SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID
In this work, the FeEDDSNP nanocomplex was synthesized by dissolution peptization of a freshly precipitated sol of iron hydroxide Fe(OH)3 in an aqueous solution of the racemic form of Н4EDDS. The complex was characterized by electron absorption spectroscopy and IR spectroscopy. It was shown that th...
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Ukrainian Chemistry Journal| _version_ | 1871465977443516416 |
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| author | Trunova, Olena Berezhnytska , Оleksandra Rohovtsov , Oleksandr |
| author_facet | Trunova, Olena Berezhnytska , Оleksandra Rohovtsov , Oleksandr |
| author_institution_txt_mv | [
{
"author": "Olena Trunova",
"institution": "V.I. Vernadsky Institute of General and Inorganic Chemistry NAS of Ukraine"
},
{
"author": " Оleksandra Berezhnytska ",
"institution": "V.I.Vernadsky Institute of General and Inorganic Chemistry of NAS of Ukraine, Akad. Palladin Avenue, 32\/34, Kyiv, Ukraine, 03142"
},
{
"author": "Oleksandr Rohovtsov ",
"institution": "V.I.Vernadsky Institute of General and Inorganic Chemistry of NAS of Ukraine"
}
] |
| author_sort | Trunova, Olena |
| baseUrl_str | https://ucj.org.ua/index.php/journal/oai |
| collection | OJS |
| datestamp_date | 2026-07-22T08:23:52Z |
| description | In this work, the FeEDDSNP nanocomplex was synthesized by dissolution peptization of a freshly precipitated sol of iron hydroxide Fe(OH)3 in an aqueous solution of the racemic form of Н4EDDS. The complex was characterized by electron absorption spectroscopy and IR spectroscopy. It was shown that the structure of the nanocomplex is identical to the structure of the FeEDDS complex obtained using a two-stage technology. The position of the absorption maxima of iron nanoparticles practically does not change depending on the storage time at room temperature, which indicates the stability of the synthesized nanocomplex. The nanodispersed FeEDDSNP complex is more soluble in water (275 g/l) compared to the FeEDDS complex obtained by the classical method (150 g/l), which greatly facilitates its use as a biologically active compound. To determine the stability of the system depending on the pH, the electrokinetic potential was measured to select the optimal pH of the medium and concentrations to obtain stable dispersed systems. It is shown that at low pH (1.5–4.0) there is a drop in the electrokinetic potential, and when the pH increases, the   |
| doi_str_mv | 10.33609/2708-129X.89.08.2023.97-108 |
| first_indexed | 2025-09-24T17:43:52Z |
| format | Article |
| fulltext |
97
UDK 541.49: 546.723 – 54-386 doi: 10.33609/2708-129X.89.08.2023.97-108
SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III)
WITH ETHYLENEDIAMINEDISUCCINIC ACID.
O.К. Trunova*, О.S. Berezhnytska, О.О. Rohovtsov
V.I. Vernadsky Institute of General and Inorganic Chemistry of the National Academy
of Sciences of Ukraine,
32/34 Academic Palladin ave., 03142 Kyiv, Ukraine
*e-mail: trelkon@gmail.com
In this work, the FeEDDSNP nanocomplex was synthesized by dissolution peptization of
a freshly precipitated sol of iron hydroxide Fe(OH)3 in an aqueous solution of the racemic
form of Н4EDDS. The complex was characterized by electron absorption spectroscopy and
IR spectroscopy. It was shown that the structure of the nanocomplex is identical to the struc-
ture of the FeEDDS complex obtained using a two-stage technology. The position of the ab-
sorption maxima of iron nanoparticles practically does not change depending on the sto
rage time at room temperature, which indicates the stability of the synthesized nanocomplex.
The nanodispersed FeEDDSNP complex is more soluble in water (275 g/l) compared to the
FeEDDS complex obtained by the classical method (150 g/l), which greatly facilitates its use
as a biologically active compound. To determine the stability of the system depending on the
pH, the electrokinetic potential was measured to select the optimal pH of the medium and
concentrations to obtain stable dispersed systems. It is shown that at low pH (1.5–4.0) there is
a drop in the electrokinetic potential, and when the pH increases, the ξ-potential changes its
sign, which is due to the recharging of the colloidal particle and the decrease in the size of the
particles. The system is stable in the range of pH 4.5–7.5 and a wide range of concentrations
(1∙10-1–1∙10-3 M). At a metal concentration of 6–8 wt.%, the system is thixotropic-reversible
and does not require additional stabilization, since EDDS itself has surface activity. Using the
methods of dynamic light scattering and scanning electron microscopy, a study of the disper-
sion of FeEDDSNP complex nanoparticles, their distribution by radii, shape and morphology
was carried out. It is shown that the particles of the nanocomplex have a morphology close to
spherical with dimensions of ~30 nm.
Keywords: iron (III), nanoparticles, synthesis, peptization, colloidal solution, ethylenedi-
aminedisuccinic acid.
98 ISSN 2708-129X. Укр. хім. журн., 2023
SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID.ORGANIC CHEMISTRY
INTRODUCTION. Biocoordination com-
pounds of vital metals (microelements) as
medical and biological agents form the basis
of modern socially and technologically sig-
nificant innovative developments. Combining
metal ions with an organic compound enables
the production of supramolecular associates,
which are inherently close to the endogenous
coordination compounds that exist in the liv-
ing organism and in general in biosystems.
