Separation and Purification Technology 179 (2017) 328–334

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Separation and Purification Technology

journal homepage: www.elsevier.com/locate/seppur

Application of high gradient magnetic separation for oil remediation

using polymer-coated magnetic nanoparticles
Seyyedali Mirshahghassemi a, Armin D. Ebner b, Bo Cai c, Jamie R. Lead a,⇑
a
Center for Environmental Nanoscience and Risk (CENR), Department of Environmental Health Sciences, Arnold School of Public Health (PHRC 511), University of South Carolina,
921 Assembly St, Columbia, SC 29208, United States
b
Department of Chemical Engineering, 3C06 Swearingen Engineering Center, University of South Carolina, Columbia, SC 29208, United States
c
Department of Epidemiology and Biostatistics, Arnold School of Public Health, University of South Carolina, Discovery 1, Room 460, 915 Greene Street, Columbia, SC 29208,
United States

a r t i c l e i n f o a b s t r a c t

Article history: Oil can be released into the environment from different sources such as runoff, accidental oil spills and
Received 29 September 2016 oily wastewater discharges produced during industrial activities and can have dramatic impacts on the
Received in revised form 13 January 2017 environment. The limitations of current clean-up techniques have inspired researchers to study the
Accepted 22 January 2017
application of nanotechnology for oil remediation. Previously, we reported excellent oil-removal effi-
Available online 10 February 2017
ciency of a reference MC252 oil using polyvinylpyrrolidone (PVP)-coated magnetic nanoparticles (NPs)
from an oil-water mixture under a wide range of environmentally relevant conditions. In the current
Keywords:
report, the same type of NPs were used with a high gradient magnetic separation (HGMS) technique
Nanoparticles
Iron oxide
for the rapid removal of oil from oil-water mixtures in a continuous flow system. Using a high magnetic
Oil spill field (0.56 T) and 1 h mixing time, fluorescence and inductively coupled plasma-optical emission
Remediation spectrometer (ICP-OES) data showed approximately 85–95% oil and NP removal under all conditions.
Magnetic separation Gas chromatography–mass spectrometry (GC–MS) results show 88 and near 100% removal of alkanes
Polymer (C9-C22) for experiments in the presence or absence of stainless steel wool, respectively. Continuous
use over 7 h of operation (17 L oil-water mixture was treated) showed no reduction in oil and NP removal
capacity. Results showed that increasing the magnetic field and inserting stainless steel wool significantly
increased oil and NP removal efficiencies. This study shows that using HGMS is a promising technique for
oil remediation using PVP-coated magnetic NPs.
Published by Elsevier B.V.

1. Introduction
The use of oil and other hydrocarbons are a necessary and inte-
gral part of our daily lives, although they also bring significant
problems with the risk of spills and other releases to the environ-
ment, with concomitant economic and environmental damages
[1]. Crude oil and petroleum products can be released into the
aquatic systems from different sources such as accidental oil spills,
runoff and industrial activities such as petroleum refineries, metal
manufacturing and automotive industries [2]. Oily discharges can
damage aquatic systems and can also contaminate groundwater
and drinking water resources and impact population centers [3].
The most common clean-up techniques for removing oil in oil
spills are skimming, in-situ burning, dispersants and sorbents [4].
However, there are challenges associated with these methods
⇑ Corresponding author.
E-mail address: jlead@mailbox.sc.edu (J.R. Lead).
including low removal efficiency, high operational cost and time
and environmental constraints [5,6]. Similar to the clean-up tech-
niques for oil spills, different wastewater treatment techniques
have been proposed for treatment of oily wastewater including
electrochemical treatment [7], microfiltration [8], sorbent materi-
als [9] and membrane bioreactor [10]. Although great progress
has been made in the application of these techniques, they have
limitations such as high operating costs, operating issues (e.g.
membrane fouling) and slow removal rate [11].
In recent years, the application of nanotechnology in water and
wastewater treatment has been widely investigated including for
the removal of dyes [12,13], heavy metals [14] and crude oil
[15,16]. Magnetic nanoparticles (NPs) are particularly interesting
due to their inherent low toxicity and magnetism allowing easy
separation of NPs from fluids [16,17]. For example, Calcagnile
et al. functionalized polyurethane foam by means of oleic
acid-capped superparamagnetic iron oxide NPs and polytetrafluo-
roethylene (PTFE) particles which showed high water-repellency

