Effect of Oligomers and Polymers of Ethylene Glycols on Micellar
Characteristics of Aqueous Solutions of Sodium Pentadectyl Sulfonate
VIGEN BARKHUDARYAN
Department of Molecular Physics
Yerevan State University
1 Alek Manukyan St., Yerevan 0025
ARMENIA
Abstract: The influence of oligomers and polymers of ethylene glycols with a different molecular mass on the
structural transformations of aqueous solutions of surfactant, sodium pentadecylsulfonate, studied by
viscometry and light scattering methods depending on their content in the system. It established that ethylene
glycol with a molecular mass of 2,000 and 40,000 does not affect the structure of the system. For ethylene
glycol with a molecular mass of 4,000, 6,000, and 20,000, a clearly expressed complex course of the
dependence of the intrinsic viscosity of the micelle system on the polymer content was established. It assumed
that with the changes in the concentration of ethylene glycols in the system, micelles are compacted due to a
change in the balance of hydrophobic-hydrophilic interactions. In parallel with the change in apparent micelle
masses and asymmetry coefficients determined by the light scattering method, the intrinsic viscosity also
changes depending on the system's composition. The practical application of this research is that it allows the
performance properties of sodium pentadecyl sulfonate (SPDS) to be adjusted, thereby expanding and
improving its applications.
Key-Words: - ethylene glycol (EG), polyethylene glycol (PEG), sodium pentadecylsulfonate (SPDS),
viscometry, light scattering, surfactant.
Received: June 25, 2022. Revised: August 13, 2023. Accepted: September 19, 2023. Published: October 3, 2023.
1 Introduction
This work is devoted to the study of the influence of
various amounts of water-soluble oligomers and
polymers of ethylene glycols with different
molecular masses on the structural transformations
of aqueous solutions of an anionic surfactant -
sodium pentadecylsulfonate (SPDS). The effect of
oligomers and polymers at various masses on the
surfactants was studied by viscometry and light
scattering methods.
Polyethylene glycol (PEG), also known as
polyethylene oxide (PEO) or poly (oxyethylene)
(POE) is a synthetic, hydrophilic, and biocompatible
polyether. Typically, materials with molecular
weights less than 20,000 g/mol are referred to as
PEGs, whereas those with molecular weights above
20,000 g/mol are referred to as PEOs. These
polymers are soluble in water as well as in many
organic solvents, such as ethanol, acetonitrile,
toluene, acetone, dichloromethane, hexane, and
chloroform.
As is well known, the uses of surface-active
substances (surfactants) have numerous industrial
applications. Due to the property of self-
aggregation, they were used extensively in a variety
of areas. They are used in detergents for cleaning
processes, emulsions, waste-water treatment,
lubricants for automobiles, electronic printing,
biotechnology, cosmetics, petroleum industries, and
more [1, 2, 3, 4]. Their performance can be
bolstered with the addition of polymers. Surfactants
and their micelles can change the surface tension,
phase behavior, and rheology of a solution [2, 5, 9].
The addition of polymers particularly charged
polymers has been shown to enhance bulk and
interfacial properties for a variety of applications [6-
10].
Currently, in various technological processes (in
micelle-polymer flooding, emulsifying, foaming,
and other solutions), polymers are used together
with surfactants. Therefore, it is considered relevant
to study the interaction of surfactants with
macromolecular compounds to obtain information
about the structural changes occurring in solutions
and the possibility of their regulation. In addition,
mixed surfactant-polymer systems are relatively
simple analogs of biological structures that allow
one to form model ideas about the mechanism of
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self-assembly and functioning of bio membranes
[11–13].
Many publications are devoted to the study of the
interaction of polymers with low molecular mass
anionic and cationic surfactants [14]. Most of them
belong to polyelectrolyte (PE) complexes with
oppositely charged surfactants. It assumed that the
volume of the PE macromolecule serves as the
center of surfactant condensation, in which
intramolecular micelle-like clusters formed. As the
PE macromolecule is saturated with detergent ions,
it is hydrophobized, compressed, and neutralized.
When the critical charge density is reached, the
macromolecule collapses.
