Journal of Colloid and Interface Science 276 (2004) 456464

www.elsevier.com/locate/jcis
Surfactants treatment of crude oil contaminated soils
Kingsley Urum
a,
, Turgay Pekdemir
a
, Mehmet opur
b
a
Chemical Engineering, School of Engineering and Physical Sciences, HeriotWatt University, Edinburgh EH14 4AS, United Kingdom
b
Chemical Engineering Department, Engineering Faculty, Atatrk University, 25240 Erzurum, Turkey
Received 8 October 2003; accepted 19 March 2004
Available online 21 April 2004
Abstract
This study reports experimental measurements investigating the ability of a biological (rhamnolipid) and a synthetic (sodium dodecyl
sulfate, SDS) surfactant to remove the North Sea Ekosk crude oil from various soils with different particle size fractions under varying
washing conditions. The washing parameters and ranges tested were as follows: temperature (5 to 50

C), time (5 to 20 min), shaking speed

(80 to 200 strokes/min), volume (5 to 20 cm
3
), and surfactant concentration (0.004 to 5 mass%). The contaminated soils were prepared in
the laboratory by mixing crude oil and soils using a rotating cylindrical mixer. Two contamination cases were considered: (1) weathered
contamination was simulated by keeping freshly contaminated soils in a fan assisted oven at 50