http://dx.doi.org/10.1016/j.seppur.2017.01.067
1383-5866/Published by Elsevier B.V.
 S. Mirshahghassemi et al. / Separation and Purification Technology 179 (2017) 328–334 329

and fast oil absorption [18]. We have synthesized polyvinylpyrroli- 6.25 mL ammonium hydroxide (25–30%, BDH) was added drop-
done (PVP)-coated iron oxide NPs capable of sorbing over 150 wise with vigorous stirring and the solution was stirred for
times its own volume of crude oil [16]. We have also developed a 25 min at 90 ± 5 °C. After the mixture cooled down, the precipitates
cost-effective, efficient, low toxicity and facile hydrothermal syn- were washed once with ultrapure water and separated magneti-
thesis technique to produce PVP-coated iron oxide NPs [19]. The cally and redispersed in water by sonication. The NP suspensions
synthesized iron oxide NPs show excellent oil removal efficiency were stored for the HGMS experiment. NP characterization data
under different environmentally relevant conditions, including a are provided in the Supporting Information.
wide concentration range of natural organic macromolecules In a typical oil removal experiment, crude oil from the Deepwa-
(NOM) and different ionic compositions [19,20]. The oil removal ter Horizon spill (sample ID number: A0068H, Aecom Environ-
mechanism of PVP-coated magnetic NPs is likely based on the
hydrophobic effect forcing oil from the aqueous phase onto the
PVP layer, which is bound to the core. Magnets can then be used
to separate the nanomaterial, with associated oil, from the water
[20]. Despite the excellent oil removal performance in the previous
studies, these techniques were only tested in the laboratory scale
and their performance at a larger removal scale remains unclear.
In this study, a high gradient magnetic separation (HGMS) tech-
nique, which can be utilized to remove oil in a continuous and lar-
ger volume, was tested as a function of the operating parameters
(e.g. magnetic field strength, mixing time and stainless steel (SS)
wool content). The HGMS system has an externally applied mag-
netic field which can be energized using a fine ferromagnetic wire
matrix (e.g., SS wool) inserted into the column. This technique has
been widely used in wastewater treatment [21,22], drug delivery
[23] and other industries such as paper manufacturing and food
industry [24].

2. Experimental

The hydrothermal synthesis technique and NP characterization

have been published previously [19] and a short summary is given
here. In a typical synthesis process, 28.8 mM PVP (Mw 10 kDa,
Sigma-Aldrich) was dissolved in 6.25 mL ultrapure water (Milli-
pore) while the solution was stirred at 80 ± 5 °C. Then, 160 mM
FeCl2
4H2O (98%, Alfa Aesar) and 640 mM FeCl3
6H2O (>98%,
BDH) were added to the solution and stirred at 80 ± 5 °C. Subse-
quently, 19.2 mM PVP was added while the solution was stirred
and the temperature was kept constant at 80 ± 5 °C. Finally,

