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The Journal of The Textile Institute


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A comparative study on natural fibre density


measurement
a a b b
M. Truong , W. Zhong , S. Boyko & M. Alcock
a
Department of Textile Sciences , University of Manitoba , Winnipeg, MB, Canada
b
Composite Innovation Centre Manitoba Inc. , Winnipeg, MB, Canada
Published online: 03 Aug 2009.

To cite this article: M. Truong , W. Zhong , S. Boyko & M. Alcock (2009) A comparative study on natural fibre density
measurement, The Journal of The Textile Institute, 100:6, 525-529, DOI: 10.1080/00405000801997595

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The Journal of The Textile Institute
Vol. 100, No. 6, August 2009, 525–529

A comparative study on natural fibre density measurement


M. Truonga , W. Zhonga∗ , S. Boykob and M. Alcockb
a
Department of Textile Sciences, University of Manitoba, Winnipeg, MB, Canada; b Composite Innovation Centre Manitoba Inc.,
Winnipeg, MB, Canada

This is a study for the comparison of existing test methods for measuring the density of natural fibres to be used as
reinforcement in biocomposite materials. Normally, any such method is evaluated by referring to its accuracy, cost, speed
Downloaded by [University of California, San Francisco] at 07:34 14 December 2014

of test result (i.e. how quick a method is to give the result), and whether it is convenient and safe to use. Through literature
review, we identified five such methods: (1) diameter and linear density, (2) Archimedes, (3) helium pycnometry, (4) gradient
column and (5) liquid pycnometry. The same sample (oilseed flax fibres) was tried using these methods to measure its density.
As a result of the study, two methods are recommended: Archimedes (with the use of canola oil as immersion fluid) and the
helium pycnometry. The former was found to be simple, quick to give the result and incur lower cost, and therefore promising
for general use in measuring the density of natural fibre, but the latter, although capable of providing more repeatable results,
be at a much higher cost.
Keywords: flax fibres; natural fibres; density; composite materials

Introduction reinforcement (fibre), dC the density of the composite, dM


There has been a growing urgency to develop new bio- the density of matrix, R the weight percent matrix in the
based composite materials for their advantages of being composite and r the weight percent reinforcement (fibre) in
renewable, recyclable, sustainable and ecoefficient. Natural the composite.
fibre reinforced composites are emerging as a viable al- However, there is currently no standard test method
ternative to glass fiber reinforced composites especially in for natural fibre density in the industry. The purpose of
automotive parts and building materials (Goutianos, Peijs, this study is, therefore, to recommend an appropriate test
Nystrom, & Skrifvars, 2006; Magurno, 1999; Mohanty, method for the measurement of natural fibre density (Li,
Misra, & Drzal, 2002). Bast fibres, including flax, hemp, Mai, & Ye, 2000; Soykeabkaew, Supaphol, & Rujiravanit,
coil and jute fibres are among the most popular natural fi- 2004; Wool et al., 2002).
bres in such applications because of their high stiffness and Five density test methods used for high-modulus fi-
strength. bres or plastics were found through a review of academic
Fibre and void volume fractions are important pa- literature journals and standardised tests (e.g. ASTM).
rameters in evaluating the quality of composite materials, They are diameter/linear density (Soykeabkaew et al.,
whereas accurate fibre and void volume fraction evaluations 2004), Archimedes (ASTM-D3800–99, 2005), helium py-
are based on the knowledge of fiber density, as represented cnometry (Rude, Strait, & Ruhala, 2000), gradient col-
in the equations according to ASTM D3171 (1990) and umn (ASTM-1505–03, 2005) and liquid pycnometry (Rude
ASTM D2734 (1994): et al., 2000). Of these, three were chosen for this study: di-
ameter/linear density, Archimedes and helium pycnometry.
Fibre volume in a composite (% ) They were compared by referring to the quality of results,
 cost, how quick a method is to give the result, and whether
WR dR it is convenient and safe to use.
=  − 100 (1)
WC dC
Void content in a composite (% ) Materials and methods
 
