Composites: Part A 45 (2013) 153161

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Composites: Part A
journal homepage: www.elsevier.com/locate/compositesa

Characterization of blue agave bagasse bers of Mexico

Satyanarayana Kestur G. a,, Thais H.S. Flores-Sahagun b, Lucas Pereira Dos Santos b, Juliana Dos Santos b,
Irineu Mazzaro c, Alexandre Mikowski c,d,1
a

PIPE/Department of Chemistry, Federal University of Parana (UFPR), Centro Politcnico, Jardim das Americas, P.B. No. 19081, CEP: 81531-980, Curitiba, PR, Brazil
Department of Mechanical Engineering, Federal University of Parana (UFPR), Centro Politcnico, Jardim das Americas, P.B. No. 19011, CEP: 81531-980, Curitiba, PR, Brazil
c
Universidade Federal do Paran, Centro Politcnico, Departamento de Fsica, P.O. Box 19091, CEP: 81504-990, Curitiba, PR, Brazil
d
Universidade Federal de Santa Catarina, Centro das Engenharias da Mobilidade, CEP: 89218-000, Joinville, SC, Brazil
b

a r t i c l e

i n f o

Article history:
Received 6 November 2011
Received in revised form 1 July 2012
Accepted 1 September 2012
Available online 9 October 2012
Keywords:
A. Fibers
B. Mechanical properties
B. Microstructures
D. Thermal analysis

a b s t r a c t
This paper presents physical, chemical, thermal and tensile properties of Mexican cooked blue agave
bagasse bers extracted from this plant. The bers are 1012 cm long and 592.34 lm in diameter. The
elliptical cells in the ber are regularly arranged with varying lumen size. The cellulose and lignin contents of the ber are 73.60% and 21.10% respectively. Fibers showed decreasing average values of ultimate
tensile strength and constant values of Youngs modulus and average % strain values with increasing
mean gauge length and decreasing mean diameter. Above results are discussed in the light of various factors that affect the properties. These bers are found to be thermally stable due to their higher values of
crystallinity and lignin. Main aim of this work is to characterize these partially degraded bers with a
view to nd possible uses for such bers such as compostable and biodegradable composites of corn
starch/cooked blue agave residues.
2012 Elsevier Ltd. All rights reserved.

1. Introduction

1.1. Background, status of characterization and uses

Signicant efforts in recent years to develop composites reinforced with plant materials have prompted study of the structure
and properties of various plant bers. The heightened awareness
of the need to preserve and recycle natural resources has enlarged
the range of plant ber resources [14] for such applications. The
reasons for such studies include renewability and abundant availability of plant bers, and stringent environmental regulations,
have been mentioned elsewhere [5,6]. There has been specic
characterization of individual plant bers including those of Brazil
origin by the authors themselves such as coir and sisal [14,712]
as well as part of studies on composites [5,6]. Extending their work
on characterization of lignocellulosic bers, the authors have
started research on the characterization of two of the bers obtained from Mexico, This paper deals with the blue agave
bagasse12 bers (Agave tequilana).

A. tequilana (also termed A. tequilana or Agave Americana L as

used by Bessadok et al. [12] or blue agave is native to Mexico. A.
tequilana Weber azul is a succulent plant (Fig. 1a) that spreads
radially and is 1.21.8 m tall at maturity.
It is mainly used to produce the distilled spirit tequila, since under Mexican law, only the blue agave, which has an intense blue
color, can be used to produce tequila [1316]. Commercially, the
important part of A. tequilana Weber azul for tequila production
is the stem (Fig. 1b) commonly termed head or pin, the Spanish word for pineapple, which it resembles. It is also reported that
after the agave juice is obtained, a brous waste is left after cooking the head.
It should be noted that these cooked blue agave bagasse piles
are seen in the tequila industrial plant from which the bers are
also extracted, which are used in this study. On the other hand,
the raw blue agave stem is extracted from the elds and go by
truck to the tequila facilities where the sweet juice is extracted
and the bagasse is the residue. From this, bers (called bagasse
composed of ber and pith) are obtained after shredding, milling
and extracting the juice from the cooked agave heads.
A number of studies [12,1321], though not systematic, have
been reported (including some patents) on this plant looking into
various aspects such as harvesting the plant, management, economic aspects, process for obtaining the bers from leaves of
the plant characterization and possible utilization of parts (e.g.
leaves obtained after the extraction of juice) and other byprod-

