 *Corresponding author.

Email: s.hajar@upm.edu.my

eISSN: 2550-2166 / © 2018 The Authors. Published by Rynnye Lyan Resources

  Food Research 3 (2) : 157 - 163 (April 2019)
  Journal homepage: http://www.myfoodresearch.com

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Mechanical and thermal properties of tapioca starch films plasticized with

glycerol and sorbitol

1Zahiruddin, S.M.M., 1,2*Othman, S.H., 1Tawakkal, I.S.M.A. and 1Talib, R.A.

1Department of Process and Food Engineering, Faculty of Engineering, Universiti Putra Malaysia, 43400,

UPM Serdang, Selangor, Malaysia.
2Materials Processing and Technology Laboratory, Institute of Advanced Technology,

Universiti Putra Malaysia, 43400, UPM Serdang, Selangor, Malaysia.

Article history:

Received: 2 June 2018

Received in revised form: 31

October 2018

Accepted: 1 November 2018

Available Online: 6

November 2018

Keywords:

Film packaging,

Biopolymer,

Starch,

Glycerol,

Tensile,

Sorbitol,

DOI:
https://doi.org/10.26656/fr.2017.3(2).105

Abstract

Recently, the use of natural polymer such as starch to produce packaging film has received

much attention as a substitute for conventional petroleum-based packaging film since

starch is biodegradable and sustainable. However, the poor characteristic of starch such as

high brittleness will limit the application of the film. This problem can be solved by

adding plasticizers. In this work, the effects of different types of plasticizers (glycerol,

sorbitol and 1:1 mixture of glycerol-sorbitol) on mechanical and thermal properties of

tapioca starch films prepared by solvent casting method were investigated. The films were

characterized in term of mechanical (tensile strength (TS), elongation at break (EAB),

Young Modulus (YM) and thermal properties (thermo-gravimetric analysis (TGA)). Film

plasticized with sorbitol exhibited higher TS and YM but lower EAB value which

contributed to higher thermal stability than glycerol-plasticized film. This was due to the

strong interactions between the polymer chains resulting from the high molecular weight

of sorbitol. Hence, films became more rigid and thus promoted to a greater thermal

resistance.

1. Introduction

 Recently, numerous studies on the development

of biodegradable film packaging especially made from

biopolymers have been done. Generally, there is a huge

interest in biodegradable film packaging due to the

excessive use of conventional petroleum-based as food

packaging material which is non-biodegradable and

contributed to land disposal problems. The new study on

global analysis of plastics made from petroleum reported

that out of 6.3 billion metric tons of plastics have

become a wastage and on top of that, only 9% has been

recycled (Geyer et al., 2017). In order to prevent the

increasing number of plastic wastes, biopolymer-based

materials have been introduced as an alternative to

replace the petroleum packaging material due to its

biodegradability and sustainability. Film packaging

produced from biopolymers can be disposed into an

organic waste accumulation for further composting,

leaving behind organic by-products such as carbon

dioxide (CO2) and water (H2O) (Othman, 2014).

The biopolymers to be used for the film formation

are usually derived from renewable and abundant

resources such as proteins, lipids, and polysaccharides

(Nemet et al., 2010). Among these biopolymers,

polysaccharide mainly starch has the potential to be used

for film formation due to its non-toxicity,

biodegradability, renewability, availability, and low cost

(Bonilla et al., 2013; Li et al., 2015). Starch is a natural

carbohydrate which serves as the main energy storage

found in various plant sources such as grains (wheat and

rice), fruits and vegetables (corn), as well as roots and

tubers (potatoes and tapioca) (Mohammadi Nafchi et al.,

2013; Borges et al., 2015). Tapioca starch (Manihot

esculenta C.) was chosen to be used in this study because

it can be easily found in tropical climate country such as

Brazil, Thailand, Indonesia, and also in Malaysia. Films

made from polysaccharides mainly starches are able to

form a continuous polymer matrix even without the

addition of plasticizer (Cerqueira et al., 2011).

