot test method dates back to the early 1950s. It is one of
the oldest techniques used to identify excessive engine
soot, evaluate the dispersancy of lubricant, and detect
the presence of glycol and other contaminants in
engine crankcase lubricants.18,19 Spot test method has
characteristic of simple operation, low‐cost, and field
determination. The precision of spot test depended on
the experience of the operator, which limited the applica-
tion to a certain extend. Some scholars tried to use image
processing method to determine the oil spot diameters to
calculate the dispersancy property quantitatively.20
Four steps, spot test, image processing, relation model
establishing, and OOT calculating, were contained in the
method to test OOT of gasoline engine oil. To illustrate
the proposed method procedure, a commercial Shell
HELIX ULTRA SAE 5W‐30 all‐synthetic engine oil was
taken as an example to present the details of the proposed
method.
Step 1: 3 to 5 engine oil samples of different mileages
were collected and taken to spot test. The oil samples were
collected with soft rubber tubes and syringes after engine
stopped about 1 to 2 hours. Approximately 10‐mL oil
sample was removed from the crankcase and put into a
15‐mL centrifuge tube for spot test. At room temperature
and no wind environment, a 1‐mL pipette was immerged
into the oil sample about 20‐mm deep and pulled up
vertically. The fifth or sixth oil drop was taken to the
centre of a piece of 90‐mm diameter quantitative filter
paper, which was put on a 65‐mm plastic cup to hang
the centre of the filter paper in the air. After the oil drop
diffused in the filter paper for 2 hours, 2 or 3 oil ring
may formed on the filter paper. The oil spot images of
different mileages were shown in Figure 1. The oil spot
image was taken by a mobile phone and transmitted to
computer through Bluetooth or Internet.
Step 2: The oil spot image was processed with Matlab
software. As Figure 2A shown, the colour oil spot image
obtained by mobile phone camera was converted to grey
image. The oil spot contained 3 parts, oil ring zone (label
1), diffusion ring zone (label 2), and deposition ring zone
(label 3). The grey histogram (Figure 2B) was outputted
according to the converted grey image. The segmentation
threshold values were assured according to the wave
trough (label 4) of the grey histogram. The oil spot was
segmented in 4 parts with the segmentation threshold
values obtained above and outputted as binary image.
The 4 parts were the blank zone, the oil ring zone, the
diffusion ring zone, and the deposition ring zone of oil
WEI ET AL. 3

FIGURE 1 Oil spots of different mileages [Colour figure can be viewed at wileyonlinelibrary.com]

FIGURE 2 Oil spot image process [Colour figure can be viewed at wileyonlinelibrary.com]

spot, respectively. For the segmentation part had some
noise (labels 5, 6, and 7 in Figure 2), which may decrease
the precision of the image processing. So the noise should
be removed. The white area was the diffusion zone of the
oil spot image presented in Figure 2D. The labels 5 and 6
in Figure 2D were the exterior noise to the diffusion zone,
and the label 7 in Figure 2E was the inner noise. To
remove the exterior noise, the area of the white zone
was calculated by the function “STATS = regionprops
(BW, ‘area’)” contained in Matlab software. The area of
the white zone was taken as the threshold to remove the
exterior noise. With the function “BW = bwareaopen
4 WEI ET
(BW, area)”, the noise area zone, which were smaller than
the threshold, were removed (Figure 2E). After the
exterior noise were removed, the image was reversed with
the function “BW = ~BW” and the inner noise was
removed with the function “BW = bwareaopen (BW,
5000).” Finally, reversed the image again, the full
denoised diffusion zone of oil spot was obtained
(Figure 2F). With the same method, the denoised deposi-
tion zone, diffusion zone, and oil zone were shown in
Figure 2G‐I.
The denoised binary image was converted to grey
image and calculated the grey average value Ginitial of
the oil spot zone. The grey average value of the blank filter
paper Gblank and the grey value of the filter paper without
oil spot Gbackground were calculated in Matlab. As the
mobile phone camera would have errors at different
conditions, the oil spot grey average value was corrected
with the equation Gaverage = (Gblank−Gbackground) + Ginitial
to decrease the error. The correction grey average value of
the oil spot was obtained.
Step 3: The OOT of the lubricating oil samples, which
collected in step 1, were tested with NETZSCH HP 204
PDSC. The experiment pressure was 3.5 MPa, and the
heating rate was 10 K/min. The relation model of the grey
average value and the OOT can be established.
Step 4: To measure the oil sample unknown OOT.
Based on the relation model established above, the OOT
could be calculated with the grey average value. After
the oil spot grey average value was known, the OOT could
be calculated easily by the established model. The oil
sample needed to be tested was collected and taken to
FIGURE 3 Oil spot images under strong light [Colour figure can be viewed at wileyonlinelibrary.com]
FIGURE 4 Oil spot images under low light [Colour figure can be viewed at wileyonlinelibrary.com]
AL.
spot test in field as the step 1 presented. The grey average
value was obtained by spot test and image process method
as the step 2 given above. The OOT was calculated by
bringing the grey average values of spot image to the
relation model equation established in the step 3. The
OOT of engine oil tested in filed was achieved.
3 | R ESULTS A ND DISCUSSION
3.1 | Spot test under different light
conditions
The spot image played an important role in the proposed
method. The spot image may have huge difference while
taking pictures under different light conditions. Two
groups of spot tests with a SAE 5W‐20 mineral oil were
taken under different light intensity to study the
reliability of the proposed method. Four oil samples
(0, 1096, 2010, and 3219 km) of SAE 5W‐20 mineral oil
special for Hyundai engine were taken to spot test. The
spot images with strong light and low light were shown
in Figures 3 and 4, respectively. As Figures 3 and 4
presented, the oil spot images taken under strong light
were brighter, and the oil ring were more obvious than
the oil spot images taken under low light. Four oil
samples given above were taken as modelling data to
establish the relation model with OOT. The spot image
under strong light and low light was processed with the
method given above. The results of image processing were
presented in Table 1. The errors of Gaverage of strong light
image between Gaverage of low light image were less than
WEI ET AL. 5