Corresponding author. Present address: Ananda Kuteera, G001, Insight Academy Road, Bikasipura, ISRO Layout, Bangalore 560 061, India. Tel.: +91 80 26622130
35x3012; fax: +91 80 26614357.
E-mail addresses: kgs_satya@yahoo.co.in (S. Kestur G.), tsydenstricker@
gmail. com (T.H.S. Flores-Sahagun), santoslucas4@hotmail.com (L.P. Dos Santos),
julianastos@hotmail.com (J. Dos Santos), mazzaro@sica.ufpr.br (I. Mazzaro),
mikowski@joinville.ufsc.br (A. Mikowski).
1
Universidade Federal de Santa Catarina, Centro das Engenharias da Mobilidade,
CEP: 89218-000, Joinville, SC, Brazil
2
Throughout this paper the word bagasse when used refers to blue agave ber
unless otherwise mentioned.
1359-835X/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesa.2012.09.001

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S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

economic aspects of this waste; (iii) there is no report from one research group on the characterization of cooked blue agave bagasse
extracted from the stem (head or pia) obtained from Mexico
although there are some papers about the use of the bagasse ber
as reinforcements in composites without mentioning whether
these bers were obtained from tequila factory where the bers remain stored in piles whereby degradation process of the bers
inevitably could have occurred and (iv) despite all these, a serious
environmental problem is posed by the waste blue agave leaves
that are left in the eld after harvesting the heads for tequila production, even when some quantity of these are used for ber
extraction. Considering all these, a systematic study is undertaken
with the objectives to characterize the blue agave bagasse ber extracted from the stem base, which are obtained from one major
country. These include chemical composition, density, structure
and morphology; thermal as well as tensile properties of these bers, which were supplied by a tequila industry in Mexico. It
should be understood that this kind of study may pave the way
for nding suitable applications for such bers obtained from left
out of cooked blue agave bagasse from the Tequila production
and thus, the bers might have undergone a degradation process
in the storage step.
2. Experimental

Fig. 1. Photographs of (a) Mexican agave tequilana (blue agave) plantation

showing cutting operation to get the stems. (b) Stems lying in a factory from which
bers are extracted. [Reproduced from (a) http://www.royalresortsnews.
com/wp-content/uploads/2010/10/agave-farming-tequila-mexico.jpg (b) http://a1.
sphotos.ak.fbcdn.net/hphotos-ak-snc6/226087_10150320505500861_709255860_
9667455_3138674_n.jpg] (Accessed on 20th October 2011). (For interpretation of
the references to colour in this gure legend, the reader is referred to the web
version of this article.)

ucts [17]. Limited studies on the tensile properties of these bers

including the effect of surface treatments on these properties are
also reported [13,15] including one such study on the ber bundles obtained from Tunisia with and without the chemical treatment of the bers [12]. Another study has reported on the
preparation and characterization of composite of this ber in high
density polyethylene with and without esterication as reinforcement [21].
While many patents are available describing the utilization of
sub-products of blue agave leaves, other uses of the bers are also
reported [17,22,23], which include possible production of good
quality ber from commonly discarded leaves after obtaining the
pia and as reinforcements in thermosetting resins. While many
of these attempts are at laboratory stage without enough information to evaluate their feasibility, there is continuous research to
nd alternative uses for this ber. This has been the subject of
many researchers, since 40% (on wet weight basis) of the total blue
agave consumed corresponds to the residual bagasse, most of
which is treated as waste and hence thrown into elds, which is
not a value added use [12,13].
Further, it is also reported [17] that these plants would provide
important economic status in the future with considerable development opportunities.
From the foregoing, the following becomes evident: (i) the blue
agave bers is produced in Mexico as a byproduct of one of their
most important beverage industry; (ii) scanty and scattered data
is reported on the properties along with some potential benecial

The agave bagasse bers used here were obtained from a tequila factory in the city of Tequila, Jalisco state, Mexico. The bers
were obtained in the tequila industry as follows: after the cooking
of the agave stem (pia), the sweet agave juice obtained goes to the
fermentation process, while the brous waste called bagasse is
left in the eld forming big mountains until transportation by
trucks. As a residue, no special care is taken to avoid its partial degradation and so, the material undergoes some degradation process
before these bers are used for any application.
They were light brown in color. The dimensions (length and
diameter) were measured using a projection (optical) microscope,
which could read up to 2nd decimal point. The morphology studies
were carried out on the received bers using both optical and scanning electron microscopes. For the optical microscopy study, the
specimens were prepared using a mixture of polyester resin with
2% catalyst and 2% initiator poured into a mold into which a bunch
of bers was kept vertically until the resin set. After curing, the
samples were ground successively using silicon carbide papers of
grit size ranging from 220 to 600 mesh sizes. Then the specimens
were polished with a sylvet cloth mounted on disk polisher using
diamond paste (6, 3 and 0.25 lm size). The polished specimens
were observed in reected light using a Leica DMRX optical microscope. For electron microscopy, ber samples were mounted on
brass studs and after gold coating were observed under a JEOL
scanning electron microscope (model JSM 6360 LV) at 15 keV
and current of 0.65 A.
The density of the bers was determined as per the standard
ABNT NBR 11931, which is similar to ASTM D 1505 and ASTM D
792 where the density of the bers is estimated by the density gradient method used for polymeric materials. In this method, chloroform having density of 1484 kg m3 and methylene chloride
having density of 1330 kg m3) were used as solvents. The method,
in short consists of immersion of a portion of the sample in a beaker containing a mixture of miscible solvents of different densities.
Then, volume of each solvent used is measured and the beaker is
lled until the bers stay oating at the center of the liquid mass
(density of the ber is equal to that of the liquid mass). Then, with
the known volumes and density values of the solvents, the density
of the ber is calculated.
For tensile testing of the bers, the procedure followed was that
the bers 50 mm in length were cut and mounted on a piece of