However, tapioca starch films produced without

plasticizer are usually brittle and exhibit poor mechanical

strength as well as thermal stability. This is due to the

strong hydrophilic behavior of starch makes this material

sensitive when coming into contact with water resulting

in low flexibility and yield a brittle film (Avella et al.,

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2005). In order to overcome the film brittleness,

plasticizer can be introduced as an additive in the tapioca

starch film. The incorporation of plasticizer into the

starch film is to enhance the flexibility of starch by

reducing the intermolecular forces within polymer matrix

as a result of increasing the mobility of polymer chains

(Sanyang et al., 2016). Plasticizers consist of hydrophilic

compounds such as polyols (glycerol and sorbitol) are

commonly used in starch film formation and has been

found to be particularly effective to serve as plasticized

hydrophilic polymer (Zhang and Han, 2006).

A number of research has been conducted regarding

the effect of polyols plasticizers especially glycerol and

sorbitol to the properties of biopolymer starch film.

Recent studies by Lagos et al. (2015), investigated the

mechanical properties of tapioca starch films added with

glycerol and sorbitol at different relative humidity

conditions. Borges et al. (2015) also studied the

influence of different starch sources and plasticizers

(glycerol and sorbitol) on the properties of biodegradable

films. Although there were several studies which

investigated the effect of polyols plasticizers on the

tapioca starch films, the studies mostly focused on a few

properties such as mechanical, physical, and barrier

properties. To the best of our knowledge, this study was

conducted to investigate the relationship between

mechanical and thermal properties on different types of

tapioca starch-plasticized films. Furthermore, there were

limited studies reported on the incorporation of varying

plasticizers in tapioca starch compared to other

biopolymer starch-based films. In this study, the effects

of different types of plasticisers (glycerol, sorbitol, and

1:1 mixture of glycerol-sorbitol) on the mechanical and

thermal properties of tapioca starch films were

investigated.

2. Materials and methods

2.1 Materials

Tapioca starch was purchased from LGC Scientific

Sdn. Bhd. Selangor, Malaysia. Food grade glycerol and

sorbitol were used as film plasticizers and were supplied

from R&M Chemicals, United Kingdom with a

molecular weight of 92.10 g/mol and 182.17 g/mol

respectively. Distilled water served as the solvent for

preparing film solutions.

2.2 Preparation of tapioca starch films with different

types of plasticizers

The films were prepared by diluting 25 wt. % (based

on dry basis of tapioca starch) of different types of

plasticizers which were glycerol, sorbitol, and 1:1

mixture of glycerol and sorbitol (glycerol-sorbitol) in

100 mL of distilled water. After that, 3.0 g of tapioca

starch was added into the plasticizer solution and then

stirred using stirrer hot plate (Favorit, Model HS0707V2,

Malaysia) at 80ºC for 30 mins to completely gelatinize

the starch. The gelatinized starch-plasticized solution

was then allowed to cool down at room temperature

before sonication using ultrasonic probe (QSonica, USA)

with 50% amplitude for 20 mins. Then, tapioca starch

films were obtained by casting method, whereby 40 mL

of the gelatinized solution was poured into 14 cm

diameter of petri dish and dried in the laboratory under

air conditioning system at 20ºC for 48 hrs. The sample

film was then separated from the petri dish and kept in a

desiccator (25ºC, RH = 53%) for further testing. The

thickness of each film was measured at five different

positions using Mitutoyo Digimatic Micrometer (Model

MDC-1” SX, USA). The thickness of the films produced

ranged from 0.007 to 0.008 mm. All the analyses were

carried out at least in triplicate.

2.3 Characterization of films

2.3.1 Mechanical properties

Mechanical properties of tapioca starch-plasticized

films which include tensile strength (TS), Young

modulus (YM), and elongation at break (EAB) were

determined using TA XT Plus Texture Analyzer

(Texture Technologies, UK). Tapioca starch-plasticized

sample films were cut into rectangular shape (100 x 15

mm2) using film specimen cutter following the ASTM

standard of D882 (ASTM, 2001). The samples were

clamped between the grips and the experiment was run

with the clamp distance of 50 mm and the cross-head

speed at 0.20 mm/sec. TS is the measurement of

maximum load that the sample can withstand before

failure while being stretched by the texture analyzer. It

was calculated by dividing the maximum load for

breaking the film by its cross-sectional area. Percentage

of the EAB was expressed as the change in the original

length of the sample at the break and was determined by

dividing the film elongation at rupture with the initial

grip separation. The rigidity of the films was analyzed by

the measurement of film stiffness which attributed to

YM value.

