J Nanopart Res (2013) 15:2054

DOI 10.1007/s11051-013-2054-y

RESEARCH PAPER

Sedimentation and aggregation of magnetite nanoparticles

in water by a gradient magnetic field
I. Medvedeva Yu. Bakhteeva S. Zhakov
A. Revvo I. Byzov M. Uimin A. Yermakov
A. Mysik

Received: 11 July 2013 / Accepted: 7 October 2013 / Published online: 24 October 2013
Springer Science+Business Media Dordrecht 2013

Abstract Magnetite (c-Fe3O4) nanoparticles are

promising effective sorbents for water cleaning of
heavy metal, radionuclides, organic and biological
materials. A good sorption capacity can be achieved
due to their high specific surface area. Application of
gradient magnetic fields helps to separate the magnetic
nanoparticles from the water suspension, which is rather
hard to do using the conventional mechanical filtration
and sedimentation methods without coagulants. The
sedimentation dynamics of magnetite nanoparticles
with sizes of 1020 nm in aqueous media in the
presence of a gradient magnetic field was studied by
optical and NMR relaxometry methods. The gradient
magnetic field was produced by a series of strip
permanent magnets with B B 0.5 T, dB/dz B 0.13
T/cm and in some cases enhanced by a steel grid with
sharp edges (dB/dz B 5 T/cm). Dynamic Light Scattering in the water suspension with different nanoparticle
concentrations (c0 = 0.11 g/l) revealed the characteristic features in the aggregate formation, which is
reflected in the sedimentation behavior. The

I. Medvedeva (&)  Yu. Bakhteeva  S. Zhakov 

I. Byzov  M. Uimin  A. Yermakov  A. Mysik
Institute of Metal Physics, Ural Branch of the Russian
Academy of Sciences, S. Kovalevskaya 18,
620990 Ekaterinburg, Russia
e-mail: ivmed@imp.uran.ru
A. Revvo
Ural State Mining University, Kuibysheva 30,
620144 Ekaterinburg, Russia

sedimentation rate of the nanoparticles in water and in

magnetic fields is higher for less concentrated suspensions (c0 = 0.1 g/l) than for more concentrated ones
(c0 = 1 g/l), which might be connected with the formation of a gel structures due to a strong magnetic attraction
between ferromagnetic nanoparticles. In 180 min this
resulted in the reduction of the iron concentration in
water down to 0.4 mg/l, which is close to hygienic and
environmental norms for drinking water and fishery.
Keywords Magnetite  Nanoparticles 
Magnetic attraction  Aggregation  Gradient
magnetic field  Sedimentation  Colloids

Introduction
Application of nanosorbents for water cleaning from
mineral and organic impurities is a fast developing
field. The sorption capacity of the powder is defined by
the specific surface which for particle diameter in
nanosize range comes up to hundreds of m2/g.
However, the small particle size creates difficulties
to separate the solid phase from the water suspension
using conventional mechanical filtration and sedimentation methods without coagulants. If the nanoparticles have magnetic moments, their separation from
aqueous solution can be enhanced by gradient magnetic fields (Yavuz et al. 2006; Yantasee et al. 2007;
Medvedeva et al. 2012).