They are less toxic than their constituents and
usually have a wide range of biological activity
[1–3]. The effectiveness of the effect of a mi-
croelements on any living organism directly
depends on the form in which the trace ele-
ment is. The twenty-first century is the period
of use in various bio-medical fields of effective
preparations of microelements based on che-
lated compounds, which are easily absorbed
by living organisms. The most promising che
lating agents are aminopolycarboxylic acids,
for example ethylenediaminediansuccinic acid
(H4EDDS), which contains fragments of aspar-
tic and succinic acids in the molecule, known
as adaptogens. In a living organism, it per-
forms not only the function of delivering trace
elements but also carries a biologically active
load. Under the action of enzymes in the liv-
ing organism, EDDS breaks down into essen-
tial amino acids (arginine, leucine, isoleucine,
valine, histidine, asparagine, alanine), which
are components of the metabolic chain [4,
5]. EDDS forms fairly stable complexes with
biogenic metals in a wide pH range (3–10),
which in terms of biochemical structure and
chemical purity are very similar to organome-
tallic compounds that are synthesized in plant
or animal cells. Therefore, upon entering a
living cell, these substances will be perceived
by it not as foreign elements, but as "its own",
which will ensure their biogenic compatibility
and accordingly, high digestibility [1, 6, 7]. For
example, complexes of metals with ethylene-
diaminedisuccinic acid have an antimicrobial
effect against fungi and bacteria [8] and an an-
tiviral effect against cytomegalovirus [9]. They
can be used in homeopathic doses on all types
of soil for any plants, or as feed additives for
animals, without harming nature [10–12].
With the development of modern technolo-
gies for the synthesis of nanomaterials, interest
has arisen in studying the properties of me
tals in the ultradisperse range in the form of
powders, solutions and suspensions [13–15].
Of particular interest to researchers are nano-
systems of a given composition with predictable
properties and a certain size of nanoparticles,
since the permeability, activity, solubility and
toxicity of nanoparticles depends on this [16,
17]. The targeted production of metal complex-
es in the nano-range with a certain size, degree
of aggregation and particle shape for the crea-
tion of new functional materials (optical and
nanoelectronic devices, chemical and biological
sensors, catalysts) is an important task, since
many physicochemical characteristics of mate-
rials depend on these parameters [ 18, 19].
Among the various forms of nanosized ma-
terials for various fields of biology, veterinary
medicine and medicine, solutions of nanopar
ticles of metal complexes are of interest. Their
advantage lies in a relatively narrow distribu-
tion of particles in size and shape, and a long
period of preservation of biological activi-
ty. However, the main problem in obtaining
nanodispersed metal complexes is that nano-
particles are unstable in solution and tend to
form large aggregates. To obtain stable nano-
particles of a certain size and shape in the form
of colloidal solutions, it is necessary to contain
99https://ucj.org.ua
O.К. Trunova, О.S.Berezhnytska, О.О. Rohovtsov UCJ № 08 / Vol. 89
stabilizing agents (surfactants) in aqueous dis-
persions, which, when adsorbed on the surface
of the particles, prevent their association for
several months [20–22]. Various organic com-
pounds are often used as such stabilizers – thi-
ols, thiourea derivatives, amines, thiocyanates,
carboxylates, etc. Stabilizers are sorbed on the
surface of growing particles and reduce their
surface energy, thereby reducing the likelihood
of aggregation and precipitation [23–26].
The purpose of this work is to develop a
method for the synthesis of biologically active
Fe(III) complexes with ethylenediaminesuc-
cinic acid in the nanoscale range (30–200 nm),
which will facilitate the effective penetration of
the microelement through the cell membranes
of living organisms by endocytosis.
EXPERIMENT AND RESULTS DISCUS-
SION. The classic version of the synthesis of
3d-metal complexes with ethylenediaminedi-
succinic acid is a two-stage process consisting
of the condensation reaction of ethylenedi-
amine and maleic acid in an alkaline medi-
um (1) and an exchange reaction between an
organic molecule and an inorganic metal salt
(2) (Fig. 1) [27, 28].
Fig. 1 – Scheme of the synthesis of 3d-metal complexes with ethylenediaminedisuccinic acid.
which are components of the metabolic chain [4, 5]. EDDS forms fairly stable complexes with
biogenic metals in a wide pH range (3–10), which in terms of biochemical structure and
chemical purity are very similar to organometallic compounds that are synthesized in plant or
animal cells. Therefore, upon entering a living cell, these substances will be perceived by it not
as foreign elements, but as "its own", which will ensure their biogenic compatibility and,
accordingly, high digestibility [1, 6, 7]. For example, complexes of metals with
ethylenediaminedisuccinic acid have an antimicrobial effect against fungi and bacteria [8] and an
antiviral effect against cytomegalovirus [9]. They can be used in homeopathic doses on all types
of soil for any plants, or as feed additives for animals, without harming nature [10–12].
With the development of modern technologies for the synthesis of nanomaterials, interest
has arisen in studying the properties of metals in the ultradisperse range in the form of powders,
solutions and suspensions [13–15]. Of particular interest to researchers are nanosystems of a
given composition with predictable properties and a certain size of nanoparticles, since the
permeability, activity, solubility and toxicity of nanoparticles depends on this [16, 17]. The
targeted production of metal complexes in the nano-range with a certain size, degree of
aggregation and particle shape for the creation of new functional materials (optical and
nanoelectronic devices, chemical and biological sensors, catalysts) is an important task, since
many physicochemical characteristics of materials depend on these parameters [ 18, 19].