R r Oilseed flax fibres were used in the present study, as it is one
= 100 − dC + (2)
dM dR of the most frequently used bast fibres in the development
of natural fibre reinforced composites. Prior to testing, the
where WR is the weight of the reinforcement (fibre), WC flax fibre sample was conditioned in an oven at 60◦ C until
the weight of the composite specimen, dR the density of the the moisture content was reduced to below 5%. The fibre


Corresponding author. Email: zhong@cc.umanitoba.ca
ISSN 0040-5000 print / ISSN 1754-2340 online
Copyright 
C 2009 The Textile Institute
DOI: 10.1080/00405000801997595
http://www.informaworld.com
526 M. Truong et al.

was dried to ensure that all specimens to be tested were at Method 3: helium pycnometry (Rude et al., 2000)
a consistent moisture level. The flax fibres were then kept Specimen for this test was also a bundle of fibres, and 10
in sealed specimen bags so that they would remain at a samples were tested to give an averaged value. This test
constant moisture level during the test. method was similar to the Archimedes method, but was
applied using a gas medium rather than a liquid one. He-
lium gas was used to test the fibre volume through what
Method 1: linear density and diameter calculation was called the helium gas pycnometer. A known volume
(Soykeabkaew et al., 2004) of helium gas was contained in the pycnometer’s refer-
The specimen, a long-single fibre, was cut into small ence cell. During a test, the gas was released slowly from
splices, placed onto a microscope slide, and projected onto the reference cell into the sample cell where the fibres were
a screen through the microscope. Its diameter was mea- located. The pressure of the helium gas that remained in
sured using a ruler in millimetres. Linear density was cal- the reference container was used to determine the volume
culated by measurement of the masses and lengths of the of the fibre sample. Mass of the sample was measured on
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specimens tested. Namely, 100 fibres were tested to deter- a balance, and the density of the fibre was determined by
mine an average diameter and 10 fibres to determine the dividing the mass by the volume (Rude et al., 2000).
average linear density. The average linear density and di-
ameter were used to calculate the volume density of the
Method 4: gradient column (ASTM-1505–03,
fibre ρ f (Arbelaiz et al., 2005; ASTM-D1577–01, 2005;
2005)
ASTM–D2130, 2005; Soykeabkaew, 2004):
ASTM 1505–03 (2005) is usually used. In such a test, den-
sity of the specimen (a bundle of fibres) must be matched
M
ρf = πd 2
(3) with that of the liquid. The apparatus used is a column
4
l composed of liquids of different densities. The specimen is
submerged in the column, and the closest calibrated glass
where M is the mass of a fibre specimen, d the average float serves to determine the density of the sample. No way
diameter, and l the length of a fibre specimen. is known to directly measure the weight or volume of the
fibre sample. Since we have to depend on the closest cal-
ibrated glass float to tell the density of the sample tested,
accuracy of the test has to be questionable. In addition, it re-
Method 2: Archimedes (buoyancy) quires costly equipment developed specifically for the type
The sample, a bundle of fibres, was weighed in air and of specimens to be tested. Thus the test was not selected in
then in a liquid that was used to wet the sample and was this study.
smaller in density than the sample. The difference of the
two media was the buoyancy force. The weighing process
was conducted on an analytical balance with a resolution of Method 5: liquid pycnometry (Rude et al., 2000)
0.0001g, and was adapted for suspension weighing through
This test method is similar to the Archimedes and helium
a stainless steel suspension wire approximately 0.4 mm
pycnometry methods, and specimen used is also a fibre
in diameter. The buoyancy force was converted to sample
bundle. There is one thing in particular, however, the test
volume by dividing the liquid density. The sample density
specimen must be less dense than the test fluid. Since the
ρ f was acquired by dividing sample weight in air with
fibre sample is weighted in air and then placed into a liquid
sample volume (ASTM-D3800–99, 2005):
pycnometer, this method permits a direct measurement of
the fibre sample’s volume (namely, the liquid that is dis-
(M3 − M1 ) ρl placed in the pycnometer gives a reading of the sample
ρf = (4)
((M3 − M1 ) − (M4 − M2 )) volume). Then density of the fibre is calculated by the mass
and volume. This test method was not chosen in the present
where ρ l is the density of liquid, M1 weight of suspension study because the choice of test fluids is limited by the
wire in air, M2 the weight of suspension wire in liquid (to density of the flax fibres, and it is similar to other selected
immersion point), M3 the weight of suspension wire plus methods.
item whose density was to be determined in air and M4
weight of suspension wire plus item whose density was to Results and discussion
be determined in liquid. Trial results for the three chosen test methods are sum-
The immersion liquids tried in this study were canola marised in the appendix, and performances of these meth-
oil, water, ethanol, methanol, acetone and glycerol. Seven ods are summarised in Table A1. The tests were timed to
fibre samples were tested for each immersion liquid. acquire the average time to conduct each test and allow
The Journal of The Textile Institute 527