Fig. 2. Effect of magnetic field strength on the oil and NP removal efficiencies (a) oil
Fig. 1. Schematic diagram of the HGMS system: (A) stirred oil-water-NPs mixture; and NP removal for the last collected sample, (b) oil removal efficiency and (c) NP
(B) peristaltic pump; (C) magnet; (D) SS wool (if used); (E) treated solution. removal efficiency (mixing time: 1 h and mass of SS wool: 100 mg).
330 S. Mirshahghassemi et al. / Separation and Purification Technology 179 (2017) 328–334
ment) was mixed with ultrapure water in a vial via sonication
(Branson 2800, 40 kHz, ambient conditions) for 30 min to prepare
the oil-water sample. The oil concentration used was
0.15 ± 0.05 g L 1 which is based on literature data [25] and is sim-
ilar to our previous works [19,20]. The NP concentration used was
18 ppm, which had been previously optimized [19,20]. Following
the preparation of an oil-water mixture, the NP suspension was
added to the mixture and mixed for specific periods of time
(5 min or 1 h) using a mechanical stirrer. The suspension contain-
ing the NPs was then pumped into a glass column (upflow
40 mL min 1 with a velocity of 0.14 cm s 1 via a peristaltic pump;
300 mm length and 11.1 mm I.D.) within the magnet assembly,
with no water recirculation. The eluent was then collected in sev-
eral small sample bottles to measure oil and NP removal efficien-
cies. A 0.18 or 0.56 T permanent magnetic assembly consisting of
two 2  4  0.5 inch NdFeB blocks with a minimum gap of 5/8 inch
was used as the magnetic source. The magnetic field strength was
changed by adjusting the gap between the two magnets and the
magnetic field was measured using a Model 4048 Bell Gauss/Tesla
meter. For additions of SS wool, an AISI 434 stainless steel wool
(average fiber width: 120 mm), packed at different packing densi-
ties (50 and 100 mg SS wool in the column) was placed in the col-
umn and magnetically energized. The external magnetic field
created large magnetic field gradients around the SS wool which
improved the removal efficiency [26]. In the absence of SS wool,
NPs were collected by the magnetic field on the wall of column.
Fig. 3. GC–MS results. (a and b) Chromatograms and (c and d) mass spectrometry results for the solution remaining after HGMS (mixing time: 1 h and mass of SS wool:
100 mg).
In the presence of SS wool, NPs were collected either on the wall
of column or were trapped in the SS wool. Each HGMS experiment
was replicated three times. Following the HGMS experiment, the
column was removed from the magnetic field and collected NPs
were removed by rinsing with ultra-pure water. The variables
studied include the applied magnetic field strength, mixing time
and SS wool content. Fig. 1 shows a schematic of HGMS system
used in this study.
To study the performance of HGMS process, oil and NP concen-
trations before and after HGMS was measured. Oil concentration
was measured by fluorescence spectroscopy and individual alkanes
removal efficiencies were further quantified using gas chromatog-
raphy–mass spectrometry (GC–MS). For the fluorescence measure-
ments, emission spectra of oil-water mixtures were recorded over
the range of 350–650 nm at the excitation wavelength of 337 nm
using a Horiba Jobin Yvon Fluorolog-3 spectrofluorometer. This
excitation wavelength has been used to detect polycyclic aromatic
hydrocarbons of crude oil [27]. A calibration curve was obtained
based on samples with known oil concentration and the oil
removal efficiency was quantified. GC–MS analysis was performed
on an Agilent 6890 N gas chromatography system and an Agilent
5975 mass spectrometer equipped with an autosampler (Agilent
7683B) to quantify the removal efficiency for individual hydrocar-
bons. The samples were prepared via extraction in dichloro-
methane (>99.8%, Sigma-Aldrich). The analytical column was an
Agilent TG-5MS (30 m  0.25 mm I.D., 0.25 mm film thickness)
 S. Mirshahghassemi et al. / Separation and Purification Technology 179 (2017) 328–334 331

