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Water-diesel separation. part 2: Impact of fuel

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Water/Diesel Separation. Part 2:

Impact of Fuel Additives on the Physical Properties of

Water/Diesel Emulsions

Steffen Schütz, Dagmar Winkler, Pius Trautmann, Jochen Reyinger, Uwe Staudacher
Hindenburgstraße 45, D-71638 Ludwigsburg, Germany
Phone: (+49) 7141 98-3610
Fax: (+49) 7141 98-183610


Modern diesel combustion engines with high pressure injection systems are sensitive to diesel
fuel with dispersed water droplets which can lead to insufficient lubrication, hazardous corrosion
or fouling effects [for2002, ver2010, wil2009]. It is common to use fibrous filter media and filters
to separate water droplets from diesel fuels to protect the high pressure injection components,
thus achieving their designed service life. Generally two wide-spread filtration techniques for
water/diesel separation are applied. Either a single hydrophobic filter medium is used as barrier
layer for the water droplets or a two-stage coalescence concept. This coalescence system
combines a hydrophilic (oleophobic) and a hydrophobic (oleophilic) filter layer. This combination
enables a separation of water droplets with an increased droplet size due to coalescence
[kle2005]. Regarding the investigations discussed hereafter, the experiments were usually
performed with a hydrophilic filter medium.
In the existing test standards [sae1488, iso4020, iso16332, sta2007, sto2009, yan2010] for
water/diesel systems and separators, the impact of the real fluid properties of modern and
future diesel fuels and water/diesel systems are not properly considered. Diesel components
(mainly biodiesel blends) and fuel additives have changed dramatically during the last decade.
This is important when the influence of fuel additives on the stability and the separation
behaviour of water/diesel emulsions with coalescence filters are investigated.
One basic property of water/diesel emulsions is the interfacial tension between water and diesel
fuel (which is characterized with its value after a contact time of 60 s between the two fluids as
per the relevant standards). New investigations show the dynamic behaviour of this parameter.
The second basic material property is the contact angle which also can be a dynamic
parameter. The contact angle is often neglected in actual investigations on water/diesel
separation. Its value describes the wettability of filter media with water droplets and depends on
the three-phase system water, diesel and fiber material.
In this presentation we demonstrate how fuel additives influence these two properties as they
are determined by the types of fuel additives, their adsorption kinetics and further parameters.
With further experiments, considering the emulsion stability it is proved that there is no distinct
correlation between the dynamic interfacial tension and the stability of a water/diesel emulsion.
Otherwise a correlation between the dynamic character of the contact angle and the emulsion
stability can be shown.
The investigations show that the dynamic transport processes, e. g. diffusional transport, at the
three-phase interface water/diesel/filter medium is impacted by two time scales. One time scale
is the interfacial age of the water/diesel interface. The second time scale is the adsorption time
which describes the contact between the diesel fuel and the filter medium surface.
Finally it is shown that multiple emulsions can result where small diesel droplets are included in
water droplets which are dispersed in the continuous diesel phase. The multiple emulsions are
generated with specific operational conditions, material properties and additive species.
Chapter two gives an overview on water/diesel systems. The characterization of these systems
by the dynamic interfacial tension is presented in chapter three. Chapter four is dedicated to the
discussion on the dynamic contact angle in the water/diesel/surface system. In chapter five
some investigations on the stability of water/diesel emulsions and three-phase emulsions are