S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

hard cardboard with a central window. Then the cardboard was

gripped by an Instron machine (model 5565) and the sides of the
cardboard were cut before applying the nal load. Stressstrain
curves of the bers were obtained using 1 kN load cell (having precision of 0.02 N) and cross-head speed of 5 mm/min. All the tests
were carried out at room temperature (25 C) and relative humidity of 43% with an average minimum load of 0.02 N and maximum
of 2.43 N. Because of the variations in diameter of the bers along
their length and also between bers, three sets of bers were
tested with each set having a narrow diameter range. At least 10
samples were used for each set. From the stressstrain curves obtained, the average Youngs modulus (YM), ultimate tensile
strength (UTS) and% elongation were evaluated for each set. To calculate the strength values, the values of the force (F) and the area
of the curve were used, while the% elongation was calculated using
the standard method with monitoring the extension through the
displacement shown without the use of the extensometer.
For chemical analysis, the bers were chopped using knives.
The brous residues were sieved into different fractions (20, 35
and 60 mesh) and separated. The initial mass of material before
the grinding was determined (170 g). Fibers of 35 mesh size were
used for the determination of chemical composition, as this fraction was the largest. All determinations were carried out in triplicate using 25 g of the bers and average values are listed.
Moisture content of the bers was determined as per Standard:
TAPPI T212 om-02 and using the equation:

Min% W f  W o   100=W o

where M is the moisture content and Wf and Wo are the weights of

the bers in wet and dry conditions. All experiments were performed in triplicate.
The ash content of the bers was determined as per TAPPI T211
om-02 standards and calculated using the equation:

Ash% A  100=B

where A is the mass of ash and B is the original mass of the ber
sample.
The TAPPI T207 cm-99 standard was followed for the determination of soluble products in cold/hot water. Solubility in cold
water or hot water was then calculated using the equation:

S% P  P1 =P  100

where P is the initial mass of the sample, P1 is the mass after the test
and S is the percentage of soluble products in cold/hot water.
Solubility in 1% NaOH solution as per TAPPI T212 om-02 standard determines the degree of attack of the lignocellulosic materials by fungi or other deleterious agents. Also, this is important due
to the wet nature of the residue and possible degradation during
transportation. According to the standard mentioned above, lowmolecular-weight carbohydrates consisting mainly of hemicellulose and degraded cellulose in wood and pulp are extracted by
hot alkali solutions. In the case of wood, its solubility could indicate the degree of fungus decay or of degradation by heat, light,
oxidation, etc. With the decay or degradation of wood, an increase
in the percentage of the alkali-soluble material occurs. Further, the
extent of cellulose degradation during any chemical process (pulping and bleaching, etc.) is indicated by the solubility of pulp,
which has been related to strength and other properties of pulp.
Accordingly, Solubility in 1% NaOH solution was determined as
per the standard mentioned and using the equation also used for
determining the solubility in water mentioned above.
Following the TAPPI T204 cm-97 and TAPPI T264 cm-97 standards a mixture of ethanol/toluene was used to extract fats,
greases, some resins and gums, while hot water was used to extract tannins, gums, sugars, starches and colored materials. The
amount of extracts (%) was obtained using an equation mentioned

155

in the standards (TAPPI T204 cm-97 and TAPPI T264 cm-97) similar to the one used for% soluble in water, with P being the initial
mass of the sample, P1 the mass after extraction and S the percentage soluble in ethanol/toluene. The material resulting from the total extracts was then used to determine the lignin content.
Both soluble and insoluble lignin contents were determined as
per the TAPPI T222 om-02 standard. The amount of soluble lignin
was then calculated using the equation [24]:

C LS 4:53  A215  A280=300

where CLS is the lignin concentration in the sample in g L1; A215 is

the absorption by solution at 215 nm and A280 is the absorption by
solution at 280 nm.
On the other hand, the cellulose fractions (a, b and c) of the blue
agave ber were determined as described in the TAPPI T203 cm-99
standard.
X-ray diffraction (XRD) studies were carried out using a Shimadzu diffractometer (Model XRD-7000), with monochromatic Cu Ka
radiation (k = 1.5418 ), at operating conditions 40 keV and 20 mA
to determine the crystallinity of the ber following regular diffraction method. For this, a sample was prepared by cutting a small
transversal piece (0.51 mm), to make a sample with volume of
100 mm3, seeking to obtain the best random distribution from
the bers to estimate the crystallinity index. The measurement
was done with slits from 1 and the equipment was operated at
40 keV and 20 mA.
Thermogravimetric analysis (TGA) was carried out in a Metler
Toledo instrument (Model SDTA 851) with a heating rate of
20 C/min. In this case, two atmospheres were used. The rst one
was nitrogen (inert) atmosphere, which prevents combustion and
allows the degradation of components to take place one by one
and thus making it possible to identify the degradation regions of
the ber components, while under atmosphere of air/oxygen both
the reactions occur at the same time similar to oxidative atmosphere, since it is not possible to separate the different degradation
processes of the ber components such as hemicellulose, cellulose
and lignin, because all the reactions would be very complex and
they would be overlapped in the temperature ranges of these reactions [9,10]. Finally, the samples were maintained at 800 C for 10
more minutes. Experimental conditions used are: nitrogen (50 mL/
min) in the range of 40600 C and air (50 mL/min) from 600 to
800 C, after which the samples were maintained at 800 C for a
further 10 min.
Differential scanning analysis (DSC) was performed in a Metler
Toledo instrument (Model 822e) in the range of 40550 C at a
heating rate of 10 C/min in a nitrogen atmosphere at a pressure
of 104 Pa.

3. Results
It should be noted that the bers characterized for various properties in this paper are those bers obtained from tequila factory
(as explained in Section 2), where the bers (cooked bagasse) remain stored in piles whereby degradation process of the bers
inevitably could have occurred and mostly discarded as waste.
In view of this, the properties determined show differences from
those reported earlier on these types of bers (these were raw,
but not cooked ones). From the point of view of the readers, who
are new to this eld of lignocellulosic bers and hence may not
be aware of various factors that affect the properties of the ber,
detailed explanation is given in the next Section 4 to help them
in understanding the observed results. In view of this, all the results obtained in this study are described with the detailed discussions even though it may be often found to be redundant.

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S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

3.1. Density
The density of the ber was found to be 880 kg m3, which is
higher than that reported earlier (740 kg m3) for this ber [12],
but lower than that reported for other types of agave bers [25].
3.2. Morphology studies
Fig. 2 shows a histogram of the sizes of blue agave bagasse bers according to sieving. It can be seen that 32.9%, 47.8% and
19.3% of the bers sieved through mesh sizes of 20, 35 and 60
respectively were retained in sieve size 0.85 mm, 0.43 mm and
0.21 mm respectively. As can be seen from the gure, some bers
are very thick and others quite thin. Thus, each sieve retained
the bers according to their size, although during sieving the bers
may pass from one sieve to another vertically (lengthwise). The
very thick ones could have any size, but were mostly retained in
20 mesh size.
Furthermore, Fig. 3 shows a cross section (Fig. 3a) and longitudinal sections (Fig. 3b and c) of this ber. It can be seen from Fig. 3a
that thick walled cells are closely packed and have irregular lumen.
Fig. 3b is a scanning electron micrograph of a longitudinal section
of the ber, similar to that observed in many plant bers, showing
the longitudinal arrangement of a large number of brils, with
binding and pithy material in between. Some surface defects are
also evident, which might have occurred during the extraction process. At higher magnication (Fig. 3c), one can see the internal
structure showing the helical winding of microbrils. Average
length of the bers was found to be 1012 cm.

Similarly, the solubility in hot water is also higher than that reported by Iiguez-Covarrubias et al. (5.84%) for uncooked raw head
ber [20], while the ethanol/toluene extracts are comparable to
ethanol/benzene extracts (2.95% compared to 3.1%).
In the case of total lignin content, it is higher [21%] than that reported in ber both from raw [1616.8%] and cooked heads [7.2%]
[13,20]. Also, all the values of chemical constituents are higher
than those reported earlier by Cedeo Cruz and Alvarez-Jacobs
[18]. It is also interesting to note that while the total chemical
composition (cellulose content + lignin + ash) in the present study
adds to 100%, the same was not true in other studies [13,20],
since many of the constituents were not given. In practice, the total

3.3. Chemical composition

Table 1 summarizes the complete chemical analysis of blue
agave ber residues (bagasse) determined in the present study. It
can be seen that the ash content obtained [5.30%] is higher than
that reported (2%) for ber from raw heads without cooking [13],
but, is lower than that reported (8.8%) for the cooked material
[20]. On the other hand, the insoluble lignin content obtained is
similar to that reported for uncooked raw heads [13], while it is
higher than that reported [20] for the cooked material [7.2%].
There are also differences in the cellulose content obtained from
the reported ones. The a cellulose content obtained in the present
study (49.43%) is lower than that reported (64.9%) when raw heads
without cooking were used [13], but it is higher than that reported
[20] for cooked material (41.90%).

