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Investigation on Physio-chemical and Mechanical Properties of

Raw and Alkali-treated Agave americana Fiber

Article  in  Journal of Reinforced Plastics and Composites · March 2010

DOI: 10.1177/0731684410362817

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 Journal of Reinforced Plastics and
Composites
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Investigation on Physio-chemical and Mechanical Properties of Raw and Alkali-treated

Agave americana Fiber
K. Mylsamy and I. Rajendran
Journal of Reinforced Plastics and Composites 2010 29: 2925 originally published online 5 March
2010
DOI: 10.1177/0731684410362817

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 Investigation on Physio-chemical and
Mechanical Properties of Raw and
Alkali-treated Agave americana Fiber

K. MYLSAMY
Department of Mechanical Engineering, K.S. Rangasamy
College of Technology, Tiruchengode, Tamil Nadu, India

I. RAJENDRAN*
Department of Mechanical Engineering, Dr. Mahalingam College
of Engineering and Technology, Pollachi, Tamil Nadu, India

ABSTRACT: This paper aims at introducing new natural fibers for use as fillers in a polymeric
matrix enabling production of cost-effective, biodegradable, and lightweight composites for load
carrying structures. Agave (Agave americana) leaf fiber, one such kind, is rich in cellulose, relatively
inexpensive, and abundantly available. In this study, investigations on extraction of agave leaf fiber
are carried out and its physical, chemical, and mechanical properties such as the cross section, length
distribution, weight distribution, density, cellulose, hemicellose, lignin, and wax are determined
experimentally. Analysis of the tensile force of the fiber, elongation of the fiber, and water absorp-
tion of the fiber in load direction and fiber length are also carried out. The effect of alkali treatment
on the fiber at varying concentrations, temperature, and holding time are also studied. A scanning
electron microscope is used to analyze the morphology of raw and treated fibers.

KEY WORDS: natural fibers, mechanical properties, chemical properties, alkali treatment, SEM.

INTRODUCTION

ATURAL FIBERS PLAY an important role in developing high performing fully bio-
N degradable ‘green’ composites, which will be key materials in solving the current
ecological and environmental problems. The natural fiber reinforced composite is a
lightweight, naturally attractive, cost-effective application of renewable materials.
It will help to improve cultivation of fiber plants and also the economy of the country.
Synthetic fibers used in composite materials pollute the environment because of their non-
biodegradability. Environmental hazards in production of glass, carbon, aramid fiber
reinforced plastics and their recycling have seriously been realized in the world. As an
alternative, natural fiber composites were developed, in which plant fibers such as jute,
bamboo, banana, oil palm, hemp, kenaf, and flax were used. Nowadays wood substitute is

*Author to whom correspondence should be addressed. E-mail: irus_rajendran@yahoo.co.in

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Journal of REINFORCED PLASTICS AND COMPOSITES, Vol. 29, No. 19/2010 2925
0731-6844/10/19 2925—11 $10.00/0 DOI: 10.1177/0731684410362817
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2926 K. MYLSAMY AND I. RAJENDRAN

found to be commercially cost-effective and plays an increasingly major role as an alter-

