Mixed Micelles of Triton X‐100 and Sodium Dodecyl Sulfate and Their Interaction with Polymers

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Mixed Micelles of Triton X‐100 and Sodium DodecylSulfate and Their Interaction with PolymersRakesh Sharma a , Dharmesh Varade a & Pratap Bahadur aa Department of Chemistry, South Gujarat University, Surat, 395007, IndiaPublished online: 06 Feb 2007.

To cite this article: Rakesh Sharma , Dharmesh Varade & Pratap Bahadur (2003) Mixed Micelles of Triton X‐100 and SodiumDodecyl Sulfate and Their Interaction with Polymers, Journal of Dispersion Science and Technology, 24:1, 53-61, DOI:10.1081/DIS-120017943

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Mixed Micelles of Triton X-100 and Sodium

Dodecyl Sulfate and Their Interactionwith Polymers

Rakesh Sharma,* Dharmesh Varade, and Pratap Bahadur

Department of Chemistry, South Gujarat University, Surat, India

ABSTRACT

Micellization of polyoxyethylene tert-octylphenyl ether, Triton X-100 [TX-100], and sodium

dodecyl sulfate [SDS] and their mixtures at varying mole fraction was investigated by surface

tension measurements at 30�C. Changes in the critical micelle concentration (CMC) with the

composition of the two surfactants so determined were analyzed by applying the Rubingh’s

regular solution theory to obtain interaction parameter, b (¼�3.81) showing synergism.

Sodium dodecyl sulfate shows a remarkable interaction with polyethylene oxide [PEO, mol.

wt.¼ 6000] and polyethylene oxide–polypropylene oxide–polyethylene oxide block copolymer

[P65: EO19PO30EO19, total mol. wt.¼ 3400, % EO¼ 50], while no such interaction was

observed for TX-100. Interaction weakens in mixed micelle and diminishes when the mole

fraction of TX-100 in mixed system increases. Turbidimetric studies show that the presence of

TX-100 in SDS improves calcium ion tolerance.

INTRODUCTION

Surfactants are widely used in numerous technical

applications such as detergents, cosmetics, pharmaceuti-

cals, textile auxiliaries etc. Mixed surfactant systems are

more versatile than single surfactant and have been exten-

sively examined in past two decades.[1–3] The superiority in

performance of mixtures of surfactants is attributed to the

synergistic interaction. Both critical micelle concentration

(CMC) and distribution of surfactant between the micellar

and aqueous phases play an important role in describing the

behavior of such binary surfactant systems. As a result of

their widespread use in different industries, research on

mixtures of surfactants has stimulated the interest of

researchers, and in recent years many papers have been

published for various mixed surfactant systems.[4–15]

Often mixed systems comprising nonionic and anio-

nic surfactants are used in order to achieve a higher

surface activity and hence an improved performance.

Such mixtures show strong deviations from ideality[16]

and the CMCs are considerably lower than those

predicted from ideal mixing theory. Often negative

*Correspondence: Rakesh Sharma, Department of Chemistry, South Gujarat University, Surat, 395007, India.

DOI: 10.1081=DIS-120017943 0193-2691 (Print); 1532-2351 (Online)Copyright # 2003 by Marcel Dekker, Inc. www.dekker.com

53

JOURNAL OF DISPERSION SCIENCE AND TECHNOLOGYVol. 24, No. 1, pp. 53–61, 2003

©2002 Marcel Dekker, Inc. All rights reserved. This material may not be used or reproduced in any form without the express written permission of Marcel Dekker, Inc.

MARCEL DEKKER, INC. • 270 MADISON AVENUE • NEW YORK, NY 10016

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interaction parameter, b, calculated by applying the

nonideal mixed micelle theory developed by Rubingh[17]

has been used to explain the synergism. Furthermore, it is

also of interest to investigate the interaction of water-

soluble polymers with surfactants. Polymers are added to

achieve different effects such as rheology control, surface

modification and adsorption.[18] The interactions between

nonionic hydrophilic polymers and ionic surfactants have

been studied extensively.[19,20] Anionic surfactants form

complexes with neutral water-soluble polymers, which

render the formation of micelles at much lower surfactant

concentration compared to the corresponding single

surfactant system. On the other hand nonionic surfactants

often do not interact with neutral water-soluble

polymer.[18]