100

78.41g

90
80
70

53.98g

60
50

31.60g

40
30
20
10
0

20 mesh

35 mesh

60 mesh

Fig. 2. Histogram of sieved blue agave ber sizes. (For interpretation of the
references to colour in this gure legend, the reader is referred to the web version of
this article.)

Fig. 3. Morphology of Mexican blue agave ber. (a) Scanning electron micrograph
of the cross section of blue agave bagasse ber showing central lacuna and lumens
in cells. (b) Longitudinal section of the ber showing arrangement of cells with
some surface defects including the channels and defects.

S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

Table 1
Chemical composition of Mexican blue agave.

Content

Present study (%)a

Moisture
Ash
Solubility in cold water
Solubility in hot water
Solubility in 1% NaOH
Ethanol/toluene extracts
Soluble lignin
Insoluble lignin
Total lignin
Cellulose
a-Cellulose
b-Cellulose
c-Cellulose

10.1 0.05
5.30 0.07
9.74 0.27
10.64 0.26
35.73 0.38
2.95 0.17
5.12 0.40
15.98 1.20
21.10 1.13
73.60 0.01
49.43 0.54
15.21 1.26
8.96 1.12

On the other hand, a single ber diffraction pattern showed

dark wide concentric rings (halos) on the lm coming from the ber (not included due to poor quality of the gure). The Laue pattern obtained showed a pattern typical of cellulose bers, while
some points distributed on the lm came from a very organized
crystalline material, probably from internal microcrystalline impurities in the ber. This conrmed that spots observed in the Laue
method correspond to the sharp peaks observed in the diffractogram. However, it was not possible to identify symmetry of the
points on the lm, suggesting that the observed dark points might
have come from different small crystallites distributed in the ber.
3.5. Thermal studies

All values are average of triplicates.

of all the constituents determined by chemical analysis of lignocellulosic materials, such as the ber studied here, should be 100%.
Normally totals of 95102% are not uncommon [26] due to partial
loss of a constituent, overlapping of some constituents in analysis,
impurities present in residues and failure to account for some of
the compounds present in the material.
3.4. X-ray diffraction (XRD) studies
Fig. 4 shows the X-ray diffractogram of the ber obtained in this
study. Several sharp peaks can be seen together. The crystallinity
index (Xc) of Mexican blue agave ber was calculated at 2h values
between 5 and 70 using the equation given below, following the
reported method by Alexander [27]:

X c Ic =Ic Ia  100%

157

where Ic is the scattering of crystalline portion and Ia is the scattering of amorphous part. This method in brief is the one that is based
on the possibility of drawing a line between the spread of the crystalline and amorphous material in a certain angular interval, where
there is the amorphous halo and crystalline peaks. In the present
case, a program Dxta Version 2.6 that comes with the analysis software of XRD Shimadzu equipment was used with delineation of the
proles corresponding to diffraction of the crystalline portion (Ic)
and also the scattering of amorphous part (Ia). The crystallinity obtained from the above is found to be 70% for the ber.

Fig. 5a and b present TGA and DSC data of the Mexican blue
agave bagasse ber. It may be noted that the TG analysis gives
information about thermal stability of the bers and composition
in terms of volatile substances, organic constituents and inorganic
residues. Accordingly, it can be seen from the TGA curve that the
ber undergoes mass loss at three different temperatures, viz.,
10.8% starting at 80 C (moisture content in the ber), 63.8% at
360 C and nally 20% at 620 C.
Between 100 and 220 C, the blue agave bagasse ber presents
thermal stability (see Fig. 5a) suggesting that these bers can be
used safely up to the maximum temperature of 220 C. This temperature can be taken as that for thermal stability of blue agave ber, which is similar to that observed for Brazilian banana bers,
but slightly lower than those of sugarcane bagasse and sponge
gourd bers (250 C). This high thermal stability may probably
due to its high value of crystallinity (70%) and high lignin content.
Further, it is reported that the estimation of the amount of bulk
free water in cellulose-based materials can be measured by the
vaporization temperatures in DSC [28]. In the case of blue agave
bagasse bers, one endothermic peak was observed in DSC curve
(Fig. 5b) at 89. 2 C, corresponding to the dehydration of ber (in
agreement in the range at which 10.8% mass loss observed in
TGA curve). This is in contrast to only one peak observed at
300 C for three Brazilian bers (attributed to decomposition of
cellulose [11] and two endothermic peaks at 69.1 C and
358.0 C) for bleached cellulose obtained from sugarcane [35]
and at 126 C and 325 C for wood [29] corresponding to dehydration and decomposition, respectively. In the present case, the
amount of energy DH = 328.1 J/g was used during evaporation of
this water.
3.6. Tensile property studies

Fig. 4. X-ray diffractogram of Mexican blue agave ber.

