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International Journal of Innovative Research in Advanced Engineering (IJIRAE) ISSN: 2349-2163

Volume 1 Issue 8 (September 2014)


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Biodegradable Surfactant from Natural Starch for the


Reduction of Environmental Pollution and Safety for Water
Living Organism
Md. MohsinHossain
Department of Applied Chemistry & Chemical
Engineering, (ACCE)
University of Rajshahi, Rajshahi -6205,
Bangladesh

Md. Ibrahim H. Mondal


Department of Applied Chemistry & Chemical
Engineering, (ACCE)
University of Rajshahi, Rajshahi -6205,
Bangladesh

Abstract: The chemical contamination of water from a wide range of toxic derivatives, in particular soap, surfactants,
heavy metals, aromatic molecules and dyes, is a serious environmental problem owing to their potential human
toxicity. Therefore, there is a need to develop natural polymeric surfactant from starch that can free from toxic
pollutants found in wastewaters, ponds, drains, canals and rivers. Among all the treatments proposed, adsorption is one
of the more popular methods for the removal of pollutants from the waste water and soap-detergent free water. On
the other hand, water living organism can live smoothly without chemically substances (soap, surfactants) in the
mentioned sources by using naturally polymeric surfactants (prepared from potato starch). Adsorption is a procedure
of choice for treating industrial effluents, and a useful tool for protecting the environment. In particular, adsorption
on natural polymers and their derivatives are known to remove pollutants from water. The increasing number of
publications on adsorption of toxic compounds by modified polysaccharides shows that there is a recent increasing
interest in the synthesis of new low-cost adsorbents used in wastewater treatment and using natural polymeric
surfactants from natural sources for better washing in garments, textiles and household washing. The present review
shows the recent developments in the synthesis of adsorbents containing polysaccharides, in particular modified
biopolymers derived from chitin, chitosan, starch and cyclodextrin. New polysaccharide based-materials are
described and their advantages for the removal of pollutants from the wastewater discussed. The main objective of this
review is to provide recent information about the most important features of these polymeric materials and to show
the advantages gained from the use of adsorbents containing modified biopolymers in waste water treatment where
chemical substances (surfactant like CTAB, Tween-20, SDS) mixing when they are used as washing purposes in
textile industries. From the experimental results of viscosity, surface tension and other physical properties it
indicated that adding starch in detergent as soap filler these properties have changed which also indicated the more
washing activity of polymeric starch (potato) were cheaply available indoor market in Bangladesh. Biodegradable
starch interactions with ionic surfactants (CTAB, SDS) by the way of H-bond formation to ensure complexation
and reduced the harmful criteria of living organism in water also to ensure maximum protection of water pollution.
The formed complexes from starch-ionic surfactant-water were analyzed and characterized by XRD and SEM
instruments. Some of the complexes exhibited excellent emulsifying efficiency and polymeric surfactants
performance properties with this biodegradable natural starch polymer.
Keywords- biodegradable, CMC, Natural Starch, SEM, surfactants, water pollution and XRD.

I.INTRODUCTION
Water pollution due to toxic metals such as soluble soap-detergents in water in ponds, rivers, canals and organic
compounds remains a serious environmental and public problem Moreover, faced with more and more stringent
regulations, water pollution has also become a major source of concern and a priority for most industrial sectors such as
textile Industry, soap Industry, detergent Industry. Heavy metal ions, aromatic compounds (including phenolic
derivatives, and polycyclic aromatic compounds) and dyes are often found in the environment as a result of their wide
industrial uses. They are common contaminants in wastewater and many of them are known to be toxic or
carcinogenic. For example, chromium (VI) is found to be toxic to bacteria, plants, animals and people [1]. Mercury
and cadmium are known as two of the most toxic metals that are very damaging to the environment [2]. In addition,
heavy metals are not biodegradable and tend to accumulate in living organisms, causing various diseases and
disorders. Therefore, their presence in the environment, in particular in water should be controlled. Chlorinated
phenols are also considered as priority pollutants since they are harmful to organisms even at low concentrations. They
have been classified as hazardous pollutants because of their harmful potential to human health [3,4]. 2,4,6-trinitrotoluene (TNT) is a nitro-aromatic molecule that has been widely used by the weapon industry for the production of
bombs and grenades. This compound is recalcitrant, toxic and mutagenic to various organisms [5,6]. Many synthetic
dyes, which are extensively used for textile dyeing, paper printing and as additives in petroleum products are recalcitrant
organic molecules that strongly color waste water.Strict legislation on the discharge of these toxic products makes it
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International Journal of Innovative Research in Advanced Engineering (IJIRAE) ISSN: 2349-2163


