DOI: 10.

7251/JEPM2002044H Journal of
UDC: 66.061.085:546.799.4 Engineering & Processing
Management

REVIEW PAPER

Cloud Point Extraction as a Method for Preconcentration of Metal

Ions
Nusreta Hasić1 | Emir Horozić2

1
Faculty of Natural Sciences, University
of Tuzla, Univerzitetska 4, 75000
Abstract
Tuzla, Bosnia and Herzegovina Cloud point extraction (CPE) is an attractive technique that reduces solvent con-
2
Faculty of Technology, University of sumption and exposure, disposal costs, and process time. This method has an im-
Tuzla, Univerzitetska 8, 75000 Tuzla, portant practical application and is used to separate and concentrate the analyte as
Bosnia and Herzegovina a step before its determination, and after the formation of a poorly water-soluble
complex. Use of nonionic surfactants as ”green solvents” which represent an effec-
Correspondence tive alternative to toxic organic solvents (in classical extraction), along with other
N. Hasić advantages, such as low cost and low flammability, makes this method attractive
Email: and worth further research and optimization. This paper presents a detailed de-
nusreta.suljkanovic@yahoo.com scription of the principles, procedure, advantages, disadvantages and application
of CPE.

Keywords: Cloud point, surfactant-rich phase, nonionic surfactants, metal extrac-

tion, ”green” method.

1. INTRODUCTION
Cloud point extraction (CPE) is a unique extraction
method that provides economical sample preparation
with high extraction efficiency. In this method, the sepa-
ration of the two phases is based on the aggregation be-
havior of the surfactant in aqueous solution, which de-
pends primarily on the temperature and then on the con-
centration of the surfactant (Hagarová, Kubová, Matúš,
& Bujdoš 2008). If a solution in which the surfactant
concentration is above the critical micellar concentration
(CMC) is heated to a certain temperature (cloud point
temperature, TC P E ), then the surfactant molecules form
micelles that create an additional phase, which is man-
Figure 1. Separate phases in CPE.
ifested by turbidity of the solution, i.e. a cloud point
is reached (Shokrollahi & Ahmadi 2017). This phase is
called the surfactant-rich phase because it contains most
of the surfactant, is heavier than the aqueous phase, and while polar substances and ions will remain in the aque-
therefore separates the phases as shown in Figure 1. ous phase (Reffas, Benabdallah, Youcef, & Ilikti 2010).
Unlike the surfactant-rich phase, the diluted aque- In this way, CPE using non-ionic surfactants attracts sig-
ous phase contains a low concentration of the surfac- nificant attention as an alternative to conventional ex-
tant corresponding to the critical micellar concentration traction processes for separation and preconcentration
(CMC) (Haddou, Canselier, & Gourdon 2014). Non-polar of substances(Shokrollahi, Joybar, Haghighi, Niknam, &
molecules can enter the micelles and thus be co-extracted, Niknam 2013).

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Cloud Point Extraction as a Method for Preconcentration … Hasić & Horozić 45

2. CLOUD POINT the turbidity of pure nonionic surfactant from the alkyl
The cloud point is the temperature at which the surfactant ethoxylate class. For a set of 62 structures composed of
solution, whose concentration is close to or above its crit- linear alkyl, branched alkyl, cyclic alkyl and alkyl ethoxy-
ical micellar concentration (CMC), becomes cloudy and late chains, the cloud point can be estimated with an
separates into two phases (Bader, Edbey, & Telghederb accuracy of + 6.38 ◦ C using the logarithm of the num-
2014). Under these conditions, the micelles aggregate ber of ethylene oxide residues. At lower temperatures,
to form a turbid phase with a high concentration of sur- the molecules of each nonionic surfactant form hydro-
factant that separates from the aqueous phase (Arnold & gen bonds with the water layer using their polar groups
Linke 2007). The term cloud point refers to the disper- (polar heads) and polyoxyethylene units (Shokrollahi &
sion of light created by the formation of a colloidal sys- Refahi 2019). When the temperature increases, there is
tem, the so-called Tyndall effect. The Tyndall effect is an increase in entropy, which causes dehydration of the
the name for the scattering of light on colloidal particles polyoxyethylene chains and destroys the layer of water
(Kraemer & Dexter 2002). Rays of light, colliding with molecules. From this point, Van der Waals forces weaken
colloidal particles, are reflected in all directions. If a nar- between the molecules, which makes an important con-
row beam of light is passed through a colloidal solution tribution to the micellar formation of agglomerates, and,
and the solution is observed perpendicular to that beam, consequently, the separation of the solution phases occurs
the light in the solution appears to be cloudy (Heidorn (Kori 2019). The cloud point can be changed by the ad-
2006). The turbid portion of the surfactant solution, also dition of electrolytes, the presence of alcohol, other sur-
called the surfactant rich phase, may be present as the up- factants, polymers and some organic and inorganic com-
per or lower phase of the solution, as shown in Figure 2 pounds that can cause an increase or decrease in the cloud
(Garavito & Ferguson-Miller 2001). point temperature. These effects are known as ”salting-
out” (Bezerra, Arruda, & Ferreira 2005).