It should be noted the bers used in the present study are not
the same as those used by some of earlier researchers [12
14,19,20] in that, present ones were received after the extraction
from the blue agave leaves left in the eld after the extraction of
juice. Considering the large variation of gauge length and diameter
of the bers used (as-received only, but not cut) for the tensile testing, as shown in Fig. 6a and b, tensile properties were determined
in three groups of diameters (no relation to either brils or other
structural aspects of bers) of the same gauge lengths and different
gauge lengths with constant diameter, using the respective stress
strain curves. The typical stressstrain curve for Mexican blue
agave ber bers is shown in Fig. 7, wherein the strain rate at
the point of maximum load is 0.09 min1 or 1.5 ms1. This is similar to that observed for banana ber, showing continuous increase
in stress with increasing strain until the maximum stress is
reached, when it breaks.
The mean tensile properties were evaluated from such curves.
The statistical treatment of these values is tabulated in Table 2.
However, it may noted that the data shown (Youngs modulus

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S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

Fig. 5. (a) TGA and (b) DSC curves of Mexican blue agave ber.

and Tensile strength) in the table demonstrates these properties do

not differ signicantly with diameter of the bers at 0.05 level with
means are not signicantly different as shown in the Tables 3a and
b.
Further, it can be seen that the mean value of Youngs modulus
(2.62.9 GPa) and % strain (1215) remain nearly constant for all
three sets. On the other hand, even though the mean ultimate tensile strength values decrease from 58.1 MPa to 41.5 MPa with
increasing mean gauge length (5198 mm) and decreasing mean
diameter (426.6328.7 lm), as can be seen from Table 3b, it may
be assumed that this property also does not differ signicantly
although diameter vs tensile strength showed inverse relationship
as observed by many others [9,10,35,36]. It thus becomes evident
that the mean UTS values obtained in the present study are much
lower than those reported range of values earlier, but the mean
values of YM and % strain are in comparable range with the re-

ported range of values for the bers with diameter range of 60

140 lm [12].

4. Discussions
It is well known that the properties of lignocellulosic bers depend signicantly on many factors, such as variety, climate, harvesting and maturity, extraction process, and the experimental
conditions during testing, among others [18]. In addition, in the
case of bers studied in the present investigations, other factors
to be considered include degradation occurred by the cooked blue
agave bagasse thrown in the Tequila industrial plant (Remain
stored in piles whereby degradation process of the bers inevitably
occurred), effect of variety and environment, etc. Accordingly, the
differences in various properties studied in this investigation in re-

S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

Fig. 6. Size distribution of Mexican blue agave ber: (a) Length distribution. (b)
Diameter distribution. (For interpretation of the references to colour in this gure
legend, the reader is referred to the web version of this article.)

Fig. 7. Typical stressstrain curve of Mexican blue agave bers. (For interpretation
of the references to colour in this gure legend, the reader is referred to the web
version of this article.)

spect of blue agave bagasse bers of Mexico and the earlier reported results on this ber can be understood on the basis of above

