FACULTY OF CHEMICAL & PROCESS ENGINEERING TECHNOLOGY
UNIVERSITI MALAYSIA PAHANG
TECHNICAL PAPER
FINAL YEAR PROJECT 2 (BTO4826)
Name and ID
S1: MOHD SYAHIR AMIR BIN SUNGIP (TH19003)
Number
S2: FENNYLIA ANAK ALIN (TH19017)
PERFORMANCE TEST OF EMULSIFIERS ON BITUMEN
Title EMULSION MIXTURE
DR. MALYANAH BINTI MOHD TAIB
Evaluator
TEST PERFORMANCE OF
NON-IONIC EMULSIFIER FOR BITUMEN
EMULSION MIXTURE
Syahir Amir Sungip, Fennylia Alin, Ts. Mohd Najib Razali.
Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang, 26300 Kuantan,
Pahang
Corresponding author, email*:
[email protected],
[email protected],
[email protected]Abstract: system for the sector. A longer test duration is
Bitumen emulsion mixture is a mixture of also recommended in order for the Emulsified
bitumen, water and an emulsifying agent. The Modification Bitumen to show a preferable result.
bitumen is suspended in water in the form of
small droplets, creating a stable mixture that can Keywords: Emulsified Modification Bitumen,
be easily transported and applied. Emulsifying optimum percentage, rate of drying, bituminous
agent is used to keep the bitumen suspended in coating.
water and prevent it from separating out. This
research aims to find the optimum percentage of 1. INTRODUCTION
emulsifier for bitumen emulsion formulation and
also to enhance the rate of drying for the Bitumen is a byproduct of the crude oil
Emulsified Modification Bitumen. The bitumen distillation process. At room temperature, it is a
mixture was prepared for the formulation in four black visco-elasticity solid that transforms into a
sets of six beakers each. The first set was viscous liquid as the temperature rises. Bitumen
prepared with the mixture of bitumen with has unique adhesive and waterproofing qualities,
penetration of 60/70, eco base oil at 3 different making it an excellent substance for
volume, deionized water and mixed with non- gluing aggregate together. Since it has diverse
ionic emulsifiers. The second set was prepared connotations in different parts of the world, the
with the same volume of bitumen grade 60/70, term "bitumen" is not entirely clear. In Europe,
eco base oil, and emulsifier but modified with the term "bitumen" is defined as previously stated,
different volume of deionized water and also however in Canada, the term "bitumen" refers to
added with different volume of drying promoter. heavy crude oils. Instead of bitumen, the term
The method was repeated by replacing the "asphalt" is used in the United States. Bitumen is
emulsifier with another emulsifier (cationic) sometimes confused with tar, which is a
Next, the EMB and CEMB will be coated and completely separate product. The dry distillation
dried on the top surface of a substrate (drywall) of coal or wood produces tar. (Cahya, 2022).
and will be compared with an industrial grade Other components, such as wax crystals and
bitumen emulsion. From the analysis, EMB with naphthenic acids, can react as natural surfactants
4% of emulsifier is the best formulated bitumen and affect the interfacial property of the bitumen
emulsion when combine with drying promoter. water system, but only when the pH of the
The result shows a percentage area removal of aqueous phase is high or low. (Lu et al., 2017).
less than 2%. 4% of non-ionic emulsifier also is Thus, in the chemical interaction of the surfactant
able to mix the bitumen emulsion and deionized with the bitumen in the formation of emulsions,
water with only 1% of water resolved from the bitumen type, and source are critical elements.
mixture. The results obtained from this study
proved that the non-ionic emulsifier is better than In the pavement construction industry,
the cationic emulsifier. However, more research bitumen emulsion is becoming more common.
is needed to provide a better understanding of the Cold recycling mixes, tack coating, and surface
factors and to make it easier to build the best treatment are just a few of the applications.
Bitumen emulsions are a novel way of rate of water evaporation is influenced by
distributing bitumen in water to liquify it. boundary conditions like temperature and
Bitumen emulsions have a considerable benefit relative humidity. The water loss in the early
over hot bitumen since their activities need less solidification stage is faster when the mixture's
energy due to their reduced viscosity. (Al- water consumption is high (Graziani et al., 2018).
Mohammedawi & Mollenhauer, 2022). Although
bitumen is often a relatively small part of asphalt The issue of emulsion formulation is usually
mixtures, bitumen engineering qualities play a solved by choosing the right components
significant role in their performance. (Behnood, (surfactant, bitumen, and aqueous phase) in the
A. 2019). right amounts. The optimum formulation should
produce an emulsion with the desired emulsion
Bitumen emulsion is a combination of fine breaking time, either during mixing or
bitumen particles and water. However, because compaction, as well as proper aggregate coating,
bitumen is a petroleum product, it does not mix which will result in a strength increase over time.
with water and is sticky, it is difficult to dissolve Initial workability, or the ability to stockpile the
into thin droplets. An emulsifier is employed to material, and the eventual growth of mechanical
solve this problem. A surface-active agent is what strength in situ, on the other hand, create
an emulsifier is. By preventing the bitumen from contradictory needs. By separating and treating
mixing with other droplets, the emulsifier retains the various components separately, it is possible
it in its fine droplet condition. Because the to make the formulation and emulsification
droplets are so little, they float on water. An technique optimization very simple (Al-
emulsion is a combination made up of two or Mohammedawi & Mollenhauer, 2022).
more liquid phases (Suryakanta, 2016). The uses
of emulsions are found in several chemicals,
energy, and environmental industries such as the 2. METHODOLOGY
food, health care, chemical synthesis, and
firefighting sectors (Goodarzi et al, 2018). 2.1.Materials
Emulsifiers of many types have been employed Table 1 summarizes the characterization of
to emulsify bitumen. Anionic emulsifiers were the raw materials that required for the
the most frequent in the beginning, but cationic formulation of the Emulsified Modification
emulsifiers have steadily gained ground since the Bitumen. The raw materials include the industrial
1950s. Bitumen emulsification can also be done grade bitumen with the penetration of 60/70, eco
with emulsifiers. When these emulsifiers come base oil, nonylphenol ethoxylate emulsifier, and
into touch with dirt and stone, they become less drying promoter.
immobilized, making the emulsions very stable.
