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Standardization of Oil Sorbent Performance Testing

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 Journal of
Testing and Evaluation
Alireza Bazargan,1,2 Jun Tan,1 and Gordon McKay3

DOI: 10.1520/JTE20140227

Standardization of Oil Sorbent

Performance Testing
VOL. 43 / NO. 6 / NOVEMBER 2015

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 Journal of Testing and Evaluation

doi:10.1520/JTE20140227 / Vol. 43 / No. 6 / November 2015 / available online at www.astm.org

Alireza Bazargan,1,2 Jun Tan,1 and Gordon McKay3

Standardization of Oil Sorbent

Performance Testing

Reference
Bazargan, Alireza, Tan, Jun, and McKay, Gordon, “Standardization of Oil Sorbent Performance Testing,”
Journal of Testing and Evaluation, Vol. 43, No. 6, 2015, pp. 1–8, doi:10.1520/JTE20140227. ISSN 0090-
3973

ABSTRACT
Manuscript received May 14, 2014; Millions of barrels of petroleum and its products are transported across the globe every day.
accepted for publication July 23, 2014;
published online October 10, 2014.
The hazard of oil spills is a looming threat that can lead not only to the loss of valuable
products, but also seriously damage the environment and ecosystems. There are various
1
Department of Chemical and
Biomolecular Engineering, Hong Kong
ways of combating oil spills one of which is the use of sorbents. The ASTM F716-09 and
Univ. of Science and Technology, ASTM F726-12 standards have been developed for absorbent/adsorbent performance and
Clearwater Bay, Hong Kong.
uptake capacity testing. However, most researchers do not use the procedures proposed by
2
Department of Chemical Engineering the ASTM when reporting their findings. Currently, the majority of the manuscripts
and Biotechnology, New Museums Site,
published on oil sorbent testing do not use any uniform standard. Herein, we argue that the
Pembroke Street, Univ. of Cambridge,
Cambridge CB2 3RA, United Kingdom. ASTM standards have some shortcomings that make them unattractive for researchers to
3
use. These problems are discussed and possible solutions are proposed for more
Department of Chemical and
Biomolecular Engineering, Hong Kong homogeneous and accurate reporting of results.
Univ. of Science and Technology,
Clearwater Bay, Hong Kong
(Corresponding author), Keywords
e-mail: kemckayg@ust.hk absorption, adsorption, oil spill remediation, methodology, petroleum clean up

Introduction
The massive need for energy in today’s world has resulted in the exploration, extraction, and
transport of millions of tons of oil across the globe. In the event of an accidental spill, in addition
to the loss of valuable liquid products, serious environmental, health, safety, and economical
problems may be caused. Large spill disasters can take many years or even decades to clean up.
Almost all sectors of society are concerned with such events including environmentalists, scien-
tists, industries, stock holders, and the general public. Petroleum spills can have direct adverse