native material in the composite industry.
Vegetable fibers can be divided into various types based on their origin in the plant. Seed
fibers are those that are borne on the seed coat as hairy structures or on the inner walls of
the fruit; each fiber consists of a single, long, narrow cell, as in cotton and coir. The bast
fibers are found in the inner bast tissue of certain plant stems and are made up of over-
lapping cells, for example, flax, hemp, jute, etc. The leaf fibers are a part of the
fibro-vascular system of the leaves, as seen in sisal and henequen. All vegetable fibers
are made up of mainly cellulose and hemicellose, lignin, pectins, and wax. All natural
fibers are susceptible to microbial decomposition. Murali Mohan Rao and Mohana Rao
[1] studied the process of extraction, cross-sectional shape, length distribution, and the
density and tensile properties of vakka, date, and bamboo fibers.
Agave americana is a succulent plant of a large botanical genus of the same name,
belonging to the family Agavaceae. Agave is the native of central and north America.
It is abundantly found in arid and semi-arid regions. It has also been successfully imported
to India. The plant has a large rosette of thick fleshy leaves with a spiny margin and ends
in a sharp point.The leaves are long, tough, and rigid, with sharp and hard pointed ends,
which can easily penetrate through clothes and leather. In general, the leaf fibers are
coarser than the bast fibers. The agave reacts dynamically to its environment in the dry
season where in it puckers up to reduce the amount of surface area for evaporation.
In times of excess heat or sun, they adapt the angle of their leaves to either get more
sun or reduce its effects. Agave fiber is extracted by rural people for manufacture of ropes
and coarse textiles. Many automotive and household components are produced using
natural composites, mainly based on polyester and fiber-like flax, hemp, pineapple, coir,
and sisal. The application of natural fiber composites in these industries is lead by motives
of price, weight reduction, and biodegradability.
This study aims at the application of agave fiber in composites. Thus investigations on
the harvesting and processing of the fiber and its chemical, mechanical, and physical
properties are carried out to analyze its suitability in natural fiber composites.
The alkali treatment of the natural fiber removes lignin and hemicellulose from the sur-
face. Sgriccia et al. [2] discussed the characteristics of treated and raw fiber surfaces and
also measured the water absorption of natural fiber composites. The water absorption of
natural fiber composites is found to be more than the glass fiber composites. Alkali treat-
ment of the natural fiber chemically modifies the fiber surface and removes the impurity
from it. Investigations reveal that the effect of alkali treatment on the fiber increases the
efficiency of the composite matrix [3,4].
Mohd Edeerozey et al. [5] investigated the kenaf natural fiber reinforced composite with
varying NaOH concentrations and analyzed the morphological structure of the fiber using
scanning electron microscope (SEM). The tensile strength of raw and treated kenaf fiber
was evaluated and the optimum concentration of alkali was found to be 6% NaOH
[6]. Studies on the surface modification of henequen fiber by alkali treatment and silane
coupling agent with improved mechanical strength of fibers were carried out [7—9]. Juarez
et al. [10] studied the efficiency of the alkali treatment to improve the tensile properties on
Agave lecheguilla fibers. Alkali-treated fibers were of high tensile strength which estab-
lished their application with Portland cement and showed increased durability when
exposed to the environment. Sgriccia and Hawley [11] analyzed microwave and thermal
curing of natural fiber (hemp, flax, kenaf, and henequen) reinforced epoxy composite

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Investigation of Raw and Alkali-treated Agave americana Fiber 2927

materials. The mechanical properties were investigated using differential scanning calo-
rimeter (DSC), thermo gravimetric analysis (TGA), environmental scanning electron
microscopy (ESEM), and the swept frequency diagnostic method.
The performance of natural fiber reinforced polymer composite was evaluated at var-
ious weather and humidity conditions [12—15]. Bisanda [16] evidenced that the alkali
significantly increases the mechanical interlocking and chemical bonding of the sisal
fiber. It is also found to improve the adhesion characteristics, surface tension, compressive
strength, and water resistance. The different treatment of alfa (Stipa tenacissima)
fibers has been characterized by means of infrared spectroscopy, surface energy, and
microscopy analysis. Bessadok et al. [17] found that chemical treatment reduced the
water absorption in alfa fibers.

EXPERIMENTS

Fiber Extraction

To extract the fiber, mature agave leaves were collected from the wild and the thorns on
the leaf margins and tips removed. The leaves were sun-dried for 2 days to remove excess
moisture. Then retting of the leaves was carried out by immersing them in water for a
minimum of 2 weeks. This facilitates maceration of the fleshy layers of the leaves. The
retted leaves were then manually beaten to remove the flesh. The cured fibers were
washed thoroughly and meticulously combed to free the flesh followed by air-drying for
2 to 3 days at room temperature. The dried fibers were thinned by ramming in order to
remove the unwanted short and broken fibers. The entire fiber extraction process takes
20—25 days.

Surface Modification

The raw agave fiber was washed with water several times and dried at room temperature
for 48 h. The surface modification consisted of alkali treatment of the fiber with varying
concentration of NaOH. It was found that with varying NaOH concentrations the fiber’s
properties change. The raw fiber were treated and immersed with 5%, 10%, and 15%
NaOH solution for 30 min and then washed with considerably dilute hydrochloric acid to
remove the residual alkali. Then, the fiber was rinsed twice or thrice with cold water. The
rinsed fibers were dried at room temperature for 2 to 3 days.