As a result, they've been commonly applied in
situations where the bitumen emulsion is meant 2.2. Emulsified Modification Bitumen (EMB)
to penetrate dirt, dust, and even clay. Emulsions Formulation
and clay emulsions have been utilized in the past
Table 2 and Table 3 summarizes Non-Ionic
for certain uses, but they are not currently
EMB formulations with varying ratios of bitumen
produced in large quantities (Cahya, 2022).
(60/70) and eco base oil. Table 4 and Table 5
Because the drying process of bitumen recap the cationic EMB formulation that been
emulsion has such a strong influence on the used for the experiment. The samples are
strength development of emulsion-based examined by using three standard test methods;
mixtures for pavement structure, it can be thickness of compacted bituminous mixture
utilized to assess bitumen emulsion quality. The specimens, drying of organic coatings and
drying behavior of bitumen emulsions, on the measuring adhesion by using a tape test. All the
other hand, was hardly considered. The drying standard test methods follow the American
process of several bitumen emulsions with a thin Standard for Testing and Materials (ASTM). All
layer is investigated using the emulsion drying the standard test methods follow the American
and film formation theory (Li et al., 2021). The Standard for Testing and Materials (ASTM) to
compare the formulated EMB with the industrial Emulsifier 2% 3% 4%
Percentage
grade bitumen emulsion (Atlas).
Bitumen 180 180 180
60/70, g
For Set A, the industrial grade 60/70
bitumen is blended with eco base oil to produce Eco Base Oil, 120 120 120
g
new modified bitumen. The modified bitumen is
mixed with nonylphenol ethoxylate emulsifier Nonyl Phenol 2 4 6
Ethoxylate, g
and deionized water to produce a new formulated
bitumen emulsion. For the set B of Emulsified Deionized 167 165 163
water, g
Modification Bitumen, the volume of the raw
materials is adjusted to mixed with drying
promoter. This procedure is done in order to
Table 3: Non-Ionic EMB formulation with drying promoter Set
uniform the weight for all the formulated B (469g).
bitumen.
Ratio (wt%) 3.8:2.6:0.04:1 3.8:2.6:0.08:1 3.8:2.6:0.13:0
Table 1: The characterization of raw materials for the formulation .26:2.3 .12:2.3 .17:2.3
of bitumen emulsion.
Emulsifier 2% 3% 4%
Test Unit Bitumen Eco Nonyl Chitosan Drying Percentage
60/70 Base Phenol Promoter
Oil Ethoxylate Bitumen 60/70, 180 180 180
g
Cas Number – 8052– 70514-9016–45–9 9012-75-8001–
42–4 12-4 4 22–7 Eco Base Oil, g 120 120 120
Specific Gravity at g/cm31.01– 0.85– 1.055 1.4 1.0622 Nonyl Phenol 2 4 6
25 C (ASTM D70) 1.06 0.87 Ethoxylate, g
Boiling Point ℃ >340 >280 230 – 250 115.5 250 Deionized 59 57 55
(ASTM D7798/ water, g
ASTM D7398)
Drying 108 108 108
Melting Point ℃ >110 – – – – Promoter, g
(ASTM D87- 09 /
ASTM E324-16
Moisture Content % – 0.31 – 4.2 –
(ASTM D789) Table 4: Cationic EMB formulation without drying promoter Set
A (469g).
Viscosity (ASTM D Pas 233.00 4.29 243 110 37.7
244/ASTM D445) Ratio (wt%) 3.8:2.6:0.04:3 3.8:2.6:0.08:3 3.8:2.6:0.13:3.47
.56 .52
Flash Point ℃ 262 240 113 – 260
Cleveland Open Emulsifier 2% 3% 4%
Cup (ASTM D92- Percentage
16)
Bitumen 180 180 180
60/70, g
Penetration at 25 C, dmm 64 – – – –
100 g, 5 sec (ASTM Eco Base Oil, 120 120 120
D5-13) g
Softening Point℃ 50.5 – – – – Chitosan, g 2 4 6
Ring & Ball Test
(ASTM D36) Deionized 167 165 163
water, g
Table 5: Cationic EMB formulation with drying promoter Set B
(469g).
Ratio (wt%) 3.8:2.6:0.04:1 3.8:2.6:0.08:1 3.8:2.6:0.13:0
.26:2.3 .12:2.3 .17:2.3
Table 2: Non-Ionic EMB formulation without drying promoter Emulsifier 2% 3% 4%
Set A (469g). Percentage
Ratio (wt%) 3.8:2.6:0.04:3 3.8:2.6:0.08:3 3.8:2.6:0.13:3.47 Bitumen 60/70, 180 180 180
.56 .52 g
Eco Base Oil, g 120 120 120 well as those connected to elastomeric alteration.
Chitosan, g 2 4 6 As deionized water was mixed thoroughly with
the bitumen emulsion and the emulsifier, it needs
Deionized 59 57 55
water, g to be prioritized to know in which group does the
Emulsified Modification Bitumen belongs to.