In an array of presentations at the AFS Annual Conference in 2010 the reasons for the water
intake in diesel and the mechanisms and possible drawbacks of water/diesel separating
systems were discussed. The main reasons for the water content in diesel are condensation of
humid ambient air and water intake during tank ventilation, storage and transportation.
Due to the high energy generated within the fuel delivery circuit of diesel combustion engines,
especially by the fuel supply pump, water droplets are produced and water/diesel emulsions are
generated. The formation of these emulsions is especially caused by the high rate of fuel
recirculation of modern engines. The evolving diesel fuel quality of the last decade, through
introduction of biodiesel blends and higher additive contents, to improve lubricating properties,
stabilized the water/diesel emulsions. One stabilization mechanism is the generation of smaller
water droplets with diameters of few microns, another one is the surface active potential of fuel
additive types included in biodiesel and in additives which lower the interfacial tension between
water and diesel. Especially those surfactants can change the surface properties of
coalescence filter media (commonly used to separate dispersed water droplets from diesel
fuel). Those coalescent filter media are often designed with a hydrophilic filter layer. They cause
the small water droplets to coalesce and a subsequent hydrophobic barrier medium. Many
experimental investigations have shown, that these filter media can lose their coalescing
characteristics after some operating time.
The increasing amount of water in diesel results in damages on relevant parts of diesel
combustion engines, especially due to corrosion, cavitation and biological growth.
Figure 1 shows the principal set-up of a coalescence filter-based water/diesel separation
system. The diesel fuel with dispersed water droplets is brought to the filter medium. Due to the
droplet coalescence, the increased water droplets settle down under gravity and can be
extracted. Water-free diesel fuel is provided to the injection system. This process works very
well with low or no additive reference diesel. The usage of commercially available diesel fuels
with increased additive contents often leads to failures of the water separation system. With the
usage of additives, the physical properties of the water/diesel systems are changed and the
surface properties of the coalescence filter media are modified and the originally hydrophilic
filter medium becomes hydrophobic [pet2009].
Figure 2 shows the typical course of the separation efficiency of many coalescence filter media
with time. They are exposed to water/diesel systems with commercially available diesel fuels.
Similar behaviour was observed by [panwfc2008, pan2008, pansae2009, sta2009].
The broad variety of physical and chemical properties of water/diesel systems couple with the
impact parameters on the water/diesel separation systems provide a basis to understand the
challenges of water/diesel separation. The water/diesel emulsions themselves are stabilized by
• additive components which are used to improve the lubrication capability of diesel fuels,
especially with ULSD (ultra low sulphur diesel), to improve the cetane number and the
deposit control
• biodiesel blends which depend on the feedstock from which the biodiesel originates
(vegetable oil or animal fat) [sha2008, kal2007]

• low-molecular by-products which are generated during the transesterification reaction to

gain biodiesel [panafs2009, sha2008]
All these parameters influence the properties of water/diesel emulsions, e. g. [sch2010,
• the stability of water/diesel emulsions as they decrease the interfacial tension and the
energy content of the interface
• the contact angle at the three-phase interface water/diesel/filter medium
• the adsorption kinetics of surfactants at the water/diesel interface and at the surface of
coalescence filter media
• the droplet size spectrum as they reduce the droplet diameters which are generated in
the diesel fuel circuits

Figure 1: Working principle of water/diesel separation with a coalescence filter.

Separation efficiency [%]





Some minutes to some hours Time

Figure 2: Time-dependent separation efficiency of many coalescence filters with commercially

available diesel fuels.

In the following investigations the characteristics of different diesel fuels with various additive
types are investigated with a focus on the interfacial tension, the contact angle and the
emulsion stability. Besides the influence of the fluid system itself the dynamic short and long
time behaviour of the interfacial tension and the contact angle is highlighted.
Various additive components are available either to modify distinct properties (low temperature
stability, lubricity, …) of diesel fuels or as additive packages with a mixture of different, usually
unknown additive species and multiple effects. The diesel fuels selected should be similar to
commercially available diesel fuels. The diesel fuels and additive types were used in the
investigations according to Tables 1 and 2.

Table 1: Diesel fuels used in the investigations.

Diesel B0 B0 Diesel fuel without any biodiesel content

Diesel B20 B20 Diesel fuel with 20 vol.-% biodiesel content

CEC Reference Diesel CEC Reference diesel fuel with low additive content

Table 2: Diesel fuel Additives applied in the investigations.