Among the various forms of nanosized materials for various fields of biology, veterinary
medicine, and medicine, solutions of nanoparticles of metal complexes are of interest. Their
advantage lies in a relatively narrow distribution of particles in size and shape, and a long period
of preservation of biological activity. However, the main problem in obtaining nanodispersed
metal complexes is that nanoparticles are unstable in solution and tend to form large aggregates.
To obtain stable nanoparticles of a certain size and shape in the form of colloidal solutions, it is
necessary to contain stabilizing agents (surfactants) in aqueous dispersions, which, when
adsorbed on the surface of the particles, prevent their association for several months [20–22].
Various organic compounds are often used as such stabilizers – thiols, thiourea derivatives,
amines, thiocyanates, carboxylates, etc. Stabilizers are sorbed on the surface of growing particles
and reduce their surface energy, thereby reducing the likelihood of aggregation and precipitation
[23–26].
The purpose of this work is to develop a method for the synthesis of biologically active
Fe(III) complexes with ethylenediaminesuccinic acid in the nanoscale range (30–200 nm), which
will facilitate the effective penetration of the microelement through the cell membranes of living
organisms by endocytosis.
EXPERIMENT AND RESULTS DISCUSSION. The classic version of the synthesis of 3d-
metal complexes with ethylenediaminedisuccinic acid is a two-stage process consisting of the
condensation reaction of ethylenediamine and maleic acid in an alkaline medium (1) and an
exchange reaction between an organic molecule and an inorganic metal salt (2) (Fig. 1) [27, 28].
Fig. 1 – Scheme of the synthesis of 3d-metal complexes with ethylenediaminedisuccinic acid.
This method for the synthesis of Fe(III) ethylenediaminedisuccinates is the most
common. However, the size of complex particles cannot be controlled due to the high rate of the
reaction. With today's development of nanotechnology, the task of obtaining biologically active
compounds in the form of nanosystems becomes urgent, since nanoparticles are the most
(1)
(2)
This method for the synthesis of Fe(III)
ethylenediaminedisuccinates is the most com-
mon. However, the size of complex particles
cannot be controlled due to the high rate of
the reaction. With today's development of
nanotechnology, the task of obtaining biolo
gically active compounds in the form of nano-
systems becomes urgent, since nanoparticles
are the most acceptable forms of perception
of biogenic metals by a living cell. Based on
these considerations, we synthesized a Fe(III)
nanocomplex with EDDS from a freshly pre-
cipitate iron hydroxide sol. The synthesis is
based on the process of dissolution peptization
of Fe(OH)3 in an aqueous solution of the race-
mic form of ethylenediaminedisuccinic acid.
The synthesis of FeEDDSNP was carried out ac-
cording to the following scheme:
1. Preparation of highly dispersed iron(III)
hydroxide.
To a hot (600C) supersaturated solution
containing 3 moles (252 g) of NaHCO3 in 1 li
ter of distilled water, with vigorous stirring,
1 mole of a hot solution of iron(III) chloride
FeCl3∙6H2O (270 g), dissolved in 500 ml of wa-
ter, was slowly added. The reaction proceeds
according to the equation:
3NaHCO3 + FeCl3
.= Fe(OH)3 +3NaCl + 3CO2.
The mixture was stirred for 10 minutes,
then the solution was cooled to room tempera
ture. After cooling, the resulting precipitate of
100 ISSN 2708-129X. Укр. хім. журн., 2023
SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID.ORGANIC CHEMISTRY
Fe(OH)3 was separated from the mother solu-
tion by centrifugation and washed repeatedly
with distilled water using the suspension-cen-
trifugation method until the wash water react-
ed negatively to Cl- ions.
2. Preparation of a colloidal solution of the
Fe(III) complex with ethylenediaminedisuccinic
acid.
An equimolar amount of dry H4EDDS
(292 g) was added to the wet Fe(OH)3 gel quan-
titatively transferred into a 1-liter beaker. The
mixture was stirred and left for 20–30 minutes
until completely liquefied. After this, the solu-
tion was heated to a temperature of 50–60 0C
with intense stirring. The pH of the medium
was adjusted using dry sodium carbonate to
7.0–7.5. In this case, the surface layer of the
sediment dissolved, resulting in the formation
of the monoprotonated FeHEDDS complex,
which is the electrolyte necessary for the pepti-
zation of the rest of the sediment:
Fe(OH)3 + H4EDDS→FeHEDDS + 3H2O.
Then peptization of the sediment was car-
ried out – loosening the sediment and trans-
forming it into a stable colloidal solution. To
do this, 50 ml of solution was diluted with
0.001 M NaOH solution to 1000 ml and pH =
8.5. The colloidal solution was filtered through
a 0.45 μm hydrophilic filter (to eliminate poly-
dispersity). When dissolving peptization, it
is very important to introduce the peptiz-
ing agent gradually in small portions, since
its sudden introduction or excess will lead to
complete dissolution of the precipitate and the
formation of a true molecular ionic solution.
Since, in this case, the peptizer is a monopro-
tonated complex formed in the solution, a slow
process at a constant temperature guarantees a
positive result. This synthesis does not require
the selection of a separate stabilizer to increase
the stability of the disperse system, since EDDS
has a diphilic structure and is an internal sur-
factant in a wide range of pH (3.2–8.5) and
concentrations.
As is known, a measure of the stability of a
colloidal system is the electrokinetic potential
(ξ), which depends on the pH of the medium,
the influence of electrolytes and temperature.