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C
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2 Journal of Testing and Evaluation
effects on marine life as well as chronic effects on entire ecosys-
tems [1,2]. In order to combat oil spills, several strategies can be
applied. The strategy selected is dependent on the type of spilled
petroleum product, geography of spill site, weather conditions,
and various other factors. If the spill takes place on open waters,
the more volatile fraction is prone to weathering and evapora-
tion, while the heavier components will form slicks and/or sink
to the bottom of the sea [3]. The detrimental effects of oil spills
can be diverse ranging from genetic modification of microbial
and enzymatic activities in the natural microbial community in
oil-contaminated sediments [4] to decrease in strength and per-
meability of effected soils [5].
Oil spills are an important area of research with hundreds
of manuscripts published on the topic each year. The proceed-
ings of the “International Oil Spill Conference,” which is one of
the many outlets for publishing such studies, contains more
than 3000 manuscripts to date [6]. A wide array of problems
resulting from oil spills have been investigated in areas such as
the Persian Gulf (although some have incorrectly referred to the
“Persian Gulf” with other false names such as the “Arabian
Gulf” [7]).
Methods for combating spills can be categorized into
mechanical, chemical, physicochemical, biological, etc [8]. The
use of dispersants, sorbents, solidifiers, booms, and skimmers
are widespread [9–11]. Booms are used to limit the oil from
spreading and skimmers are used to collect it. Using sorbents
for the collection of spilled oil is another option [12–18]. In
recent years, hundreds of various natural and synthetic materi-
als have been tested as possible oil sorbents [19–26].
Although the testing of sorbents for oil spill clean-up is a
popular area of research, unfortunately many inconsistencies
exist in reporting the experimental data. In this manuscript, the
discrepancies of these studies are discussed and areas of concern
are highlighted. Regrettably, too often the results of studies are
compared without any consideration of the differences in the
methodologies used. Although the ASTM F716-09 [27] and
ASTM F726-12 [28] exist as standard test methods, they are not
universally used among researchers. Possible reasons as to why
the ASTM standards are ignored will be mentioned and solu-
tions for overcoming the shortcomings will be suggested.
Analysis of Current Methods
The ASTM F716 and ASTM F726 standards pertain to absorb-
ent and adsorbent performance testing respectively (refer to the
Terminology section of this paper for definitions). The current
paper is specifically focused on the sorption capacity of the
sorbents. Therefore, sections of the ASTM standards which
address other issues are not considered. For example, from
ASTM F716, only section 11.3 is relevant to this paper. Section
11 of ASTM F716 contains subsections related to oily material
absorption (11.2), rate of release testing (11.3), penetration
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(11.4), release to other materials (11.5), and fluids more dense
than water (11.6). ASTM F726 is more directly related to the
topic of the current paper. Nonetheless, sections such as
dynamic degradation testing (9.2) and extraction and reuse
(10.1–10.4) are not commented upon.
SORBENT TYPES
The current standards divide sorbents into 4 types [28]. Type I
sorbents are those with length and width much greater than
their thickness such as films, sheets, pads, etc. Type II are loose
sorbents that are unconsolidated particulate material and are
handled with scoops or similar equipment. Type III is defined
as enclosed sorbents such as pillows and booms, which confine
the sorbent material by an outer permeable fabric or netting.
Finally, Type IV are those sorbents such as pompoms with an
open structure that allows the intrusion of high viscosity oils.
TERMINOLOGY
Before considering any of the details regarding the ASTM meth-
ods for oil uptake capacity measurements, it is suitable to note
the scattered (and often incorrect) terminology used for describ-
ing the phenomenon of oil sorption onto the sorbents among
researchers. In the literature, the words “adsorption” and
“absorption” have unfortunately often been used loosely and
interchangeably. Absorption is a bulk phenomenon which is the
result of the assimilation of the liquid molecular species
throughout the bulk of the sorbent. Meanwhile, adsorption is a
surface phenomenon which is the result of the accumulation of
liquid molecular species at the surface rather than in the bulk of
the sorbent. Using a more general term such as “sorption,”
which can be considered as encompassing both adsorption and
absorption, is more suitable. Therefore it is advised that unless
future researchers have distinct reasons to use either absorption
or adsorption specifically, they refrain from using either term,
and the word sorption is used. A sorbent can be defined as a
material “used to recover liquids through the mechanisms of
adsorption or adsorption, or both” [28]. The liquid uptaken by
a sorbent (in particular type II, III, and IV sorbents) is often the
result of both adsorption and absorption phenomena. Table 1
provides examples of various studies that have used the terms
absorption, adsorption, and sorption.
The ASTM standards give the following definitions for ad-
sorbent and absorbent [27]:
TABLE 1 Examples of varying terminology used to describe the
uptake of the oily liquid by the sorbent.
Terminology Used References
Absorption [29,30]
Adsorption [31,32]
Sorption [33,34]