C for 14 days, mimicking the weathering

effect in a natural hot environment, and (2) nonweathered contamination which was not subjected to the oven treatment. The surfactants were
found to have considerable potential in removing crude oil from different contaminated soils and the results were comparable with those
reported in literature for petroleum hydrocarbons. The removal of crude oil with either rhamnolipid or SDS was within the repeatability
range of 6%. The most inuential parameters on oil removal were surfactant concentration and washing temperature. The soil cation
exchange capacity and pH also inuenced the removal of crude oil from the individual soils. However, due to the binding of crude oil to soil
during weathering, low crude oil removal was achieved with the weathered contaminated soil samples.
2004 Elsevier Inc. All rights reserved.
Keywords: Soil washing; (Bio)surfactants; Crude oil; Soil; Oil removal; Weathered; Nonweathered
1. Introduction
With the growing interest in environmental remediation,
various approaches have been proposed for treating pe-
troleum hydrocarbon contaminated sites [1]. Among these
treatment methods, soil washing has been proposed as a
promising innovative remediation technology due to its po-
tential for treating not only oil contaminated soils but also
those contaminated by heavy metals [24]. Soil washing
is less time consuming compared with bioremediation and
phytoremediation, which are largely affected by climatic
factors. The traditional soil washing process has been stud-
ied extensively in recent years [58], showing that it can
be applied as an ex situ or in situ process, involving wa-
ter or aqueous surfactant solutions to desorb and concentrate
the contaminants into bulk liquid phase without chemically
modifying them [9]. The behavior of surfactant solutions in
different systems has been investigated [1013].
*
Corresponding author. Fax: +44-131-451-3219.
E-mail address: k.urum@hw.ac.uk (K. Urum).
Naturally occurring surfactants are classied as biosur-
factants. Biosurfactants display excellent surface activities
despite their bulky molecular structure in comparison to
synthetic ones. As they originate from living organisms,
biosurfactants have advantages of biodegradability, easily
produced using renewable resources, possible regeneration,
high specicity and less toxicity [1416]. The use of bio-
surfactants eliminates the need for surfactant removal from
efuents, due to their innocuous nature. Their productions,
commercial application, biodegradation potential of hydro-
carbon and metal removal from soil have been studied
[1721].
The effects of surfactants on the biodegradation and
washing of crude oil contaminated soils have been re-
ported [17]. In [11], sodium dodecyl sulfate (SDS) among
other commercial surfactants was evaluated for treating pe-
troleum hydrocarbon contaminated soil through soil wash-
ing. The work reported in [2225] used surfactants to treat
single and double component hydrocarbon-contaminated
soils. In addition, [26] carried out studies and gave an exper-
imental design and technical description of a soil-washing
0021-9797/$ see front matter 2004 Elsevier Inc. All rights reserved.
doi:10.1016/j.jcis.2004.03.057
K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464 457
site. In the study, the authors used a surfactant solution
to transfer a matrix of crude oil contaminants to a liquid
phase, the surfactant solutions were then used to enhance the
biodegradation of the oil. The study concluded that the appli-
cation of surfactants in soil washing depends on the physio-
chemical nature of the surfactants and the contaminated
soil. The efciency of a biosurfactant solution produced by
Pseudomonas aeruginosa has been tested in removing the
Exxon Valdez oil from gravel [27]. The microbial surfactant
showed considerable enhancement in reducing the amount
of oil in soil at varying experimental conditions.
Generally, the use of surfactants for crude oil contam-
inated soil washing has not been fully exploited yet. This
paper aims to evaluate the effectiveness of rhamnolipid and
sodium dodecyl sulfate (SDS) solutions in removing Ekosk
crude oil from contaminated soils through the soil washing
process. The soil washing technique and the different soil
fractions used in this study will yield a novel and informative
description on the application of biosurfactants in washing
crude oil contaminated soils. This is believed to have major
academic and industrial implicational values for the treat-
ment of oil contaminated sites, sand produced with oil, drill
cuttings and waste drilling mud, and enhanced oil recovery.
2. Materials and methods
2.1. Preparation of contaminated soil
The different soil fractions were studied because of their
varying characteristics such as pH, cation exchange capac-
ity and crude oil content. Method 9045 in [36] and Method
9081 [37] were used to determine the soil pH and cation
exchange capacities (CEC), respectively. Cation exchange
capacity shows the net negative charges in soil. This is one
of the most important soil chemical characteristics and re-
lates to the amount of organic matter and clay present in the
soil. CEC may be inuenced by soil pH.
Two sources of soils were used in this study. The rst was
from the mineral division of Hepworth Minerals and Chemi-
cals Ltd., UK. Analysis of soil particle size was conducted in
a standard laboratory by Malvern Instrument Ltd., UK. The
soil characteristics were range of particle size 0.00001 to
0.3 mm and bulk density 2.00 g/cm
3
. About 60% of the total
soil mass was less than 0.050 mm. This soil was classied as
Soil 1. The second soil sample was fromSilvaperlo, supplied
by Williams Sinclair Horticulture Ltd., UK. This soil is of
horticultural grade, lime free, washed and graded quartzite
grit sand with maximum nominal size of 5 mm. This soil
was sieved using an Endecott test sieve shaker following the
methods of [28,29] and named as Soil 3. Soil 3 was further
sieved and grouped into two major fractions based on parti-
cle sizes as Soil 2 (less than 2 mm) and Soil 4 (24 mm).
2.2. Soil contamination
A xed mass (2 kg) of each soil fraction was measured
and placed in a drum mixer. The method in [30] was used
to contaminate soil samples with North Sea Ekosk crude
oil blend (83.58 10
2
kg/m
3
at 15

C) at 20

C. The con-
tamination process was carried out using a horizontally po-
sitioned drum mixer (Grochopp & Co., 4060 Viesen 1) at
1400 rpm for about one hour. The properties of the different
soil samples and the Ekosk crude oil are shown in Tables 1
and 2, respectively.
2.3. Weathering procedure
Samples of the contaminated soils were oven treated at
50