Drying 108 108 108
Promoter, g
The newly emulsified modification bitumen also
needs to be analysed using Fourier-transform
infrared spectroscopy to ascertain how the non-
ionic emulsifier affected the binder’s chemical
2.3.Testing plan composition. Figure 4.1 and figure 4.2 show the
At a temperature of 110 C, the bitumen 60/70 peak value and other group that belongs in the
is heated in the oven for two hours. Then, using EMB. (Maciejewski & Chomicz-Kowalska,
an IKA C-MAG HS 7 mechanical stirrer with a 2021).
three-blade stirrer, preheated bitumen of 180g is
combined with eco base oil. At a mixing rate of As part of the building process, it is checked
450 rpm and a controlling temperature of 190 C, that the appropriate quantity of bitumen emulsion
modified bitumen is created. For 90 minutes, this has been applied to the substrate using the
situation is maintained. The modified bitumen is standard test technique for the thickness of the
then permitted to cool to 100 C. Following that, a compacted bituminous mixture specimen
sample of modified bitumen containing 180g is (ASTM D 3549-03). A drywall with a 1 mm
weighed, swirled, and heated at 75 C while being thickness is prepared for use in this test procedure.
mixed at a velocity of 450 rpm. At the same time, The samples of bitumen emulsion are then put on
167 mL, 165 mL, or 163 mL of deionized water the drywall's surface. The samples of bitumen
is diluted with 2%, 3%, 4% of nonylphenol emulsion are flattened in accordance with the
ethoxylate or chitosan emulsifier. The emulsifier caster's thickness. The drywall finally leaves
solution is dissolved and then added to the behind the bitumen emulsion coated on the
modified bitumen. A newly formulated bitumen surface of the drywall. The bitumen emulsion
emulsion is created after the material has been coating materials are applied to the substrates
given 60 minutes to thoroughly mix. (drywall), and the drying of organic coatings is
verified using the standard test techniques
For the part of dictating the physical (ASTM D1640-03). For 180 minutes, the
characterization of the newly formulated bitumen samples are cooked in an oven at 60 ℃. The
emulsion, emulsion stability test (ASTM D 1479) coated bitumen emulsion samples on the
was conducted. All the formulated EMB samples substrate are then checked using seven testing
were tested for emulsion stability. Each measures, including set-to-touch time, dust-free
formulation received a 300 mL sample to time, tack-free time, dry-to-touch time, lacquers,
evaluate gravity stability at room temperature. dry-hard time, and dry-through time.
The amount of water that settles demonstrates the
stability of the emulsion. The samples were left To determine if bitumen emulsion, a coating
inside the fume hood and the result were taken substance, adheres enough to drywall, the
after 3 days. Using, the Equation 1, the standard test technique for assessing adhesion by
percentage of water separation was calculated by tape test (ASTM D3359-09) is utilized. A coating
subtracting the separation efficiency (e) from the must stay attached to a substrate for the duration
volume of water in the measuring cylinder: of its planned service life in order to perform the
intended protective or decorative function. A
Equation 1: Water separation (%), e = method to assess the adhesion of a coating to
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑟𝑒𝑠𝑜𝑙𝑣𝑒𝑑, (𝑚𝐿) / 𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 different substrates or surface treatments, or of
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟, (𝑚𝐿). different coatings to the same substrate and
treatment, must be looked into because the
Due to the findings of the spectroscopic tests, substrate and its surface preparation have a
it was possible to determine the specific significant impact on the adhesion of coatings.
functional groups linked to bitumen oxidation as
Applying and removing pressure-sensitive for three hours at four distinct temperatures
tape over cuts in the film is how this testing (60 ℃, 45 ℃, 30 ℃, and 27 ℃) inside the oven.
technique is carried out. Applying and removing
pressure-sensitive tape over cuts in the film is A non-contact digital laser infrared thermometer
how this testing technique is carried out. The rate is then used to measure the temperatures of the
of adhesion will then be calculated using the drywall's top, back, and coating (bitumen
testing method's depicted scale. emulsion). The value for the heat transfer through
the drywall can be calculated by using the
After performing all of the regular test Equation 2.
procedures, ageing is used to continue the study.
One of the most important elements that affects Equation 2:
𝑘𝐴(∆𝑇)
how the bitumen emulsion behaves on the Conduction: q = 𝑡
substrate is ageing. At three distinct temperatures Convection: q = (hA∆𝑇)
(55 ℃, 27 ℃, and 10 ℃) the ageing process is where,
gauged. Utilizing the Accelerated Weathering q = amount of heat (W)
Tester, the ageing process at 55 ℃ is evaluated. 𝑊
k = thermal conductivity of material, 𝑚𝑘
According to ASTM G 154, the Accelerated 𝑤
Weathering Tester is carried out with an h = convective heat transfer coefficient, 𝑚2 𝑘
𝑊 DT = temperature difference (K)
irradiance intensity of 0.89 𝑚2 , a step time of 8
t = thickness (m)
hours, a setup temperature of 55 ℃, and a test
A = area (𝑚2 )
time of 168 hours.
This method is comparable to 10,343 hours or 3. RESULTS AND DISCUSSION
431 days under actual conditions. Additionally,
the Accelerated Weathering Tester, which has
four variable parameters including UV light, 3.1 Emulsion Stability Test
heater, water, and condensation, aids in the Table 6 and Table 7 shows the volume of
research of EMB performance against water resolved and percentage of water separate
deterioration brought on by climatic from NEMB Set A and the CEMB Set A. Using ,
circumstances. The bitumen emulsion samples the percentage of water separation was calculated
are aged in the laboratory for seven days at a by subtracting the separation efficiency (e) from
temperature of 27 ℃ . The bitumen emulsion the volume of water in the measuring cylinder by
samples are kept in the chiller for seven days using Equation 3.
during the ageing process at 10 ℃. Every day,
weights of all the bitumen emulsion samples are Water separation (%), e = 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
measured and recorded for each of these three 𝑟𝑒𝑠𝑜𝑙𝑣𝑒𝑑, (𝑚𝐿) / 𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟,
temperatures. (𝑚𝐿).