2.3.2 Thermal properties

Thermal properties of tapioca starch-plasticized

films were investigated via thermo-gravimetric analysis

(TGA) using Thermo Gravimetric Analyzer (Mettler

Toledo, Model TGA/DSC 1 HT, United States). At first,

sample film was weighed to approximately 10.0 mg. The

film was placed in aluminium pans and was heated at a

constant rate of 10ºC/min from 25-400 ºC under 50 ml/

min of nitrogen atmosphere. The degradation

temperature (ºC) and percentage weight loss (%) were

determined from two types of curve; thermo-gravimetric

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analysis (TGA) and derivative thermo-gravimetric

(DTG).

2.3.3 Statistical analysis

The statistical analysis of the obtained experimental

results was performed by using Minitab software

(Minitab Inc, USA). Analysis of Variance (ANOVA),

Tukey mean comparison test (p<0.05) was performed to

verify the significant differences among the mechanical

values. T-test (p<0.05) was performed to verify the

significant differences among thermal values.

3. Results and discussion

3.1 Mechanical analysis

Films packaging need to withstand the normal stress

applied during the application, handling and storage

period in order to maintain the quality of the films and

food’s properties. In this work, three types of plasticizers

(glycerol, sorbitol, and 1:1 mixture of glycerol-sorbitol)

have been used to produce tapioca starch-plasticized

films. Table 1 shows the TS, EAB, and YM for different

types of tapioca starch-plasticized films (control film

without plasticizer, glycerol-plasticized film, sorbitol-

plasticized film, and glycerol-sorbitol-plasticized film).

Tensile strength is defined as the maximum tensile stress

that a film can sustain during the tension grip test

whereas elongation at break is the maximum change in

length of the film before breaks (Bourtoom and Chinnan,

2008; Arham et al., 2016). Elongation at break is usually

inversely proportional to tensile strength whereby the

increase in TS value will decrease the EAB.

Table 1 shows that control film exhibited the highest

TS of 33.29 MPa. However, TS value decreased with the

addition of plasticizers. The addition of plasticizer

reduced the tensile strength of the films due to the

interaction between the starch polymer and plasticizer

molecules which weaken the hydrogen bonding thus,

promoted the molecular mobility of the polymer matrix.

Increasing molecular mobility between polymer chains

resulted in the increase in film flexibility as well as film

elongation which then made the film less brittle (Lin and

Tung, 2010).

TS value for sorbitol-plasticized film (18.92 MPa)

was higher than glycerol-plasticized film (15.84 MPa)

due to the rigidity of sorbitol that gave strong effect to

the tapioca starch film (p<0.05). According to Mali et al.

(2005), the firmness of sorbitol plasticizer was

influenced by several factors such as molecular weight

and molecular size of sorbitol. They reported that the

molecular weight of sorbitol was higher compared to

glycerol. The high molecular weight of sorbitol

plasticizer caused an increase in molecular mobility of

amorphous and crystallization of the starch matrix.

Therefore, films produced with the addition of sorbitol

were strong and rigid than glycerol-plasticized films due

to the molecular size of sorbitol which was higher than

glycerol. As a result, the incorporation of sorbitol in the

film was lower than glycerol plasticizer. This condition

makes the film less flexible and more rigid compared to

glycerol. Other than that, bigger size of sorbitol molecule

affected molecular ring conformation of sorbitol

molecules which strictly hindered an insertion between

starch chains. As a result, sorbitol plasticizer was less

effective in disturbing the interruption between starch

molecules which resulted in a strong film (Wittaya,

2013).

Apart from that, TS of films incorporated with

glycerol plasticizer exhibited the lowest value of TS due

to the hygroscopic character of glycerol which led to an

additional water to bind with starch matrix thus reducing

the strength of the films (Mali et al., 2005). Meanwhile,

TS value for glycerol-sorbitol-plasticized film was in

between the glycerol and sorbitol-plasticized films which

was 14.80 MPa because the combination of these

plasticizers resulted to balancing the low TS of glycerol

plasticized film and high TS of sorbitol plasticized film

(Sanyang et al., 2016). They also reported that a

combination of glycerol and sorbitol plasticizers

improved the low tensile strength of glycerol-plasticized

film and compromised the high tensile strength of

sorbitol-plasticized film.

