DE LA SALLE UNIVERSITY

Gokongwei College of Engineering

Chemical Engineering Department

Engineering Thermodynamics Laboratory

Final Laboratory Report

Experiment # 7
Determination of Flash Point, Fire Point, and
Carbon Residue of Lubricating Oils

Group Name N3P Section EA1

NAME SIGNATURE Criteria Score

1. Cellona, Kimberley B. Content (50%)
2. Dar, Lloyd Ross M. Presentation (25%)

3. Javier, Mona Lyndsay C. Relevance (25%)

4. Lopez, Maristela Ann F. Total (100%)

5. Soriano, Elijah Jeremie D. Percentage Equivalent

3 July 2018 10 July 2018

Date of performance Date of Submission

Dr. Lawrence P. Belo

Instructor
Engineering Thermodynamics Laboratory

Determination of Flash Point, Fire Point, and

Carbon Residue of Lubricating Oils
Kimberley B. Cellona, Lloyd Ross M. Dar, Mona Lyndsay C. Javier,
Maristela Ann F. Lopez, Elijah Jeremie D. Soriano
Department of Chemical Engineering, Gokongwei College of Engineering, De La Salle University,
2401 Taft Avenue, Manila 1004, Philippines

ARTICLE INFO ABSTRACT

AY 2017–2018 | Term 3
LBYCHED EA1
Final Laboratory Report
Experiment # 7
Date Performed: July 3, 2018
Date Submitted: July 10, 2018
Keywords
flash point, fire point, open-cup,
carbon residue, carbon residue test,
viscosity
The two-part experiment tested both the flash and fire points and carbon residue of
three commercial lubricating oils, namely Petrolube, Shell, and Sphinol. For the first
part, the samples were placed in an open cup, where it was heated until both flash
and fire points were achieved. Meanwhile, for the second part, the weighed samples
were allowed to combust inside a series of crucibles, dried, and re-weighed. Overall,
Sphinol had the most optimum performance for both tests, exhibiting the lowest flash
and fire points. In addition, Sphinol also had the least carbon residue present after
combustion, which signifies its minimal capacity to develop residues under extremely
high temperatures while undergoing the most complete combustion as compared with
the other samples. The results were supported with the oil’s low viscosity among the
samples as determined from the previous experiment, indicative of its weaker
intermolecular forces which allow for the capability to flow easier in pipes for
various uses.

I. INTRODUCTION hydraulic liquids is desired for it means that the

A lubricating oil is sometimes referred to as the blood
of an engine. They reduce friction between engine parts
which is what causes them to wear easily. Noise
operation is significantly reduced by using lubricating
oils. Lubricating oils are also used for cleaning engine
parts. [1] Before a lubricating oil could be used in a
certain engine, it is important to review its qualities first.
[2] Three important properties of lubricating oils are the
flash point, fire point, and carbon residue.
Flash and Fire Points
Both the flash and fire points of lubricating oils are
important in determining fire resistance and volatility.
Flash point is the lowest temperature at which the
lubricating oil gives off vapor, and when mixed with air
ignites, but not continuously. Fire point, on the other
hand, is the lowest temperature when the combustion of
the lubricating oil is sustained. [3] Flash point also
determines transportation and storage temperature
requirements of the lubricating oil. A high flash point for
[1]
resistance of the liquid to combustion is high. Lubricants
with flash points lower than 100 F will require special
handling instructions. Moreover, as the flash point
increases, the fire point follows. The fire point is usually
8 to 10% higher than the flash point. In measuring the
flash and fire points of lubricating oils, the closed-cup
and open-cup methods are used. The closed-cup method
records a flash point lower than a flash point recorded
using the open-cup method since it prevents vapor from
escaping as compared to the latter. However, in this
experiment, the open-cup method is applied.
Carbon Residue
The tendency of lubricating oils to form carbon
deposits at high temperatures and inert atmospheres is
called the carbon residue of a fuel. This may be
expressed as the Micro Carbon Residue (MCR) or the
Conradson Carbon Residue (CCR), which are
numerically almost the same. [4] Although the
relationship between carbon residue and engine
performance is poor, the carbon residue number is
considered in determining the combustibility and
carbonaceous deposit-forming tendencies of a lubricating
oil. A lubricating oil who has a higher MCR or CCR
number has a higher tendency of forming carbon residue.
Higher MCR or CCR values also mean that the fuel is
harder to oxidize and has a slower burning rate, which
may cause both incomplete combustion and damage of
the engine. [2] Modern engines can tolerate a wide range
of MCR or CCR values. However, a high carbon residue
value may cause problems in older engines, which may
experience difficulty in burning fuel for carbon residue
having a value higher than 12%m/m. [5] All fuels have
carbon residue. To lower its value, the fuel must be
mixed with a distillate. [2]

In this experiment, the students are expected to (1)

determine the flash point of various lubricating oils using
the open cup method, (2) determine the fire point of
various lubricating oils using the open cup method, (3)
compare the flash point and fire point of different
lubricating oils, and (4) determine the carbon residue of
lubricating oils after combustion.
Figure 1. Cleveland Open-cup Flash Tester
In the carbon residue test, a Conradson Residue
setup was used as shown in Fig. 2. The porcelain
crucible is put inside, and the setup was heated
using a Bunsen burner.