Polyethylene glycol (PEG) is the simplest water-
soluble non-ionic synthetic polymer, having a broad
range of applications. It is used to cover the surfaces
of colloidal particles to improve their
biocompatibility since the modified surface shows
increased resistance to the adsorption of protein [15,
16]. It also used for covalent modification of
biological macromolecules, peptides, liposomes,
and other drug delivery systems [17-19]. Colloidal
particles covered by PEG are not suppressed by the
immune system, and their circulation time is
increased up to 8–10 h, making them suitable for
prolonged drug release [20 - 22]. Mixtures of PEG
with anionic surfactants in aqueous solutions are
used for various applications [23]. The solubility
and colloidal properties of PEGylated particles
depend strongly on the polymer molecular mass.
Nanoparticles, oligomers, and low-molecular-
weight compounds are usually covered with
medium-sized polymers, with a mass of 20–50
kg/mol. Larger nanoparticles of sizes 50–100 nm are
usually covered by low molecular weight PEG (3–
10 kg/mol) since a further increase of the
hydrodynamic radius leads to a reduction of the
particle circulation lifetime [24, 25]. Small
nanoparticles can be covered by low-molecular-
weight PEG (1.5–20 kg/mol), leading to an increase
in the lifetime of magnetic nanoparticles introduced
into the body [26, 27]. PEG molecules having a size
in the range of 2–8 kg/mol, at concentrations of 4–8
wt%, are used for the crystallization of proteins and
biological macromolecules. In this process, the
polymer occupies a large volume in the solution,
displacing the protein. This induces the segregation
and subsequent aggregation and formation of a solid
crystalline phase [28].
2 Materials and Methods
We studied SPDS (C15H31SO3Na) manufactured by
VEB Leuna (Germany) and PEGN ([-CH2-CH2-O-
]n) manufactured by "LOBA-Chemie" (Austria)
without preliminary purification.
As known, PEG is a very common food
supplement, used as a thickener in many fields.
Surfactants are surface-active agents having the
unique property to adsorb at the interface. This is
due to the amphiphilic nature of surfactant
monomers. They have a polar head group and a non-
polar hydrophobic tail present in their structure. The
surfactant monomers can aggregate to form
colloidal-sized clusters in solutions, known as
micelles. The formation of micelle occurs over a
sharp range of concentrations of surfactant known
as critical micelle concentration (CMC) due to the
delicate balance between hydrophobic and
hydrophilic interactions. The surfactant monomers
dispersed in a solution below this concentration.
As is well known, viscometry is the leading
method for determining average molecular mass in
industrial applications. As a standalone method, it
delivers values, typically by using an Ubbelohde
capillary viscometer. In industrial applications, the
measurement of [η] provides a quick and easy route
to the Molecules. For viscosity measurements, a
minimum requirement is the knowledge of the
dependence of [η] on (M).
We carried out viscometric studies of solutions
using a modified Ubbelohde viscometer with a
hanging level, which allows the initial solution to be
diluted directly in the viscometer itself; the capillary
diameter was 0.56 mm. All measurements were
carried out at temperature
295 0.01K
. The outflow
time of the solvent-bidi stilled water under these
conditions - was 101.1 sec. The initial concentration
of the studied solutions was ~1.0 g/dl. Before
measurements, both the solvent and the solutions
were filtered with a Schott glass filter No.2. Intrinsic
viscosity was found by double graphical
extrapolation of values and infinite dilution.
The structure and interaction parameters of
micelles in solutions of anionic surfactant PEG in
water were studied by viscometry and light
scattering methods. The effect of the addition of
PEG, on micelle solutions, was investigated. A
change in the power-law type behavior of the
aggregation number on the SO concentration was
observed at 2 wt. percentage of PEG in the
surfactant/polymer mixtures. The screening effect
concerning the micelle interaction took place with
the addition of a large amount of PEG (about 10 wt.
percentage in the mixture).
To study the above systems, light-dispersion
studies were also used. Light scattering
measurements were performed in the light scattering
instrument FPS-3 (constructed by the Central
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Constructional Bureau of Academy of Sciences,
Russian Federation at an incident light length of
=436 nm.) with unpolarized incident 30–1500C with
benzene as reference (IU=48, 5x10-6cm-1). The
refractive index increment (
Cn
) measured in a
Pulfrich differential refractometer in bidi stilled
waterby using a mercury-discharge lamp with blue
light (435, 8 nm), giving dn/dc = 0,109 sm3g-1. To
purify the solvent and solutions, they were
successfully filtered through the glass filtered of
different sizes (No 3-5) thermostated at
K295
.