Volume 1 Issue 8 (September 2014)
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then necessary to develop various efficient technologies for the removal of pollutants from waste water. Different
technologies and processes are currently used. Biological treatments [79], membrane processes [1013], advanced
oxidation processes [1417], chemical and electrochemical techniques [1820], and adsorption procedures [21
49] are the most widely used for removing metals and organic compounds from industrial effluents. Amongst all the
treatments proposed, adsorption using sorbents is one of the most popular methods since proper design of the
adsorption process will produce high-quality treated effluents. Adsorption is a well-known equilibrium separation
process. The adsorbents may be of mineral, organic or biological origin: activated carbons [2126], zeolites
[27,28], clays [2933], silica beads [34,35], low-cost adsorbents (industrial by-products [3641], agricultural
wastes [42,43], biomass [44,45]) and polymeric materials (organic polymeric resins [46,47], macro porous hypercross linked polymers [48,49]) are significant examples. Table.1 shows a non-exhaustive list of some selected
examples of adsorbents used in wastewater treatment.
Recently, numerous approaches have been studied for the development of cheaper and more effective polymeric
surfactant for better washing containing natural polymers. Among these, polysaccharides such as chitin [5052] and
starch [5355], and their derivatives (chitosan [56,57], cyclodextrin [5860]) deserve particular attention. These
biopolymers represent an interesting and attractive alternative as cleansing substances because of their particular
structure, physico-chemical characteristics, chemical stability, high reactivity and excellent selectivity towards aromatic
compounds and metals, resulting from the presence of chemical reactive groups (hydroxyl, acetamido or amino
functions) in polymer chains. Moreover, it is well known that polysaccharides which are abundant, renewable and
biodegradable resources, have a capacity to associate by physical and chemical interactions with a wide variety of
molecules [61,62] Hence adsorption on polysaccharide derivatives can be a low-cost procedure of choice in water
decontamination for extraction and separation of compounds, and a useful tool for protecting the environment [63].
Besides, the increasing number of publications on adsorption of toxic compounds by these natural polymers shows
that there is a recent interest in the synthesis of new adsorbent materials containing polysaccharides. Polysaccharides,
stere oregular polymers of mono saccharides (sugars), are unique raw materials in that they are: very abundant natural
polymers (they are referred to as biopolymers); inexpensive (low-cost polymers); widely available in many countries;
renewable resources; stable and hydrophilic biopolymers; and modifiable polymers. They also have biological and
chemical properties such as non-toxicity, biocompatibility, biodegradability, poly functionality, high chemical reactivity,
chirality, chelation and adsorption capacities. The excellent adsorption behavior of polysaccharides is mainly attributed
to: (1) high hydrophilicity of the polymer due to hydroxyl groups of glucose units; (2) presence of a large number of
functional groups (acetamido, primary amino and/or hydroxyl groups); (3) high chemical reactivity of these groups; (4)
flexible structure of the polymer chain. From the above mentioned features, it is proved that many researchers have paid
their attention on this field. In spite of half century of great effort, many academic aspects such as, chemistry, chemical
reactions, bond formation on starch-surfactants interaction are still open for discussion. The purpose of the present
investigation is to explore the effect of starch interaction with various surfactants and the better understanding the
mechanism between starch and surfactants complexes formed as polymeric surfactants studied by the ternary phase
diagram, interfacial surface tension and viscosity measurement and characterized by the XRD and SEM analysis.