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Page 2 of 8

The most suitable materials for this purpose are iron

and magnetic iron oxidesmagnetite, c-Fe3O4 and maghemite, c-Fe2O3 (Tang and Lo 2013). Iron and its oxides
are environmentally friendly as they are present in natural
waters and soils. They are not expensive in bulk and so
currently many methods of synthesis of iron oxide
nanoparticles have been developed (Song et al. 2011;
Woo et al. 2004; Sun and Zeng 2002; Ullrich and Horn
2013). It is well established that magnetite Fe3O4
nanoparticles (NP) adsorb efficiently heavy metals,
actinides, organic and mineral impurities. Surface-modified magnetic nanoparticles can adsorb viruses and other
biological objects (Tiwari et al. 2008; Savage and Diallo
2005; Tang and Lo 2013). The sorption capacity of the
iron-based nanopowders for many heavy metals is rather
high in comparison with other conventional agents, e.g.,
activated carbon- and resin-based sorbents (GT-73).
Some studies report that for heavy metals (Hg(II), Pb(II),
Cd(II), and Cu(II)) on the adsorption on the humic acidcoated 10-nm Fe3O4 NP qm = 43.697.7 mg/g (Lui et al.
2008) and for Fe3O4 NP functionalized with dimercaptosuccinic acid (surface area 114 m2/g) the sorption
capacity is qm = 227 mgHg/g, which is a 30-fold larger
value than that for GT-73 (Yantasee et al. 2007).
While many contributions are devoted to the
sorption processes, the subsequent important stage of
the water cleaning technology i.e. the nanosorbent
separation from water is poorly investigated (Mandel
and Hutter 2012; Tang and Lo 2013). In the few works
authors concentrated on studying the effect of pH and
impurities (NOM, counterions) on the rate of ironbased NP sedimentation in water (Yin et al. 2012).
These factors are effective to change the electrostatic
charge of the particles which is essential for the
particles aggregation in aqueous media. At the same
time, the aggregation of the particles with the magnetic polarization is strongly affected by the magnetic
attraction forces, which might be changed by the
external magnetic field variation. In our previous
paper the effect of a gradient magnetic field produced
by a system of radial permanent magnets on the
sedimentation dynamics of magnetite nanoparticles
with different sizes (1080 nm) was investigated
(Medvedeva et al. 2012). For the application the more
practical magnetic system would be the alternating
strip permanent magnets with opposite polarization to
produce a gradient magnetic field.
In this work, the sedimentation dynamic of magnetite nanoparticles with the sizes of 1020 nm in

123

J Nanopart Res (2013) 15:2054

aqueous media in the presence of a gradient magnetic

field B B 0.5 T, dB/dz B 0.13 T/cm was studied by
optical and nuclear magnetic resonance (NMR)
relaxometry methods. The NMR relaxometry method
allows registering fast the residual magnetite powder
concentration in water after sedimentation process.
Special attention is paid to the starting solid-phase
concentration variation, the magnetic field gradient,
and to the aggregate formation under the magnetic
field action. This study is important both for a deeper
understanding of the aggregation process and for the
optimization of a nanosorbent sedimentation conditions for the practical application.

Experimental section
Samples preparation and characterization
The powder samples of Fe3O4 with average particle
sizes near 1020 nm were prepared by the gas condensation method (Kortov et al. 2008). A strongly overheated drop of molten iron was evaporated in a buffer Ar
gas media containing some percent of oxygen. A
variation of the partial argon pressure and the velocity
of its flow near the evaporation zone allowed changing
the average particle size. The partial Argon pressure was
70 Torr, the velocity was 0.33 m/s.
The phase composition and the crystal structure
were examined by X-ray using DRON-6 diffractometer at Cu Ka-radiation. The X-ray analysis showed
that the powder samples had a cubic structure and the
lattice parameters were close to that of the bulk
magnetite (Fig. 1a). The secondary phase (a-Fe)
content was about 5 %.
The transmission electron microscopy (TEM) images
were taken in a high-resolution electron microscope
PHILIPS CM30 (200 kV). The TEM images showed
that the powders consisted of the particles of an
octahedral shape with the diameters (d) ranging from
several nm to tens nm (Fig. 1b). From the TEM images
the size-distribution histograms N (d) were obtained
(Fig. 1b, inset). The major part of the powders had the
sizes 1020 nm. The size of the dry particles was
estimated also from the regions of coherent scattering
from the width of the XRD reflections. The obtained size
1020 nm is in agreement with the results of the gas
desorption BrunauerEmmettTeller (BET) method for
the specific surface: 6070 m2/g.

J Nanopart Res (2013) 15:2054

(a)
Intensity, arb. uni.

Fig. 1 Characterization of
the magnetite nanoparticles.
a XRD pattern of magnetite,
b TEM image and SAED
pattern of the magnetite
nanopowder, insetThe
size-distribution histogram
for the dry nanopowder;
c the size-distribution
function V(dh) for the
nanopowder in water
obtained from DLS analysis;
d hysteresis loop of the
nanopowder at room
temperature

Page 3 of 8

(b)
311

a(Fe 3O4 ) = 0.837 nm

440

220
511

400

533
222

40

60

331 422

80

442 620

100

120

622
444

140

2Q, deg.