3. PHASE SEPARATION MECHANISM

The cloud point phenomenon occurs when a solution
containing nonionic or zwitterionic surfactants, i.e. sur-
factants, by heating to the appropriate temperature, di-
vide or separate into two phases (Jamali, Gholinezhad,
Balarostaghi, Rahnama, & Rahimi 2013). The concentra-
tion of surfactants in the solution must be above their crit-
Figure 2. Position of the surfactant solution phases at the
ical micellar concentration (CMC) in order for micelles to
cloud point. form or later to separate the phases (El-Naggar, Lasheen,
Nouh, & Ghonaim 2010). Anionic surfactants can also
The most experimentally modified condition to reach be used to preconcentrate metal ions by the CPE method.
the cloud point is temperature. The temperature at which This type of surfactant requires the presence of a high con-
the phase separation occurs is a function of the surfactant centration of acids to reach its cloud point (Casero, Sicilia,
concentration (Muslim 2015). Some empirical links be- Rubio, & Perez-Bendito 1999). The cloud point extraction
tween surfactants and their cloud points can be found in methodology used to remove metal ions from the solution
several published papers. In their work, scientists Gu and consists of several basic steps. The first step is the ad-
Sjöblom (1992) showed that there is a linear relationship dition of a suitable surfactant in a certain concentration,
between the cloud point and the logarithm of the number which exceeds its CMC, to an aqueous solution containing
of oxyethylene units for surfactants, such as alkyl oxyethyl metal ions (Moghimi 2008). If the addition of a particular
ethers, as well as a linear relationship between the cloud chelating ligand is required, it can be initially dissolved in
point and the number of carbon atoms in the hydrophobic an organic solvent or directly in water, depending on the
chain. Further, Schott (2003) also determined a linear re- solubility. The next step is to heat the prepared extrac-
lationship between the cloud point of water-soluble poly- tion solution above its cloud point. Surfactant rich phase
oxyethylated nonionic surfactants with the average num- and aqueous phase occur. The phase separation process is
ber of oxyethylene units per molecule. The cloud point performed by centrifugation (Figure 3) (Sheikh, Gouda,
of polydispersed surfactants may be related to their hy- Mostafa, & El Din 2015).
drophilic and lipophilic balance (Materna, Cote, & Szy- In some cases, prior to the separation process itself,
manowski 2004). Huibers, Shah, and Katritzky (1997) it may be necessary to add a small amount of a separat-
developed a general empirical connection for estimating ing agent such as salts or alcohols. The content of the

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46 Hasić & Horozić Cloud Point Extraction as a Method for Preconcentration …

is a fast process, from 2 to 5 minutes (Järup 2003). Per-

forming such fast extraction, with high efficiency and a
temperature of 20-25 ◦ C, contributes to increasing the use
of the CPE method (Maniasso 2001; Pramauro & Prevot
1995).