I I . EXPERIMENTAL
2.1Materials
Potato starch as powder formwaspurchased fromUNI-CHEM, China and its degreeof substitution (DS) was
0.80.Starch sol uti on was prepared byheating thestarchin waterin anautoclave at1200 C for30min. All solutions were
prepared at least24h before measurement was performed. The surfactants sodium dodecyl sulphate (SDS), N-cetylN,N,N-trimethyl ammoniumbromide (CTAB) and Tween-20 were purchased as analyticalgrade and were used without
further purification.The water used was ion exchanged and distilled. Its conductivity, and reduced viscosity were 2.0
s and 4.0 dm3/mol, respectively and its surface tension was 71.510-3 0.5N/mat300C. All other chemicals were
analytical grade and were used without further purification.
METHODS
2.2.1 Surfaceandinterfacialtensionmeasurement
Surface tension was measured with a drop weight method (Stalagmometer i nstruments).In the calculation of surface
tension ,the correction factors of Huh and Mason [65] were used. The reproducible result between measurements of
thesamesamplewas0.5mN/m. The results of the surface tension measurement were presented as () values calculated
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International Journal of Innovative Research in Advanced Engineering (IJIRAE) ISSN: 2349-2163


Volume 1 Issue 8 (September 2014)
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from mg . Where, f is equal to 1 , v i s the volume of the drop and r is its radius, mg is the weight of falling
3
2rf

drop and is its surface tension. A drop of the weight(mg) given by the above equation has been designated as the
ideal drop. Repeated measurements (2-4 times) were conducted on each sample from which equilibrium surface or
interfacial tension values were obtained by averaging the values at very long periods, where the surface and interfacial
tension values showed little or no change with time. Prior to running tests with the starch solutions, the instrument was
calibrated with water and then checked by measuring the interfacial tension between water and pure starch.

2.2.2Viscosity
Viscosities were determined with an Ostwald viscometer according to British standard (Fisher Scientific TM 200) with
a fluctuation of 0.10 C was used. The flow of time was recorded by a timer accurate up to 0.01 second. At certain
surfactant/starch ratios the aggregates formed were very mobile flocks, which tended to form in the samples. This could
be partly avoided by draining the capillary fully between measurements. The results of the viscosity values calculated
from

red

(t t 0 )
t0

. where t is the measured efflux time of solutions and t0 is the efflux time of the pure solvent (water)

and C is the weight concentration of the surfactant, starch & surfactants mixed polymer.

2.2.3 Ternary Phase Diagram


2.2.3.1 Sample Preparation
For the development of ternary phase diagrams, the sample components were taken into the test tube by varying
composition in such a way that the total composition remains 100%. The components were added by varying
weight or volumes. The samples were prepared by varying 5% composition of two components simultaneously
keeping the third component constant, alternatively in a test tube. The open end of the test tube was then closed
with rubber cork in such a way that the vapour would come out and would enter into the test tube, here the cork
reacted with the sample. The samples were then shaken for well mixing of the components and placed into the
diagram are put according to the composition and mark. After completion of the 228 samples according to the
diagram on the wooden frame. The open end of the test tube was then closed tightly with cork, so that this would
remain no leakage or the lower part of the cork did not touch the sample solution and after that these samples were
then left to equilibrate in a thermostat box at 30C for at least ten days and would be shaken from time to time. The
equilibrium was established within this period.
2.3 Characterization
2.3.1 SEM analysis
Scanning Electron Microscope (SEM, JEOL, JSM 6301F, Japan), Fine coaster (JFC 1200,JEOL, Japan), Aluminum
specimen stub, Double-sided adhesive tape.
2.3.1.1 Procedure for sample determination
Scanning Electron Microscope (SEM) of potato starch, surfactant sample and starch-surfactant complexes samples were
less than 4% moisture content before examined. Dried sample and sprinkle were taken onto the double-sided adhesive
tape attached to the specimens tub. The excess sample was removed and the sample was placed in fine coater of gold
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coating for150seconds. The coated sample was then placed in the sample chamber of the SEM .The sample was
examined at magnification of 2,500 and 6,000 with the accelerating voltage of 10 Kv.
Model and specification:
2.3.2 XRD analysis
2.3.2.1Preparation of sample for XRD
The preparation of starch sample ,the dried sample is saturated with water by stirring repeatedly with a glass rod; this
step is performed by 2g of