While the literature abounds with studies on the

interaction between anionic surfactants and neutral poly-

mers,[21–24] there is not much reported on mixed micelles

of anionic and nonionic surfactants in presence of

uncharged polymers.[25,26] Bakshi[27,28] have examined

the interaction between cationic mixed micelles with

water soluble polymers using conductance measure-

ments. In this paper we investigate properties of aqueous

solutions of a binary surfactant mixture consisting of

Triton X-100 (TX-100) and sodium dodecyl sulfate

(SDS) by surface tension measurements. To examine

how the micelle surface charge influences the inter-

action of surfactant with polymers, we have used

TX-100þ SDS systems at varying mole ratio for study-

ing interaction with water-soluble polymers polyethylene

oxide [PEO, mol. wt.¼ 6000] and polyethylene oxide–

polypropylene oxide–polyethylene oxide triblock copoly-

mer [Pluronic P65: EO19PO30EO19, mol. wt.¼ 3500].

Clouding behavior of TX-100 in the presence of SDS has

been studied before[29] where a drastic increase in cloud

point of TX-100 was observed in the presence of little

amount of SDS (at concentration less than CMC). The

increase in cloud point may be attributed to the insertion

of the surfactant monomer into the TX-100 micelle and

modifying the surface charge density leading to inter-

micelle repulsion.

EXPERIMENTAL

Anionic surfactant, SDS was from Sigma (USA) and

used as supplied. Nonionic surfactant, polyoxyethylene

tert-octylphenyl ether, TX-100 was supplied by Fluka.

These surfactants did not show any minimum in surface

tension–concentration plot and provided a well-defined

break point at CMC values (Table 1). The weakly surface

active polymer, polyethylene oxide [PEO, mol.

wt.¼ 6000] and polyethylene oxide–polypropylene

oxide–polyethylene oxide triblock copolymer, Pluronic1

P65, EO19PO30EO19, (BASF Corp., Mount Olive, NJ)

were used as received.

Triple distilled water (surface tension¼ 71.8 mNm�1

at 30�C) from an all PYREXTM glass apparatus was used

for the preparation of solutions.

Surface tension was measured using drop weight

method at 30� 0.1�C. Surface tension measurements had

an accuracy of �0.1%.

The turbidity of the solution was measured with an

Erma colorimeter, Japan with a filter 660 mm, at ambient

temperature (30� 0.2�C) by mixing the solutions of

anionic=nonionic surfactant and CaCl2 with vigorous

stirring at regular intervals.

RESULTS AND DISCUSSION

Theory of Mixed Micelles

Surface tension at different total surfactant concen-

trations for aqueous solutions of single and mixed

surfactant systems at different mole fractions was mea-

sured to obtain CMC.

According to Rubingh’s regular solution theory

for mixed micelles,[17] the mixed CMC (C12) for

TX-100þ SDS system obtained by mixing two surfac-

tants is given by Eq. (1),

1

C12

¼a1

f1C1

þ1 � a1

f2C2

ð1Þ

Table 1. CMC12, mole fraction of TX-100 in mixed micelle (X1), interaction parameter (b) and averageparameter (bav) for nonionic–anionic surfactant systems at 30�C.

Mole fraction a (TX-100) CMC12 (mM) Ideal value (mM) X1 b bav

1.0 0.38 — — —

0.8 0.38 0.47 0.8090 �3.97

0.5 0.42 0.72 0.7381 �3.97 �3.81

0.2 0.72 1.59 0.6325 �4.22

0.1 1.30 2.66 0.5843 �3.10

0.0 8.00 — — —

54 Sharma, Varade, and Bahadur



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where a1 is the mole fraction of surfactant 1 in the total

mixed solution and f1 and f2 are the activity coefficients

of surfactant 1 and 2 in mixed micelle. C1 and C2 are the

CMCs of the single surfactants 1 and 2, respectively.

In the case of ideal behavior, f1¼ f2¼ 1 and hence

Eq. (1) reduces to the form:

1

C12

¼a1

C1

þ1 � a1

C2

ð2Þ

as proposed by Clint[30] for ideal mixed micelles.