Fiber Diameter Distribution

A sample of 100 fibers was randomly taken from an agave fiber stack and the diameter
measured using the air wedge method. The limitation of the natural fiber is the variation in
diameter, which depends on the nature of growth, age of the plant, and the environmental
conditions. In agave fibers the diameter varies throughout the length of the fiber. Three
varying lengths from the top, mid-span, and tail end of the fiber were measured. The fiber
was placed between the two optically plane glass plates and a wedge was formed, then the
diameter was measured from the interference fringes of alternate bright and dark bands
caused by the air wedge. The light source used was a sodium vapour lamp. The size of the

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2928 K. MYLSAMY AND I. RAJENDRAN

fiber plays a major role in determining the tensile strength of the fiber [18]. The diameter of
the fiber was calculated using Equation (1):
l
t¼ ð1Þ
2
where t ¼ thickness of the fiber (m), l ¼ distance between of the fiber and the tied end of the
glass plate (m),  ¼ wavelength of sodium light 58931010 m and  ¼ band width (m).
. The average diameter of the fiber was calculated to be 0.204 mm
. The maximum diameter of the fiber was calculated to be 0.334 mm
. The minimum diameter of the fiber was calculated to be 0.126 mm

Fiber Length Distribution

An agave fiber sample of 10 g was selected at random. The number of fibers in the
consignment was counted. The length of each fiber was measured at room temperature by
a metre scale with an accuracy of ±1 mm. During measurement care was taken to make
sure that elongation does not take place while stretching the fiber to its full length. Fibers
varying in length under 100 mm were grouped into one category. The shortest fiber mea-
sured was 326 mm and the longest fiber was 1576 mm. The length of the fiber was skewed
towards the longer fibers. Maximum number of fibers were found to be in the range of
1101—1200 mm. The distribution of length is shown Figure 1.

Fiber Weight Distribution

The sample of 10 g was weighed in an electronic weighing balance of sensitivity ±0.001 g

and it accounted to have 225 individual fibers. The distribution of weight of the fiber is

60

50

40
Number of fiber

30

20

10

0
301–400 401–500 501–600 601–700 701–800 801–900 901–1000 1001–1100 1101–1200 1201–1300 1301–1400 1401–1500 1501–1600

Length of the fiber (mm)

Figure 1. Length distribution of the agave fiber.

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Investigation of Raw and Alkali-treated Agave americana Fiber 2929

shown in Figure 2. Maximum fiber was found to lie under the length category of
1101—1200 mm and was measured to be 38.9 wt%.

Test for Chemical Properties

TEST FOR CELLULOSE

One gram of agave fiber sample was taken in a sterile dry container to which 1.72% sodium
chlorite (NaClO2) solution was added and it was acidified with a few drops of concentrated
sulphuric acid. The solution was refluxed for 1 h. Then the suction process was carried out
and the excess fluid was removed. To the resulting concoction ammonia was added and
washed with distilled water. The residue was dried and the final weight was noted:
R
C¼  100 ð2Þ
D
where C ¼ cellulose content (%), R ¼ weight of residue (g), D ¼ dry weight of the sample (g).

TEST FOR HEMICELLULOSE

One gram of the fiber sample was dried in an oven for 4 h at 100 C and the resulting
sample was treated with 4% NaOH solution at room temperature for 1 h and later cured
with 5% HCl. HCl was removed by suction and the resulting sample was treated in an
oven for an hour. The difference in the initial and final weights presented the quantity of
hemicellulose.

TEST FOR LIGNIN

One gram of agave fiber sample was soaked in 12.5 mL of 72% sulphuric acid for 1 h at
room temperature. Then 300 mL of distilled water was added and left undisturbed for 2 h.
The solvents were drained carefully and the sediment was weighed. The quantity of the
sediment is interpreted as the quantity of lignin.

3.5

2.5
Weight of the fiber (g)

1.5

0.5

0
301–400 401–500 501–600 601–700 701–800 801–900 901–1000 1001–1100 1101–1200 1201–1300 1301–1400 1401–1500 1501–1600

Length of the fiber (mm)

Figure 2. Weight distribution of agave fiber.

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2930 K. MYLSAMY AND I. RAJENDRAN

TEST FOR WAX

One gram of the fiber sample was taken in an extraction condenser. To this sample,
200 mL of petroleum ether was added and refluxed for 5 h at 70 C. Then the sample was
dried and weighed. The difference in weight gives the quantity of wax.

Test for Physical Properties

TEST FOR DENSITY

The density of agave fiber was measured using the water displacement method.
One gram of the sample was completely immersed in water and the volumetric displace-
ment was noted. The ratio of weight and volume presented the density of the sample.

TENSILE TEST OF AGAVE FIBERS

The tensile test was conducted with a cross velocity of 50 mm/min using a gauge length
of 200 mm at 65% RH ± 2% RH and 20 C ± 1 C temperature of using Uster Tensorapid
3 machine applying constant rate of extension. The yarn count of the fiber was calculated
by the cut and weigh method. The results obtained for a 20 fiber consignment in single,
three, and five sample at three levels of chemical treatment, namely raw, 5% NaOH, and
10% NaOH treated are shown in Tables 1—3, respectively.