st a r ch with 100 ml of hot water which is 100% distilled and stirred at room

temperature for 1h,centrifuging the suspensions and decanting the supernatant solutions. This process is repeatedly three times.
Then the starch solution is dried in oven at temperature 80oC.2h after proper drying the powder sample iskeptinasealedbottle.
The syntheses of cationic surfactants were undertaken by the following procedure: 2gofSodium dodecyl sulphate was first
dispersed in100 ml of deionized water then under mechanical stirring for about 1h. A pre-dissolved starch
solution of same amount was slowl y added to that suspension near about at 80oC. The reaction mixtures were
stirred for 1h at 80oC using mechanical stirring after proper drying the powder sample is kept in a sealed bottle then dried
products were stored in vacuum desiccators.
Starch powders to be used for X-ray diffraction (XRD) measurements were equilibrated in desiccators containing
saturated solutions of K2CO3 at 20-22oC.Under these conditions, the relative humidity (RH) at 20Cwas shown to be
44% and the final water content of pea, maize, potato, and wheat starches was 1314,12,15,and 12%,respectively.
Wet starch powder (from potato) for XRD measurements was produced by first equilibrating the starch in excess water.
The starch suspension was then centrifuged (3000 g) and the supernatant removed. The starch precipitate appeared as a
hard wet powder that was slightly more moist at the top. This moisture was dried with tissue paper. The wet starch
powder had a water content of 49%. It was apparent that the proportion of water was slightly overestimated, because the
precipitated starch granules would have a small amount of free space between them, which would be filled with free
water. This over estimation, however, can be considered to be very small as the granules in the precipitate were closely
packed. Since the water content with in the crystallites is fixed, near about 24% the proportion of water in the amorphous
part of starch can be estimated at 5560%. It was assumed that total crystalline of starch and complexes. Apparatus was
Wide-angle X-ray diffractometer (JEOL, JDX 3530, Japan), Silicon sample cell and Computer with program MDI Jade
6.5 (Japan)
From the polymer chemists point of view, the chemical substitution of chitin and starch offers enormous challenges.
These are provided by the presence of the numerous functional groups of starch molecules, which are available for
chemical reactions. However, their reactivity depends on experimental conditions. This makes, in general, selective
substitution relatively difficult

and different mono, di or tri-derivatives can then be obtained, yielding modified

polysaccharides (starch). The modification of the existing polysaccharides is one possible method of obtaining more
polar sorbents. The possible chemical derivatization of starch and chitin is also an interesting property because it is wellknown that the grafting of ligands can improve their adsorption properties. By incorporating some functional
(hydrophobic) groups either into the backbone of the network structure or as pendant groups it is possible to prepare
materials with strong adsorption properties. The chemical modification of the starch also allows preparation of
derivatized polysaccharide called cyclodextrin.