II. METHODOLOGY

2.1 Materials and Reagents

Three samples of lubricating oils were used: shell,
Sphinol, and Petrolube. Three porcelain crucibles
with covers were also used, each used for a different
sample. In handling hot crucibles, a crucible tong
was used. Finally, a glass desiccator was used in
cooling the samples to avoid moisture.

2.2 Equipment
In determining the flash and fire points of the three
samples, the open-cup method was used. Figure 1
shows the Cleveland Open-cup Flash Tester used in
the experiment. Figure 2. Conradson Carbon Residue setup

2.3 Experimental Procedure

Flash and Fire Points
The lubricating oil was poured into the oil cup until
the brim of the cup. The electric heater was turned on
before placing the oil cup on top. The heater was then
allowed to heat evenly by moving the flame around
the lubricating oil, avoiding the thermometer as it
may cause the glassware to break. The temperature
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[2]
 when the first flash of vapor appears is recorded as
the flash point. After getting the flash point, the
heating of the lubricating oil is continued until a small
fire appears. The temperature when the first flash of
fire appears is then recorded as the fire point. These
steps were done for the shell, Sphinol, and Petrolube
samples.
Carbon Residue Test
Three porcelain crucibles, each with two glass beads
inside, were weighed. Approximately ten grams of
lubricating oil samples were poured into separate
crucibles. The first porcelain crucible was placed
inside an iron crucible, which is also inside a
Skidmore crucible. The set-up was then heated using
a Bunsen burner. As heating continued, flames
appeared and was allowed to settle down and cool
down for ten minutes in the glass desiccator before
weighing the porcelain crucible again. These steps
were done for the shell, Sphinol, and Petrolube
samples.
III. RESULTS & DISCUSSION
From the flash and fire points test, the flash points
observed from the experiment range from 132oC to
158oC, while the fire points followed higher from 192oC
to 222oC. Among the lubricating oils tested, Petrolube
exhibited the highest flash point followed by Shell and
Sphinol, respectively. On the other hand, Shell had the
highest fire point, followed by Petrolube and Sphinol
with close values. Further, the differences between the
flash point and fire point are 76 oC for Shell, 60oC for
Sphinol, and 38oC for Petrolube accordingly. Table 1
lists the individual data obtained for each sample for this
test.
Afterwards, the carbon residue test showed that the
carbon residue left after combustion of each lubricating
oil by weight percent of the original sample are 1.3, 0.56,
and 1.8 for Shell, Sphinol, and Petrolube accordingly.
Thus, Petrolube produced the most amount of soot in
contrast to Sphinol with the least byproduct deposited.
Table 2 shows the data recorded for each lubricating oil
sample for this test.
Cruz, Dela Cruz, Francisco(your last names only)
[3]
From the positive values for ∆T, the results are
consistent with having fire points higher than the flash
points initially obtained. Specifically, Petrolube may be
considered to have had the most amount of highly
volatile constituents in its composition, due to having the
closest flash point and fire point, which could also be
indicative of high evaporation losses upon use [2,6].
Conversely, the highest temperature difference observed
for Shell may be correlated to a high amount of heavy
volatile fractions and low evaporation losses. However,
these fractions may be part of the constituents of the oils
or impurities gained from other or previous use in
experiments.
Overall, the high flash points also indicate that the
lubricating oils are not flammable under ambient
temperature, exhibiting high resistance to combustion
and evaporation under normal temperatures [2].
Definitively, under the Globally Harmonized System for
Classifying and Labelling of Chemicals (GHS), liquids
with flash points above 93 oC are not classified as
flammable or hazardous in the workplace [7,8]. Hence,
the results indicate that the lubricating oils tested are
reliable for use over a wide range of temperatures under
132 oC, the lowest flash point.
Subsequently, in comparing the samples, it is
recognized that different factors in preparation, such as
the base oil used—whether mineral (paraffin, naphthene,
aromatic) or synthetic, and the fractions used in the
composition as mentioned above, among others affect the
properties of the end-product [6,9-10]. Thus, in
comparing commercial, non-reagent grade samples, a
useful comparison may be done using another property
determined for the end-product itself which can be
related to the flash point, as the manufacturing processes
and additives used by private companies are rarely
detailed in reference literature. From this, a property that
can be used is viscosity. Viscosity is known to vary
directly with the flash point [2]. The significance of flash
and fire points, however, is highlighted in its appreciable
dissimilarity among different hydraulic liquids, allowing
for differentiating lubricating oils with comparable
viscosities [2]. Further, the relationship may be explained
by the stronger intermolecular forces found in highly
viscous fluids, which hinders the molecules from freely
flowing past one another and consequently requires more
energy, leading to a higher flash point observed, to break
bonds and form initial the vapors observed at the flash
Dr. Lawrence P. Belo
point, followed by the actual ignition of the oil at fire Lastly, individual observations from the experiment
point. From a previous experiment, the order of viscosity are as follows:
of the lubricating oils tested was determined to be led by (1) The temperature for the oil was constantly increased
Petrolube as the most viscous, followed by Shell, and by placing the sample on a heating plate, while
Sphinol respectively. Thus, the results corroborate that panning the open flame back and forth onto the oil.
the highest value for flash point obtained for Petrolube is The desiccator was also in use, to dry and cool the
consistent with its evaluated viscosity from the previous sample in the crucible for the carbon residue test.
experiment. Similarly, on the other end, Sphinol with the The desiccator's lid was needed to be properly
least flash point and fire point temperatures in this opened and closed, for it to fully dry the sample.
experiment, was previously determined to be the least (Cellona).
viscous. (2) For the flash and fire point test, the flame was
constantly moved throughout the entirety of the
Meanwhile in the determination of the carbon residue
experiment. Both flash and fire points were also
of the lubricating oils, carbon residue or soot, is
challenging to determine, since for the flash point,