As is known, the light scattering of polymer
mixture solutions has its characteristics [30-35].
Therefore, we limited ourselves to determining the
apparent mass average micelle masses (
app.
М
),
asymmetry coefficients (
Z
), and second virial
coefficients (A2) of the initial SPDS system and at
the content of various amounts of PEG in the
studied systems with the molecular mass of 40,000,
20,000 and 6,000. Table 1 shows the results of these
studies. Table 1.
Values
app
М
,
2
and
for PEG/surfactant
mixtures of different compositions at different PEG
molecular mass.
Mol.
mass
of
PEG
PEG
PDSN
М,%
М
5
app
М 10
3
4
22
sm
А 10 , g mol
40 000
100
0,28
1,20
1,62
60
0,23
1,16
1,60
40
0,19
1,07
1,41
0
0,15
0,86
1,05
20 000
100
0,14
1,26
1,51
60
0,21
1,24
1,44
40
0,17
1,18
1,21
0
0,15
0,86
1,05
6 000
100
0,07
1, 24
1,21
60
0,18
1,31
1,15
40
0,16
1,20
1,08
0
0,15
0,86
1,05
The mass average molecular mass (
app.
М
) was
determined by both the methods of Zimm and
Debye on the assumption about the shape of the
macromolecules be a Gauss coil. Similar results
were obtained. So, in a further investigation, the less
complex Debye method was applied.
The refractive index increments (
Cn
) of the
studied solutions were determined on a temperature-
controlled Pulfrich IRF-23 refractometer at a
temperature of
295 0.01K
. The error in
determining the refractive indices. The value was
determined as the tangent of the slope of the linear
dependence of the refractive index of the test
solution on the concentration of the dissolved
substance, expressed in g/cm3.
Light scattering studies were carried out on an
FPS-3 photoelectric light scattering device designed
by the Central Design Bureau of the Academy of
Sciences of Russia at an incident light length of
=436 nm. The solvent used was bidistilled water at
a temperature of
295 0.01K
. Benzene was used as a
calibration liquid, for the absolute value of the light
scattering coefficient of which Ju = 48.5 10-6 cm-1
was taken (for incident natural light with a length of
=436 nm. In light-dispersion studies, solutions and
solvents were purified by successive filtration
through porous glass filters of various numbers (3–
5) directly into a cuvette, which was pre-rinsed with
the first portions of the filtrate. The samples studied
by the light scattering method were transparent
micellar solutions. It should note that the filtration
of solutions, as well as work with them, required the
development of a certain technique, since an
aqueous solution of amphiphilic foams strongly
during manipulations with the solution.
3 Results and Discussion
It is widely accepted [29, 30] that the viscosity of
solutions is the measure of interaction between
polymers and surfactants, and the formation of
complexes between them. In this work, the
influence of polyethylene glycols with a different
molecular mass on the hydrodynamic behavior of
aqueous solutions of SPDS is studied by the
viscometry method.
Fig.1 shows the dependence of intrinsic viscosity
(
[]
) of SPDS-water one-micelle systems on the
PEG content in the system. On the same graph,
dotted lines are drawn between the values of the
initial surfactant solution and pure PEG in water. It
would correspond to the dependence on the
composition of the mixture with non-interacting
components of the mixture (it is assumed that the
total viscosity of the mixture is the additive sum of
the viscosity of the components).
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Fig.1: Dependence
[]
of micellar solutions of
SPDS/water on the content in the PEG system with
the following molecular masses: 1-2000, 2-4000, 3-
6000, 4-20000, 5-40000.
As can be seen from the data presented (Fig.1),
for PEGs with molecular masses of 2000 and 40000,
linear dependences of intrinsic viscosities on the
PEG/SPDS ratios are observed, indicating the
absence of interactions between the components of
the systems. Obviously, with an increase in the
molecular weight of the polymer, after a certain
value, due to the deterioration of the solubility of the
polymer, macromolecules and free micelles coexist
in the system, which does not interact with each
other. At very low values of the molecular weight of
the polymer, we do not exclude the interaction of
macromolecules with micelles, but it is obvious that
when small macromolecules aggregated on micelles,
the shape and size at 40% content in the mixture of
PEG. After this interval, growth was observed with
increasing polymer concentration in the mixture. A
negative deviation from the additive value, and even
more so, the presence of a minimum in the
dependence on the PEG content in the system
indicates the presence of an interaction between the
components of the systems.