“Absorbent—a material that picks up and retains a liquid
distributed throughout its molecular structure causing the solid
to swell (50 % or more). The absorbent is at least 70 % insoluble
in excess liquid.
Adsorbent—an insoluble material that is coated by a liquid
on its surface including pores and capillaries without the solid
swelling more than 50 % in excess liquid.”
The ASTM standards stress that F716 should only be
applied to absorbents, whereas F726 is suitable solely for
adsorbents. However, this type of distinction is not suitable. For
all practical purposes, a material that swells 49 % is very similar
to one which swells 51 %; yet if the ASTM standards are to be
followed, such similar materials will not be subjected to the
same tests and will be evaluated differently. This is a flaw of the
current structure of the standards. Perhaps it would be better to
merge the F716 and F726 standards into one standard which
encompasses both absorbents and adsorbents instead of placing
an arbitrary cut-off point at 50 % swelling.
UPTAKE CAPACITY MEASUREMENTS
There are various methods for evaluating sorption capacities.
The simplest methodology used for testing the uptake capacity
of the sorbents follows similar steps [35,36]. The uptake
capacity is also referred to as the absorbency ratio, and is
reported as the mass of liquid uptaken per mass of sorbent. The
sorption capacities are either measured by hanging reading
scales, top loading balances with a hook, or with normal bench
top scales. First, the dry sorbent is weighed and placed in a net.
Then, the net holding the sorbent is submerged into the liquid
and allowed to stay for a duration of time. Next, the net is
removed from the liquid and allowed to drain. Finally, after the
excess liquid has been drained, the uptake capacity of the sor-
bent is calculated. Other variations of this methodology have
also been used [37–47]. For Type I sorbents, no net is required,
and the sorbent can be directly hung to drain. In ASTM F726’s
oil adsorption short test (9.3), a contact time of 15 min between
the liquid and sorbent is suggested, followed by a dripping time
of 15 s or 2 min depending on the viscosity of the oil. In the
TABLE 2 The contact and dripping times in various studies for liquid sorption calculations. Note that the dripping times vary from seconds to hours
which may radically affect the reported uptake capacity.
Contact Time
Unreported
Unreported 10 s of dripping followed by wiping the bottom of the mesh to remove excess oil
15 min (short test) or 24 h (long test)
10 min
5 min
10 min
10 min
2 or 15 h
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BAZARGAN ET AL. ON OIL SORBENT PERFORMANCE TESTING 3
long test (9.4), a 24 h contact time is provided instead of 15 min
with the other features of the test remaining the same.
Section 11.2 of ASTM F716 suggests a completely different
method of assessing the absorbing material’s inherent capacity
referred to as the absorption efficiency. Since the current paper
is focused on gravimetric experiments for adsorption capacity
measurements, the test regarding absorption efficiency is not
elaborated upon.
CONTACT AND DRIPPING TIMES
Most sorption studies include a step in which the sorbent is
contacted with the oil denoted here as the “contact time,” fol-
lowed by a step in which the sorbent is removed from the liquid
bath and allowed to drip designated as the “dripping time.”
Longer contact times ensure that the sorbent has uptaken the
maximum amount of the liquid, i.e., it has reached saturation. If
an adequate contact time is not employed, the sorbent will show
less-than-saturated uptake capacities. If the contact time is
extended longer than needed for saturation, the uptake capacity
will not be affected as it cannot increase any further. However,
since most researchers are keen on reporting higher uptake
capacities, all studies allow for enough contact to ensure satura-
tion has been reached. Contrary to the contact time, which can
be chosen above the saturation point, the dripping time is cru-
cial and should not be chosen arbitrarily. The dripping step is
used to ensure that the liquid which is loosely held by the sor-
bent is lost due to the gravitational pull. If the drainage is not
adequately long, the values reported for the uptake capacity will
be inaccurately high. Table 2 provides a list of studies which
have implemented different contact and dripping times for
measuring uptake capacity. Evidently, a large range of contact
and dripping times are employed. These inconsistencies lead to
major differences among the reported results.
Studies which do not incorporate adequate dripping times
and measure the uptake capacity quickly after the removal of
the sorbent from the liquid basin, report higher (and often