Table 1. Mechanical property of agave raw fibers.

Tensile Yarn
Number force CV% % of CV% of Tenacity B-work count
of fiber (N) of strength elongation elongation (N/den) (Nm) (denier)

Single 5.69 38.53 7.07 29.28 0.0165 0.049 344

Three 22.66 26.97 7.29 25.01 0.0258 0.186 878
Five 31.10 34.30 7.68 17.61 0.0236 0.283 1317

Table 2. Mechanical properties of agave 5% NaOH-treated fibers.

Number Tensile CV% of % of CV% of Tenacity B-work Yarn count

of fiber force(N) strength elongation elongation (N/den) (Nm) (denier)

Single 7.03 48.51 6.35 38.39 0.0261 0.048 269.1

Three 26.97 34.53 6.24 13.81 0.0316 0.163 853.48
Five 38.42 29.0 7.21 13.53 0.0291 0.311 1320.27

Table 3. Mechanical properties of agave 10% NaOH-treated fibers.

Number Tensile CV% of % of CV% of Tenacity B-work Yarn count

of fiber force (N) strength elongation elongation (N/den) (Nm) (denier)

Single 4.63 39.91 8.71 21.46 0.0173 0.040 267.3

Three 13.89 23.48 8.59 9.77 0.0201 0.124 662.8
Five 19.98 22.67 8.21 12.88 0.0155 0.246 1284.8

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Investigation of Raw and Alkali-treated Agave americana Fiber 2931

Scanning Electron Microscope

In SEM a fine probe of electrons scans the surface of the sample and the signals
emanating from the incident site are processed and quantified. The major difference is
that instead of imaging the entire specimen at once the electron beam is scanned back and
forth over the specimen, imaging only one point at a time. The interactions of the electrons
with the surface are registered and from this data an image can be constructed. A higher
depth of field is required to observe irregular and consequently increased working dis-
tance. The accelerating voltage employed has an important bearing on the image char-
acteristics. The SEM analyses of the samples were taken for raw and treated fibers.

RESULTS AND DISCUSSIONS

Fiber Chemical Properties

The process of alkalization is based on the same principle as the mercerization process for
cotton fibers. The natural fibers are treated with an alkaline solution, such as NaOH,
resulting in change of fiber properties [19]. Agave fibers are composed of cellulose (68%),
hemicelluloses (15%), lignin (5%), wax (0.26%), and moisture (8%). The effect of the alkali
treatment on cellulose fiber is a swelling reaction during which the natural crystalline struc-
ture of the cellulose relaxes. The alkali solution influences cellulosic components within the
natural fiber and moreover influences non-cellulosic components (hemicellulose, lignin, and
wax content). Chemical tests were conducted with various NaOH concentrations of 5% and
10% agave fibers. The cellulose of the fiber did not affect the alkali-treated fiber but resulted
in change of other chemical properties, shown in Table 4. So the alkali-treated fiber had
good adhesion properties and improved strength of fiber.

Fiber Mechanical Properties

The yarn count of the fiber decreased with the alkali treatment and yarn count plays an
important role in the tenacity of fibers. The tenacity of the fiber depends on tensile force
and yarn count. So the yarn count of the fiber is inversely proportional to the tenacity of
the fiber. The alkali-treated agave fiber gave better tenacity compared to the raw agave
fiber. The tensile test was carried out with 20 samples of dry untreated, 5% and 10%
NaOH-treated agave fibers such as single fiber, three fibers (yarn), and five fibers (yarn)
each. The elongation of fiber was found to be 7.07%, 7.29%, and 7.68% of raw fiber for
single fiber, three fibers (yarn), and five fibers (yarn), respectively. Increase in tensile force

Table 4. Chemical properties of raw and alkali-treated agave fibers.