C for 14 days using a fan assisted Genlab Widnes oven

and a mass reduction observed through the evaporation of
lighter oil components. This study was conducted to simu-
late the effect of exposure of contaminated soil samples to
the environment for a period of time, e.g., during oil spill
incidents or for cases when aged crude oil contaminated
soil needs remediation. The amounts of crude oil in each
of the oven treated soil samples are shown in Table 1. In
this regard, the oven treated soil samples are referred to as
weathered (w) whereas those that were not oven treated
are nonweathered (n).
2.4. GC analysis of contaminated soils
The GC/MS study was conducted using a VG Quattro
Tandem mass spectrometer (Waters, Manchester, UK) with
the following operating conditions: Electron impact ioniza-
tion, electron energy 70 eV, scan range 40 to 500 amu at
1 scan/s. Helium at a ow rate of 1.5 cm
3
/min was used
Table 1
Characteristics of soil samples
Soil 1 Soil 2 Soil 3 Soil 4
Soil size fractions (%) Clay (0.002 mm) 9
Silt (0.06 mm) 51 6 6
Sand (0.0602 mm) 40 94 72
Gravel (2 mm) 22 100
Mass of crude oil per
gram of soil (mg)
Nonweathered (n) 92.20 89.10 87.50 37.60
Weathered (w) 89.87 88.76 86.68 37.53
pH 6.13 7.14 7.43 7.18
CEC (meq/100 g soil) 7.58 14.32 10.17 6.28
458 K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464
Table 2
Properties of Ekosk crude oil [31]
Origin North sea (Norway)
API gravity (

C) 37.70
Specic gravity at 15

C 83.62 10
2
Viscosity at 20 and 50

C 8.16 10
2
and 3.62 10
2
cm
2
/s
Water content (mass%) 2.30 10
1
Table 3
Parameters studied at different levels
Studies Parameter levels tested
First Second Third Fourth
Washing temperature (

C) 5 20 35 50
Volume of solutions (cm
3
) 5 10 15 20
Concentration of solutions (mass%) 0.004 0.02 0.10 0.50
Shaking speed (strokes/min) 80 120 160 200
Washing time (min) 5 10 15 20
as a carrier gas. Samples were injected on-column onto a
30 m HP5 fused silica capillary column, 0.25 mm i.d. (Agi-
lent, UK), and the temperature held at 55

C for 2 min, then

increased from 55 to 300

C at 5

C/min, thereafter held at

300

C for 40 min. Crude oil/n-hexane extract (1 l) was in-

jected into the equipment for each investigation.
2.5. Washing method
Contaminated soil samples (5 g) were measured using
OHAUS/TS400D-Precision standard balance and poured
into 45-cm
3
centrifuge test tube. A known volume and
concentration of each surfactant solution was added to the
contaminated soil in the test tube. The test tube was shaken
laterally, with a horizontal displacement of about 2.25 cm,
in a temperature regulated water bath shaker from Grant In-
strument at different speeds (strokes/min) over a period of
time. Table 3 shows the parameter level investigated.
After each washing, the contents of the test tube (Soil 1)
were allowed to settle for 12 h and about 3 min for Soil 2,
Soil 3 and Soil 4. The settling time was chosen based on the
soil particle sizes distribution [28]. The washed solution was
decanted from the test tube after the dened settling time.
The soil was then rinsed with 5 cm
3
of distilled water by lat-
eral shaking for 3 min at the same washing conditions and
the rinse water decanted after the appropriate particle set-
tling time. The rinsing of the soil in the test tube was carried
out to remove the oil from the walls of the test tube as well
as the remaining surfactant solution from the soil. Another
reason for the rinsing was to prevent the formation of an
emulsion with the extracting solvent later when determining
the remaining oil on the soils.
2.6. Determining oil removal
The oil remaining in the soil was determined by solvent
extraction using n-hexane. n-Hexane (10 cm
3
) was added
to the rinsed soil, and then shaken laterally for 5 min and
the n-hexane/crude oil extract was removed. This process
was repeated four times; the fourth extract gave the same ab-
sorbance reading as a pure n-hexane (zero absorbance). All
the n-hexane/crude oil extract was collected into one volu-
metric ask and made up to 50 cm
3
with n-hexane. A sample
from the 50-cm
3
extract was centrifuged for 20 min at a
speed of 3000 rpm. This was to remove any suspended parti-
cles, which may interfere with the absorbance measurement.
Although n-hexane is a highly nonpolar solvent, our choice
for it was due to its low toxicity and ease of availability in
comparison with other solvents listed in Ref. [32]. However,
other authors have used n-hexane in the extraction of petro-
leum products from soil [33,34].
Absorbance of the centrifuged extract was measured at
400 nm using the HACH DR/2000 spectrophotometer. The
400-nm wavelength was chosen based on investigations us-
ing a stock solution of n-hexane/crude oil mixture, which
showed that the highest absorbance occurred at 400 nm. The
concentration of crude oil at this absorbance was determined
from the function obtained from the calibration curve of the
stock solution of n-hexane/crude oil at 20