Therefore, studies were carried out on the sta-
bility of the system and changes in particle size
depending on the pH of the solution (Fig. 2,
Table 1). The ξ-potential and particle size were
determined by dynamic light scattering using
a Zeta Sizer Malvern device at a temperature
of 250C. To do this, 15 ml of the solution was
placed in an autotitrator tube and measure-
ments were carried out with a pH interval of
0.5, titrating the test system with a solution of
0.25 M HCl.
Fig. 2 – Change in ξ-potential (1) and particle
size (2) depending on the pH of the medium in the
Fe(III) – EDDS system.
As can be seen from Fig. 2, the system is sta-
ble at pH≥4.5 (|ξ|≥30 mV). At low pH, a drop
in the electrokinetic potential is observed,
and, as a consequence, coagulation of the col-
1 2 3 4 5 6
0
500
1000
1500
2000
pH
r,
nm
-40
-30
-20
-10
0
10
20
30
1
2
Fig. 2 – Change in -potential (1) and particle size (2) depending on the pH of the medium in the Fe(III) –
EDDS system.
As can be seen from Fig. 2, the system is stable at pH≥4.5 (||≥30 mV). At low pH, a
drop in the electrokinetic potential is observed, and, as a consequence, coagulation of the
colloidal system occurs. With increasing pH, the -potential changes sign, which may be due to
both recharging of the colloidal particle and a decrease in particle size due to decoagulation.
There is evidence in the literature that a polymolecular layer can form on the surface of a particle
[29], but in our case such a statement is doubtful, since polymolecular adsorption from solutions
is impossible.
In Fig. 3 and Table 1 show the size distribution of FeEDDSNP nanoparticles.
Fig. 3 – Size distribution of FeEDDSNP nanoparticles.
An analysis of the distribution of nanoparticles shows that in this system there are two regions
with a predominant radius of particles of approximately the same size. In the region of low pH
values (1.2–3.7), large particles (940–1900 nm) are formed with a wide distribution among
fractions. In this case, a drop in the electrokinetic potential occurs due to compression of the
electrical double layer, which, in turn, is associated with the sensitivity of the -potential to the
pH of the medium for systems containing amphoteric compounds. Recharging a particle under
the influence of pH, unfortunately, leads to coagulation processes and a decrease in the stability
of the entire dispersed system. In the pH range = 4.5–7.5, the system is dominated by
nanoparticles with sizes of ~ 32 nm, that is, the system is monodisperse and quite stable. Based
on the charge of the zeta potential, we can assume the following micelle
formula:{[(mFeLn[FeL]-(n–x)К+]∙xК+}. As can be seen from the formula, the potential-
determining ion (PDI) is the complex particle [FeL]-, which is typical for nanodispersed systems
based on organic ligands with surface-active properties.
101https://ucj.org.ua
O.К. Trunova, О.S.Berezhnytska, О.О. Rohovtsov UCJ № 08 / Vol. 89
loidal system occurs. With increasing pH, the
ξ-potential changes sign, which may be due to
both recharging of the colloidal particle and a
decrease in particle size due to decoagulation.
There is evidence in the literature that a poly-
molecular layer can form on the surface of a
particle [29], but in our case such a statement
is doubtful, since polymolecular adsorption
from solutions is impossible.
In Fig. 3 and Table 1 show the size distribu-
tion of FeEDDSNP nanoparticles.
1 2 3 4 5 6
0
500
1000
1500
2000
pH
r,
nm
-40
-30
-20
-10
0
10
20
30
1
2
Fig. 2 – Change in -potential (1) and particle size (2) depending on the pH of the medium in the Fe(III) –
EDDS system.
As can be seen from Fig. 2, the system is stable at pH≥4.5 (||≥30 mV). At low pH, a
drop in the electrokinetic potential is observed, and, as a consequence, coagulation of the
colloidal system occurs. With increasing pH, the -potential changes sign, which may be due to
both recharging of the colloidal particle and a decrease in particle size due to decoagulation.
There is evidence in the literature that a polymolecular layer can form on the surface of a particle
[29], but in our case such a statement is doubtful, since polymolecular adsorption from solutions
is impossible.
In Fig. 3 and Table 1 show the size distribution of FeEDDSNP nanoparticles.
Fig. 3 – Size distribution of FeEDDSNP nanoparticles.
An analysis of the distribution of nanoparticles shows that in this system there are two regions
with a predominant radius of particles of approximately the same size. In the region of low pH
values (1.2–3.7), large particles (940–1900 nm) are formed with a wide distribution among
fractions. In this case, a drop in the electrokinetic potential occurs due to compression of the
electrical double layer, which, in turn, is associated with the sensitivity of the -potential to the
pH of the medium for systems containing amphoteric compounds. Recharging a particle under
the influence of pH, unfortunately, leads to coagulation processes and a decrease in the stability
of the entire dispersed system. In the pH range = 4.5–7.5, the system is dominated by
nanoparticles with sizes of ~ 32 nm, that is, the system is monodisperse and quite stable. Based
on the charge of the zeta potential, we can assume the following micelle
formula:{[(mFeLn[FeL]-(n–x)К+]∙xК+}. As can be seen from the formula, the potential-
determining ion (PDI) is the complex particle [FeL]-, which is typical for nanodispersed systems
based on organic ligands with surface-active properties.
Fig. 3 – Size distribution of FeEDDSNP nanoparticles.