Wax Moisture
Chemical Cellulose Lignin Hemicelluloses content content Density
properties (wt%) (wt%) (wt%) (wt%) (wt%) (g/cm3)

Raw fiber 68.42 4.85 15.67 0.26 7.69 1.20

5% NaOH treated fiber 86.27 4.05 Nil 0.14 8.74 1.30
10% NaOH treated fiber 84.58 4.25 Nil 0.01 8.64 1.32

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2932 K. MYLSAMY AND I. RAJENDRAN

of fiber was favored by 5% NaOH treatment whereas 10% NaOH treatment showed
reduced tensile force (Figure 3). Also, the alkali treatment was found to improve the tensile
force of fibers by 10—15%. The alkali treatment of fibers increased the surface smoothness
of the fiber and also improved the chemical interaction matrix and definitely improved the
mechanical properties of the composite material.
The tensile force for 5% NaOH-treated fiber at a holding time of 30 min was found at various
temperatures at intervals of 20 C. Since the tensile force was maximum at 80 C, it was
selected as the most promising alternative, as illustrated in Figure 4. Similarly elongations

90

80

5% NaOH-treated fibers
70

5% NaOH-treated fibers
60
Tensile force (N)

10% NaOH-treated fibers

Untreated fibers
50

10% NaOH-treated fibers

Untreated fibers
5% NaOH-treated fibers

10% NaOH-treated fibers

40

30
Untreated fibers

20

10

0
Single fiber Three fiber Five fiber
Number of fibers

Figure 3. Tensile force of raw and treated fibers.

6.8

6.6

6.4
Tensile force (N)

6.2

5.8

5.6

5.4
0 20 40 60 80 100 120
Temperature (°C)

Figure 4. Tensile force of 5% NaOH-treated agave fiber at varying temperature.

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Investigation of Raw and Alkali-treated Agave americana Fiber 2933

at the same temperatures were noted. The elongation increased sharply from 50 C to 60 C
and then gradually increased as temperature increased, as shown in Figure 5. The tensile
force at 80 C and different holding time at intervals of 20 min were found. This proved that
30 min holding time is the most suitable holding time, this is shown in Figure 6.

Surface Morphology of Fibers

The surface morphology of raw and treated agave fibers using SEM were carried out.
The microscopic image of raw fiber showed the presence of irregular cell wall
features and also the presence of some extra cellular non-fibrous impurities. The alkali
treatment (5%, 10%, and 15% NaOH) was found to give a uniform smoothness to the
fiber surface and also to have leavened away the impurities that were found in raw fibers.

30

25
Elongation (mm)

20

15

10

0
0 20 40 60 80 100 120
Temperature (°C)

Figure 5. Elongation of 5% NaOH-treated agave fiber at varying temperature.

5
Tensile force (N)

0
0 20 40 60 80
Holding time (min)

Figure 6. Tensile force of 5% NaOH-treated agave fiber at varying holding time.

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2934 K. MYLSAMY AND I. RAJENDRAN

The alkali treatment of the fiber was found to refine its mechanical and physio-chemical
properties. This favors its application in the composite industry.

CONCLUSION

The physio-chemical and mechanical properties of raw and treated agave fiber were
investigated and the SEM analysis of the fiber was also carried out.
. Diameter of the fiber was not uniform throughout the length of the fiber. The diameter
of the fiber was found to have a major influence on the mechanical strength of the fiber.
. Agro climatic factors, environmental factors, and the harvesting period are found to
influence the qualities of natural plant fibers. Thus, in this study the length and weight
distribution of the agave fiber were analyzed. On an average, the fiber length was found
to be more than 1 m and the maximum weight distribution was found to be between 0.9
and 1.4 m.
. The chemical composition of both raw and alkali-treated agave fibers were studied.
According to the current observation, the cellulose content of agave fiber was rich when
compared to the other natural fibers. It was also found that the alkali treatment reduced
the hemicellulose, lignin, and wax content of the fibers. The alkali-treated fiber was
found to have a more attractive color and a smoother surface texture than the raw one.
. The density of the agave fiber was found to be lower than that of the synthetic fibers
available and so this fiber can be preferred to manufacture lightweight composite
materials in the near future. Another added advantage is that the agave fiber is
biodegradable.
. The tensile force analysis of both the raw and alkali-treated fibers was performed with
varying factors. The treated fibers were found to have more tensile force than the raw
fibers. The optimum was found at 5% NaOH treatment. When the tensile force of 5%
NaOH-treated fiber was observed at varying temperatures, 80 C was found to be opti-
mum. The third factor analyzed was the holding time. It was observed that the 5%
NaOH-treated fiber at 80 C gave an optimum strength at the holding time of 30 min.
. Surface morphology of fiber was studied using SEM. The images of the fiber were
analyzed. The cell wall, cross section of the fiber, and interlinks between fiber cells
were observed. The surface smoothness of the fiber and impurities of the fiber was
also observed. It was found that the treated fiber was smoother and more pure by
surface than the untreated fiber.

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UD Flax Fiber Reinforced Composite by Applying an Alkali Fiber Treatment, Composites. Part A: Applied
Science and Manufacturing, 37(9): 1368—1376.

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