coated with 5% phenylmethylsiloxane stationary phase. High pur-
ity helium (99.9%) at a constant flow rate of 1.5 mL min 1 was used
as the carrier gas. The injection port was maintained at 250 °C in
splitless mode and 1 ml of extracted sample was injected. Spectra
were obtained in the electron impact mode (70 eV) scanning from
40 to 400 m/z. The oven temperature was operated from 40 to
300 °C rising at 10 °C/min. A full scan mode was used and alkanes
were monitored in the initial oil-water mixture and the last col-
lected sample after HGMS.
To measure NP removal efficiency, NPs in the initial oil-water-
NP mixtures and suspensions remaining after the HGMS treatment
were digested by fresh aqua regia and the total iron concentration
was measured, after dilution, using a Varian 710-ES inductively
coupled plasma-optical emission spectrometer (ICP-OES). The
removal efficiency of both oil and NP was measured simultane-
ously from the same collected solutions. Mean and standard errors
of data are provided.
The comparison of operating parameters on the oil and NP
removal efficiencies was conducted using the one-way analysis
of variance (ANOVA) with random effects, which is the simplest
case of the linear mixed effects model. The typical ANOVA analysis
was not used for multiple group tests because each effluent had
repeated measures based on three repeated experiments, which
are somewhat correlated. This violated the independent assump-
tion in the ANOVA. By including random effects into the ANOVA,
we could accommodate the correlation within subject (i.e. the cor-
relation among repeated measures for each effluent) and the vari-
ation across different collected samples. Statistical analysis was
performed by using R software (version 3.2.1). The statistical sig-
nificance was set as p < 0.05.
3. Results and discussion
To study the effect of magnetic field strength on the oil and NP
removal efficiencies, HGMS experiments were performed using
two different magnetic field strengths (0.18 and 0.56 T) which
are comparable to previous studies [28,29]. In this set of experi-
ments, the mixing time was 1 h and, for the experiment in the
presence of SS wool, 100 mg of SS wool was inserted in the column.
Based on the fluorescence and ICP-OES results (Fig. 2a) in the
absence of SS wool, using a magnetic field of 0.18 T and 0.56 T,
the oil removal percentage was 81.4% ± 2.9 and 87.3% ± 4.0, while
the NP removal efficiency was 48.8% ± 3.8 and 84.4% ± 5.2, respec-
tively. At the higher magnetic field (0.56 T), the insertion of 100 mg
SS wool into the column changed oil and NP removal from
87.3% ± 4.0 to 89.5% ± 3.0 and from 84.4% ± 5.2 to 92.9% ± 2.6,
respectively, compared to the experiment in the absence of SS wool
(Fig. 2a). These results, showing a high oil removal and low NP
removal at low magnetic strength and no increase in oil removal
at the higher NP removal% and higher field strength

Fig. 4. Effect of mixing time on the oil and NP removal efficiencies (a) oil and NP removal for the last collected sample, (b) oil removal efficiency, (c) NP removal efficiency and
(d) mass spectrometry results for the solutions remaining after HGMS (magnetic field strength: 0.56 T and mass of SS wool: 100 mg).
332 S. Mirshahghassemi et al. / Separation and Purification Technology 179 (2017) 328–334

(Fig. 2b and c), suggest that only a fraction of the NPs are respon-
sible for oil sorption. Most likely this is due to the (a) heterogeneity
of oil-NP agglomerates or (b) the polydisperse nature of the PVP
coating on the NPs, with a specific fraction of the (highly coated)
NPs active in separation. The low magnetic field presumably
removes the larger oil-NPs agglomerates resulting high oil removal
efficiency. At the high magnetic field, more of the individual dis-
persed NPs are also removed. Moreover, results indicated that
increasing the magnetic field strength and inserting SS wool in
the column provides a small but highly significant enhancement
of oil and NP removal efficiencies (P-value < 0.0001). The external
magnetic field creates larger magnetic field gradients around the
SS wool which improves the oil and NP removal [26]. Increasing
the magnetic field increases oil and NP removal. However a nar-
rower gap between the magnets is required meaning that lower
volumes of the oil-water mixture can be treated compared to the
condition using a lower magnetic field. A trade-off therefore exists
between volume treated and efficacy of treatment which must be
optimized on a case by case basis.
Fig. 3 shows the chromatograms for the oil-water mixtures
before and after HGMS and removal percentages for the individual
hydrocarbons obtained by GC–MS. Chromatography peaks for all
suspensions after treatment were significantly reduced compared
to the original oil-water mixture, showing the removal of alkanes
(Fig. 3a and b). Using a lower magnetic field (0.18 T) and in the
absence of SS wool, results indicate that approximately 60% of all
detected alkanes (C9-C22) were removed (Fig. 3c). Adding
100 mg of SS wool to the column, hydrocarbon removal efficiency
increased by approximately 10% (Fig. 3c). Fig. 3d shows that using
0.56 T magnetic field, in the presence and absence of SS wool, there
was approximately 100% and 80% removal of all detected alkanes
(C9-C22), respectively.
Fig. 4 shows the effect of mixing time (5 min and 1 h) on oil and
NP removal efficiencies. In this set of experiments, a magnetic field
of 0.56 T in the presence of 100 mg of SS wool was used. For a
5 min mixing time, 90.7% ± 1.8 and 88.6% ± 1.7 oil removal and
75.3% ± 1.6 and 62.6% ± 3.3 NP removal was achieved in the pres-
ence and absence of SS wool, respectively (Fig. 4a). GC–MS results
also showed that using a five minute mixing time, greater than 86%
and near 80% of alkanes (C9-C22) were removed with and without
SS wool, respectively (Fig. 4d). By increasing the mixing time to 1 h,
there was a small but significant improvement in NP removal effi-
ciency, 92.9% ± 3.0 and 84.4% ± 5.2 in the presence and absence of
SS wool, respectively (P-value < 0.0001). Increasing the mixing
time presumably enhanced interactions between oil and NPs
resulting in a more strongly bound oil-NP complex. Subsequently,
the NPs aggregated and removal efficiency improved. However,
increasing the mixing time did not significantly alter the oil
removal efficiency (P-value > 0.05). This again suggested that a
fraction of NPs are responsible for oil sorption. GC–MS results show