An analysis of the distribution of nanopar-
ticles shows that in this system there are two
regions with a predominant radius of particles
of approximately the same size. In the region of
low pH values (1.2–3.7), large particles (940–
1900 nm) are formed with a wide distribution
among fractions. In this case, a drop in the elec-
trokinetic potential occurs due to compression
of the electrical double layer, which, in turn, is
associated with the sensitivity of the ξ-poten-
tial to the pH of the medium for systems con-
taining amphoteric compounds. Recharging
a particle under the influence of pH, unfor-
tunately, leads to coagulation processes and a
decrease in the stability of the entire dispersed
system. In the pH range = 4.5–7.5, the sys-
tem is dominated by nanoparticles with sizes
of ~ 32 nm, that is, the system is monodisperse
and quite stable. Based on the charge of the
dzeta potential, we can assume the following
micelle formula:{[(mFeLn[FeL]-(n–x)К+]∙xК+}.
As can be seen from the formula, the poten-
tial-determining ion (PDI) is the complex par-
ticle [FeL]-, which is typical for nanodispersed
systems based on organic ligands with sur-
face-active properties.
In a more acidic environment, protonated
(usually poorly soluble) complexes are present.
Therefore, at pH = 1.5–4.0, the particle size in-
creases significantly, and the electrokinetic po-
tential drops sharply. In this case, at pH <1.5,
the particle is recharged in the system both
due to a sharp decrease in pH and under the
influence of ions of a non-indifferent electro-
lyte, which is ferric chloride. There are several
different protonated forms of the complex in
102 ISSN 2708-129X. Укр. хім. журн., 2023
SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID.ORGANIC CHEMISTRY
solution, making their identification difficult.
Due to the fact that the electrokinetic potential
in the acidic region changes its sign, and it is de-
termined by the sign of the POI charge, then,
obviously, the micelle formula takes on the fol-
lowing form:{[(mFeLnFe3+3(n–x)Cl-] 3xCl-}.
Based on the data in Fig. 3 and table. 1 we
can talk about a fairly high aggregative stability
of the dispersed system in the pH range 4.0–
7.5 in a wide range of concentrations (1⋅10-1–
1⋅10-3 M). In most cases, when the critical mi-
celle concentration is reached, smaller thermo-
dynamically stable particles are formed that
are less prone to coagulation [30]. It should
be noted that at a metal concentration of
6–8 wt.%, the system is thixotropic-reversible.
It is known that thixotropic transformations,
as a rule, do not destabilize the system; some-
times, on the contrary, such systems are more
stable. This is due to the formation of rigid gel-
like structures, where the particles are fixed at a
certain distance from each other, which elimi
nates coagulation processes. The dispersity of
the system practically does not change during
thixotropic transformations.
When it comes to the sensitivity of the sys-
tem to the pH of the environment, the situation
is slightly different. In particular, everything
depends on the charge and size of the poten-
tial-determining ion. As a rule, when a parti-
cle is recharged due to the pH of the medium,
agglomeration takes place in the system, and,
consequently, a change in dispersion, which is
confirmed by the results of the study. Thus, the
presented results indicate the stability of the
FeEDDSNP nanodisperse complex in the pH
range = 4.5–7.5, the particle size is optimal (the
possibility of toxic effects of small particles is
excluded), which allows its use as a biologically
active additive for living organisms.
Тable 1.
Changes in particle size and electrokinetic
potential depending on the pH of
the medium in the FeEDDS system.
№ рН r, nm ξ,mV
1 7.5 32.04 -31
2 6.2 3.31 -31
1 5.7 32.29 -31
2 5.42 34.38 -30
3 4.89 33.03 -29
4 4.47 32.78 -30
5 3.7 639.6 -26
6 3.42 1789 -15
7 2.9 1804 -8
8 1.42 1909 9
9 1.88 1654 15
10 1.42 1198 20
11 1.2 940 22
It should be noted that the nanodispersed
FeEDDSNP complex has a higher solubility
(275 g/l) compared to the FeEDDS complex
obtained using two-stage technology (150 g/l),
which greatly facilitates its use as a biologically
active compound.
The FeEDDSNP nanodisperse complex iso-
lated from solution was analyzed by electron
absorption spectroscopy, IR spectroscopy and
scanning electron microscopy (SEM). Electronic
absorption spectra were recorded on a Specord
M-40 UV-VIS spectrometer in quartz cuvettes
(l = 1 cm) in the range of 50000–11000 cm-1.
IR spectra were recorded on a Specord M-80
spectrometer in the region of 4000–400 cm-1
in tablets with KBr. Microphotographs were
recorded on a Tescan Mira 3 LMU scanning
electron microscope (SEM).
The electronic absorption spectra of
FeEDDSNP are similar to the spectra of Fe(III)
ethylenediaminedisuccinate synthesized using
the classical method (Fig. 4).
103https://ucj.org.ua
O.К. Trunova, О.S.Berezhnytska, О.О. Rohovtsov UCJ № 08 / Vol. 89
Fig. 4 – UV-VIS spectra of FeEDDS (1) and
FeEDDSNP depending on storage time (2 – 3 days,
3 – 1 month, 4 – 6 months). СFe=5∙10-3 mol/l,
рН=6.5, Т= 220С± 30С.
Absorption maxima (νmax) at 24600 and
29840 cm-1 relate to d-d transitions (6A1g →
4A1g
and 6A1g→
4T1g, respectively) of the Fe3+ ion in
an octahedral environment [31]. A small split-
ting νmax at ~30000 cm-1 is due to the overlap of
the charge transfer band from the metal to the
ligand (30960 cm-1) and the 6A1g→
4T1g term. At
the same time, the intensity of the absorption
bands and the position of the absorption maxi
ma of iron nanoparticles practically did not
change depending on the storage time at room
temperature, which indicates the stability of
the synthesized nanocomplex.