Anti-bacteria additive Biocide Biocide

Commercial additive package C1 Additive package for mineral oil industry

Commercial additive package C2 Additive package for mineral oil industry

Commercial additive package E Emulsifier

Commercial additive package DE Mixture of demulsifier/emulsifier


The interfacial tension (IFT) is a measure characterizing the energy content of an interface. For
the generation of water droplets in diesel, an energy input is required. This energy input is
partially stored in the increased interface of a fine disperse water droplet system. So the bigger
the water/diesel interface becomes with decreasing droplet diameters the stability of the
dispersed two-phase system decreases. But this is only true in a fluid system with two pure
According to standards the interfacial tension between water and diesel is measured by a ring
tensiometer [astm971]. In this static measuring technique a ring made of platinum is drawn
through the water/diesel interface slowly and the maximum force on the ring is recorded.
Dependent on the geometry of the ring, the interfacial tension can be recalculated. Usually the
interfacial tension is measured at an interfacial age of 60 s. The term “interfacial age” describes
the age of the water/diesel interface. During this period molecular diffusion causes the transport
of surfactants to the interface which usually lowers the interfacial tension. In addition the

interfacial tension depends as well on the temperature as diffusion becomes faster with rising
temperature and also on the concentration of the surfactants.
In our investigations we have applied a dynamic measuring technique, the droplet volume
method (DVM). Within this procedure the interfacial tension is determined by the generation of
water droplets in diesel. A pre-defined amount of water is pumped into the diesel through a
nozzle. The interfacial tension can be calculated form the droplet size, capillary shape and from
the droplet generation rate (number of droplets over time).
Figure 3 shows the interfacial tension of water in different diesel fuels with various additive
types and concentrations measured with the ring tensiometer. The time-dependent behaviour is
obvious, the interfacial tension drops with the interfacial age, i. e. the droplet formation time.
The interfacial tension also depends on the additive types.

Interfacial Tension [mN/m]



0 50 100 150 200 250

Interfacial Age [s]

Figure 3: Dynamic interfacial tension dependent on the interfacial age for reference diesel with
various additives (green curve: additive C1 with 0.015 mass-% blue curve: additive E with 0.039
mass-%, red curve: additive DE with 0.038 mass-% and yellow curve: B0 diesel).

The same behaviour is shown in Figure 4. The interfacial tension of three different commercially
available diesel fuels (green, red and blue symbols) according to the EN 590 standard is
determined with the DVM dependent on the droplet formation time (interfacial age) for a lower
time range up to 90 seconds. The IFT was determined three times for each diesel brand (round,
triangular and diamond shapes) and the measuring values are reproduced well. The
dependency of the interfacial tension on the time and on the diesel quality is observed.
The question for the behaviour of the interfacial tension within an interfacial age of about 1
second or less arises from practical reasons because in the real separation process with
coalescence filters the water droplets hit the filter fibers within such a tight time slot. To get a
closer insight, short time measurements were performed with the droplet volume method. The
result is given in Figure 5. For measuring times below 0.5 s signal noise appears as the
dynamic limit of the measurement technique is reached. Dependent on the kind of water/diesel
system a maximum interfacial tension arises within a time slot of 1 s to 5 s. With increasing
additive concentrations from additive-free CEC reference diesel to a B20 biodiesel blend with
20 vol.-% biodiesel content the interfacial tension decreases clearly. Due to the increased
diffusion velocity of surfactants to the water/diesel interface with higher surfactant

concentrations, the maximum plateau develops more quickly with increasing additive
concentrations from CEC to B20 diesel.
The dynamic behaviour of the droplet-fiber contact is shown by numerical simulations based on
computational fluid dynamics [win2010].

22 And within the

first time interval ???
Interfacial Tension [mN/m]






0 10 20 30 40 50 60 70 80 90

Droplet Formation Time [s]

Figure 4: Dynamic interfacial tension dependent on the droplet formation time for three different
commercially available diesel fuels according to EN 590, each water/diesel system was
measured three times according to the different symbols.

CEC reference diesel /1
Interfacial Tension [mN/m]

CEC reference diesel /2

EN 590 diesel /1

25 EN 590 diesel /2

20 EN 590 blend 2008 /1


15 EN 590 blend 2008 /2


B20 diesel /1
B20 diesel /2
0,1 1 10 100

Droplet Formation Time [s]

Figure 5: Dynamic interfacial tension dependent on the droplet formation time for four diesel
fuels with different additive contents (red curve: CEC reference diesel with low additive
concentration, blue curve: commercially available diesel blend from 2008 according to EN 590,
green curve: actually commercially available diesel according to EN 590, yellow curve:
Biodiesel blend with 20 vol.-% biodiesel content).