C given by
(1) =0.38585 (mass%).
The percentage crude oil removed from soil was calcu-
lated using the equation
(2) Crude oil removed (%) =

(O
i
O
r
)/O
i

100%,
where is the concentration of crude oil remaining in the
soil (mass%), is the corresponding absorbance at 400 nm.
O
i
is the initial oil in the soil (g) before washing and O
r
and the oil remaining in the soil (g) after washing. The soil
washing experiment was repeated twice and the repeatability
and experimental error were within the range 6 and 4%,
respectively.
2.7. Surfactants
The selection of surfactants (rhamnolipid and sodium do-
decyl sulfate) was based on their origin of material of pro-
duction. Figs. 1 and 2 show the chemical structures of rham-
nolipid and sodium dodecyl sulfate (SDS), respectively. All
the surfactants were used as supplied without further puri-
cation.
The biosurfactant of microbial origin (rhamnolipid) was
a blend of C
26
H
48
O
9
and C
32
H
58
O
13
. It was composed of
15%active ingredient, supplied by Jeneil Biosurfactants Co.,
USA. The biosurfactant is readily biodegradable and has a
very low environmental impact, low toxicity and low skin ir-
ritation with excellent wetting and emulsication properties.
Rhamnolipids are glycosides of rhamnose (6-deoxyman-
nose) and -hydroxydecanoic acid.
Sodium dodecyl sulfate (C
12
H
25
NaO
4
S) is 97% pure,
a synthetic surfactant supplied by Fluka Co., Switzerland.
K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464 459
Fig. 1. Chemical structures of rhamnolipid.
Fig. 2. Chemical structure of sodium dodecyl sulfate.
3. Results and discussion
3.1. Effect of weathering
The weathering of the contaminated soil was due to evap-
oration of volatile compounds of oil, which were lost within
the rst 24 h. Over 14 days, the evaporation rate reduced.
The mass reduction of the contaminated soils was not notice-
able as shown in Fig. 3. Soil 1 (ne particle sizes) showed a
greater reduction in mass while Soil 4 (gravels) showed less
mass reduction indicating less crude oil content in the soil
sample. To ascertain the reduction of hydrocarbons fromsoil
after fourteen days, a GC/MS study was carried out for both
the weathered and nonweathered contaminated soil samples.
Results of the GC study shown in Fig. 4 indicated that
most carbon compounds lower than C
16
were lost. This re-
sult was similar to the work reported in [35], in which they
contaminated washed sharp sands with Kuwait crude oil.
The contaminated soil was heated to 60