Table 1 also shows that control film exhibited the

lowest EAB value of 12.54% followed by sorbitol

23.21% and then glycerol-plasticized film with EAB

value of 50.21%. These results were consistent with the

study by Borges et al. (2015) who found that films from

potato and tapioca starch exhibited lower TS and higher

EAB values when prepared with glycerol compared to

those produced with sorbitol. This finding shows that

glycerol-plasticized film has a greater plasticizing effect

than sorbitol whereby glycerol can soften the film and

make it more elastic than sorbitol due to its smaller size,

which allows it to exert a greater influence on the EAB

than the molecule of sorbitol (Heydari et al., 2014).

Besides, Dias et al. (2010) discovered that the highly

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Plasticizer TS (MPa) EAB (%) YM (MPa)

Control 33.29±0.35a 12.54±0.20a 1604.07±209.11a

Glycerol 15.84±2.81b 50.21±14.09b 153.04±39.66b

Sorbitol 18.92±0.98b 23.21±3.54c 779.39±86.32c

Glycerol+ 14.80±4.35b 29.70±7.27c 677.38±220.32c

Table 1. Tensile strength (TS), elongation at break (EAB), and

Young modulus (YM) of different types of plasticized tapioca

starch films

Values were mean ± standard deviation. Different superscripts

mean statistically different (p<0.05).

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hygroscopic nature of glycerol-plasticized films was also

plasticized by water since water is one of the plasticizing

agents in starch-based materials, which explains its low

TS and high EAB values. In contrary, the addition of

sorbitol plasticizer reduced EAB of the film due to the

molecular structure of sorbitol that was similar to

glucose units, which promotes the interaction within

polymeric starch chains thus, resulting to the increase in

strength and stiffness of the film with low flexibility

(Ooi et al., 2012). From Table 1, EAB value for glycerol

-sorbitol-plasticized film showing a similar trend with

TS value which was in between the glycerol and sorbitol

plasticized films. Generally, as the film structure softens,

TS decreases and EAB increases. A higher EAB value

indicates that the film is more flexible when subjected to

tension or mechanical stress. This implies that the film

might resist mechanical damage when subjected to a

rough handling during application on food processing

especially for easily damaged food products (Aisyah et

al., 2018).

YM is the measure of film stiffness, which is the

extent to which films resist deformation when the

response to an applied force. The higher the YM, the

higher the stiffness and rigidity of the materials. Based

on Table 1, YM for control tapioca starch film was the

highest amongst the other films which were 1604.07

MPa. Film stiffness can be related to its TS by which the

stiffness of control tapioca starch was the highest and

directly proportional to its strength.  When plasticizers

were added, films rigidity were reduced as the YM

values showed a decrement to 779.39, 677.38, and

153.04 MPa with the addition of sorbitol, mix of glycerol

-sorbitol and glycerol, respectively. Prakash Maran et al.

(2013) have also reported that the glycerol-plasticized

film was less stiff than sorbitol. This was due to its

intensively hygroscopic characteristic as compared with

the sorbitol, which acted as a lubricant to improve the

movements between polymer chains. As a result, there

was a significant increase in EAB and reduction in YM

values for glycerol-plasticized film. YM value for the

glycerol-sorbitol plasticizer was in the middle between

glycerol and sorbitol similar to the trend of TS and EAB

values as reported by Sanyang et al. (2016) whereby the

mixture of glycerol and sorbitol plasticizers gave a

balance effect to the flexibility and rigidity of the films.

3.2 Thermal analysis

In this study, thermo-gravimetric analysis (TGA)

was used to determine the thermal decomposition or

degradation and stability of different types of tapioca

starch-plasticized films. The results of thermal

degradation for different types of tapioca starch-

plasticized films were presented in plot curves of weight

loss (%) and derivative weight loss of the films as a

function of temperature (ºC) as shown in Figure 1. From

the TGA curves, it can be seen that the weight loss of the

films decreased with the increase in temperature which

shows that the degradation of the films occurred when

heated.