Besides the interfacial tension the contact angle is the other relevant parameter which
describes the wettability of a solid surface in a three phase system. Regarding standards in
water/diesel separation, the impact of the contact angle is neither specified nor characterized in
any way. Only in the paper [shi2004] the improved separation efficiency in coalescence filtration
with low static contact angles and full wettability of the filter fibers with the disperse phase is
described as a relevant mechanism to coalescence filtration.
Figure 6 shows two extreme cases: On the left the wetting case with a water droplet in diesel
fuel on a hydrophilic surface (contact angle Θ<90o) and on the right the non-wetting case with a
water droplet in diesel fuel on a hydrophobic surface (contact angle Θ>90o) is shown by photos.
The static contact angle Θ is analytically described by Young’s equation:
σs,d = σs,w + σ w,d cos Θ

Here σs,d is the interfacial tension between the solid surface and the diesel fuel, σs,w is the
interfacial tension between the solid surface and water and σw,d is the interfacial tension
between water and diesel.

Figure 6: Water droplet in diesel on a wetting and on a non-wetting surface.

The static contact angle depends on:

• the chemical surface properties, e. g. the molecular structure of a surface
• the physical surface properties, e. g. the surface roughness
• disperse and continuous phase
In fact the contact angle is a dynamic parameter also depending on the transportation state of a
surface such as
• interfacial velocity
• material properties of the fluid phases, e. g. the diffusion coefficients of surfactants

Regarding especially the separation of water/diesel systems with filter elements there are
characteristic time scales of some physical processes which influence the measured values of
the contact angle. These time scales are shown in Figure 7.

1 2 3 4

Adsorption Time AT

Interfacial Age IA

Wetting Time WT

1: Start contact filter medium (surface)/diesel

2: Generation water droplet in diesel
3: Droplet deposition on filter medium
4: End of measurement

Figure 7: Different time scales which are relevant for the characterization of dynamic contact
angles in the three-phase system water/diesel/filter medium.

The first relevant time scale is the adsorption time AT. This time scale describes how long a
solid surface (e. g. filter medium) is exposed to a diesel fuel. It is called adsorption time
because within this time range, additive components and surfactants from the diesel fuel adsorb
on the surface of the filter medium. This time range ends when a water droplet hits the surface
of the filter medium. From this time point 3 on the wetting time WT starts in Figure 7.
Before a droplet is deposited on the solid surface it is generated within the diesel fuel. The
contact time of the droplet from the moment just after its formation within the diesel fuel is
denoted as interfacial age (IA). The interfacial age ends with the droplet deposition on the solid
surface and covers the time interval 2 to 3 in Figure 7.
The influence of the interfacial age and the wetting time on the contact angle is shown in Figure
8 for a droplet of distilled water on a glass surface in B0 diesel with low additive concentration.
The photos show a droplet on a glass surface with an interfacial age of 20 s, 100 s and 245 s.
The photos are taken after wetting times of 0 min, 5 min, 10 min and 30 min. The quantitative
value of the contact angle dependent on the wetting time is shown in the diagram on the right.
The temperature is 25 oC.

B0: IA = 245 s, T = 25°C 170

B0-Diesel GA245s
B0: IA=245s,
Contact Angle [°]

0 min 5 min 10 min 30min 140
B0: IA = 100 s, T = 25°C B0-Diesel GA100s
B0: IA=100s,
B0-Diesel GA60s
B0: IA=60s,
0 min 5 min 10 min 30min 100

B0: IA = 20 s, T = 25°C 90 B0-Diesel GA20s

B0: IA=20s,
80 T=25°C
0 10 20 30 40

0 min 5 min 10 min 30min Wetting Time WT [min]

Figure 8: Influence of the interfacial age IA and the wetting time WT on the contact angle of a
water droplet on a glass surface in B0 diesel.