bloated) sorption capacity values. For example, studies within
our research group show that when testing the uptake capacity
Dripping Time References
Unreported [48]
[49]
30 s or 2 min (for heavy or weathered oil) [28]
1 min [50]
5 min [51]
10 min [31]
15 min [52]
1 or 3 h [53]
4 Journal of Testing and Evaluation
of RMG380 marine residual fuel with rice husk sorbents, the
measured uptake capacity will decrease by 50 % if the sorbent is
allowed to drip for 30 min instead of 30 s [54]. Such large varia-
tions cannot be overlooked. As such, when comparing the
reported data in literature regarding uptake capacities, one must
be aware of the employed dripping time.
In order to overcome the problem arising from employing
different drip times, it is suggested for researchers to report
the measured uptake capacity of each sample recorded at dif-
ferent drainage periods. This solution would effectively result
in drainage profiles exhibiting the kinetic data of liquid reten-
tion. Such a curve, shown in Fig. 1, would appear as follows:
immediately after the removal of the sorbent from the liquid
basin, the gravitational forces acting on the system result in
fast removal of large amounts of oil from the sorbent. As
more oil is lost and the drainage progresses, the oil remaining
in the sorbent becomes less susceptible to dripping. With the
passing of time, less oil is lost due to downward gravitational
forces. The process continues until gravity is no longer strong
enough to remove any more oil from the sorbent. The equilib-
rium uptake capacity (Ce) can be defined as the uptake
capacity at the point when no more drops of liquid are lost
due to further drainage. This point in time has been referred
to as “the point of no dripping” [34] and can also be called
the equilibrium time (te). It is expected that uptake capacities
for various samples will exhibit different degrees of depend-
ence on the dripping time. Some sobent–sorbate systems may
have very sharp declines in the initial moments of drainage,
while others may drain less quickly.
Reporting the full dripping profile for the sorbent–sorbate
system will allow a better assessment of the sorbent’s perform-
ance. It should also be noted that the speed at which the liquid
is lost is not only a function of the sorbent, but also a function
of the sorbate properties. A sorbent may lose a particular
FIG. 1 The measured uptake capacity of a sorbent versus dripping time (also
referred to as the retention profile). C1 and C2 show the uptake
capacity if 30 s and 2 min of dripping are allowed, respectively. Ce is
the equilibrium uptake capacity reached at the time when dripping
stops (te).
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sorbate quickly, while exhibiting more resistance towards the
dripping of another sorbate.
NET MESH SIZE AND SORBENT AMOUNT
If a net is employed to hold the sorbent during the test, some
liquid will be trapped between the sorbent particles and the net
body. If the net has small holes or if not enough sorbent is used,
the amount of trapped liquid between the net and sorbent will
be a significant portion of the amount of liquid retained by the
entire experimental setup. The liquid held at the contact points
between the sorbent and the net is not technically uptaken by
the sorbent; however, in the uptake capacity calculations, this
amount of liquid trapped between the net and the sorbent will
be unwantedly included. Hence, in such a case, the final
reported uptake capacity will be offset.
As the amount of sorbent which is being tested increases,
the mass of liquid trapped in between the net and the sorbent
becomes less influential on the final calculated sorption
capacity. Ultimately, if enough sorbent is used in the experi-
ment or if the net mesh size is increased, this amount of trapped
liquid becomes unimportant. For better accuracy, it is also
important to ensure that the weight of the net is not a large
fraction of the final weight of the system (including the wet
sorbent). If the weight of the net is much higher than the
sorbent, slight measurement errors may result in large errors in
accuracy.
As an example, in Fig. 2, data regarding the measured
uptake capacity of RMG380 marine residual fuel by rice husk
sorbents produced in our research group is provided [55]. Tests
were conducted 3 times and the average values are reported.
Evidently, the less sorbent that is used, the higher the measured
sorption capacity will be. As the amount of sorbent increases,
the trapped liquid between the net and sorbent becomes less
significant and the values begin to steady-out. Thus the more
sorbent is used, the more accurate the reported uptake capacity
will be.
FIG. 2 Measured uptake capacity versus amount of sorbent used.
 BAZARGAN ET AL. ON OIL SORBENT PERFORMANCE TESTING 5