Table 6: Volume of water resolved and percentage of water
separate from NEMB Set A
To ascertain the bitumen emulsion's
insulation properties, a heat transfer investigation NEMB Initial volume Volume of water Water
Set A of water, mL resolved, mL separation, %
will be performed. The tool is made up of an oven, 2% 167 8.35 5
drywall measuring 10 cm × 5 cm × 1 cm, 3% 165 4.95 3
aluminium foil tape, and a non-contact digital 4% 153 1.63 1
laser infrared thermometer. Six drywall samples
will have bitumen emulsion applied to their top
Table 7: Volume of water resolved and percentage of water
surfaces, with one drywall sample being left separate from CEMB Set A
uncoated as a control. To stop heat loss to the
CEMB Initial volume Volume of water Water
surroundings, aluminium foil tape will then be Set A of water, mL resolved, mL separation, %
applied to the sides and back of the drywall 2% 167 8.35 5
sample. Following that, the samples are heated 3% 165 6.6 4
4% 153 3.26 2
From the result shown in table 6 and table 7, Table 8: FTIR results of functional group for Non-Ionic
the bitumen emulsion from both sets that been Emulsified Modification Bitumen (NEMB)
mixed with the 4% of emulsifier produced less Se Percenta Ran Peak Appearan Group Class
volume of water resolved. Meanwhile, the t ge ge ces
NEMB with 4% of emulsifier produce less water
2% 2923. Medium C-H Alka
3000 -2500
resolved with 1% compare to the CEMB. This 81 Stretchi ne
indicate that the 4% formulation of non-ionic ng
emulsifier is better than the cationic emulsifier. Se 3% 2923. Medium C-H Alka
t 65 Stretchi ne
A ng
3.2 Fourier Transform Infrared Spectroscopy
4% 2923. Medium C-H Alka
From the Figure 1, the bitumen temperature 82 Stretchi ne
and percentage of emulsifiers had a substantial ng
impact on the formation of group and the peak in 2% 2924. Medium C-H Alka
all of the tested EMB, according to the statistical 13 Stretchi ne
ng
analysis shown in Table 4.2. Through a detail
analysis, other functional group also can be found Se 3% 2923. Medium C-H Alka
t 98 Stretchi ne
in the EMB if the wavelength narrowed to a B ng
specific range. The statistical significance of the
4% 2924. Medium C-H Alka
peak and range demonstrated that those mixture 14 Stretchi ne
of Emulsified Modification Bitumen are ng
belonging to the same group. (Maciejewski &
Chomicz-Kowalska, 2021).
3.3 Adhesion Test
Table 9 and Table 10 shows the result for
adhesion test for NEMB formulated bitumen
emulsion. The classification of the adhesion test
results is according to the tables. All the standard
test methods follow the American Standard for
Testing and Materials (ASTM) to compare the
formulated EMB with the industrial grade
bitumen emulsion (Atlas).
Table 9: Adhesion test (ASTM D 3359-09) for NEMB Set A.
Figure 1: FTIR results on NEMB
SET A Classification of Total removed Area
NEMB Adhesion Test from six parallel Removed
cut (%)
2% 47
3% 20
4% 16
Figure 2: FTIR results for CEMB
Table 10: Adhesion test (ASTM D 3359-09) for NEMB Set B.
Table 12: Adhesion test (ASTM D 3359-09) for CEMB Set B.
SET B Classification of Total removed Area
NEMB Adhesion Test from six parallel Removed
SET B Classification of Total removed from Area
cut (%)
CEMB Adhesion Test six parallel cut Removed
2% 5
(%)
2% 5
3% 4
3% 4
4% 2
4% 2
Table 9 and Table 10 summaries the
adhesion test results for NEMB samples. From From the Table 11 and Table 12, this
Table 9, it shows that the EMB with 2% emulsifier results recap the adhesion test for CEMB samples.
clearly has the most percentage area removed Table 11 shows the result for CEMB without
with 47%. Meanwhile, 3% and 4% has lesser area drying promoter. The EMB of 2% emulsifier has
removed with 20% and 16% each. Table 10 shows the most percentage area removed with 45%.
the classification for EMB with drying promoter. Meanwhile, the area removed from adhesion test
Each of the samples has lower percentage of area for EMB with drying promoter are less than 10%
removed with less than 10% compared to the as shown in the Table 12. EMB with 4%
EMB without drying promoter. At the meantime, emulsifier with drying promoter are clearly the
4% of emulsifier has the lowest percentage of best formulated bitumen emulsion among the
area removed for both set. This result clearly cationic EMB.
shows that the formulation of Emulsified
Table 13: The summary of the adhesion test results for all
Modification Bitumen with 4% of emulsifier with samples.
drying promoter has the best adhesion towards
drywall. The result also suggests that the EMB EMB Set Emulsifier Area removed (%)
NEMB Set A 2% 47
formulation without drying promoter has the 3% 20
poorest adhesion towards drywall as the coated 4% 16
Set B 2% 5
area removed are higher than EMB formulation 3% 4
that been mixed with the drying promoter. 4% 2
CEMB Set A 2% 45
3% 20
Table 11: Adhesion test (ASTM D 3359-09) for CEMB Set A. 4% 16
Set B 2% 5
SET A Classification of Total Area 3% 4
CEMB Adhesion Test removed from Removed (%) 4% 2
six palallel Atlas Bitumen - 5 - 15
cut
2% 45
The adhesion test findings for all samples are
summarized in Table 13. According to Table 13,
the Atlas industrial grade bitumen emulsion is
3% 20
analyzed and the total area removed from the
drywall are between 5% and 15%. Meanwhile, in
NEMB and CEMB of 4% emulsifier with drying
4% 16
promoter, where a total of 2% of the area has been
cleared, has the best adherence to the substrate
(drywall). This was followed by 3% and 2% from
each set respectively.