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III. RESULTS AND DISCUSSIONS


Some of the prepared starch-surfactant mixture lowered the surface tension of water, namely at lower concentration of
the sample(Table1). The functional properties of some of the prepared surfactant and starch mixed surfactant solutions
were tested for emulsifying efficiency, washing power and anti redeposititative efficiency. The emulsifying efficiency
was characterized by the stability of the paraffinic Tween-20/water emulsions and other surfactant mixture at definite
ratio. The results of reduced viscosities in CTAB and SDSsummarizedin Table 2 and 3 which show that some of the
surfactant made emulsions of the oil/ water type stable even after 24h. Their efficiency was comparable to that of the
commercial emulsifier Tween-20. Some of the tested mixture showed excellent washing power exceeding that of the
anionic detergent, name SDS containing dodecyl chains. The anti-redepositive efficiency was higher than the starting
SDS, but moderate in comparison to starch used as a co-builder in detergents [64]. in case of ionic surfactant (SDS,
CTAB) the changing is remarkable due to maximum interactions occurred with starch polymer. Here, we mentioned that
temperature has a remarkable effect in the complexes of starch-ionic surfactant, here it is obtained according to Arrhenius
rule increasing temperature reduced viscosity and specific viscosity is reduced due to the freeness of solution which has
been seen in Table 2 and 3.
Table 1: The value of surface tension of surfactants (Cationic, Anionic and Non-ionic)) with added starch
% Log Conc. of surfactant solution

% Conc. of
surfactant solution

Surface tension of
SDS mixed with
starch soln.

Surface tension of
CTAB mixed
with starch soln.

Surface tension of
Tween-20 mixed
with starch soln.

-2.00
-1.69
-1.52
-1.39
-1.30
-1.22
-1.15
-1.09
-1.04
-1.00

0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
0.09
0.10

48.11
47.02
44.35
44.21
42.13
41.95
41.73
41.55
41.52
40.51

48.19
46.15
44.67
43.89
43.15
42.37
41.69
41.46
41.45
41.41

52.11
49.19
48.75
47.61
45.63
44.84
44.45
44.05
43.05
42.07

Table2 at temperature range (25oC-85oC) solution viscosity of starch mixed CTAB


Reduced Viscosity (polymer)

Temp
o
C

reduced Viscosity (polymer-surfactant mixture)

0.0625%

0.125%

0.250%

0.500%

1.000%

0.0625%

0.125%

0.250%

0.50%

1.00%

25

1644.528

813.616

411.320

213.134

116.297

1549.392

912.256

539.508

298.854

182.692

35

1385.072

823.416

481.496

288.598

170.153

1298.592

786.768

454.012

240.734

159.576

45

1229.392

718.792

426.532

247.572

151.884

1177.504

703.104

392.944

216.802

135.538

55

1065.072

645.592

374.624

218.512

133.615

1021.824

608.992

344.088

192.870

125.923

65

926.688

572.392

341.036

201.418

121.115

918.048

541.016

307.448

168.940

108.615

75

857.504

525.328

313.556

184.324

110.538

822.912

488.728

279.968

155.264

99.961

85

771.024

478.272

286.076

168.94

99.961

753.728

441.672

252.488

141.588

90.346

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Table 3 at temperature range (25o-85oC) solution viscosity of starch mixed surfactant (SDS) compounds
Temp
o
C

Reduced Viscosity (polymer)

reduced Viscosity (polymer-surfactant mixture)

0.0625%

0.125%

0.250%

0.500%

1.000%

0.0625%

0.125%

0.250%

0.500%

1.000%

25

1644.528

813.616

411.320

213.134

116.297

1549.392

912.256

539.508

298.854

182.692

35

1385.072

823.416

481.496

288.598

170.153

1298.592

786.768

454.012

240.734

159.576

45

1229.392

718.792

426.532

247.572

151.884

1177.504

703.104

392.944

216.802

135.538

55

1065.072

645.592

374.624

218.512

133.615

1021.824

608.992

344.088

192.870

125.923

65

926.688

572.392

341.036

201.418

121.115

918.048

541.016

307.448

168.940

108.615

75

857.504

525.328

313.556

184.324

110.538

822.912

488.728

279.968

155.264

99.961

85

771.024

478.272

286.076

168.94

99.961

753.728

441.672

252.488

141.588

90.346

Scanning Electron Microscopy (SEM)