Control film clearly demonstrated two-steps weight

loss at particular degradation temperature range of 73-

151ºC and 280-370ºC with respect to degradation of

weakly bound water and decomposition of polymeric

starch material respectively (Pelissari et al., 2009).

However, glycerol-plasticized film shows three-step

weight loss which varied in the temperature range of 68-

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Figure 1. Thermo-gravimetric curves for different types of tapioca starch films including i) control film; ii) glycerol-plasticized

film; iii) sorbitol-plasticized film; and iv) glycerol-sorbitol-plasticized film.

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145ºC, 205-260ºC, and 290-380ºC, ascribed to

degradation of weakly bound water, glycerol plasticizer

degradation, and polymeric starch decomposition (Cyras

et al., 2008; Sanyang et al., 2016).

According to Sanyang et al. (2016), the degradation

temperature of unplasticized and plasticized sugar palm

starch (SPS) films for glycerol occurred between 125 to

290ºC indicated by the second step. They reported that

the three-step thermal degradation system also

demonstrated by the film with glycerol-sorbitol

plasticizer by which the degradation of glycerol takes

place at the temperature range between 220-275ºC might

be due to the contribution of glycerol content in the film.

Zhong and Li (2014) also found that the degradation

temperature of glycerol-rich phase of kudzu starch-based

edible films occurred at the second step of temperature

ranges from 150 and 280°C. The trend of these results

can also be observed from the derivative weight loss

curve which shows a slight slanted slope starting from

200°C where the degradation of glycerol happened at

this step. The thermal degradation rate of polymeric

material was at its highest when further heated to a

temperature more than 280ºC whereby the drastic weight

reduction of all films can be seen in Table 2.

Similar trends were also discovered by various

studies from Cyras et al. (2008); Nascimento et al.

(2012); Suppakul et al. (2013); Dang and Yoksan

(2015); and Sanyang et al. (2016). They discovered that

the mass loss at the initial step can be associated by the

loss of weakly bound water and low molecular weight

compounds of the film, whereby the degradation of the

molecular chain of plasticizer occurred at the second step

and the thermal degradation for the last step was

subjected to the elimination of hydrogen groups,

decomposition, and depolymerization of the starch

carbon chains.

It can be observed in Figure 1 that there was no

significant difference (p>0.05) on the weight loss of

maximum degradation peaks among the films. However,

glycerol-plasticized film contributed to the lowest

thermal degradation rate among all at the last step of

polymeric degradation temperature between 280 and

370ºC. From Table 2, the maximum weight losses at the

polymeric degradation temperature were 17.13%,

23.05%, 16.63%, and 22.21% for control, glycerol,

sorbitol, and glycerol-sorbitol-plasticized films,

respectively. In other words, the presence of glycerol in

tapioca starch films reduced the thermal resistance due to

the molecular interaction between glycerol and starch

compound which weakened the strong intermolecular

bonds between starch molecules and lowered the thermal

resistance of glycerol-plasticized film (Sanyang et al.,

2016). Based on Figure 1, sorbitol-plasticized film had

the highest thermal stability than other films at respective

temperature. These results resembled the mechanical

analysis whereby sorbitol-plasticized film also showed

the highest tensile strength among others due to the

sorbitol content which contributed to the optimum

thermal stability.

4. Conclusion

It was found that control tapioca starch film

exhibited low EAB but high TS values. Nevertheless, the

addition of plasticizers in the tapioca starch films alters

the mechanical properties of the film. Incorporation of

high molecular weight plasticizer particularly sorbitol

slightly increased the TS of the films but reduced the

elongation and flexibility as compared to glycerol.

Similarly, sorbitol-plasticized film also exhibited the

highest thermal resistance than glycerol because the

presence of high molecular weight of sorbitol in between

starch polymer chain produced a stronger film due to the

decrease in molecular mobility of the polymer chains

thus improved the thermal stability.

Acknowledgement

The authors gratefully acknowledge the financial

support provided by the Ministry of Higher Education,

Malaysia under Fundamental Research Grant Scheme

(Project no. 03-01-16-1873FR, Vote no. 5524980)

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