3.4 Aging Test
One of the major determining variables that
affects how bituminous materials behave is
ageing. Simply put, ageing will aid in the
understanding and description of the alterations
that occur in the coating material (EMB) when it
is exposed to external influences over time, such
as heat and sunshine. The effects from outside
Figure 3: NEMB Set A on 55 ℃
change depending on the location, height, and
time of year. Therefore, it is essential to imitate a
condition in the lab that is as near to the real
condition as possible. The ageing test for the
samples was carried out at three distinct
temperatures of 55 ℃, 27 ℃, and 10 ℃ in order
to satisfy these requirements. (Razali et al., 2020).
3.4.1 Accelerated Weathering Test
From the graph of weight gain shown in the Figure 4: NEMB Set B on 55 ℃
Figure 3 and Figure 4, the emulsifier had
increasing of weight in the first seven days of
analysis. On the day 8, the NEMB shows a drop
in the reading of weight. The same process also
occurs for the CEMB. This result shows that the
bitumen emulsification starts to undergo
oxidization process after a certain period due to
the characteristic of bitumen.
Figure 5: CEMB Set A on 55 ℃
Based on the table 14 and table 16, the reading
shows that each of the EMB samples determined
the correlation line of the linear graph with the
different types of aging test. Table 15 and table
17 summarize the results of the aging test for all
of the samples. Sample with the lowest
percentage of weight loss is determined as the
best formulation. The results provided after 10
days of testing shows that the CEMB 2% of
emulsifier from Set A has the lower percentage Figure 6: CEMB Set B on 55 ℃
of weight loss with linear equation of y = 3.52x -
23.82. By setting the y-axis (weight loss) to 100%, 3.4.2 Natural Weathering
the aging period (days) can be determined. After To investigate the impact on the EMB under
a detailed calculation, the aging period for the ambient circumstances, ageing at 27℃ was
CEMB 2% emulsifier from Set B is 489 days. chosen. This temperature was chosen to match
Meanwhile, atlas bitumen has the aging period of the environment outside the operating room. The
428 days. results of the bitumen emulsion sample’s weight
(g) after 10 days of natural weathering at 27℃.
Graph in the Figure 7 and Figure 8 shows the
trendline of weight for the non-ionic EMB and
the graph in Figure 9 and Figure 10 shows the
linear regression for cationic EMB. For all
bitumen samples, the weight gain (g) shows an
upward trend on the first seven days. After the
seven days, the graph began to show downward
line which indicate that the EMB starting to
undergo oxidization process.
The aging for the each of the EMB can be
predicted by following the trendline from the
graph. By using a linear correlation from the
graph in the figure below, it is possible to forecast
the ageing period. For natural weathering test,
Atlas bitumen indicates the aging periods of 1683 Figure 9: CEMB Set A on 27 ℃
days. Based on the table 14 and table 16, the
reading shows that each of the EMB samples
determined the correlation line of the linear graph
with the different types of aging test. Table 15
and table 17 summarize the results of the aging
test for all of the samples. Sample with the lowest
percentage of weight loss is determined as the
best formulation. For natural weathering test, the
results provided after ten days of testing shows
that the CEMB 2% of emulsifier from Set A has
the lower percentage of weight loss with linear Figure 10: CEMB Set B on 27 ℃
equation of y = 4.7365x - 34.997. By setting the
y-axis (weight loss) to 100%, the aging period 3.4.3 Cooling at 10 ℃
(days) can be determined. After a thorough The ageing test at 10 ℃ was selected to reflect
calculation, the aging period for the CEMB 2% the state of an operating room, which is typically
emulsifier from Set B is 438 days. Meanwhile, kept at 16 ℃. The findings of the weight loss (g)
atlas bitumen has the aging period of 1683 days. of the bitumen emulsion samples after 10 days of
cooling at 10 ℃ are shown in the Figure 11, Figure
12, Figure 13, and Figure 14. The graph shown in
the Figure 11 and Figure 12 indicates an increasing
trend in the weight (g) for the bitumen samples of
the non-ionic EMB. Meanwhile, Figure 12 and
Figure 13 highlight the trendline for cationic
EMB on the ten days of analysis. To calculate the
aging period for the EMB coating, a downward
trendline need to obtain and thus the experiment
was prolonged until the graph shows the desired
linear regression. The experiment took a progress
for ten days of duration and so that the aging
Figure 7: NEMB Set A on 27 ℃
period for the EMB coating can be determined.
Based on the Figure 11 and Figure 12, the non-
ionic EMB stipulate a significant low weight gain
through the seven days of experiment and start to
decrease after day 7. The NEMB for Set A has
higher value of weight compare to the NEMB for
Set B.
Figure 13 and Figure 14 highlighted the graph
trend for cationic EMB also shows the same
Figure 8: NEMB Set B on 27 ℃
trendline which is consequential to note that the
non-ionic bitumen emulsifier and cationic
bitumen emulsifier would have an increasing
weight due to the molecule of water from
surrounding. The best formulation of EMB can
be determined by reviewing the Table 15 and
Table 17 which already summarize the results of
the aging test for all of the samples. Sample with
the lowest percentage of weight loss is
determined as the best formulation. For cooling
aging test, the results provided after ten days of
testing shows that the CEMB 2% of emulsifier
from Set B has the lowest percentage of weight
loss with linear equation of y = 4.5236x - 31.903. Figure 14: CEMB Set B on 10 ℃
By setting the y-axis (weight loss) to 100%, the
aging period (days) can be determined. After a Based on the aging analysis at three different
thorough calculation, the aging period for the conditions, the industrial grade bitumen emulsion
CEMB 2% emulsifier from Set B is 420 days. (Atlas) lasts longer compared to the best
Meanwhile, atlas bitumen has the aging period of formulated bitumen emulsion cationic EMB of
1488 days. 2% without drying promoter. This statement is
supported by the fact that the aging periods for
Atlas using the accelerated weathering tester,
natural weathering and cooling are 428 days,
1683 days and 1488 days, respectively.