Figs. 1a, 1b and 1c show the individual surface image of starch, SDS and starch-SDS mixture, respectively studied by
SEM. It can be seen from Figs. 1a, 1b and 1c that the surface images of the starch and surfactant are quite different from
each other. The surfaces of the starch, SDS and mixture of these two looks like granules, pop-corn and needle like
respectively. It is clear that, at a certain temperature and concentration, the starch interacts with the surfactant through the
formation of H-bonds and changes its surface structure.

(a) starch

(b) Surfactant (SDS)

(C) starchwithSDS mixture

Fig. 1.SEM Image of (a) starch, (b) surfactant (SDS) and (c) starch with SDS mixture

H-bond formation with Surfactant

Fig.2: H-Bond formation starch with cationic surfactants. Fig.3: Only cationic surfactant molecule.

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From fig. 2 and fig. 3, it can be seen that starch molecule have many hydroxyl groups and hydrogen atoms which bind
with surfactant molecule through H-atom called H-bond formation. So bond break down is easily of hydrophilic and
hydrophobic parts of surfactant molecule, finally cleansing activity increased although starch are biodegradable and ecofriendly. XRD Figures 4, 5 and 6 has been given below for better understanding starch, SDS, CTAB complexes as
variation of concentration.

Fig.4StarchXRD
Fig. 4StarchXRD

The interactions between

Fig.5Starch-SDScomplexesXRD
Fig.5Starch-

Fig.6Starch-CTABcomplexesXRD

SDScomplexesXRD
starch and all type of surfactants and their mixtures were studied by using surface

tension, solution viscosity measurements and to do the ternary phase diagram, FT-IR analysis for H- bond detection
and identification , SEM analysis for characterization for smoothness of surfaces and XRD analysis for crystallization
of complexes structure. The composition and structure of the complexes of starch and surfactants mixture were
studied by using phase equilibrium determination, Scanning electron microgram (SEM) and X-ray diffraction (XRD)
measurements. Critical association concentrations (cac) are well below the critical micellisation concentrations (CMC)
of the surfactants. Associative phase separation occurs in extremely dilute systems when the charge ratio between the
surfactants and the polymer is close to one. The effect of mixing on micellization of the binary surfactant solution
can be described by taking into account the effects of the volume difference between the hydrocarbon chains.

V. CONCLUSION
The investigations presented in this paper show that strong ionic interaction occurs between cationic and anionic
surfactants (CTAB, SDS) except nonionic surfactant (Tween-20) and starch polymer, leads to phase separation
and precipitation of the formed amorphous complexes. Complex formation on starch depends on the chain length
difference in exactly in the same way as for free mixed micelles .The separated complex phase is a hydrophobic,
highly viscous and gel like containing 40 to 60% water. The highly and low water content of the complex phase
indicates that the interactions between the starch and ionic surfactants are very strong and they are capable more
effective washing properties in textile industry, dishwash in household, garments and laundry shops than normal
chemical detergent available in our indoor market. The polymeric surfactants which are newly prepared from
potato starch is also biodegradable and eco-friendly for environment not only this thisnatural surfactant from
natural sources help our green chemistry to safety for water living organism due to washable surfactant from
polymeric potato starch where small amount of chemical detergents also present.

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VI. ACKNOWLEDGMENT
The author is acknowledged to ministry of Science communication and Information Technology, Bangladesh for funded
financial fellowship assistance for doctoral research work to continuous three fiscal year . I also Thanks to my beloved
spouse SP Farida Yasmin BPM who inspired me to perform my Ph.D research work and my Supervisor Prof. Dr. Md.
Ibrahim H. Mondal who helped me to reach my goal.
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