IMPORTANCE OF LIQUID PROPERTIES
Each sorbate–sorbent system will exhibit a different dripping
profile. The profile is dependent on many factors including (but
not limited to) the liquid’s viscosity, density, and surface ten-
sion. As such, if the liquid being used as the sorbate is not fresh,
the properties may have changed significantly from the data
provided by the producer. For example, it was observed in our
research group that if RMG380 marine residual fuel was left
exposed to the laboratory atmosphere for 20 days, the measured
sorption capacities increased by more than 10 %–15 % com-
pared to when fresh liquid was used. This is because the more
volatile fraction of the liquid gradually evaporated and left
behind the heavier and thicker fraction. In other words, the vis-
cosity and density of the weathered liquid increased. It is well
known that more viscous liquids lead to higher measured sorp-
tion capacities. Therefore, the properties of the liquid as well as
environmental conditions such as temperature which can affect
the liquid viscosity should be kept as constant as possible.
In order to better understand the extent of which volatili-
zation occurs, the evaporation of the RMG380 marine residual
fuel was monitored over a span of several months. Figure 3
shows the weight loss of the marine residual fuel left in a petri
dish exposed to the laboratory atmosphere for a long duration
of time. The figure shows that although 5 % of the marine
diesel evaporated in the first 20 days, it took nearly ten times
as long (about 200 days) for the next 5 % to evaporate. The
evaporation significantly altered the properties of the liquid.
Although the fresh residual fuel is pourable, after 200 days of
evaporation, the liquid will no longer pour out of the petri
dish unless it is physically forced out. Hence when oil sorption
tests are carried out, the properties of the liquid should be
carefully measured and reported. Exposure to air when storing
the liquids for future experimentation must be minimal. If
experimentation is to be carried out after large time intervals,
it is suggested for liquid properties to be re-measured. If vola-
tile liquid is used, the evaporation profile will be more pro-
nounced and influential.
Shortcomings of the ASTM
Standards
The number of studies that use the ASTM F716 and
ASTM F726 standards to measure oil uptake capacities are
limited. Effectively, these standards are unpopular among the
majority of researchers working on developing new oil sorbent
materials. The unpopularity of the standards may be due to the
lack of familiarity with the standards, or due to shortcomings
associated with ASTM F716 and F726. Three of the most
important shortcomings that have been identified in the stand-
ards are as follows:
1. In the ASTM standards, the mesh size of the net to hold
the sorbents is not defined. The only mentioned criteria is
that “the mesh should retain the sorbent, yet allow free oil
to drain away from the sorbent” [27]. As previously dis-
cussed, this is not an adequate limitation, as different
mesh sizes result in different dripping profiles of the sor-
bent and result in different amounts of oil being trapped
between the net and the sorbent.
2. The ASTM standards require at least 4 g of sorbent to be
used in every experimental run. However, often in labora-
tory experiments, the prepared sorbents are not produced
in large scales. Hence, using 4 g for every run (and taking