The nature and strength of the interactions between

the two surfactants in a mixed system are determined by

calculating the values of the b parameter (a measure of

these interactions), using the CMCs obtained from surface

tension (g) to log concentration (log C ) plots of aqueous

solutions of the individual surfactants and their mixtures.

By considering the phase separation model for micelliza-

tion, Rubingh[17] derived the relationship shown in Eq. (3)

ðX1Þ2 ln½ða1C12=X1C1Þ

ð1 � X1Þ2 ln½ð1 � a1ÞC12=ð1 � X1ÞC2

¼ 1 ð3Þ

where X1 is the mole fraction of surfactant 1 in the mixed

micelle. Equation (3) was solved iteratively to obtain the

value of X1, from which the interaction parameter b was

evaluated using the relationship [Eq. (4)]

b ¼lnða1C12=X1C1Þ

ð1 � X1Þ2

ð4Þ

The value of b is a measure of extent of interaction

between the surfactants resulting in their deviation from

the ideal behavior, with negative values indicating syner-

gism and positive values antagonism.

Mixed Micelles of Triton X-100þ

Sodium Dodecyl Sulfate

Generally, anionic surfactants possess higher CMCs

than nonionic surfactants. This is because for nonionic

surfactants, aggregation is mainly due to hydrophobic

interaction among hydrocarbon chains. This is more

feasible because the hydrophobic groups are easily sepa-

rated from the aqueous environment, whereas for ionic

surfactants, high concentrations are necessary to over-

come the electrostatic repulsion between ionic head

groups during aggregation.

Figure 1 shows a typical plot of surface tension vs.

log surfactant concentration for different mole fraction of

TX-100þ SDS mixture. The data obtained from the

Figure 1. Plots of surface tension (g) vs. log concentration (C ) for the TX-100þ SDS system in water for different mole fractions

(X1) of TX-100. Key: þ , 1.0; ., 0.8; u, 0.5; j, 0.2; m, 0.1; , 0.

Mixed Micelles of Triton X-100 and SDS 55



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surface tension measurements are reported in Table 1.

The measured CMCs of SDS and TX-100 agree well

with literature values.[31] Figure 2 shows the variation of

CMC obtained experimentally as a function of the mole

fraction of the TX-100. The decrease in CMC of mixed

system with increase in mole fraction of TX-100 indi-

cates synergism. A tenfold decrease in the CMC of SDS

was registered when the mole fraction of TX-100 was as

low as 0.2, where the synergistic effect was most.

However, the CMC of mixed system at any composition

could not be reduced more than that of pure TX-100. It is

also clear from this figure that experimental mixed CMC

values are always lower than the ideal CMCs. A similar

behavior was observed for nonylphenol with different

degree of ethoxylation.[32]

The calculated values of the mole fraction of surfac-

tants in the mixed micelle (X1) at four different mole

fractions in the bulk (a) are recorded in Table 1. The plot

between X1 and a is shown in Fig. 3. The X1 and a remain

almost same for mixed systems with mole fraction 0.8

but the micelles are rich in TX-100 when the mole

fraction of SDS in bulk is 0.5 or even more. A marked

variation from the dotted line (depicting the ideal beha-

vior) can be clearly seen.

The calculated Rubingh’s interaction parameter

b values for the four mole fractions are recorded in

Table 1. These values are essentially same for all the four

mole fractions showing the validity of Rubingh’s solution

theory. The average b value so calculated was �3.81. For

mixtures of a ionic and a nonionic surfactant the average b

values are considerably smaller and fall in the range

�5< b<�1. Such negative value of interaction para-

meter, b, for nonionic and ionic surfactant has been

observed before.[1,33] This negative deviation from ideality

indicates certain attractive interaction between the two

surfactants forming the mixed system. First, the nonionic

component shields the repulsion between the negatively

charged head groups of the anionic surfactants in the

micelle and second, there is an attractive contribution

due to ion–dipole interaction.

Nonideal CMCs calculated using average b value

(�3.81) are more or less identical to experimental CMCs

(Fig. 2) which explains the validity of Rubingh’s regular

solution theory.