C for about 7 days

and the results from GC/MS analysis indicated that crude oil
extracted from the weathered contaminated soil showed that
most aliphatic compounds smaller than C
16
were reduced to
trace levels.
As the weathering process persists, the chemical and
physical nature and the appearance of the weathered conta-
Fig. 3. Mass reduction of contaminated soils.
minated soil change compared to the nonweathered samples.
Resulting in a contaminated soil with oil of higher molecular
weight, density and viscosity, leading to the greater binding
strength of crude oil to soil. It is assumed that the inorganic
(such as sulfur and metals) content of the oil is more con-
centrated than in the nonweathered soil.
3.2. Effect of concentration of surfactant solutions
The control (distilled water, W) washing showed a crude
oil removal of about 5%fromthe weathered soil (w) samples
of Soil 1 and Soil 2, and about 18% for Soil 3 and Soil 4.
However, for the nonweathered (n) samples of Soil 1 and
Soil 2, crude oil removal of 55 and 60% was achieved. Using
surfactant solutions, crude oil removal was enhanced beyond
the critical micelle concentration of 0.02 and 0.2 mass% for
rhamnolipid (R) and SDS, respectively. As the concentration
of the surfactant solutions increases the overall performance
of rhamnolipid and SDS in removing crude oil from the
460 K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464
Fig. 4. GC analysis of Ekosk crude oil contaminated soil.
weathered soil samples were in the following order: Soil 4
> Soil 3 > Soil 2 > Soil 1.
Crude oil removal from the weathered and nonweathered
soil samples (Fig. 5) increased as the concentration of sur-
factant solutions increased. The low removal of crude oil
from the weathered soil samples was a result of the complex
nature of the oil, due to loss of volatile components during
weathering. The weathered contaminated soils reduce the in-
teraction and penetration of the surfactant solutions at the
interfaces between crude oil and soil, therefore reducing the
crude oil removal efciency with surfactant solutions.
Generally, Rn and SDSn can be approximated within the
repeatability range of 6%, except for Soil 4, which indi-
cated about 10% more oil removal in favor of SDS. As the
soil particle sizes increased and the concentration of solu-
tions increased, crude oil removal from the weathered and
nonweathered soil samples appeared to respond similarly.
This study was comparable with [27], suggesting that the
desorption of crude oil from soil with aqueous surfactant so-
lutions may be effective in treating soils with larger particle
sizes (Soil 4) than the ner (Soil 1) ones.
The greater crude oil removal from Soil 4 (with 100%
gravel) may be due to the lower oil content, neutral pH and
CEC. Higher CEC indicates greater organic matter content
in soil and high pH as noticed with Soil 2 and Soil 3. Soil pH
affects CEC, the soil has an exchange site that becomes ac-
tive as the pHincreases. Soil 1 showed the lowest pHof 6.29.
Its CEC was expected to be higher than 7.58 meq/100 g
soil because the soil has larger surface area and thus more
sites readily exchangeable in comparison to Soil 2 and Soil 3
which both demonstrate CEC of 14.32 and 10.17 meq/100 g
soil, respectively. Clay and organic matters in the soil have
negative charges, so naturally attracts positively charged ions
and repels negatively charged ions. Therefore, this may also
lead to stronger binding of the oil with the ner soil samples
(Soil 1).
3.3. Effect of temperature
Fig. 6 shows variation in crude oil removal for all the soil
fractions, as the washing temperature increased. The trend in
oil removal was similar for the different washing solutions in
each of the soil samples; it follows that increase in temper-
ature will reduce the crude oil viscosity thereby increasing
the oil mobility and interaction with surfactant solution. For
most of the nonweathered samples, SDS and rhamnolipid
had a constant crude oil removal above 20

C whereas the
weathered samples indicated that more crude oil could be
removed if temperature was increased beyond 50

C.
At 50

C, crude oil removal from the nonweathered soil

samples was twice that of the weathered samples, with Soil 3
and Soil 4 showing constant oil removal above 20

C. There-
fore, crude oil removal from the weathered soil samples was
enhanced for soil with large fractions (Soil 4). The large
K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464 461
Fig. 5. Crude oil removed (%) at different surfactant concentration (mass%) for weathered and nonweathered soil samples. Washed at 20

C with 20 cm
3
solution, shaken at 200 strokes/min for 20 min.
Fig. 6. Crude oil removed at different temperature for weathered and nonweathered soil samples. Washed with 20 cm
3
0.1 mass% solution, shaken at
200 strokes/min for 20 min.
462 K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464
Fig. 7. Crude oil removed versus volume of washing solution for weathered and nonweathered soil samples. Washed at 20