FIG. 3
Natural evaporation of RMG380 marine residual
diesel exposed to laboratory atmosphere.

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6 Journal of Testing and Evaluation
into consideration that each run must be repeated at least
3 times for accuracy) is often impractical.
3. In the ASTM F726 standard, only 30 s (or 2 min in the
case of heavy and weathered oil) of dripping is allo-
cated after the removal of the sorbent from the liquid
basin. However, this amount of time is often inad-
equate and leads to inaccuracies in reporting the
results. As such, the uptake capacities reported by using
the ASTM F726 method are often bloated and much
higher than the actual practical pickup capacity of the
sorbent. Unlike ASTM F726, which has overlooked this
issue completely, in clause 11.3.2, ASTM F716 does
indeed mention that the sorbent needs to be allowed to
drain until cessation of dripping in order to record the
“practical pickup.”
In order to overcome the problems associated with the
ASTM standards, adjustments and revisions are required.
Proposed Solutions
The lack of adjustments to ASTM F716 and F726 could result
in the continuation of their unpopularity. This unpopularity has
led to disorder in experimental methodologies used for the eval-
uation of sorbents in the scientific community. The differences
in methodologies have often resulted in data from each study
being different from the next. These differences sometimes
make findings misleading and hinder the possibility of mean-
ingful comparisons being drawn among research results
reported by different groups. Thus, the following suggestions
could be considered in order to ensure more sound and compa-
rable studies are conducted and reported:
1. Instead of the loose and inexact use of the words adsorb-
ent and absorbent, the more general terms of sorbent
should be used. The sorption process of oils is usually a
combination of both adsorption and absorption phenom-
ena. If researchers wish to use the words adsorbent or
absorbent, specific justification should be provided in
order to explain why the specific word has been utilized.
ASTM F716 vaguely states that “increase in volume of the
solid absorbent is the property that distinguishes an
absorbent from an adsorbent.”
2. During the removal of the sorbent from the liquid bath
and subsequent drainage, the practical pick up capacity is
measured when no more drops of liquid are lost during
drainage. This point may also be referred to as the “no-
drip point” or as the “point of no dripping.” It would be
preferable for researchers to report this practical capacity
as well as the uptake capacity at other points in time dur-
ing drainage. Reporting the uptake capacity at the no-drip
point would be beneficial in the sense that the uptake
capacity of no sorbent would be over-estimated (or delib-
erately over reported). The time to reach this equilibrium
is also of importance. Hence, here we define two
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parameters of importance to be reported in oil sorption
performance testing:
Equilibrium Uptake Capacity: denoted by Ce or Qe, is
the uptake capacity of the sorbent calculated at the no-
drip point. The equilibrium uptake capacity, which can
also be referred to as the “practical uptake capacity,” is a
function of both sorbent and sorbate properties.
Equilibrium Time: denoted by te, is the time required
for dripping to stop. In other words, te is the duration of
time starting from when the sorbent is removed from the
liquid bath, until the no-drip point is reached. The equilib-
rium time, also known as “the point of no dripping,” is a
function of the sorbent and sorbate properties as well as
the net mesh size in case one is used.
3. It is preferable for researchers to report the dynamic loss
of liquid from the sorbent. This means that the calculated
uptake capacity should be reported at several points
between the initial removal of the sorbent from the liquid
bath, until all dripping has stopped (equilibrium uptake
capacity). Reporting how the sorbent loses the liquid with
time provides vital information regarding the retention
behavior of the sorbent. Sorbents that lose liquids faster
would presumably be less favorable than those which
have slower desorption due to dripping.
4. It is understandable that researchers may want to use as
little sample in each sorption capacity experiment as pos-
sible in order to not exhaust their sample supplies. None-
theless, in order to verify that the mass of the sorbent
used in the experiments is not leading to an overstate-
ment of the uptake capacity, a small number of test runs
employing more mass of the sorbents should be carried
out. This is to make sure that the measured uptake
capacity does not decrease when more sorbent is used
and that the amount of liquid stuck between the mesh
and the sorbent does not significantly affect the experi-
mental results. Moreover, when a larger mass of sorbent
is used, slight measurement errors lead to less significant
accuracy issues.
5. Since volatilization can drastically change the liquid prop-
erties and in-turn lead to overstated uptake capacities, the
properties of the actual sorbate used in the sorption
experiments (in particular density and viscosity) should
be measured and reported. If the sorbate is used for sev-
eral experimental runs, it would be sound practice to
measure the liquid properties before the first and after the
final run in order to ensure the liquid properties have not
changed significantly.
Conclusion
The environmental disasters looming due to oil spills are an
area of concern for many researchers as well as the general pub-
lic. In order to combat spills, various methods and techniques
are used. In this regard, oil sorbent materials are frequently
produced and tested. Although the standard methods of

ASTM F716 and ASTM F726 for sorbent performance testing
exist, many, if not most, researchers focused in the area of oil
sorbent production have ignored them. The disorder resulting
from the use of different methodologies is discussed and possi-
ble solutions for better homogeneity and comparability are sug-
gested. By following the suggestions provided herein, it is hoped
that some (if not all) of the inconsistencies of reporting sorbent
materials’ uptake capacities can be overcome.
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