(c) 10

(d) 80

, emu/g

V, %

40
t = 1 min

t = 60 min

-40
0
-80
1

10

10

10

d h , nm

The size of the magnetite nanoparticles in water

(dh) was determined by dynamic light scattering
(DLS) experiments performed using NanoZS apparatus (Malvern, UK). Laser beam k = 633 nm was
produced by HeNe laser, operating in back-scattering
mode at an angle of 173. The volume distribution
function has a two-modal shape with one maximum
corresponding to 200 nm, and the second maximum
corresponding to 4 lm (Fig. 1c).
The magnetization of the nanopowders was measured at room temperature in magnetic fields up to
1.5 T using a vibrating sample magnetometer. The
magnetization curves show a saturation magnetization
with a high magnetic susceptibility of the para process
(Fig. 1d). Such a magnetization curve corresponds to
the ordering of spontaneous magnetic moments in
ferro/ferrimagnetic state and contribution from the
small particles in superparamagnetic state. The contribution from superparamagnetic nanoparticles is
confirmed by Mossbauer spectroscopy, from which
its volume was estimated to be 1215 %. The
saturation magnetizations values at room and at low
temperatures are about 2030 % lower than that in a
bulk magnetite, which points to a presence of phases
with a lower magnetic moment. Evidently, these are

10

-10000

10000

H, Oe

the phases with structural and atomic (oxygen)

vacancies, magnetically disordered Fe2? and Fe3?
ions in the surface layer of the particles. In particular,
such disordering can lead to a co-existence of ferroand antiferro-magnetic interactions and the exchange
anisotropy effect, which reveals in exchange bias
observed at low temperatures in the small particle
powder (Medvedeva et al. 2012). The presence of the
surface oxygen deficiency in the magnetite nanopowders is confirmed by the Mossbauer spectra, which
evidence a distribution of Fe2? and Fe3? ions different
from that in bulk natural magnetite Fe3O4.
Sedimentation dynamics experiments
In order to study the sedimentation dynamics of
magnetite nanoparticles in water, suspensions of
different magnetite powder concentrations 0.051 g/l
in distilled water were prepared, with subsequent
excitation by ultrasonic probe for about 10 s. As a rule
for each sedimentation measurement a freshly made
suspension was used. As in the water cleaning
technologies by sorption magnetite nanopowder sorbent concentrations 15 g/l are used, in this study the
starting concentration of c(Fe3O4) = 1 g/l was chosen.

123

Page 4 of 8

J Nanopart Res (2013) 15:2054

(a)

y
B

(b)
z=5mm

0.2

0.5

z=10mm

0.4

z=15mm

Bx, Bz, T

Bx , T

0.1
0.0
-0.1

Bx

0.3
0.2

Bz

0.1
-0.2
20

40

60

80

100

120

140

x, mm

0.0
10

30

40

z, mm

Fig. 2 a Scheme of the permanent magnets system. The arrows show the magnetic field directions. b The distance dependence of the
magnetic field along the x- and z-directions

The sedimentation was registered by monitoring

the light transmission coefficient k as a function of
time. A monochromatic light beam k = 950 nm
wavelength in horizontal direction was split into two
beams, one going through pure water as a reference
signal and another going through a fluid optical cell
containing the magnetite suspension. Then the beams
were detected by a photodiode and the ratio between
the signals was amplified and PC-monitored versus
time. Before each sedimentation experiment a calibration of the optic cell using pure distilled water was
done. The magnetic systems can be placed under the
optical cell containing the magnetite suspension.
The magnetic field source (magnetic system) was
made from a set of permanent magnet bars Sm2Co17
(10 9 40 9 40 mm) with a remanence induction
Br = 1 T (Fig. 2a). Between the bars strips of the
same thickness made from magnetically soft steel
were inserted. The value of the magnetic field and the
gradient in z- and x-directions were measured using a
Hall gauge (Fig. 2b). The sedimentation was studied