Table 14: Relationship between various performance indicators
and the time of accelerated weathering ageing, natural weathering
ageing and cooling ageing.
Aging Type Set NEMB Aging Equation 𝑅2
Formul Condition
ation
Test time y = 3.125x - 1
2%
Figure 11: NEMB Set A on 10 ℃ of 168 h, 21.875
Set irradiance y = 2.2575x - 0.8909
3%
A intensity 16.77
Accelerated W y = 0.999x - 0.6
4% of 0.89 ,
Weathering m2 7.659
Ageing step time
2% y = 4x - 28 1
of 8 h,
Set 3% 4.546x - 34.096 0.8331
setting
B y = 5x - 37.5 0.8333
4% temperatu
re of 55 ℃
2% y = 4x - 29.715 0.8908
Set 3% y = 2.75x - 20.25 0.8963
A Test time y = 1.428x - 0.8909
4%
of 168 h 10.608
Natural
with y = 2.629x - 1
Weathering 2%
setting 18.399
Ageing
Set temperatu y = 1.539x - 0.6
3%
B re of 27 ℃ 11.799
y = 1.946x - 0.8909
4%
14.456
Figure 12: NEMB Set B on 10 ℃ 2% y = 3.52x - 23.82 0.965
y = 4.149x - 0.9795
Set 3%
29.779
A Test time
of 168 h y = 3.468x - 0.9797
4%
24.888
Cooling with
y = 2.223x - 0.8331
Ageing 2% setting
16.673
temperatu
Set y = 3.481x - 0.9154
3% re of 10 ℃
B 25.236
y = 3.704x - 0.9525
4%
26.854
Table 15: Result of the aging period for the non-ionic EMB
based on the different types of ageing test.
Aging Type Set EMB Aging Duration
Formulation (days)
Figure 13: CEMB Set A on 10 ℃ 2% 290
Set 3% 208 2% 321
A 4% 92 Set A 3% 300
Accelerated Weathering
2% 372 4% 303
Ageing Set Cooling
3% 420
B Ageing 2% 420
4% 462
2% 370 Set B 3% 251
Set 4% 129
3% 254
A
Natural Weathering 4% 132
Ageing 2% 244
Set
3% 142
B
4% 180 3.5 Heat Transfer Analysis
2% 328
Set
A
3% 385 As the samples are run in the oven and the
4% 321
Cooling Ageing
2% 205 influence of radiation on the samples is minimal,
Set
B
3%
4%
322
343
the effect of radiation in the computation has also
been ignored. Based on equation, the heat
transfer through the drywall is computed with
Table 16: Relationship between various performance indicators W W
and the time of accelerated weathering ageing, natural Kbitumen at 40.5 mK , Kdrywall at 40.27 mK , hair at
weathering ageing and cooling ageing. W
40.27 𝑚2 K, tbitumen at 0.001 m, A = 0.005 𝑚2 , and
Aging Type Set CEMB Aging Equation 𝑅2
Formulation Condition tdrywall at 0.009 m. Figure 15 and Figure 16 depicts
2%
y = 5.264x -
36.849
1 an escalate in the rate of heat transfer through the
Test time of
Set
3% 168 h, y = 4.862x - 0.9799 drywall for the non-ionic EMB. The graph also
A 33.467
irradiance
y = 2.822x - 0.8965
shows how the bitumen emulsion coating
Accelerated 4% intensity of
Weathering
W
0.89 , step
20.782 material aids in lowering the rate of heat transfer
m2 y = 4.8565x 0.9797
Ageing 2% time of 8 h, - 34.852 (q) through the drywall. At all temperatures, The
setting
Set
3% temperature
y = 1.5x - 0.6 EMB of 4% emulsifier performs best as a heat
B 11.5
of 55 ℃
y = 1.8421x 0.8909 insulator, followed by EMB with 3% emulsifier
4%
- 13.684 and EMB with 4% emulsifier. The same trend of
y = 4.7365x 0.9
2%
- 34.997 uprising rate of heat conductivity through the
Set
A
3%
y = 3.9998x
- 28.285
0.98
temperature of 27 ℃, 30 ℃, 45 ℃, 60 ℃ for the
Test time of
Natural 4% 168 h with
y = 3.3332x 0.9657 cationic EMB. Meanwhile industrial grade Atlas
- 23.845
Weathering setting
y = 2.857x - 0.8333
bitumen rate conductivity on different
Ageing 2% temperature
of 27 ℃
21.428 temperature was 1.09. 0.71, 0.64, and 0.57
Set y = 3.4209x 0.9657
B
3%
- 23.157 respectively. The Atlas shows the best
4%
y = 1.6668x
- 11.389
0.9 performances as a heat insulator at all
2%
y = 3.4694x 0.8627 temperatures. It is clear from the trend that as
- 25.918
Set y = 3.25x - 0.786
bitumen composition grows, so does its capacity
3%
A
Test time of
24.5 to absorb heat. This research focuses on the two
y = 3.2652x 0.9846
Cooling
4% 168 h with
- 22.652
types of heat transport known as conduction and
setting
Ageing
2% temperature
y = 4.5236x 0.9627 convection. The value of heat transfer (q), which
- 31.903
Set
of 10 ℃
y = 2.7083x 0.9657 is directly proportional to the change in
3%
B - 19.375 temperature. In contrast to bitumen coatings and
y = 1.4x - 0.8909
4% uncoated drywall with lesser bitumen
10.4
Table 17: Result of the aging period for the cationic EMB based compositions, the greater bitumen composition
on the different types of ageing test.