Fig. 5. Effect of SS wool content on oil and NP removal efficiencies (a) oil and NP removal for the last collected sample, (b) oil removal efficiency, (c) NP removal efficiency and
(d) mass spectrometry results for the solutions remaining after HGMS (magnetic field: 0.18 T and mixing time: 1 h).
 S. Mirshahghassemi et al. / Separation and Purification Technology 179 (2017) 328–334
Fig. 6. Breakthrough experiment in the presence and absence of SS wool. Vertical
gridlines show when the new oil-water-NP mixture was pumped (magnetic field:
0.56 T, mixing time: 1 h and for the experiment in the presence of SS wool, 100 mg
of SS wool was used). In the absence of SS wool, the average and standard deviation
of oil and NP removal efficiencies were 81.2% ± 1.8 and 81.2% ± 1.9 and in the
presence of SS wool, the oil and NP removal efficiencies were 89.5% ± 2.9 and
82.0% ± 2.2, respectively.
that using 1 h mixing, in the presence and absence of SS wool near
100% and greater than 88% of C9-C22 were removed, respectively
(Fig. 4d). Based on both sets of data, it appears that the aromatic
fraction is more easily removed (in the absence of full removal of
the NPs), while the aliphatic hydrocarbons are sorbed more equally
over the NPs, indicating different modes of removal.
We studied the removal efficiency of the pristine NPs in the
absence of oil to investigate if the oil enhances their removal. A
magnetic field of 0.56 T with no SS wool was used. Pumping the
pristine NPs through the column, no color change in the suspen-
sion was observed and based on ICP-OES results, approximately
10% of NPs were removed (data not shown). This suggests that
the oil coating on the NP surface enhanced agglomeration of the
NPs, enhancing the NP magnetic separation resulting in increased
removal. As the magnetic NPs are single-domain and magnetic
force upon a magnetic particle is linearly proportional to its vol-
ume, magnetic separation is more effective on the aggregated
oil-NP complexes which resulted in higher NP removal efficiency
[30]. Previous use of atomic force microscopy (AFM) and dynamic
light scattering (DLS) showed that the NPs strongly aggregate upon
oil addition [16,19] and this appears to be the likely cause of
increased magnetic removal in the presence of oil.
The effect of SS wool content on oil and NP removal efficiencies
were studied by conducting the separation experiment using a low
magnetic field (0.18 T) and 1 h mixing, with and without SS wool.
Based on both fluorescence and ICP-OES data, increasing the SS
wool content from 0 to 100 mg, the oil and NP removal efficiencies
increased from 81.4% ± 2.0 to 86.7% ± 0.9 and from 48.8% ± 2.7 to
68.1% ± 0.4, respectively (Fig. 5a). GC–MS results also reveal that
333
increasing the SS wool content increased hydrocarbon removal
efficiencies (Fig. 5d). For example, in the absence of SS wool, alkane
removal efficiencies (C9-C22) were 50–72%, while using 100 mg SS
wool, C9-C22 removal efficiencies were between 73% and approx-
imately 100% (Fig. 5d). Inserting the SS wool in the column can
energize SS wool and creates larger magnetic field gradients
around the fine ferromagnetic wires, thereby improving the
removal efficiency [26]. Statistical analysis showed that increasing
the SS wool content from 0 to 100 mg significantly increased oil
and NP removal efficiencies (P-value < 0.0001). However, the
statistical analysis does not show a significant increase in oil
removal for the experiment with 50 mg SS wool compared to the
experiment with no SS wool. For the experiment in the presence
of 50 mg SS wool, it is likely that a large fraction of the SS wool
was oriented in the direction of the flow. In this situation, that part
of the SS wool has no magnetic field of its own to collect oil.
Finally, we tested the HGMS system for a longer time by run-
ning the system for 7 h (3.5 h in two consecutive days) and treating