indicative of incomplete combustion of the fuel.
the vapor that was present was misleading due to the
Nonetheless, all fuels have carbon residue as a result of
vapor from the flame of the carbon residue test.
their refining processes [2]. From the experiment,
Similarly, the fire point was difficult to identify since
however, the amount of carbon residues determined from
once the oil burned, the temperature rapidly
the experiment are low in value, at most of 1.8% wt. of
increased. (Dar).
the original sample. This means that generally, the
(3) The carbon residue test was easier to perform than
lubricating oil samples combusted to a high extent of
the flash and fire point test. Aside from taking much
completion, wherein Sphinol could be determined to
longer, determining the fire point of the samples was
have completed the combustion the most while at the
difficult, since when this point has been reached, the
same time exhibited a low tendency to form deposits
temperature increases rapidly, making it hard to
under very high temperatures given its low amount of
record the temperature when flame first appeared
carbon residue formed. On the other hand, Petrolube was
(Javier).
the least fully combusted thereby having the slowest
(4) Increasing the temperature to observe the flash point
burning rate, attributed to difficulty in oxidizing [2].
was achieved gradually by both placing the oil
More importantly, the lubricating oil has the highest
sample on a heating plate and bringing a flame
tendency to leave carbon residues after completely
above the surface of the sample intermittently.
burning, as indicated by its highest amount of carbon
However, when the fire point was reached, the
residue developed. Therefore, similarly, it can be
flames from the oil, also occurring at the bottom of
observed that the order of oils developing carbon
the thermometer, caused a rapid rise in temperature
residues follows the trend for viscosities, as described in
which made determining and recording the fire point
the flash and fire points test. The least viscous oil left the
more challenging (Lopez).
least amount of residue, while the most viscous yielded
(5) It can be observed that the fire point temperatures
more burnt carbon byproduct [11, 12]. In view of the
are always greater than that of the flash point
significance of the intermolecular forces as described
temperatures (Soriano).
earlier, the stronger attraction between molecules present
in the heavily viscous liquid can be considered more
difficult to overcome in the combustion process under a
IV. SUMMARY AND CONCLUSION
constant oxygen supply from the surrounding air during
the experiment, as compared to a lighter, less viscous
The gathered data for the three oil samples, Petrolube,
fluid abound with weaker intermolecular forces. In
Shell, and Sphinol, all indicated that those lubricants can
addition, similar to what was suggested earlier, the
be safely used, since their flash points are above the
carbon byproduct may consist of unburnt constituents of
standard for flammability. Similarly, the observed fire
the oils, or impurities that were added to the oil from
points are within the expected values, in which it was
previous use.
higher than the flash points. By having greater flash and
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[4]
fire points, though, it can be correlated that the oil is
more viscous. Additionally, all three samples performed
well for the carbon reside test. This was due to the low
carbon content found after ignition, suggesting a high
completion for the oils' combustion.
Thus, in terms of viscosity and flash and fire points,
Sphinol may be the preferred oil among the three, given
its low viscosity yet generally high flash point. These
indicate that the oil can flow easier, requiring less energy
to pump into an internal engine, and may still be used at
high working temperatures below its flash point at 132oC.
In addition, Sphinol was found to have the least tendency
to form deposits that could cause fouling of components
under high temperatures.
V. ANSWERS TO GUIDE QUESTIONS
1. Explain the relationship of the flash point of a
lubricating oil with its viscosity.
The flash point of a lubricating oil is directly
proportional to its viscosity. The more viscous the
lubricating oil is, the higher its flash point.
2. What are the effects of too low a flash point for
the lubricating oil used in engines? Too a high a
flash point?
Lubricating oils with too low or too high flash
points are not advisable to use in engines.
Lubricating oils with low flash points will ignite
easily therefore it can cause damage to the
engine. On the other hand, lubricating oils with
too high flash points will be difficult to pump
inside the engine since flash point increases with
viscosity.
3. At what concentration of fuel vapor and air will
the mixture start to ignite?
The minimum concentration of fuel vapor and air
at which it will start to ignite is at the lower
flammable limit. It is usually close to the
saturated concentration at the flash point.
Cruz, Dela Cruz, Francisco(your last names only)
[5]
4. What is auto-ignition? What is its difference with
flash and fire points?
Auto-ignition temperature is the lowest
temperature at which a volatile material will be
vaporized which ignites without the help of any
external flame or ignition source whereas flash
and fire points requires ignition sources.
5. What is the importance of determining the flash
and fire points for used oils?
Determining the flash and fire points for oil
would determine the necessary oils for specific
application.
6. Explain the purpose of the glass beads during the
heating process.
Glass beads act like boiling chips. It allows the oil
to heat up steadily in order to prevent intense fire
build up or explosion during the experiment.
7. Besides the cooling step, why is there a need to
place the crucibles in a desiccator after heating?
The crucibles are placed in a desiccator to cool
down the heated crucible. This also prevents the
carbon residue from reacting with moisture
present in the atmosphere.
8. State the relationship between the viscosity and
the amount of carbon residue for a certain kind of
lubricating oil.
The viscosity of a fuel affects its flammability
such as when the viscosity is higher, the
flammability is relatively lower. Therefore, fuels
with lower flammability yield less carbon residue
due to incomplete combustion.
9. Describe the extent of importance of performing
the experiment and the knowledge of the amount
of carbon residue in lubricating oils.
The importance of performing this experiment is
attributed towards understanding the formation of
carbon from the burning of fuels. This is
important because the formation of carbon in
Dr. Lawrence P. Belo
 engines causes degradation, which yields lower efficiency.