It is obvious that in this case regarding a diesel fuel with low additive content the wetting time
determines the contact angle for low time scales (minutes) but not for increased wetting times.
With an increasing interfacial age the water droplet shows an increasing contact angle on the
glass surface. This is due to the diffusion transport of additives to the water/diesel interface and
the change in the surface charge with additive molecules. After droplet deposition on the
surface the contact angle remains constant and stable.
In Figure 9 we see the influence of the additive concentration. This is the temperature and the
wetting time on the contact angle for a droplet of distilled water on a glass surface. CEC
reference diesel was blended with additive C1 with concentrations of 0.015 mass-% and 0.047
mass-%. The investigations were performed at 20 oC and 40 oC. The temporal increase of the
contact angle gets faster both for higher additive concentration and temperature. This is due to
the increased adsorption kinetics with the temperature and the steeper additive concentration
gradient from diesel fuel to surface. Due to the additive content in this fluid a longer wetting time
results also in an increased contact angle. No steady state is achieved as this was the case for
the conditions with Figure 8 where B0-diesel was used. The increased additive content leads to
a long time diffusion process which results in a time dependent contact angle after 30 min as
the diffusion is not yet completed.

C1-0.047%: IA = 30 s, T = 20°C 170

K-0,047% T=20°C
Contact Angle [°]

IA = 30s,
0 min 5 min 10 min 30min 140 T=20°C
C1-0.015%: IA = 30 s, T = 40°C
K-0,015% T=40°C
IA = 30s,
110 T=40°C
0 min 5 min 10 min 30min 100
K-0,015% T=20°C
C1-0.015%: IA = 30 s, T = 20°C 90
IA = 30s,
0 20 40
0 min 5 min 10 min 30min Wetting Time WT [min]

Figure 9: Influence of the interfacial age IA, the temperature and the additive concentration on
the contact angle of a water droplet on a glass surface in a C1 diesel blend.

With Figure 10 the effect of the adsorption time on the contact angle is shown (see photos). In
these investigations an originally hydrophilic filter medium was used and wetted with a
commercially available EN 590 diesel fuel for different adsorption times AT (few seconds, 30
min, 24 h). A droplet was generated at a nozzle and deposited immediately on the filter medium
so that the interfacial age IA was low in all three cases. The droplet on the filter medium with the
longest adsorption time (24 h, top line in Figure 10) is not absorbed by the filter medium, neither
after 30 min nor after 20 h. If the filter medium is exposed to the diesel fuel for 30 min, the
droplet is absorbed after less than one minute (middle row in Figure 10). With a low adsorption
time the water droplet is absorbed within few seconds after deposition.

Figure 10: Influence of the adsorption time of a filter medium in a EN 590 diesel fuel with
additive contents and the consequences for the water absorption capability.

This investigation shows that an originally hydrophilic surface is hydrophobized by the additive
types in the diesel fuel and the absorption capacity of the filter medium for water droplets is
decreased dramatically.


The stability of a water/diesel emulsion can be measured either by droplet size distributions or
turbidity of the water/diesel emulsion dependent on time. One of the simplest methods is the
measuring of the coalescence and sedimentation behaviour of a water/diesel emulsion in an
Imhoff funnel. With this measurement technique the stability or instability of an emulsion is
captured by the time which passes during emulsion generation and gravitational sedimentation
of water droplets, which are often increased by coalescence. To be more precise the volume of
the water sediment in the lower part of the Imhoff funnel is determined dependent on time. With
increased emulsion instability the droplet coalescence is faster and the water droplets settle
down more quickly.
The diagram in Figure 11 shows the volume of water sediment in an Imhoff funnel dependent
on time. Four diesel qualities with different additive contents and different interfacial tensions
were investigated. The interfacial tension between the water and the diesel phase was
measured with interfacial ages about 160 s for all samples with the static ring method
The water/diesel system with an additive content C1 with 0.015 mass-% showed to be the most
unstable and the corresponding sedimentation curve (blue symbols) has the steepest increase.
The water/diesel system with an additive content DE with 0.033 mass-% shows almost the
same behaviour though the interfacial tension is quite lower (18.2 mN/m compared to 29.6
mN/m for the system with additive C1). The B0 system (green symbols) shows a significantly
increased stability with a flat sedimentation curve and the water/diesel system with the additive

E (0.033 mass-%) seems to be completely stable as there is no visible water sedimentation

within the observation time of 1500 s. For these two systems the interfacial tension values are
similar (23.8 mN/m and 25.3 mN/m) and lie between the interfacial tension values of the first
systems with the C1 and the DE additives.

