Chapter 2

METHODOLOGY

2.1 Preparation of Materials

Sago flour (100-mesh, 83% starch) was provided by Prof. Dulce Flores sourced from

the province of Agusan del Sur. Glycerol that was used in the experiment was of analytical

grade, available from commercial suppliers.

2.2 Preparation of Thermoplastic Sago Starch

The thermoplastic starch material was prepared using a method similar to that of

Soest and Borger (1996). Starch-plasticized blend formulations consisting of sago starch,

water, and glycerol in ratios of 20:80:40 and 40:60:40 were fed into the extruder using the

treatments shown in Table 2. The extrudates were tubular due to the round die. Consequently,

rectangular samples, 3 cm long and varying thickness and widths based on extrudate

properties, were prepared from the tubular extrudates. Three samples were used for each

treatment. The samples were subsequently placed in aluminum trays and cooled in an air-

conditioned environment at 20OC (50 ±5% RH), as suggested by Forssell et al. (1999), for 24

hours before analysis. This was to ensure that there was a constant level of temperature for

conditioning the samples. Afterwards, samples were subjected to physical strength testing and

biodegradation tests.

Table 2. Production conditions of the thermoplastic sago starch sheets.

Formulation
Glycerol (% wt
(glycerol : starch : water) Barrel Temperature(°C)
Treatment glycerol/wt starch)
1 20:80:40 20% 90
2 20:80:40 20% 110

3 40:60:40 40% 90

4 40:60:40 40% 110

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2. 3 Testing of Tensile Strength

Tensile strength is defined as the maximum strength of a material without breaking when a

certain load is trying to pull it apart (Daniels, 1989). Using an improvised tensile testing setup

patterned after ASTM D638, tensile strength and elongation at break of samples were

measured. The testing setup is shown in Figure 7. Three samples were tested per treatment.

The upper part of the sample was attached to an iron clamp on an iron stand, whereas on the

lower tip a screw clamp was attached. The spring scale was affixed on the screw clamp, and a

pulling force was made on the scale hook. The hook was pulled until the material broke into

two distinct pieces. The readings in the scale, in kilograms, just before breaking were

estimated. The tensile strength was computed using the following formula:

(MT x 9.8 m/s2)

Strength (in Pa) = ------------------------------------
HxW

Where MT was the mass reading on the scale just before breaking; 9.8 m/s2 is the

acceleration due to gravity; H was the thickness of the sample in meters; and W was the width

of the sample in meters (Rosen, 1982).

clamp

Iron stand

TPS sheet

Screw clamp

Spring scale

Fig. 2. The improvised tensile strength testing setup: (A) actual testing setup, with
inset showing a close-up view of the polymer attached to the iron clamp; (B)
schematic diagram of the testing setup, with x as the length of the TPS sample.
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2.4 Biodegradability Test

Fig. 3. Sample of compost pile.

A compost pile was prepared using garden soil placed in a box of dimensions 2m x

0.7 x 0.4m. A method by Kale et al. (2007) was followed in tracking the degration of TPS

samples in the soil, with minor adaptations from Mohee et al. (2007). Two samples each for

every treatment, approximately 3 centimeters long each, will be placed in 0.12m x 0.09m

mesh bags, and buried 0.25m deep in the compost pile.

Weights of every sample for each treatment will be recorded at zero time and after 7

days or until the starch films disappeared. The samples will be taken from the compost every

24 hours for visual observations of appearance and weight or mass reduction. Weight loss will

be used as an indication of biodegradability, based on the method by Lai et.al. 2005, using the

formula on the next page.

(wo - wf)
Weight loss (%) = -------------------- x 100
wo

Where wo is the original sample weight and wf

is the final sample weight after the soil burial.

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2.5 Resistance to Water Disintegration

The resistance of the thermoplastic starch samples to disintegration in water was

determined using the method of Fishman et al. (1996) and as suggested by Sitohy and

Ramadan (2001). Circular samples resembling discs were made, approximately 0.007 m in

diameter; it was ensured that these weighed almost the same (±0.005 kg differences). These

were submerged in 100 mL distilled water at 25OC in a beaker. The water was stirred using a

magnetic stirring bar at 1000 rpm. The time required for each disc to visually disappear was

measured through a stopwatch. However, if the discs remained undissolved after 20 minutes,

they were considered resistant to disintegration. There were three discs used for each

treatment.

Fig. 4. The resistance to water disintegration setup.

2.6 Statistical Analysis

The following statistical tests were employed to analyze and interpret the results of

the study:

Mean. This was used to determine the average tensile strength at break and the

average percent weight loss of the TPS samples.

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One-Way Analysis of Variance. This was used to determine significance of the

difference on the mean tensile strength at break and the mean percent weight loss of the TPS

samples.

Tukey’s Honestly Significant Difference. This post hoc multiple comparison

procedure for analysis of variance was used to determine whether a significant difference

between different treatments.

All data are computerized using the Mega Stat Menu. In a 95% confidence interval,

paired groups with significance level of ≤ 0.05 were considered to be significantly different.