nearly 17 L oil-water mixture (oil concentration was 0.15 g L 1). In
this set of experiments, magnetic field of 0.56 T and 1 h mixing was
used i.e., the optimum removal conditions. Fig. 6a and b shows the
oil and NP removal efficiencies for the experiment in the presence
and absence of SS wool. Removal in all cases was greater than 80%.
It is also clear that, despite fluctuations over time (probably due to
instrument drift, despite calibration, and variation due to changing
batches of sample every hour) that oil removal was slightly, but
significantly, improved in the presence of the SS wool. However,
no significant changes were observed for NP removal. The lack of
correlation indicated again that a subset of the NPs removes most
of the oil. Our results show that even after 7 h of operation (17 L of
oil-water mixture was treated), the oil and NP removal efficiencies
for both separation conditions and the ability of the system to
work were unchanged, indicating excellent removal efficiency over
time (Fig. 6a and b) and the potential of the system to be used at a
larger scale.
Clearly, the primary motivation in this technique is oil removal
and our preliminary data indicates there may be benefits in leaving
these NPs in situ in the environment (data not shown). Certainly,
oil is considerably more hazardous than these NPs. Nevertheless,
given the concerns regarding NPs as an emerging contaminant
[31–35], it may also be important to be able to remove the NPs
and prevent them being discharged to the environment in order
to meet any pertaining regulatory requirements [36]. Additionally,
for commercial applications, an improved NP capture efficiency
and oil removal would reduce costs and waste discharges. A
scaled-up version could simply use larger volumes and flow rates,
or develop this system in a massively parallel format. In this case,
the NPs would be added to the oil-water mixture and pumped
through a HGMS to separate the nanomaterial, with associated
oil, from the contaminated site. Alterations of residence time or
magnet strength can be used in practice to remove greater percent-
ages of the NPs, in scaled-up processes.
4. Conclusions
Previously, we have shown a facile synthesis of PVP-coated
magnetic NPs which are cheap, environmentally-friendly and reli-
able as a technique for oil removal under a wide range of environ-
mentally relevant conditions. This study demonstrates that these
NPs can be used in a larger scale for the removal of oil from an
oil-water mixture (or potentially from oil contaminated soil
slurries). Using a high magnetic field (0.56 T) and 1 h mixing time,
fluorescence and ICP-OES data showed approximately 85–100% oil
and NP removal under most conditions, with the higher magnetic
field and the presence of SS wool giving significantly improved
334 S. Mirshahghassemi et al. / Separation and Purification Technology 179 (2017) 328–334
separation of both oil and NPs. However, only a fraction of the NPs
were used in oil removal (particularly for the aromatic fraction),
suggesting that efficiency improvements can be made by more
exacting synthesis conditions, which will reduce cost and environ-
mental impact.
Acknowledgments
The authors thank the SmartState Center for Environmental
Nanoscience and Risk (CENR) for financial support. We thank Dr.
Mike Walla for use of GC–MS. We also thank BP (Aecom) for pro-
viding reference MC252 surrogate oil (sample ID number:
A0068H).
Appendix A. Supplementary material
Additional information on the NP characterization, the control
experiment and figures 2b, 4b and 5b with a narrower Y-axis range
are provided in the Supporting Information. Supplementary data
associated with this article can be found, in the online version, at
http://dx.doi.org/10.1016/j.seppur.2017.01.067.
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