159

mentioned factors. Some details of this on each of the property

studied are mentioned below briey.
Thus, the difference in density values for the same type of blue
agave bers may be due to the ber extraction processes used by
Bessadok et al. [12], who obtained the bers from a pretreatment
of washed blue agave leaves of Tunisia origin by using a pectinase
solution followed by another washing followed by whitening using
bleach solution, the rst washing being done by Milli-Q water for
24 h at 25 C. On the other hand, the bers used in the present
study obtained from Mexico were by cooking the stem followed
by the extraction of the juice, resulting in the bers (bagasse) followed by keeping the bers for some period, during which likely
hood of degradation by fungi could have occurred.
Study of X-ray diffraction results of the ber showing several
sharp peaks, which may be related to a material with less structural organization and are associated with the bers crystalline
character. This is probably due to some type of sugar or some other
substance adhered during the fermentation process [21].
Similarly, the difference in various chemical constituents obtained in the present study such as cellulose, lignin and ash and
the previously reported by other workers [12,13,1820] in similar
material (blue agave ber) may be due to various factors mentioned above including geographic locations, harvesting and maturity of the plants, extraction process used for obtaining the bers,
and methodology used for chemical analysis [12,19,20,30]. Possible degradation process undergone by the bers analyzed could
also be another factor [13,20]. In the case of difference in values
for solubility in hot water between the present study and earlier
reported ones could also be due to natural resins, which are generally insoluble thermosets.
The NaOH solubility indicates that the agave brous residue
was subject to degradation. This is probably due to the fact that
the analyzed residues were obtained from tequila production,
where the head was cooked without any treatment and thus not
completely dried, leading to degradation of its bagasse before they
were analyzed. Therefore, when these bers are used, it should be
known that they are partially degraded bers, without complete
drying. In this respect, Iiguez-Covarrubias et al. [20] reported that
wet agave bagasse was subjected to degradation of organic material, following a rst-order kinetic equation. The value obtained
(35.73%) in this study is very high, considering that the acceptable
amount of solubility in 1% NaOH is between 11.2% and 17.0%
according to the TAPPI T212 om-02 standard.
Another factor that might have affected the chemical composition of the bers in the present study could be due to the time delay. For example, though the bers were sun dried and transported
to Brazil from Mexico within 3 days of the cooking process, analysis of the bers was carried out after several months, so during this
period probably the action of fungi and bacteria could have degraded part of the material. This was indicated by the strong smell
emanating from the bers used for testing. Therefore, this poses an
important issue to be considered, if large amounts of agave residues are used commercially, but at the same time it also important
to use these materials, which otherwise go waste.
In the case of thermal studies, it may be relevant here to point
out that a comparison of these results with those of bleached cellulose obtained from sugarcane [31], which are similar chemically,
but different in water content, reveals different mass losses at
about similar temperatures although such comparison may not
be proper due to differences in experimental conditions. For example, Mulinari et al. [31] reported peaks and mass loss for their samples of 4.7% at 62 C, 83.9% at 378 C of and 8.6%, at 613 C
respectively, attributing them to elimination of water, degradation
of cellulose and lignin, respectively. Accordingly, observed results
in the present study can also be understood on similar lines and
also as reported elsewhere [26,32] for lignocellulosic materials as

160

S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

Table 2
Statistical treatment of tensile properties.
Parameter

Gauge length, L0 (cm)

SD (cm)

dia. (lm)

SD (lm)

YM (GPa)

SD (GPa)

TS (MPa)

SD (MPa)

Strain e (%)

SD (%)

Mean

5.1
7.1
9.8

0.7
0.6
1.1

426.6
328.7
345.8

63.3
80.1
76.1

2.6
2.7
2.9

0.8
1.0
0.9

58.1
41.5
49.9

21.0
25.9
31.8

15
11
12

7
9
6

SD Standard deviation; dia: Diameter; YM: Youngs modulus; TS: Tensile strength.

Table 3
Statistical treatment of tensile property data.
Data

Mean

(a) One-way ANOVA: Youngs modulus

A
2.62
B
2.74
C
2.92
(b) One-way ANOVA: tensile strength
A
58.09
B
41.48
C
49.92

Variance

0.64
1.06
0.84

8
13
10

440.75
672.99
1009.45

8
13
10

At the 0.05 level, the means are NOT signicantly different.

due to (i) elimination of water, (ii) degradation of cellulose and (iii)

degradation of lignin respectively.
Beyond temperature of 220 C up to 600 C, observed mass
loss can be attributed to decomposition of different types of cellulose present in the ber. Above the temperature of 600 C, degradation of the ber can be seen due to the breakage of bonds of lignin
present in the ber [33,34]. The above two mass losses can be
attributed to oxidation of the fragments in the presence of air. Further, a residue of 6% can be seen from the Fig. 5a, probably of
mineral nature, which is similar (5.5%) to that in dry samples having 10% moisture content. Thus, it may be concluded that TGA
curves indicate about the moisture content of the ber, thermal
stability and ash content of the ber.
The observed 10.8% water loss (see TGA curve) is that of the regained water as capillary water, which can be related to environmental humidity and temperature along with composition of the
ber [28]. In fact, the water content of blue agave bagasse bers,
calculated by the difference between the weight of the ber before
and after heating at 60 C until constant, was found to be 10.8%. It
should also be noted that despite the bers were dried before performing the test it would be difcult to eliminate the water content
completely from the ber due to its hydrophilic nature, which is
present even as structurally bound water molecules.
Therefore, this water is regained by other components of the ber (soluble and insoluble lignin and very small amounts of amorphous cellulose). This is because, in addition to high crystallinity of
the ber, total cellulose of bagasse is 74% with higher amount of
more crystalline alpha-cellulose (polymer), than hemicelluloses
and hence, the access of water (moisture) to its hydroxyls is much
more difcult. These would lead to absorption of less moisture by
the ber.
In the case of tensile properties, observed stressstrain curve is
understandable since lignocellulosic bers are natural polymers
that can show viscoelastic behavior, and the mechanical behavior
of polymers depends on the mobility of their macromolecules
and thus on time (speed of the tensile test) and temperature. Such
behavior has been reported for many lignocellulosic bers [8
10,35].
Obtained mean UTS values for the blue agave bers in the present study are much lower than those reported range of values earlier, but the mean values of YM and % strain are in comparable
range with the reported range of values for the bers with diameter range of 60140 lm [12]. The differences between the obtained