The IR spectra of the complexes obtained by
different methods are almost identical (Fig. 5,
Table 2).
The electronic absorption spectra of FeEDDSNP are similar to the spectra of Fe(III)
ethylenediamine disuccinate synthesized using the classical method (Fig. 4).
Fig. 4 – UV-VIS spectra of FeEDDS (1) and FeEDDSNP depending on storage time (2 – 3 days, 3 – 1
month, 4 – 6 months). СFe=5∙10-3 mol/l, рН=6.5, Т= 220С 30С.
Absorption maxima (max) at 24600 and 29840 cm-1 relate to d-d transitions (6A1g 4A1g and
6A1g4T1g, respectively) of the Fe3+ ion in an octahedral environment [31]. A small splitting max
at ~30000 cm-1 is due to the overlap of the charge transfer band from the metal to the ligand
(30960 cm-1) and the 6A1g4T1g term. At the same time, the intensity of the absorption bands
and the position of the absorption maxima of iron nanoparticles practically did not change
depending on the storage time at room temperature, which indicates the stability of the
synthesized nanocomplex.
The IR spectra of the complexes obtained by different methods are almost identical (Fig.
5, Table 2).
4000 3500 3000 2500 2000 1500 1000 500 0
0
20
40
60
80
100
M-N
M-O
sCOO
,cm-1
In
te
ns
ity
, %
2
1
H
2
O
asCOO
Fig. 5 – IR spectra of FeEDDS (1) and FeEDDSNP (2) complexes.
The absorption bands as(COO-) and s(COO-) have values of ~1600 and 1400 cm-1,
respectively, which indicates the ionic type of bond of the Fe3+ ion with the oxygen atoms of
ionized carboxyl groups. A slight shift of these bands in the spectrum of FeEDDSNP to the high-
frequency region compared to FeEDDS indicates an increase in the ionicity of the bond in the
nano-complex. This is also evidenced by a decrease in the bond energy (M-N) in FeEDDSNP
relative to FeEDDS [32].
The electronic absorption spectra of FeEDDSNP are similar to the spectra of Fe(III)
ethylenediamine disuccinate synthesized using the classical method (Fig. 4).
Fig. 4 – UV-VIS spectra of FeEDDS (1) and FeEDDSNP depending on storage time (2 – 3 days, 3 – 1
month, 4 – 6 months). СFe=5∙10-3 mol/l, рН=6.5, Т= 220С 30С.
Absorption maxima (max) at 24600 and 29840 cm-1 relate to d-d transitions (6A1g 4A1g and
6A1g4T1g, respectively) of the Fe3+ ion in an octahedral environment [31]. A small splitting max
at ~30000 cm-1 is due to the overlap of the charge transfer band from the metal to the ligand
(30960 cm-1) and the 6A1g4T1g term. At the same time, the intensity of the absorption bands
and the position of the absorption maxima of iron nanoparticles practically did not change
depending on the storage time at room temperature, which indicates the stability of the
synthesized nanocomplex.
The IR spectra of the complexes obtained by different methods are almost identical (Fig.
5, Table 2).
4000 3500 3000 2500 2000 1500 1000 500 0
0
20
40
60
80
100
M-N
M-O
sCOO
,cm-1
In
te
ns
ity
, %
2
1
H
2
O
asCOO
Fig. 5 – IR spectra of FeEDDS (1) and FeEDDSNP (2) complexes.
The absorption bands as(COO-) and s(COO-) have values of ~1600 and 1400 cm-1,
respectively, which indicates the ionic type of bond of the Fe3+ ion with the oxygen atoms of
ionized carboxyl groups. A slight shift of these bands in the spectrum of FeEDDSNP to the high-
frequency region compared to FeEDDS indicates an increase in the ionicity of the bond in the
nano-complex. This is also evidenced by a decrease in the bond energy (M-N) in FeEDDSNP
relative to FeEDDS [32].
Fig. 5 – IR spectra of FeEDDS (1) and FeEDDSNP (2) complexes.
The absorption bands νas(COO-) and
νs(COO-) have values of ~1600 and 1400 cm-1,
respectively, which indicates the ionic type of
bond of the Fe3+ ion with the oxygen atoms of
ionized carboxyl groups. A slight shift of these
bands in the spectrum of FeEDDSNP to the
high-frequency region compared to FeEDDS
indicates an increase in the ionicity of the bond
in the nano-complex. This is also evidenced
by a decrease in the bond energy ν(M-N) in
FeEDDSNP relative to FeEDDS [32].
104 ISSN 2708-129X. Укр. хім. журн., 2023
SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID.ORGANIC CHEMISTRY
Тable 2.
Basic vibrational frequencies (cm-1) and
their assignments in the IR spectra
of complexes FeEDDS.
band assignment FeEDDS FeEDDSNP
ν (COOH) – –
νas(COO) 1602
1553
1515
1655
1575
νs(COO) 1433
1379
1305
1446
1389
1316
ν(М—O) 559
656
602
707
537
626
603
711
ν(М—N) 457 449
ν(H2O)intra 3192 3224
ν(H2O)inter. 3424 3460
Analysis of micrographs (Fig. 6, a) indicates
that the synthesized FeEDDSNP complex is na-
nosized, with the particle size being ~30 nm.