(EMB 4% emulsifier) greatly reduces
Aging Type Set EMB Aging Duration temperature changes (DT) in order to reduce the
Formulation (days)
2% 489
flow of heat through the drywall, the EMB with
Set A 3% 452 4% emulsifier is the best-formulated bitumen
Accelerated
Weathering
4% 261 emulsion. The drywall can be kept above the dew
2% 450
Ageing
Set B 3% 138 point of the surrounding air as a result. This
4% 170 represents a significant advancement in the
2% 438
Set A 3% 371
mitigation of condensation dangers on the inner
Natural surface of walls. As a result, it will assist in
4% 309
Weathering
2% 264 eliminating the fungus issues that were brought
Ageing
Set B 3% 318
4% 155 on by the wall's moisture.
CONCLUSION
From the analysis that have been conducted
on Emulsified Modification Bitumen on adhesion,
aging, and heat transfer, the following conclusion
can be drawn such as:
• The NEMB with the formulation of 4%
emulsifier and drying promoter is the best
formulated bitumen emulsion for a faster
drying rate and less percentage of area
Figure 15: Heat transfer analysis on NEMB Set A with Atlas removed.
Bitumen
• The aging analysis that have been
conducted on the bitumen emulsion also
shown that the aging periods of CEMB
2% without the drying promoter for
accelerated weathering tester, natural
weathering, and cooling are 489 days, 438
days, and 321 days.
• From the heat transfer analysis, the heat
transfer value (q) for the EMB 4% of Set
B for temperature of 60 ℃, 45 ℃, 30 ℃,
Figure 16: Heat transfer analysis on NEMB Set B with Atlas and 27 ℃ are 4.8, 4, 3.325, 2.75
Bitumen respectively. The analysis shows a trend
the higher the composition of emulsifier
mixed with bitumen emulsion, the higher
the capabilities of the of the emulsion to
withstand heat insulation.
• The adhesion test conducted on each
sample shows that EMB that have been
mixed with drying agent have the best
capabilities to dry faster compare to the
EMB without drying promoter.
Meanwhile, the higher amount of drying
promoter, the faster the rate of drying
occurs as shown in the Table 13.
Figure 17: Heat transfer analysis on CEMB Set A with Atlas
Bitumen • Based on the overall analysis from the
experiment conducted, industrial grade
bitumen has highest performance in the
term of heat insulation and aging period.
• Non-ionic Emulsified Modification
Bitumen of 4% with drying promoter is
comparable to Atlas bitumen in the term
of coating adhesion.
Further research is required in order to study
the effect of different types of emulsifiers on the
Figure 18: Heat transfer analysis on CEMB Set B with Atlas performances of Emulsified Modification
Bitumen Bitumen. It is also essential to prolong the
duration of the test in order for the EMB to
manifest its oxidization process through the https://www.researchgate.net/publication/353217836_
Mechanism_Influencing_the_Drying_Behavior_of_Bit
natural weathering and cooling process. umen_Emulsion
[10] Li, F., Wang, Y., & Zhao, K. (2022). The hierarchical
structure of bitumen of different aging states at the
ACKNOWLEDGEMENT molecular level and nanoscale. Fuel, 319, 123791.
https://doi.org/10.1016/j.fuel.2022.123791
The authors would like to thank the [11] Lu, X., Sjövall, P., & Soenen, H. (2017, July). Structural
Ministry of Higher Education for providing and chemical analysis of bitumen using time-of-flight
financial support under Fundamental Research secondary ion mass spectrometry (TOF-SIMS).
ResearchGate; Elsevier.
Grant Scheme (FRGS) No. https://www.researchgate.net/publication/314305235_S
FRGS/1/2019/TK02/UMP/02/20 (University tructural_and_chemical_analysis_of_bitumen_using_ti
reference RDU1901174) and Universiti Malaysia me-of-flight_secondary_ion_mass_spectrometry_TOF-
SIMS
Pahang for laboratory facilities as well as [12] Maciejewski, K., & Chomicz-Kowalska, A. (2021).
additional financial support under Internal Foaming Performance and FTIR Spectrometric Analysis
Research grant RDU1803111. of Foamed Bituminous Binders Intended for Surface
Courses. Materials, 14(8), 2055.
[13] Mahalakshmi, R., Pugazhendhi, A., Brindhadevi, K., &
Ramesh, N. (2020). Analysis of Alkylphenol ethoxylates
REFERENCE (APEOs) from tannery sediments using LC–MS and
their environmental risks. Process Biochemistry, 97,
37–42. https://doi.org/10.1016/j.procbio.2020.06.015
[1] Al-Mohammedawi, A., & Mollenhauer, K. (2022). [14] Maiti, T. K., Parvate, S., Pragya, Singh, J., Dixit, P.,
Current Research and Challenges in Bitumen Emulsion Bhuvanesh, E., Vennapusa, J. R., & Chattopadhyay, S.
Manufacturing and Its Properties. Materials, 15(6), (2021). Plastics in Coating Applications. Reference
2026. https://doi.org/10.3390/ma15062026 Module in Materials Science and Materials Engineering.
[2] Ataei, S., Khorasani, S. N., & Neisiany, R. E. (2019). https://doi.org/10.1016/b978-0-12-820352-1.00176-0
Biofriendly vegetable oil healing agents used for [15] M. SALOU, Siffert, B., & Jada, A. (1998,
developing self-healing coatings: A review. Progress in March). Interfacial characteristics of petroleum
Organic Coatings, 129, 77–95. bitumens in contact with acid water. ResearchGate;
https://doi.org/10.1016/j.porgcoat.2019.01.012 Elsevier.