Interaction of Polymers with

Mixed Micelle

Surface tension measurements on aqueous solution

of TX-100þ SDS mixed systems at varying total con-

centrations in the presence of polymers viz. PEO and

PEO=PPO=PEO triblock copolymer (Pluronic P65) at

fixed concentration were made to study the interaction

between polymers and mixed surfactant system. For

comparison similar studies were also made on single

surfactant (SDS as well as TX-100).

Figure 4 shows the surface-active behavior of

TX-100 as a function of log concentration in the absence

and presence of PEO (0.1 wt.%) and P65 (0.01 and

0.1 wt.%). Surface tensions were also measured for aqu-

Figure 2. Variation of CMC with mole fraction (a) of

surfactant TX-100 in TX-100þ SDS system. Key: - - - -,

ideal value; ——, nonideal value; , experimental value.

Figure 3. Plot of mole fraction of TX-100 in mixed micelle

(X1) vs. mole fraction in bulk (a). Key: - - - -, ideal value;

, experimental value.




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eous solutions of polymers at different concentration in

the absence of TX-100 (data are shown in the same

figure). Polyethylene oxide solutions in water do not

show any significant decrease in surface tension indicating

its weakly surface active nature. Compared to PEO,

copolymer P65 is sufficiently surface active and reduces

the surface tension of water even at low concentrations.

Surface activity of P65 has been shown by us before,[34]

however, the copolymer does not micellize at 30�C up to

the concentration studied in this work.

For TX-100, the micellization is recalled by break in

the surface tension vs. log surfactant concentration plot

providing a CMC value 0.38 mM that agrees with litera-

ture data.[31] In the presence of polymer a single break

point could be observed in the surface tension–log

concentration plot (the slightly lower surface tension at

low surfactant concentrations is due to presence of

polymer) without any significant decrease in CMC of

TX-100. It can thus be inferred from these results that

TX-100 does not form complex with these polymers.

Very hydrophilic low molecular weight polymers gener-

ally do not show strong binding with nonionic[26] as well

as with cationic surfactants.[35]

In Fig. 5 is shown surface tension behavior of SDS

as a function of log concentration with=without added

0.1 wt.% PEO. A well-defined break point for SDS in

water indicating a CMC of 8 mM is well known. Surface

tension (g) vs. log concentration plots for SDS–PEO

system is similar to those observed by Schwuger,[36]

for SDS–PEO system, Schwuger and Lange,[37] and

Arai et al.[38] for PVP–SDS system where strong poly-

mer–surfactant interactions have been reported. As seen

in figure the variation of surface tension decreases into

three regions and provide the critical aggregation con-

centration (CAC) value 4 mM. In Fig. 6 is shown surface

tension (g) vs. log concentration of SDS plot at 30�C in

the absence and presence of P65 (0.01 and 0.1 wt.%). A

direct evidence of strong interaction between SDS and

P65 can be immediately noticed from the figure, which

Figure 4. (i) Surface active behavior of TX-100 in the

presence of different water-soluble polymers. (ii) Surface active

behavior of water soluble polymers in water. Key: , Blank;

m, 0.1 wt.% PEO¼ 6000; X, 0.01 wt.% P65; ., 0.1 wt.%P65;

j, PEO¼ 6000; u, P65.

Figure 5. Surface activity of SDS in the absence and presence

of polyethylene oxide (PEO 6000). Key: , Blank; u, 0.1 wt.%

PEO.

Figure 6. Surface activity of SDS in the absence and presence

of copolymer P65. Key: , Blank; m, 0.01 wt.% P65;

u, 0.1 wt.% P65.




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shows a break point at SDS concentration well below the

CMC of SDS. In the presence of interacting polymers,

two breaks in the surface tension vs. concentration plots

often detected: the first one at Csurf¼C1<CMC, is the

CAC, generally considered the onset of the binding of

surfactant onto the copolymer[39] the second one, at

Csurf¼C2<CMC, is assumed[40] to correspond to the

polymer saturation concentration (PSP) by surfactant. In

the copolymer P65þ SDS system, when the solution of

copolymer contains sufficiently low concentration of

SDS such that a critical level is not exceeded (below

CAC), most of the surfactant molecules apparently exist

freely in the solution. When SDS concentration exceeds

the CAC, complex formation occurs over a broad surfac-

tant concentration range in which a substantial amount of

surfactant is bound in the form of aggregates to the

copolymer chain, although a part of surfactant will still

be present in the free form. Beyond PSP at which the

copolymer has been completely saturated with surfactant

aggregates, the concentration of free micelles increases in

the bulk solution. The PSP obtained here are found to be

independent of the nature of the block copolymer used.