In addition, it should be noted that the result-
ing compounds have a homogeneous chemical
composition and a morphology close to sphe
rical. Microphotographs of the FeEDDS com-
plex (Fig. 6, b) indicate that the complex con-
sists of irregularly shaped particles with sizes
up to 10 μm. Those, for iron ethylenedimine-
disuccinate synthesized using the classical
method, compared to the nano-complex, the
particle size increases and their shape changes,
which is associated with the speed of the com-
plex formation reaction.
Fig. 6 – SEM micrographs of the FeEDDSNP complex, scale mark 500 nm (a)
and FeEDDS complex(b), scale mark 10 µm(b).
Тable 2.
Basic vibrational frequencies (cm-1) and their assignments in the IR spectra of complexes
FeEDDS.
band
assignment
FeEDDS FeEDDSNP
(COOH) – –
as(COO) 1602
1553
1515
1655
1575
s(COO) 1433
1379
1305
1446
1389
1316
(М—O) 559
656
602
707
537
626
603
711
(М—N) 457 449
(H2O)intra 3192 3224
(H2O)inter. 3424 3460
Analysis of micrographs (Fig. 6, a) indicates that the synthesized FeEDDSNP complex is
nanosized, with the particle size being ~30 nm. In addition, it should be noted that the resulting
compounds have a homogeneous chemical composition and a morphology close to spherical.
Microphotographs of the FeEDDS complex (Fig. 6, b) indicate that the complex consists of
irregularly shaped particles with sizes up to 10 μm. Those, for iron ethylenediminedisuccinate
synthesized using the classical method, compared to the nano-complex, the particle size
increases and their shape changes, which is associated with the speed of the complex formation
reaction.
а b
Fig. 6 – SEM micrographs of the FeEDDSNP complex, scale mark 500 nm (a) and FeEDDS complex(b),
scale mark 10 µm(b).
CONCLUSIONS. A procedure has been developed for the synthesis of a nanosized Fe(III)
complex based on ethylenediaminedisuccinic acid using a freshly precipitated Fe(III) hydroxide
sol. The synthesis is based on the process of dissolution peptization of Fe(OH)3 in an aqueous
solution of the racemic form of EDDS. The use of bipolar substances with a zwitterionic
structure (namely, EDDS) as a dispersant makes it possible to introduce such systems in the form
of suspensions not only into aqueous phases, but also into fatty phases. This is one of the
CONCLUSIONS. A procedure has been de-
veloped for the synthesis of a nanosized Fe(III)
complex based on ethylenediaminedisuccinic
acid using a freshly precipitated Fe(III) hydroxi
de sol. The synthesis is based on the process of
dissolution peptization of Fe(OH)3 in an aque-
ous solution of the racemic form of EDDS.
The use of bipolar substances with a zwitteri-
onic structure (namely, EDDS) as a dispersant
makes it possible to introduce such systems in
the form of suspensions not only into aqueous
phases, but also into fatty phases. This is one of
105https://ucj.org.ua
O.К. Trunova, О.S.Berezhnytska, О.О. Rohovtsov UCJ № 08 / Vol. 89
the conditions for introducing nanocomplexes
into animal feed (premixes). To determine the
stability of the system depending on pH, the
electrokinetic potential was measured to select
the optimal pH of the medium and concentra-
tions to obtain stable dispersed systems. It has
been shown that at low pH there is a drop in
the electrokinetic potential, and with increas-
ing pH the ξ-potential changes sign, which is
due to the recharging of the colloidal particle
and a decrease in particle size. The system is
stable in the pH range 4.5–7.5 and in a wide
range of concentrations (1⋅10-1–1⋅10-3 M). At
a metal concentration of 6–8 wt.%, the system
is thixotropic-reversible and does not require
stabilization, since EDDS itself has surface ac-
tivity. The methods of dynamic light scattering
and scanning electron microscopy were used
to study the dispersion of nanoparticles of the
FeEDDSNP complex, their distribution by radi-
us, shape and morphology. It was shown that
the particles of the nanocomplex have a mor-
phology close to spherical with a size of ~30 nm.
AKNOWLEDGEMENT. The work was
carried out with the financial support
of the National Academy of Sciences of
Ukraine within the state budget topic
322E «Creation of new hybrid, composite
and polymer materials doped with coordina-
tion compounds of 3d- and 4f- metals based
on β-diketonate and carboxylate acyclic li
gands». The state registration number of the
work is 0122U001299.
СИНТЕЗ І ДОСЛІДЖЕННЯ НАНОРОЗМІРНОГО
КОМПЛЕКСУ Fe(III) З ЕТИЛЕНДИАМІНДИ
БУРШТИНОВОЮ КИСЛОТОЮ
О. К. Трунова*, О. С. Бережницька,
О. О. Роговцов
Інститут загальної та неорганічної хімії
ім. В. І. Вернадського НАН України,
просп. Академіка Палладіна, 32/34, Київ
03142, Україна
*e-mail: trelkon@gmail.com
З огляду на сучасний розвиток нанотех-
нологій перед фахівцями постало завдан-
ня отримати біологічно активні сполуки у
вигляді наносистем, оскільки саме нано-
частинки є найбільш прийнятними форма-
ми сприйняття біогенних металів живою
клітиною. Таким чином актуальним стає
пошук нових шляхів формування моно-
дисперсних систем із контрольованим роз-
міром наночастинок. У роботі представ-
лено результати із синтезу та дослідження
нанорозмірного комплексу Fe(III) на осно-
ві етилендиаміндибурштинової кислоти.