123

in different water layers: h = 20, 30, and 40 mm. In

some cases a grid from magnetically soft steel was
placed beneath the cuvette with the suspension to
enhance the magnetic field gradient. The grid was
0.1 mm thick with the holes 2 9 2 mm with the sharp
edges, which resulted in a gradient increase near the
grid up to 5 T/cm (estimated).
To determine the residual concentration of magnetite
nanoparticles in water after sedimentation, the method of
NMR relaxometry was explored. This method is based on
the registration of the relaxation time T2 of the NMR echo
signal from the water protons (H?). The impurities
bearing magnetic moment dispersed in water influence
the local magnetic field gradient near the proton, which is
reflected in a change of T2. For the water samples taken
from the upper layer of the cuvette T2 was measured using
the NMR relaxometer with the resonance frequency
2.06 MHz. The values of Fe3O4 content in water were
determined using a calibration dependence T-1
2 versus
c (Fe3O4), made previously on model suspensions. From
c (Fe3O4) the values of c (Fe) were calculated.

J Nanopart Res (2013) 15:2054

1.0

2
3

0.8

0.8
k, arb.un.

k,arb.un.

Page 5 of 8

0.6

0.4

0.4
0.0
2

0.2

10
10
time, min

10

0.0
0

20

40

60

80

100

120

140

time, min

Fig. 3 Sedimentation dynamics of magnetite nanoparticles in

water monitored by the optical method: 1 in the gravity field
(and the inset), 2 under magnetic field of radial magnets in water
layer h = 30 mm, 3 under magnetic field of strip magnets in
water layer h = 30 mm

Results and discussions

Figure 3 shows the sedimentation dynamics of the
nanopowder in a gravity field and in gradient magnetic
fields produced by radial (Medvedeva et al. 2012) and
strip magnets. In the gravitation field the nanoparticles
are floating for a long time, it will take around 24 h for
the settling of 90 % of their volume ((Medvedeva et al.
2012) and the inset to Fig. 3). Gradient magnetic fields
strongly accelerate the sedimentation. The initial
sedimentation rate is higher for the radial magnetic
system in comparison with the strip magnetic system,
as the magnetic field Bmax = 0.6 T and the gradient
dB/dz is higher for the former than for the later.
However, in working water cleaning devices (e.g.,
thin-layer sedimentation tank) the configuration with
strip magnets is more practical. Therefore, the studies
were done for the magnetic field produced by strip
magnets.
It was shown earlier (Medvedeva et al. 2012) that
the sedimentation of magnetite particles with the size
near 20 nm has a complex process due to aggregation
formation processes. According to the DVLO model,
the stability of a colloid system under an external
magnetic field is defined by the minimum of the sum of
main interactions:
V Ve V v V m

where Ve is the electrostatic interactions energy, Vv is

the van der Waals energy, and Vm is the energy of
magnetic interactions. Under the action of these forces
the small particles can form the large aggregates in

aqueous media. If the particles carry magnetic

moments, as in the case of magnetite, magnetic
attraction forces are very strong and exceed other
interactions. Electrostatic forces depend on the charge
of the double layer on the particle surface and can be
varied by the sign and by the value when pH of
aqueous media is changed. From the data of DLS and
our earlier studies (Medvedeva et al. 2012) it follows
that in water nanoparticles form aggregates with the
size of 70600 nm which slightly change on acidity
variation between pH = 5 and 9. Correspondingly, the
effect of pH change on the sedimentation dynamics of
magnetite nanoparticles is pronounced but still much
less than the magnetic field effect (Medvedeva et al.
2012).
The sedimentation rate of nanoparticles in water
results from the sum of forces of different natures and
strengths: gravity, buoyancy, viscous resistance, and
thermal motion. By setting down in water by the
gradient magnetic fields, two additional effects are
important: (i) the particle magnetization enhances
their attraction; hence the aggregates with large
magnetic moments can be formed, and (ii) the
magnetic force directed to the region of the gradient
increase is added to the gravity force:


Fm l0 Vp Mp  gradB B
2
where l0 = 4p 9 10-7 is magnetic permeability of the
vacuum, Vp is the volume of the particle, Mp is the
magnetization of the material (in this case Fe3O4) in a
given magnetic field B, B is the magnetic field gradient
in the particle center.
Magnetic attraction forces depend on the magnetic
moments of interacting particles which in turn determine whether the particle is in a ferromagnetic or in a
superparamagnetic state. From magnetization data and
Mossbauer spectra (Goya et al. 2003), for magnetite
Fe3O4, the border line size between these states is
dsp & 5 nm. The particles with d \ dsp are comparatively weakly magnetized in external magnetic field
(B \ 0.5 T) at 300 K. Therefore, they slightly aggregate in water and the water suspension remains stable
for a long time (months, years). To let them settle
down rather strong magnetic fields (of the order
several T) and gradients are required (Yavuz et al.
2006). To achieve the maximal sorption capacity, it is
necessary to have the specific surface as large as
possible. The optimal size of the particle in sorbent

123

Page 6 of 8

J Nanopart Res (2013) 15:2054

1.0

(a)
C = 1g/l, B

0.8
c0 = 1 g/l

10

C = 0.1g/l, B

C = 0.1g/l,
B=0

c0 = 0.5 g/l

0.2

c/c0

c0 = 0.25 g/l

V, %

c0 = 0.1 g/l

0.1

0.0
0

10

20

30

40

50

60

Fig. 4 Time dependence of the relative residual concentration

of magnetite nanoparticles in water after sedimentation under
magnetic field in the water layer h = 20 mm

10

time, min

10

10

10

d h, nm

(b)

123

10

00
10

30

e,m

20

10

d ,
h
nm

tim

in

0
10

10

should be of the size a little larger than superparamagnetism criteria for magnetite, which is about
1020 nm. Therefore, particles in this range were
chosen for the present research.
The time dependence of the residual concentration
of iron in water after particles sedimentation in
gradient magnetic field is shown for different values
of initial magnetite concentration c0 in Fig. 4. The
sedimentation rate depends on c0: high concentrated
suspensions are settled down for a longer time than
low concentrated suspensions. For the first hour of
settling of suspension with c0 = 1 g/l the iron concentration decreases by 20 %, while for the suspension
with c0 = 0.1 g/l the iron concentration decreases by
50 %. Such behavior is different from the data of
(Phenrat et al. 2007), where in the gravitation field
more rapid sedimentation was observed for more
concentrated suspensions than for more diluted ones.
It seems that in magnetic field at higher magnetite
powder concentrations the colloid formation occurs
with a structure which sediments slower in comparison
with sedimentation of big aggregates formed in diluted
suspension. The kinetic behavior of a dispersion with
magnetic particles of micron sizes was studied theoretically and experimentally (Furst and Gast 2000;
Martnez-Pedrero et al. 2008). It was shown that in
magnetic colloids the particles are assembling in
dimers, trimers, and chains oriented along the external
magnetic field direction (Eberbeck et al. 2006). At
higher concentrations more complex structure can be
built, in particular, with magnetic flux closing, that is a
sort of a fractal structure as a network, the so-called
gelation (Phenrat et al. 2007; Gomez-Lopera et al.
2006; Berret et al. 2007).

V,%

20

Fig. 5 The volume distribution function V(dh) of nanopowder

magnetite in water suspension: a for different initial concentrations c0 in the gravity field only (B = 0) and under the gradient
magnetic field, b time evolution of the distribution function
V(dh) under magnetic field for the suspension with c0 = 0.1 g/l

Chains of iron particles and their assembling into

gelation structure were observed visually in some ironbased suspensions (Phenrat et al. 2007; Gomez-Lopera
et al. 2006; Berret et al. 2007). These considerations
were put forward for interpretation of different stages of
sedimentation dynamics curves of iron and magnetite
nanoparticles in gravity field (Medvedeva et al. 2012;
Phenrat et al. 2007). However, when magnetic fields are
absent the fast aggregation of small particles does not
occur, so the complex gel structure forms in the wide
range of the initial powder concentration c0.
The different structures of aggregates in water under
the magnetic fields at different particle concentrations
are confirmed by DLS data (Fig. 5a, b). In a suspension
with c0 = 0.1 g/l under magnetic field in the beginning, for t \ 1 min, the big aggregates, 11.5 lm are
formed and they are rapidly settling within the first
30 min. In a suspension with c0 = 1 g/l the formation
of such big aggregates practically is not observed,
which is probably connected with the formation of a