4. METAL EXTRACTION MECHANISM

Figure 3. Cloud point extraction A - Low concentration metal Above the cloud point, the surfactant molecules act as or-
ion solution; B - Metal chelates formed by the addition of a ganic solvents in the liquid-liquid extraction where the
complexing reagent; C - Addition of surfactant and binding of metals are distributed between the organic and aqueous
metal chelates to the interior of the micelle; D - Phase phases (Ojeda & Rojas 2009). The efficiency of CPE de-
separation after heating and centrifugation.
pends on the inherent interactions of metallic species with
micellar structures. The following factors must be taken
release agent must be a compromise between the ideal into account during CPE:
viscosity and the metal concentration (Stalikas 2002). As a) Constant formation of metal complexes
previously mentioned, two isotropic phases are formed
during CPE. The first phase is called the surfactant rich b) Kinetics of complexation reactions
phase and it contains the separated analyte, i.e the metal
c) Phases of transfer of metal species or chelates to mi-
ions ”trapped” inside the surfactant micelle (Yang, Jia,
cellar media
Yang, Li, & Liao 2017). For the most part after separa-
tion it forms a second phase called the aqueous phase. It It is interesting that there are distribution constants of
is important to note that only the nonionic or zwitterionic different metal chelates related to each extracted metal
surfactants that form colloidal micelles are used in CPE species. Due to the hydrated nature of the surfac-
(Yamini, Feizi, & Moradi 2020). The following nonionic tant phase, the distribution coefficients are generally
surfactants of the polyoxyethylene type are most com- lower than presented observing the conventional liquid-
monly used in the CPE method: liquid extraction method (Abbas, Madrakian, & Siampour
2006). In this extraction the constant distributions are al-
• Triton X-100 (TC P E = 69 ◦ C) ways independent of the nature of the metal ion. These
• Triton X-114 (TC P E = 25 ◦ C) facts indicate that the mechanism of distribution in CPE
differs from that in the conventional extraction method.
• Brij 30 (TC P E = 2 ◦ C) In addition, in CPE, the mechanism of chelate distribu-
tion differs from chelation (Farajzadeh & Fallahi 2006).
• Brij 35 (TC P E > 100 ◦ C)
Chelating reagents likely extracted due to specific in-
• Brij 56 (TC P E = 69 ◦ C) teractions, such as hydrogen bonds between functional
groups on chelating reagents and ether oxygen or the ter-
• Brij 97 (TC P E = 72 ◦ C) minal OH- group of a nonionic surfactant and chelate,
were extracted into the hydrophobic portion of the aggre-
• Tween 80 (nonionic surfactant based on sorbitol
gated micelles (Akita & Takeuchi 1999; Tani, Kamidate,
structures) (TC P E = 65 ◦ C) (Douglas 2016)
& Watanabe 1997).
The cloud point (TC P E ) depends on the surfactant Another aspect related to the extraction efficiency
used and covers a wide temperature range, as mentioned is the ionic strength. Its increase does not significantly
above. Nonionic surfactants generally have a lower TC P E change the extraction efficiency, and the addition of salt
than zwitterionic surfactants (Yuan, Jiang, Cai, He, & Liu makes the phase separation process easier. The degree of
2004). This temperature can vary depending on the sur- metal partition from aqueous solution to the surfactant-
factant concentration and dilution of the solution, espe- rich phase during CPE can be described by a typical dis-
cially the addition of salt. The division of the solution tribution coefficient D:
into two phases during CPE is primarily guided by hy-
drophobic interactions, i.e. Van der Waals forces, dipole- C M )s
D= (1)
dipole, and hydrogen bonds that have separate roles and (C M )w
side effects (Anastas 1999). Similar effects have been ob- where (C M )s represents the final metal concentration
served with liquid-liquid extraction in non-polar solvents. in the surfactant-rich phase, and (C M )w is its concentra-
Extraction kinetics and achieving equilibrium separation tion in the aqueous phase after the separation process.

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Cloud Point Extraction as a Method for Preconcentration … Hasić & Horozić 47