В основу синтезу покладено процес дисо-
люційної пептизації свіжоосадженого золю
Fe(ОН)3 у водному розчині рацемічної
форми EDDS. Використання в ролі диспер-
гатора біполярних речовин цвіттер-іонної
будови (а саме такою речовиною є EDDS)
дозволяє вводити такі системи у вигляді
суспензій не тільки у водні фази, але й у
жирові. Це є однією з умов введення нано-
комплексів у корми (премікси) для тварин.
Для визначення стійкості системи залежно
від рН було виміряно електрокінетичний
потенціал для вибору оптимального рН се-
редовища та концентрацій для отримання
стабільних дисперсних систем. Показано,
106 ISSN 2708-129X. Укр. хім. журн., 2023
SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID.ORGANIC CHEMISTRY
що за низьких рН (1.5–4.0) спостерігаєть-
ся падіння електрокінетичного потенціалу,
а при збільшенні рН ξ-потенціал змінює
знак, що зумовлено перезарядженням ко-
лоїдної частинки та зменшенням розміру
частинок. Система стабільна в діапазоні рН
4.5–7.5 і широкому діапазоні концентрацій
(1∙10-1–1∙10-3 М). При концентрації металу
6–8 мас.% система є тиксотропно-оборот-
ною і не потребує додаткової стабілізації,
оскільки сама EDDS має поверхневу актив-
ність. Методами динамічного розсіювання
світла та скануючої електронної мікроско-
пії проведено дослідження дисперсності
наночастинок комплексу FeEDDSNP, їхній
розподіл за радіусами, формою та морфо-
логією. Показано, що частинки нанокомп-
лексу мають морфологію, близьку до сфе-
ричної з розмірами ~30 нм.
Kлючові слова: залізо(ІІІ), наночастин-
ки, синтез, пептизація, колоїдний розчин,
етилендиаміндибурштинова кислота.
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Стаття надійшла 06.08.2023.
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| resource_txt_mv | ucjorgua/0f/fed06903d4bcec170d4679e1c2860a0f.pdf |
| spelling | oai:ojs2.1444248.nisspano.web.hosting-test.net:article-5772026-07-22T08:23:52Z SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID Trunova, Olena Berezhnytska , Оleksandra Rohovtsov , Oleksandr iron (III), nanoparticles, synthesis, peptization, colloidal solution, ethylenediaminedisuccinic acid. In this work, the FeEDDSNP nanocomplex was synthesized by dissolution peptization of a freshly precipitated sol of iron hydroxide Fe(OH)3 in an aqueous solution of the racemic form of Н4EDDS. The complex was characterized by electron absorption spectroscopy and IR spectroscopy. It was shown that the structure of the nanocomplex is identical to the structure of the FeEDDS complex obtained using a two-stage technology. The position of the absorption maxima of iron nanoparticles practically does not change depending on the storage time at room temperature, which indicates the stability of the synthesized nanocomplex. The nanodispersed FeEDDSNP complex is more soluble in water (275 g/l) compared to the FeEDDS complex obtained by the classical method (150 g/l), which greatly facilitates its use as a biologically active compound. To determine the stability of the system depending on the pH, the electrokinetic potential was measured to select the optimal pH of the medium and concentrations to obtain stable dispersed systems. It is shown that at low pH (1.5–4.0) there is a drop in the electrokinetic potential, and when the pH increases, the &nbsp; V.I.Vernadsky Institute of General and Inorganic Chemistry 2023-09-29 Article Article Inorganic Chemistry Неорганическая химия Неорганічна хімія application/pdf https://ucj.org.ua/index.php/journal/article/view/577 10.33609/2708-129X.89.08.2023.97-108 Ukrainian Chemistry Journal; Vol. 89 No. 8 (2023): Ukrainian Chemistry Journal; 97-108 Украинский химический журнал; ##issue.vol## 89 ##issue.no## 8 (2023): Ukrainian Chemistry Journal; 97-108 Український хімічний журнал; Том 89 № 8 (2023): Ukrainian Chemistry Journal; 97-108 2708-129X 2708-1281 en https://ucj.org.ua/index.php/journal/article/view/577/294 Copyright (c) 2023 Olena Trunova, Оleksandra Berezhnytska , Oleksandr Rohovtsov https://creativecommons.org/licenses/by-nc/4.0 |
| spellingShingle | Trunova, Olena Berezhnytska , Оleksandra Rohovtsov , Oleksandr SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID |
| title | SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID |
| title_full | SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID |
| title_fullStr | SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID |
| title_full_unstemmed | SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID |
| title_short | SYNTHESIS AND STUDY OF NANO-SIZED COMPLEX OF Fe(III) WITH ETHYLENEDIAMINEDISUCCINIC ACID |
| title_sort | synthesis and study of nano-sized complex of fe(iii) with ethylenediaminedisuccinic acid |
| topic_facet | iron (III) nanoparticles synthesis peptization colloidal solution ethylenediaminedisuccinic acid. |
| url | https://ucj.org.ua/index.php/journal/article/view/577 |
| work_keys_str_mv | AT trunovaolena synthesisandstudyofnanosizedcomplexoffeiiiwithethylenediaminedisuccinicacid AT berezhnytskaoleksandra synthesisandstudyofnanosizedcomplexoffeiiiwithethylenediaminedisuccinicacid AT rohovtsovoleksandr synthesisandstudyofnanosizedcomplexoffeiiiwithethylenediaminedisuccinicacid |