Let us try to explain the observed picture. It
кnown that the interaction of a polymer with a
surfactant reduces the hydration shell of the latter.
In particular, in the works of Varshavsky et al., X-
ray diffraction proved that PEG has a pronounced
water-binding property [36]. A decrease in the
hydration shell of micelles entails the compaction of
the latter and, accordingly, a negative deviation
from the additive value.
Obviously, at lower PEG contents, the system
contains free micelles and polymer coils. At certain
polymer concentrations, only mixed aggregates exist
in the system, polydisperse in terms of surfactant
content. At high polymer concentrations, mixed
aggregates and free polymer coils are present in the
mixture. It can be assumed that with a change in the
PEG concentration in the system, micelles are
compacted due to a change in the balance of
hydrophobic–hydrophilic interactions, because of
which the above pattern of changes in the
composition of the mixture is observed.
The same picture was established in a
photoluminescence study of the interaction of
sodium dodecyl sulfonate with water-soluble
polymers (poly-N-vinylpyrrolidone, polyethylene
oxide) [24]. It concluded that micelles of sodium
dodecyl sulfonate bind to polymers, and the sizes of
micelles become smaller than in the absence of the
polymer [24].
The refractive index increments (
Cn
) of the
studied solutions were determined on a temperature-
controlled Pulfrich IRF-23 refractometer at a
temperature of
295 0.1K
. The error in determining
the refractive indices
5
105
. The value was
determined as the tangent of the slope of the linear
dependence of the refractive index of the test
solution on the concentration of the dissolved
substance, expressed in g/cm3.
The solvent used was bidistilled water at a
temperature
295 0.1K
. Benzene was used as a
calibration liquid, for the absolute value of the light
scattering coefficient of which Ju = 48.5 10-6 cm-1
was taken (for incident natural light with a length of
= 436 nm.). In light-dispersion studies, solutions
and solvents purified by successive filtration
through porous glass filters of various numbers
(3–5) directly into a cuvette, which was pre-rinsed
with the first portions of the filtrate. The samples
studied by the light scattering method were
transparent micellar solutions. It should be noted
that the filtration of solutions, as well as work with
them, required the development of a certain
technique, since an aqueous solution of amphiphile
foams strongly during manipulations with the
solution.
Noteworthy is the pattern of change in
app
М
Z
,
and
2
А
, which in general show a symbatic course
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with the pattern of change
[]
depending on the
composition of the mixture. Comparison of the
results of light-dispersion studies showed that, at a
content of ~0.35% PEG in the system, the micelles
of an aqueous solution of surfactant are maximally
compacted.
4 Conclusion
Thus, the study of the effect of PEGs with different
molecular masses on the structural transformations
of aqueous solutions of PDSN depending on the
polymer content in the system showed that PEGs
with molecular masses of 2 000 and 40 000 have
absolutely no effect on the structure of the system.
For PEGs with molecular masses of 4 000, 6 000,
and 20 000, a complex character of the dependence
of the intrinsic viscosity of the micellar system on
the polymer content in it was established. It
assumed that with a change in the concentration of
PEG in the system, micelles are compacted due to a
change in the balance of hydrophilic-hydrophobic
interactions. The practical application of this
research is that it allows the performance properties
of sodium pentadecyl sulfonate (SPDS) to be
adjusted, thereby expanding and improving its
applications. Naturally, with further research of this
system, other additives will be tested to improve the
performance properties of the studied polymer. This
study is experimental. It is significantly more
expensive than theoretical ones and usually allows
you to obtain specific and reliable information in a
fairly short time. In the future, similar studies are
expected on other polymer objects to improve their
performance properties. For almost 50 years, our
laboratory has conducted similar research
experiments and collected data from the results
obtained. This method can be combined with
artificial intelligence by processing this data and
applying an appropriate machine learning model.
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International Journal of Chemical Engineering and Materials
DOI: 10.37394/232031.2023.2.8
Vigen Barkhudaryan
E-ISSN: 2945-0519
61
Volume 2, 2023