J Nanopart Res (2013) 15:2054

Page 7 of 8

200
1.0

600

120

h=30 mm

0.6

c (Fe), mg/l

k, arb.un.

c (Fe), mg/l

h=20 mm

0.8

160

0.4
0.2
0

80
40

10

20 30 40
time min

50

30 mm, B=0
30 mm
20 mm
20 mm + grid

400

200

h=30mm
h=20mm
0

0
1

10

100

50

100

150

200

time, min

time, h

Fig. 6 The residual iron concentration in water after sedimentation of magnetite nanoparticles (c0 = 1 g/l) under gradient
magnetic field in different the water layers. inset The
sedimentation dynamics under the same conditions registered
by optical method

complex gel structure of a network. From Fig. 4 it

follows that the starting sedimentation rate of the
suspension with c0 = 1 g/l is a little higher than that
for c0 = 0.5 g/l. This might be the evidence that for
this powder concentration the gelation structure is
formed; therefore, its settling is similar to the settling in
the absence of magnetic field, that is in accordance with
the results presented in Phenrat et al. (2007). Over time
under the magnetic field the larger structures have
settled and only the smaller ones (around 100 nm)
remain suspended in both in more concentrated and in
more diluted suspensions (Fig. 5b).
One cannot exclude as well that even a small
dissolution of the iron oxide nanoparticles at the
surface (Tombacz et al. 2007) can lead to some change
in the H? cation concentration, which can change the
charge of the double electric layer and, thus, would
affect the aggregative stability of this colloid system.
The residual concentration of iron in the upper layer
of water by sedimentation under external magnetic
field is illustrated in the Fig. 6 as a function of time,
where the sedimentation in different water layers is
shown. For the comparison the corresponding sedimentation dynamics registered by optical method is
shown in the inset. While in the absence of a magnetic
field the magnetite nanoparticle concentration is
decreased by 80 % within the first 20 min, under the
external gradient magnetic field in a water layer
h = 30 mm such decrease occurs within the first
4 min, and in the water layer h = 20 mmwithin the
first minute.

Fig. 7 Time dependence of the residual iron concentration in

water for the suspension of magnetite nanoparticles (c0 = 1 g/l)
under different sedimentation regimes

Comparison of water purification dynamics for

different conditions is presented in Fig. 7. The placement of the steel grid on the bottom of the cuvette
results in speeding up of the sedimentation: within the
first 10 min the concentration drops down to 36 mg/l,
that is decrease by 20 times. Then, after 180 min, the
concentration reaches a value of 0.4 mg/l, that is it
comes close to the hygienic and environment standard
for iron concentration in drinking and fishery waters
0.3 mg/l (Hygienic Norms for drinking water in
Russian Federation 2.1.4 1116).

Conclusions
Gradient magnetic field produced by a series of strip
permanent magnets (B B 0.5 T, dB/dz B 0.13 T/cm)
and in some cases enhanced by a steel grid with sharp
edges helps to separate the magnetite nanoparticles
from the water suspension. The sedimentation rate of
the nanoparticles in water and under the magnetic
fields is higher for less concentrated suspensions
(c0 = 0.1 g/l) than for highly concentrated ones
(c0 = 1 g/l), which might be related to the formation
of gel structures due to a strong magnetic attraction
between ferromagnetic nanoparticles. DLS in the
water suspension with different nanoparticle concentrations (c0 = 0.11 g/l) revealed the characteristic
features in the aggregate formation, which correspond
to the sedimentation behavior. While in a gravitational
field only the magnetite nanoparticle suspension stays
stable for several hours, under gradient magnetic fields
of strip magnets the magnetite particle concentration
in the water layer of 30 mm is reduced by 80 % within

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Page 8 of 8

the first 20 min, and in the water layer of 20 mm with

steel gridwithin the first minute. The sedimentation
of nanopowder in a gradient magnetic field enhanced
by a steel grid for 180 min resulted in the reduction of
the iron concentration in water down to 0.4 mg/l,
which is close to hygienic and environmental standard
for drinking water and fishery.
Acknowledgments The work was supported from the grant N
12-E-2-1033 of the Ural Branch of the Russian Academy of
Sciences. The authors thank N.Schegoleva, V.Gaviko, and
L.Stashkova for the TEM and XRD analysis.

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