The extraction factor (E) is given by the following expres- performed. The CPE involves only a few manual steps
sion: and uses standard equipment and glassware that can be
 ‹ found in most laboratories, namely pipettes, flasks, hot-
Vs plates and centrifuges (Mohd, Zain, Raoov, & Mohamad
E=D (2)
Vw 2018). Therefore, no specialized measuring or extrac-
where Vs /Vw is the phase volume ratio, i.e. the vol- tion devices are required. Surfactants are quite cheap and
ume of the surfactant-rich phase (Vs ) divided by the vol- have low flammability (Yamini & Ghambarian 2012). As
ume of the aqueous phase (Vw ) after the phase separation already mentioned, quantitative yields are obtained in a
step. short time and several samples can be processed at once.
At the same time, there are some other limiting factors
The fraction of the extracted analyte p is given by the
to consider (Rahnama, Eram, & Jamali 2014). The sur-
expression:
factants used can cause analytical interference and affect
D the limits of detection, especially if the analyte cannot be
p= (3) effectively isolated from the surfactant, depending on the
D + (Vw /Vs )
analysis. The extraction efficiency decreases with increas-
ing polarity of the solution and with extremely volatile or
5. ADVANTAGES AND DISADVANTAGES OF CPE thermally unstable compounds (Douglas 2016).
The use of micellar systems, in methods such as CPE, has
attracted considerable attention in recent years mainly be- 6. CPE APPLICATION
cause it is in line with the principles of ”green chemistry“ In recent years, Cloud point extraction (CPE) has be-
(Rasoolzadeh, Hashemi, & Serenjeh 2017). Green chem- come widely utilized for separation and preconcentration
istry can be defined as a set of procedures to reduce or
of trace metals (Hagarová & Urik 2006). The metal may
eliminate the use or generation of toxic substances for hu- be in ionic form or in the form of hydrophobic chelates
man health and the environment (Hussain & Keçili 2020).
which are formed in certain reactions under suitable con-
CPE is a ”green” method due to the fact that, as an ex- ditions. Thorough optimization of chemical and oper-
tractor, it uses dilute solutions of surfactants that are less
ational parameters of this method provides quantitative
toxic than classical organic solvents used in liquid-liquid separation and high efficiency of preconcentration in the
extraction. The relatively low prices of surfactants and determination of metal ions (Bezerra et al. 2005). The
the stability of their solutions should not be overlooked as use of CPE is primarily directed at metal ions and other
some of the other advantages of their application (Casero hydrophilic compounds, however significant attention has
et al. 1999). The small volume of surfactant-rich phase
been paid to small organic molecules. Priority is given
obtained by this approach allows the design of extrac- to the removal of pollutants from water using CPE, as
tion strategies that are simple, inexpensive and highly ef-
well as the extraction from solid and biological samples
ficient compared to classical extraction methods (Filik & (Pocurull, Fontanals, Calull, & Aguilar 2020). In addi-
Çekiç 2011). Another advantage of CPE over traditional tion to metal ions, this includes phthalates, polycyclic aro-
extraction processes is the high preconcentration factor matic hydrocarbons, polychlorinated biphenyls, polychlo-
that can be obtained starting from small initial sample rinated dibenzodioxins and dibenzofurans, chlorophenol
volumes (Arya, Kaimal, Chib, Sonawane, & Show 2019).
and organochlorine pesticides (Kachangoon, Vichapong,
Traditional extraction techniques often require an addi- Burakham, Santaladchaiyakit, & Srijaranai 2018). CPE
tional step of re-extracting the metal ion solution result-
applications in drug-related studies are of interest. Some
ing in a larger final volume of the solution, so that achiev- of the extracted drugs are benzodiazepines, lorazepam,
ing a high preconcentration factor uses a larger sample alprazolam, followed by preconcentration of β -lactam an-
volume (Kojro & Wroczyński 2020). Therefore, CPE is a tibiotics as well as countless studies to determine the ac-
good extraction method for concentrating a wide range of tive compounds in Chinese herbs (Douglas 2016).
metals with quantitative recovery and high preconcentra-
tion factor. This makes it possible to achieve an identical
preconcentration factor to that in other techniques with- 7. CONCLUSION
out the additional re-extraction step (Bezerra et al. 2005). The cloud point extraction methodology offers a simple,
The main limitation of CPE is the relatively low partition fast, inexpensive process and, unlike other preconcentra-
coefficient of several types of metals with some chelates. tion techniques, does not pollute the environment. All
However, this can be circumvented by the use of highly of the above contributes to the popularization of research
hydrophobic ligands (Quina & Hinze 1999). Another ad- and application of the CPE method as an alternative to
vantage of Cloud point extraction (CPE) is the way it is conventional extraction methods.

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48 Hasić & Horozić Cloud Point Extraction as a Method for Preconcentration …

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