TABLE 1 Processing results of images under strong light and low light

Strong Light Low Light

Mileage (km) Ginitial Gbackground Gaverage Ginitial Gbackground Gaverage Errors
0 173.23 200.79 172.44 140.11 167.72 172.39 −0.05
1096 161.61 200.84 160.77 129.56 169.52 160.03 −0.74
2010 156.08 201.51 154.57 119.17 162.98 156.19 1.62
3219 152.13 200.72 151.40 114.15 162.88 151.27 −0.13

1.62. It indicated that the proposed image processing 3.2 | Spot test with different oils
method had high accuracy and precision under different
The proposed method was applied in other 3 kinds of oils.
light conditions.
They were commercial SAE 5W‐30 all‐synthetic oil,
The established relation models of grey average value
and OOT under strong light and low light were shown in
Figure 5. Both of the R2 is larger than 0.90, which
indicates the model that represents the relation of data
well. The equations of the models were similar. Oil
samples of 4353 and 5396 km were taken as the tested
data to verify the relation models. The results of
calculated OOT with the established models were shown
in Table 2. As presented in Table 2, for the model
established with image taken under strong light, the
errors between calculated and PDSC tested OOT value
of 2 oil samples were −0.43°C and 0.26°C, respectively.
The low light were −1.77°C and 0.36°C. The errors of
image taken under different light environment were
small. It indicated that the proposed method had
high accuracy and precision under strong light and low
light conditions. FIGURE 6 Theoretical model of SAE 5W‐30 all‐synthetic oil

FIGURE 5 Theoretical model of SAE 5W‐20 mineral oil, A, strong light; B, low light

TABLE 2 Results of calculated OOT with the established models

Strong Light Low Light

Errors of
Mileage Correction Grey Calculated OOT Correction Grey Calculated OOT Tested OOT Strong Errors of Low
(km) Average Value Value (°C) Average Value Value (°C) Value (°C) Light (°C) Light (°C)
4354 145.82 218.27 145.28 216.93 218.7 −0.43 −1.77
5396 143.56 215.46 144.19 215.56 215.2 0.26 0.36
6 WEI ET AL.

TABLE 3 Tested results and calculated results of SAE 5W‐30 all‐synthetic oil

Correction Grey Calculated OOT Tested OOT Absolute

Mileage (km) Average Value Value (°C) Value (°C) Error (°C)
2750 143.71 228.45 228.4 0.05
2962 143.93 228.60 227.4 1.20
3503 140.07 225.98 226.6 −0.62

commercial SAE 5W‐40 semisynthetic oil, and commer-
cial SAE 5W‐40 mineral oil. Five SAE 5W‐30
all‐synthetic engine oil samples at different mileages
(0, 1084, 1305, 1923, and 2348 km) were taken as
modelling data to establish relation model of average
value and OOT shown in Figure 6. The equation of the
relation model was as follow:
y ¼ 0:68x þ 130:73;
where x is the grey average value and y is the OOT value.
The Adj. R2 was 0.96, which indicates that the model
represents the relation of data well. The lubricating oil
samples of 2750, 2962, and 3503 km were taken as the
prediction data to test the relation model. The grey
average values, the prediction OOT calculated by relation
model (Equation 1), and the PDSC results were shown in
Table 3. The absolute errors ranged from −0.62°C to
1.2°C.
As presented in Figure 7, five oil samples at different
mileages (0, 233, 606, 943, and 1258 km) of SAE 5 W‐40
semisynthetic oil were taken as modelling data. The
established model equation was as follow:
y ¼ 0:83x þ 108:71; (2)
where x is the grey average value and y is the OOT value,
and the Adj. R2 was 0.99. The engine oil samples of 1577,
(1)
1838, and 2249 km were the prediction data. The predic-
tion OOT calculated by theoretical model (Equation 2)
and the PDSC tested results were shown in Table 4. The
absolute errors ranged from −0.37°C to 0.77°C.
Four SAE 5W‐40 mineral oil samples (0, 592, 1264,
and 2056 km) were taken as the modelling data. The
established relation model of grey average value and
OOT was shown in Figure 8. The model equation was as
followed:
y ¼ 1:67x−39:89; (3)