C with 0.1 mass% solution, shaken

at 200 strokes/min for 20 min.
Fig. 8. Crude oil removed (%) at different shaking rates (strokes/min) for weathered and nonweathered soil samples. Washed at 20

C with 20 cm
3
0.1 mass%
solution for 20 min.
K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464 463
Fig. 9. Crude oil removed versus washing time for weathered and nonweathered soil samples. Washed with 20 cm
3
0.1 mass% solution at 20

C shaken at
200 stroke/min.
soil fractions have less initial crude oil content, therefore
their crude oil removal in 20 min may be faster compared to
the ner soil samples. Since the nonweathered soil samples
were freshly contaminated, crude oil removal from the ner
soils (Soil 1 and Soil 2) was enhanced. This is because of
their large surface area and less oil retention in their pores,
thereby encouraging the surfactant solution penetrating the
soiloil interface.
3.4. Effect of solution volume
To facilitate the crude oil removal, the interaction of sur-
factant in the interface between crude oil and soil was inves-
tigated by varying the volume of washing solutions from 5
to 20 cm
3
. The increase in volume of surfactant solutions
shows a corresponding increase in crude oil removal using
rhamnolipid and SDS (Fig. 7). Therefore, increase in volume
enhances the interaction between the crude oil and washing
media. In some cases with distilled water, crude oil removal
fromthe weathered soil samples was observed to be constant
indicating the noninuence of change in volume after a cer-
tain level. The weathered soil samples of Soil 3 and Soil 4
also showed a crude oil removal of about 18 and 10%, re-
spectively, after 15 cm
3
. Therefore, the plots (Ww and Wn)
in Soil 4 agree with the work of [4] that water based soil
washing is recommended for soil with particle size greater
than 2 mm.
3.5. Effect of shaking speed
The results of this study indicated that an increase in
shaking speed enhanced the removal of oil as shown in
Fig. 8. The plots (Rn, SDSn, and Wn) showed signicant
crude oil removal over the range of shaking speed (80 to
200 strokes/min) tested. As shaking speed increases, more
surface area of the contaminated soil is exposed to the sur-
factant solution; thus the surfactant solution displaces the
crude oil from soil. Rn and SDSn showed a removal within
the same repeatability range of 6%. The overall crude oil
removal from the weathered soil sample was in the follow-
ing order of soils: Soil 4 > Soil 3 > Soil 2 > Soil 1. The
enhanced oil removal has been attributed to the displace-
ment of crude oil by surfactant solutions, which was due the
scrubbing of contaminated soil surfaces that generates attri-
tion and abrasion [33,34].
3.6. Effect of washing time
Increase in washing time leads to an increase in crude oil
removal for both the weathered and nonweathered soil sam-
ples, as shown in Fig. 9. Crude oil removal from the weath-
464 K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456464
ered soil samples improved as the soil particle size fraction
increased. However, the reverse was true for the nonweath-
ered soil samples. The enhancement may be due to the least
oil content with the larger soil fractions.
4. Conclusions
Generally, the enhancement of crude oil removal using
the surfactant solutions was more effective for the nonweath-
ered soils than for the weathered soils. The overall crude oil
removal from the nonweathered soil samples was Soil 1 >
Soil 2 > Soil 3 > Soil 4, whereas the reverse was true for
the weathered soil samples. The crude oil removal from both
the weathered and nonweathered contaminated soil samples
by rhamnolipid and SDS was within the same experimen-
tal repeatability range of 6%. However, rhamnolipid may
be considered most attractive because of the advantage of
biodegradation and less environmental toxicity compared
with SDS. Therefore, results from this study are informative
in the design of a eld scale investigation.
Acknowledgment
The authors warmly thank Jeneil Biosurfactant Co., USA,
for their support and cooperation.
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