Previously Almgren et al.[41] have examined aggregation

of SDS in aqueous solutions containing block copolymer

(PEO=PPO=PEO) by fluorescence and NMR studies.

Figures 7 and 8 show surface tension vs. log surfac-

tant concentration of the TX-100þ SDS mixtures in the

absence and presence of 0.1 wt.% PEO and P65. These

systems were examined to study the effect of polymers

on mixed micelles of nonionic–anionic mixtures at vary-

ing mole fraction. In Fig. 7, for the mixed system with

mole fraction of TX-100 at 0.2, the surface tension curve

in the presence of PEO remains essentially same showing

no interaction while with P65, a weak complex binding is

present. Figure 8 shows similar curves for mixed surfac-

tant system where the mole fraction of TX-100 is held

constant at 0.8. A sharp break point giving CMCs for the

mixed system with or without added polymer is clearly

observed. Thus there is hardly any complex formation

between the mixed micelles and PEO or P65.

In the case of anionic–nonionic surfactant mixtures

and a hydrophilic polymer, the shielding of the anionic

head groups in the micelle can be due to the nonionic

surfactant or the nonionic polymer.[26] Hence we have a

competitive situation where the nonionic surfactant and

the polymer compete for the sites at the surface of

anionic micelle. From the results in Figs. 7 and 8, we

conclude that at low mole fraction (0.2) of TX-100, PEO,

and P65 are able to compete for the surface of the micelle

while at high mole fraction (0.8) of TX-100, the system is

not responding to an addition of the polymer. The adsorp-

tion of PEO at the micelle surface would release nonionic

surfactants to the solution thus increasing the total surfac-

tant activity and hence decreasing the surface tension.

The influence of nonionic surfactant, TX-100, on the

time dependant turbidity of solution of SDS (0.2 wt.%)

on addition of CaCl2 (400 ppm) is shown in Fig. 9. In the

absence of TX-100, SDS solution shows gradual

decrease in transmittance up to 5 min after the addition

of CaCl2 after which the transmittance attain a constant

value (40%). The addition of TX-100 to the SDS solution

shows enhanced calcium ion tolerance and it can be seen

Figure 7. Surface tension for the TX-100þ SDS mixtures at

a mole fraction of TX-100¼ 0.2 in absence and presence

of water soluble polymers. Key: , Blank; m, 0.1 wt.% PEO;

u, 0.1 wt.% P65.

Figure 8. Surface tension for the TX-100þ SDS mixtures at a

mole fraction of TX-100¼ 0.8 in absence and presence of

water soluble polymers. Key: , Blank; m, 0.1 wt.% PEO;

u, 0.1 wt.% P65.




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that progressive increase in TX-100 concentrations

shows a marked effect on transmittance. At 0.05 wt.%

TX-100 and above, the solutions did not develop any

turbidity (shown in inset figure).

The results show that the addition of TX-100 greatly

enhance the solubility of Ca(DS)2. Similar behavior of

nonionic surfactant was noticed before and has been

explained in terms of mixed micelle formation based on

the regular solution theory taking into consideration the

counter ion exchange at micelle. Mixed micelle may

incorporate both precipitating species (Caþ2 and DS�),

and therefore, their concentrations in solution are reduced,

causing an increase in solubility. As discussed before,

decrease in the CMC by various additives also plays an

important role in increase in the hardness tolerance.

ACKNOWLEDGMENT

Financial assistance from U.G.C. Project no. F.12-

36=98 (SR-I) is gratefully acknowledged.

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CaCl2 (400 ppm) as a function of time. Key: , 0 wt.%; m, 0.02 wt.%; j, 0.03 wt.%; u, 0.04 wt.%; X, 0.05 wt.%.




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Received January 12, 2002

Accepted July 22, 2002




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