FIGURE 7 Theoretical model of SAE 5W‐40 semisynthetic oil FIGURE 8 Theoretical model of SAE 5W‐40 mineral oil

TABLE 4 Tested results and calculated results of SAE 5W‐40 semisynthetic oil

Correction Grey Calculated OOT Tested OOT Absolute

Mileage (km) Average Value Value (°C) Value (°C) Error (°C)
1577 140.99 225.73 226.1 −0.37
1838 139.88 224.81 224.2 0.61
2249 137.43 222.77 222.0 0.77
WEI ET AL.
TABLE 5 Tested results and calculated results of SAE 5W‐40 mineral oil
Correction Grey
Mileage (km) Average Value
2664 151.44
3547 150.59
3883 146.33
where x is the grey average value and y is the OOT value.
The Adj. R2 was 0.95. The verification data, oil samples of
2664, 3547, and 3883 km, were brought to the relation
model (Equation 3) to calculate the theoretical OOT.
The PDSC test results were shown in Table 5. The abso-
lute errors were ranged from −4.52°C to 2.1°C.
The established models of oil spot grey average value
and OOT of the 4 different kinds of oils were linear. All
the Adj. R2 values were above 0.90, which means the rela-
tion models have high reliability. As the linear model
equation shows:
y ¼ ax þ b;
only 2 grey average values and OOT values were needed
to confirm the slope coefficient “a” and intercept “b” in
theory. It may cause large error for just taking 2 oil sam-
ples as modelling data. More oil samples for establishing
model and higher precision of the theoretical model
would be obtained. It would also be more time consuming
and costly. With optimal calculation, 3 to 5 oil samples
were taken to establish the relation model that can
achieve both high precision and efficiency.
The grey value in oil spot image indicated the depth of
colour after lubricating oil dispersing on the filter paper.
The colour of oil spot depended on the colour of lubricat-
ing oil and the content of sediments and contaminants in
lubricating oil. With the increase of service time, lubricat-
ing oil cannot avoid being oxidised. Antioxidants oxidised
into oxidation products and impurity compound in base
oil oxidised into deep colour organic acid or heterocyclic
compound may dark the colour of lubricating oil. The
lubricating oil was degrading with the increase of service
time. The content of sediments, contaminants, and jelly
generated after oil oxidation increase with the detergent‐
dispersant depleting. These undissolved products aggre-
gated in the centre of the filer paper and increased the
colour of the oil spot image. The OOT indicated the anti-
oxidant capacity of lubricating oil. Both the OOT and the
grey value were closely related to the oxidation of
lubricating oil. The proposed method established the
relationship of oxidation stability of lubricating oil and
in field oil spot test method.
7
Calculated OOT Tested OOT Absolute
Value (°C) Value (°C) Error (°C)
213.01 215.4 −2.39
211.60 209.5 2.10
204.48 209.0 −4.52
4 | C ON C L U S I ON S
The proposed method shows great potential for field
evaluating the oxidation stability of gasoline engine oil.
The conclusions were as follow:
1. The given approach successfully achieves the oxida-
tion stability of engine oil quantitative determination
in field by combining the advantages of spot test with
PDSC test method. The proposed method has high
accuracy and precision under different light intensity
and different kinds of engine oils. The absolute errors
of synthetic oil were less than 1.2°C, and mineral oil
(4)
was less than 4.52°C.
2. The field test procedure of the method is simple, safe,
and convenient. The method does not depend on
expensive apparatus and professional experimenters.
The oil spot images obtains by mobile phone camera
and transmits to computer by wireless communica-
tion that gives great convenience to the image pro-
cessing. With the Matlab program, the grey average
values of oil spot can be calculated in seconds. The
modelling process of the relation model was feasible
and reliable.
3. The lubricating system of vehicle is complicated. The
degradation of lubricating oil is coupled with
mechanical and chemical action. The results of this
study are based on 4 typical engine oils. More com-
monly used results needs to enlarge the number of
oils. This paper can provide a reference to evaluate
the engine oil status quantitatively and determine
the oil drain interval scientifically.
ACKNOWLEDGEMENTS
This work was supported by the National Natural
Science Foundation of China (No. 51575402) and National
Basic Research Program of China (973 program) (No.
2013CB632303).
ORCID
Lei Wei http://orcid.org/0000-0001-7139-923X
8 WEI ET
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How to cite this article: Wei L, Duan H, Chen S,
et al. A field test method to quantitatively
determine oxidation stability of gasoline engine oil.
Lubrication Science. 2017;1–8. https://doi.org/
10.1002/ls.1403