20 C1-0.015%, DE-0.033%,
t = 197 min t = 90 min
Sedimentated Water [ml]

16 Θ dynamic Θ dynamic
14 K-0,015%

DE-0.033% IA = 161 s IA = 161 s
10 σ = 29.6 mN/m σ = 18.2 mN/m
8 B0-Diesel
B0 E-0.033%,
6 E-0,033% t = 120 min t = 120 min
Θ static Θ static

0 500 1000 1500 IA = 162 s IA = 158 s
Time [min] σ = 23.8 mN/m σ = 25.3 mN/m

Figure 11: Water sedimentation volume dependent on time and correlation to the additive
content, to the interfacial tension and to the contact angle.

From this stability behaviour one can conclude that there is no correlation between the static
interfacial tension and the coalescence behaviour to describe the stability of a water/diesel
With Figure 11 these experimental results are also correlated to the contact angle. During
contact angle measurements with the water/diesel system containing the C1 and the DE
additive a dynamic contact angle was detected dependent of the wetting time. These two
systems show a quite instable character with a high sedimentation velocity. The two systems
with the B0 diesel and the E additive show a steady contact angle after some time and a high
stability with low or no water droplet coalescence and sedimentation. We can observe from
those experiments that the dynamic behaviour of the contact angle seems to correspond to an
instable emulsion whereas a steady contact angle corresponds to a stable water/diesel
Within many experiments an optically visible, white phase with a foam character could be
observed between the water sediment and the diesel phase above. The photo in Figure 12
shows a water/diesel emulsion with an E additive content of 0.033 mass-% and 2 vol.-% water
content 20 days after its generation. This effect was also observed by other authors [pan2008].
The microscopic photography taken from this white phase on the right shows that there is a
multiple diesel/water/diesel emulsion.
A multiple emulsion can be generated with different water contents, energy inputs and operating
times. In the experiments emulsions with 1 and 10 vol.-% water content were produced with an
Ultra Turrax stirrer at 4,000 and 10,000 rpm and dispersion times of 5 s and 30 s.

Figure 12: Analysis of the white phase between the water sediment and the diesel phase:
macroscopic view (left) and microscopic analysis (right).

In Figure 13 the resulting emulsions are shown according to their dispersity state and
depending on the operating and boundary conditions. All emulsions contain the E additive with
0.038 mass-%. With the low water contents the common water/diesel emulsions were
produced. With the increased water content multiple water/diesel/water emulsions were
generated. These results are independent of the blending force and the dispersion time.

Figure 13: Classification of water/diesel and diesel/water/diesel emulsions dependent on water

content, energy charge and dispersion time.

The dispersity state itself, i. e. the droplet sizes depend strongly on the stirrer speed and the
dispersion time with finer droplets corresponding to higher energy inputs.


The experimental investigations of water/diesel systems show explicitly the need to better
define the material and operational parameters. This is essential for the standards which
describe the testing procedures for water/diesel separators. As of today those standards do not
consider enough the influence of several parameters. Experimental data are often not

comparable because of the different boundary conditions used. The variation is born from the
parameter ranges allowed in the respective standards. As a consequence, the experiments
provide no evident correlation between material and operational parameters on the one side
and the water separation efficiency on the other side. The experiments have also shown the
importance of the short and long time effects on the dynamic behavior of water/diesel
separation systems. This is especially true for coalescence filter media and elements.
The existing or upcoming standards for water/diesel separators do not precisely consider the
broad variety of material and operational parameters of new diesel fuel qualities nor the
characteristics of real water/diesel emulsions and surface properties. It is essential to adapt the
existing standards with the future trends and developments of the fuel and the engine markets
This study has enabled MANN+HUMMEL to improve his offering in terms of water/diesel
separation solutions and to offer the latest technology in terms of filtration to its customers.

This investigation is the result of a cooperation project between MANN+HUMMEL GMBH

Ludwigsburg (Germany) and the University of Stuttgart (Germany) Institute of
Mechanical Process Engineering (IMVT).


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