mean UTS values and those reported earlier are understandable as

due to the bers are from two different countries and also obtained
by different extraction processes in addition to state of the bers
(degradation during storing). Hence, the arguments stated earlier
in respect of variations observed in the values chemical constituents of the ber holds good in this case also. In the case of Bessadok
et al. [12] the bers used could be fresh ones preventing any possible degradation compared to the blue agave bagasse bers used
in the present study thus having difference of time between their
production and testing. In fact, the high solubility in NaOH obtained in the chemical analysis suggested possible degradation of
the ber by fungi. Despite these variations, the bers studied in
the present investigation have comparable reinforcement potential
as some of the other lignocellulosic bers [58,25] and hence could
be considered equally good for their use as reinforcements in polymeric composites.
Despite lower tensile properties exhibited by these bers, it
would be worthwhile to understand the purpose of this kind of
study, which highlights the benets of characterizing cooked
Agave even partially degraded bagasse that may still be used, for
instance, as reinforcement (as chopped bers) in polymer (composites) based on properties exhibited by the ber as explained
above, which otherwise creates environmental problems. As a residue, no special care is taken to avoid its partial degradation and so,
the material undergoes some degradation process before these bers are used for any application. It should also be mentioned that
it is hard to dry bers outdoors in the sun after harvesting because
huge amounts (mountains) of bagasse are produced. On the
other hand, it would be expensive to dry them using electrical
heating. Even working with the present samples, we found it difcult to dry the bers properly since all of them were kept together.
Therefore, it can be concluded that although utilization of these bers may help prevent environmental problems from disposal of
large amounts of waste, their drying method is an important consideration for the economic feasibility of their use. Hence, the characterization of the ber as it is obtained (partially degraded) is
appropriate because in theory it may be possible to think that
the bagasse would be immediately dried and kept in conditions
that could prevent its degradation till its use, but in practice this
is not the case. This is because tequila is expensive liquor, while
the cooked agave bagasse is a byproduct, which is treated as a
waste, while it should be valued in view of its properties, which
still merit their uses.
5. Conclusions
 Mexican agave cooked ber (bagasse) extracted from the stem
of the plant have been characterized for their density, chemical
composition, morphology, tensile and thermal properties.
 The length of the ber was found to be 1012 cm, with mean
diameter of 592 lm and density of 880 kg m3.
 The bers contain 73.60% cellulose, 21.10% lignin and water
content of 10.8%, comparable values with many other lignocellulosic bers.
 Morphological studies indicated that the ber cells are regularly
arranged and are elliptical in shape with varying lumen size.

S. Kestur G. et al. / Composites: Part A 45 (2013) 153161

 Crystallinity of Mexican agave bagasse ber is found to be 70%.

 Tensile properties of these bers indicated them to be in the
range of some of the other lignocullulosic bers suggesting
them to be potential reinforcements to develop composites
similar to other similar bers.
 Mean values of Youngs modulus and % strain for three groups
of mean diameters (328, 345 and 426 lm) and mean gauge
lengths (5.1, 7.1 and 9.8 cm) did not show much variation
(2.62.9 GPa and 1215% respectively). On the other hand, ultimate tensile strength values for the same samples though
showed decreasing trend (from 58 MPa to 41 MPa), it may be
assumed that this property also did not differ signicantly when
the standard deviations of these values are considered.
 Thermal studies of Mexican agave bers also indicated that the
ber is thermally stable probably due to its higher crystallinity
and lignin content.
 With the understanding of various properties particularly tensile and thermal properties, it should be possible for the use
of these cooked bers for incorporating in polymers including
biodegradable ones. Thus, in view of abundant availability of
corn and cooked blue agave residues are abundant in Mexico,
a potential composite material, which could be compostable
and biodegradable composites with corn starch and cooked
blue agave residues could be produced there, whereby in addition to value addition to the residues, employment generation
could be a possibility.

Acknowledgements
The authors thank Centro de Miscroscopia Eletrnica da UFPR
for their help for the SEM studies, CNPq for nancial support for
this work and Prof. Graziela Muniz from Forest Engineering, UFPR,
Curitiba-PR for permitting use their laboratory to carry out the
chemical analysis of the bers. One of the authors (Dr. KGS)
sincerely thank Araucria Foundation, Curitiba for the nancial
support during the present work as well as the two organizations
(BMS College of Engineering, Bangalore and Poornaprajna Institute
of Scientic Research, Bangalore) with which he is presently associated in India for their encouragement.
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