[3] Behnood, A. (2019). Application of rejuvenators to https://www.researchgate.net/publication/223401763_I
improve the rheological and mechanical properties of nterfacial_characteristics_of_petroleum_bitumens_in_c
asphalt binders and mixtures: A review. Journal of ontact_with_acid_water
Cleaner Production, 231, 171–182. [16] Nabel Negm, El, A. F. M., Emam, D., & Mohamad, H.
https://doi.org/10.1016/j.jclepro.2019.05.209 N. (2012, July). Environmentally Friendly non-ionic
[4] Cahya Nur Rochmad. (2022). 1 Bitumen Emulsions. Surfactants Derived from Tannic Acid: Synthesis,
Academia.edu. Characterization and... ResearchGate; Springer Verlag.
https://www.academia.edu/5370198/1_Bitumen_Emuls https://www.researchgate.net/publication/229078849_E
ions nvironmentally_Friendly_nonionic_Surfactants_Derive
[5] Evgeny Alexandrovich Glady, Kemalov R.A, Alim d_from_Tannic_Acid_Synthesis_Characterization_and
Feizrakhmanovich Kemalov, & Kornetova, O. M. (2016, _Surface_Activity
May 25). Obtaining of Bitumen Emulsions using non- [17] Najib, M., Isa, Noor, Musfafikri, M., Mohd, H, N. A., &
ionic Surface-Active Substances. ResearchGate; R. M., Yunus. (2018). Formulation of emulsified
unknown. modified bitumen from industrial waste - UMP
https://www.researchgate.net/publication/303595966_ InstitutionalRepository.Ump.edu.my.
Obtaining_of_Bitumen_Emulsions_using_non- https://doi.org/http://umpir.ump.edu.my/id/eprint/21343
ionic_Surface-Active_Substances /1/60.%20Formulation%20of%20emulsified%20modifi
[6] Goodarzi, F., & Sohrab Zendehboudi. (2018, November ed%20bitumen%20from%20industrial%20waste.pdf
18). A Comprehensive Review on Emulsions and [18] Oliviero Rossi, C., Caputo, P., Ashimova, S., Fabozzi,
Emulsion Stability in Chemical and Energy Industries. A., D’Errico, G., & Angelico, R. (2018). Effects of
ResearchGate;Wiley. Natural Antioxidant Agents on the Bitumen Aging
https://www.researchgate.net/publication/329036427_ Process: An EPR and Rheological
A_Comprehensive_Review_on_Emulsions_and_Emuls Investigation. Applied Sciences, 8(8), 1405.
ion_Stability_in_Chemical_and_Energy_Industris https://doi.org/10.3390/app8081405
[7] Graziani, A., Iafelice, C., Raschia, S., Perraton, D., & [19] Razali, M. N., Mohd RamLi, N., Mohd Zuhan, K. N.,
Carter, A. (2018). A procedure for characterizing the Musa, M., & Hamid Nour, A. (2020). Coating and
curing process of cold recycled bitumen emulsion insulation effect using emulsified modification
mixtures. Construction and Building Materials, 173, bitumen. Construction and Building Materials, 260,
754–762. 119764.
https://doi.org/10.1016/j.conbuildmat.2018.04.091 https://doi.org/10.1016/j.conbuildmat.2020.119764
[8] Kazuo Isobe; Ryoichi Tamaki, (1998, October 16) non- [20] Saadoon, T., Gómez-Meijide, B., & Garcia, A. (2018).
ionic emulsifier for asphalt. Google.com. Prediction of water evaporation and stability of cold
https://patents.google.com/patent/US6114418A/en asphalt mixtures containing different types of
[9] Li, C., Ouyang, J., Dou, F., & Shi, J. (2021). Mechanism cement. Construction and Building Materials, 186,
Influencing the Drying Behavior of Bitumen Emulsion.
ResearchGate; MDPI.
751–761. [24] Trathnigg, B., & Rappel, C. (2002). Liquid exclusion–
https://doi.org/10.1016/j.conbuildmat.2018.07.218 adsorption chromatography, a new technique for
[21] Sajjad Jafarian, & Amir Modarres. (2020, October isocratic separation of non-ionic surfactants. Journal of
20). Study on the fatigue properties of bitumen emulsion- Chromatography A, 952(1-2), 149–163.
cement mastics using frequency sweep and https://doi.org/10.1016/s0021-9673(02)00076-6
linear... ResearchGate; Taylor & Francis (Routledge). [25] Wang, Z., Dai, N., Wang, X., & Guo, H. (2020,
https://www.researchgate.net/publication/346327953_S March). Laboratory investigation on effects of
tudy_on_the_fatigue_properties_of_bitumen_emulsion microwave heating on early strength of cement bitumen
cement_mastics_using_frequency_sweep_and_linear_a emulsion mixture.ResearchGate;Elsevier.
mplitude_sweep_tests https://www.researchgate.net/publication/339604347_L
[22] Suryakanta. (2016, January 11). BITUMEN EMULSION aboratory_investigation_on_effects_of_microwave_hea
– WHAT, WHY & HOW? - CivilBlog.org. CivilBlog.org. ting_on_early_strength_of_cement_bitumen_emulsion
https://civilblog.org/2016/01/11/bitumen-emulsion- _mixture
what-why-how/ [26] Wassenberg, Okkerman, Grosshart (2001). Chemical
[23] Susanna Lauren, (2018). What are surfactants and how study on alkylphenols. https://edepot.wur.nl/174304
do they work? . Biolinscientific.com. [27] Weissenborn, P., & Motiejauskaite, A. (2000). Drying of
https://www.biolinscientific.com/blog/what-are- Alkyd Emulsion Paints Drying of Alkyd Emulsion
surfactants-and-how-do-they-work Paints. 72(906), 65. https://www.paint.org/wp-
content/uploads/2021/09/jctJUL00-Weissenborn.pdf