REFERENCES

[1] Available online at http://what-when-how.com/automobile/purposes-of-lubricating-oil-automobile

[2] LBYCHED Manual [PDF]
[3] Available online at https://www.engineersedge.com/lubrication/flash_point_fire_point.htm
[4] Available online at http://www.bunkering.co.kr/bunker_spec/carbonresidue_1.htm
[5] Available online at http://www.kittiwake.com/bunker_fuel_carbon_residue
[6] Štěpina, V., & Vesely, V. (1992). Lubricants and special fluids. Amsterdam: Elsevier.
[7] Available online at https://ehsdailyadvisor.blr.com/2015/09/wasnt-flammable-ghs-changed-meaning-flammable-
liquids/
[8] Available online at https://www.worksafe.qld.gov.au/injury-prevention-safety/hazardous-chemicals/specific-
hazardous-chemicals/flammable-and-combustible-liquids
[9] Available online at https://www.machinerylubrication.com/Read/29113/base-oil-groups
[10] Available online at http://nptel.ac.in/courses/112102015/22
[11] Available online at https://www.linkedin.com/pulse/fuel-oil-understanding-spec-characteristics-meanings-part-
versey
[12] ASTM International. Significance of ASTM tests for petroleum products:1955. Philadelphia, ASTM, 1971.

APPENDICES

A. Raw Data

Table 1. Raw data for flash point and fire point test.
Temperature (oC)
Lubricating Oil Flash
Fire Point Difference
Point
Shell 146 222 76
Sphinol 132 192 60
Petrolube 158 196 38

Table 2. Raw data for the carbon residue test.

Weight (g)
Lubricating Oil Lubricating
Crucible Total After Burning Carbon Residue
Oil
Shell 32.49 10.21 42.70 32.62 0.13
Sphinol 32.54 10.76 43.30 32.60 0.06

Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[6]
 Petrolube 32.57 10.12 42.69 32.75 0.18

B. Sample Calculations

 Temperature difference between flash point and fire point for Shell

∆ T =Fire Point ( ℃ ) −Flash Point ( ℃ )=222 ℃−146 ℃=76 ℃

 Conrad Carbon Residue (CCR) of Shell

Carbonresidue
CCR= ×100
Weight of lubricating oil

0.13 g
¿ × 100=1.273 %=1.3 %
10.21 g

C. Photos

Figure 3. Assembling the experimental setup. Figure 4. Observing the fire point and the carbon residue test.

Figure 5. Carbon residue on crucibles used.

Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[7]
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[8]