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Journal of Colloid and Interface Science 276 (2004) 456–464 www.elsevier.com/locate/jcis Surfactants treatment of crude

Journal of Colloid and Interface Science 276 (2004) 456–464

Journal of Colloid and Interface Science 276 (2004) 456–464 www.elsevier.com/locate/jcis Surfactants treatment of crude

Surfactants treatment of crude oil contaminated soils

Kingsley Urum a, , Turgay Pekdemir a , Mehmet Çopur b

a Chemical Engineering, School of Engineering and Physical Sciences, Heriot–Watt University, Edinburgh EH14 4AS, United Kingdom b Chemical Engineering Department, Engineering Faculty, Atatürk 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 Ekofisk 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 influential parameters on oil removal were surfactant concentration and washing temperature. The soil cation exchange capacity and pH also influenced 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 [2–4]. 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 [5–8], 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 [10–13].

* Corresponding author. Fax: +44-131-451-3219. E-mail address: k.urum@hw.ac.uk (K. Urum).

0021-9797/$ – see front matter 2004 Elsevier Inc. All rights reserved.

doi:10.1016/j.jcis.2004.03.057

Naturally occurring surfactants are classified 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 specificity and less toxicity [14–16]. The use of bio- surfactants eliminates the need for surfactant removal from effluents, due to their innocuous nature. Their productions, commercial application, biodegradation potential of hydro- carbon and metal removal from soil have been studied

[17–21].

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 [22–25] 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

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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 efficiency 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 Ekofisk 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 influenced by soil pH. Two sources of soils were used in this study. The first 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

Table 1 Characteristics of soil samples

soil mass was less than 0.050 mm. This soil was classified as Soil 1. The second soil sample was from Silvaperlo, 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 (2–4 mm).

2.2. Soil contamination

A fixed 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 Ekofisk 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 Ekofisk 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 flow rate of 1.5 cm 3 /min was used

 

Soil 1

Soil 2

Soil 3

Soil 4

Soil size fractions (%)

Clay ( 0.002 mm) Silt ( 0.06 mm) Sand (0.060–2 mm) Gravel ( 2 mm) Nonweathered (n) Weathered (w)

9

51

6

6

40

94

72

22

100

Mass of crude oil per gram of soil (mg) pH CEC (meq/100 g soil)

92.20

89.10

87.50

37.60

89.87

88.76

86.68

37.53

 

6.13

7.14

7.43

7.18

7.58

14.32

10.17

6.28

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K. Urum et al. / Journal of Colloid and Interface Science 276 (2004) 456–464

Table 2 Properties of Ekofisk crude oil [31]

Origin

North sea (Norway)

API gravity ( C) Specific gravity at 15 C Viscosity at 20 and 50 C Water content (mass%)

37.70

83.62 × 10 2 8.16 × 10 2 and 3.62 × 10 2 cm 2 /s 2.30 × 10 1

Table 3 Parameters studied at different levels

Studies

Parameter levels tested

 

First

Second

Third

Fourth

Washing temperature ( C) Volume of solutions (cm 3 ) Concentration of solutions (mass%) Shaking speed (strokes/min) Washing time (min)

5

20

35

50

5

10

15

20

0.004

0.02

0.10

0.50

80

120

160

200

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 µl) 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 defined 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 flask 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)

The percentage crude oil removed from soil was calcu- lated using the equation

χ = 0.38585γ (mass%).

(2)

where χ is the concentration of crude oil remaining in the soil (mass%), γ 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.

Crude oil removed (%) =

(O i O r )/O i × 100%,

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 purifi- 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 emulsification properties. Rhamnolipids are glycosides of rhamnose (6-deoxyman- nose) and β-hydroxydecanoic acid. Sodium dodecyl sulfate (C 12 H 25 NaO 4 S) is 97% pure,

a synthetic surfactant supplied by Fluka Co., Switzerland.

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of Colloid and Interface Science 276 (2004) 456–464 459 Fig. 1. Chemical structures of rhamnolipid. Fig.

Fig. 1. Chemical structures of rhamnolipid.

456–464 459 Fig. 1. Chemical structures of rhamnolipid. Fig. 2. Chemical structure of sodium dodecyl sulfate.

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 first 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 (fine 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 from soil 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-

physical nature and the appearance of the weathered conta- Fig. 3. Mass reduction of contaminated soils.

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% from the 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

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of Colloid and Interface Science 276 (2004) 456–464 Fig. 4. GC analysis of Ekofisk crude oil

Fig. 4. GC analysis of Ekofisk 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 efficiency 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 finer (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 pH increases. Soil 1 showed the lowest pH of 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 finer 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

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

if temperature was increased beyond 50 C.

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of Colloid and Interface Science 276 (2004) 456–464 461 Fig. 5. Crude oil removed (%) at

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.

cm 3 solution, shaken at 200 strokes / min for 20 min. Fig. 6. Crude oil

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.

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of Colloid and Interface Science 276 (2004) 456–464 Fig. 7. Crude oil removed versus volume of

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.

0.1 mass% solution, shaken at 200 strokes / min for 20 min. Fig. 8. Crude oil

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.

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of Colloid and Interface Science 276 (2004) 456–464 463 Fig. 9. Crude oil removed versus washing

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 finer soil samples. Since the nonweathered soil samples were freshly contaminated, crude oil removal from the finer 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 soil–oil 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 from the weathered soil samples was observed to be constant indicating the noninfluence 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

in Soil 4 agree with the work of [4] that water based soil

and Wn)

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 significant 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-

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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 field scale investigation.

Acknowledgment

The authors warmly thank Jeneil Biosurfactant Co., USA, for their support and cooperation.

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