The Archimedes method


Strength of this method is that the equipment is easy to
set up and dissemble, and simple equations can be used
to calculate the density of the fibre. In addition, the test
apparatus is the least expensive, and the consumables re-
quired are the immersion fluids, which are also of low cost.
Furthermore, this test requires the least amount of time to
conduct. The accuracy and repeatability of measurements
are highly dependent on the immersion fluid used. Water
and ethanol provide the poorest results with respect to these
criteria, whereas canola oil gives the best, showing excellent
agreement with published values for flax fibre density in the
Figure 1. Mean and standard deviation of fibre density from
range of 1.4–1.6 g/cm3 . Another advantage of the canola
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different tests. oil is that it is harmless and does not create any health and
safety risks. But some of the alternative chemicals that are
used for this test, such as ethanol, acetone and methanol,
equipment set-up and calibration. A detailed comparison may pose a slight health risk and require worker protection
of timing and equipment capital costs are given in Table from harmful vapours.
A2. For statistical analysis of the data collected, the average A recommendation regarding this test is to select a fluid
and standard deviation were used. The results are presented with low viscosity and surface tension, because it coats the
graphically in Figure 1. To assess the accuracy of each test, fibre well, and it allows the fibre to sink into the fluid and
results were compared to the published values of flax fi- be easily immersed.
bre density, which were found to range from 1.4 g/cm3 to
1.6 g/cm3 (ASTM-D276, 2005; Collier & Tortora, 2001).
It should be noted that no experimental results were The helium pycnometry method
available for the Archimedes test using glycerol. Owing to Measurements from this test method show excellent agree-
the high viscosity of the liquid, the fibre was not easily ment with published values for flax fibre density in the range
immersed, which caused difficulty in conducting the test of 1.4–1.6 g/cm3 . This method also provides the most re-
according to the prescribed directions. Although an attempt peatable measurements for the density of the fibres as shown
was made, reliable readings were not obtained. by the small standard deviation of the results. Its strength is
that there are no harmful chemicals used to conduct the test,
and it is a quick and easy test procedure for any operator
The linear density and diameter calculation method who has become familiar with the equipment (this means,
Strength of this test method is that it is safe to conduct, then, that some worker training is required). Disadvantage
as there are no chemicals involved. No specific protective of this test method is that it requires specialised equipment.
equipment is required. It is also an easy and simple test to That is, although apparatuses used in other tests may have
set up, and the results are calculated by simple equations. alternative uses within a laboratory, the helium pycnometry
The amount of worker training required to conduct this test equipment is designed specifically for density testing. This
would be minimal. The capital cost of the equipment for this equipment is also more expensive than apparatuses for the
test method was lower than the helium pycnometry method other tests.
and comparable to the cost for the Archimedes method. The
consumables required to conduct the test, such as slides,
cover slips and distilled water, are inexpensive and readily Conclusion
available in a standard laboratory. The main weakness of This study was conducted to compare existing test meth-
this test method is that it gives poor accuracy compared ods for measuring the density of natural fibres to be used
to the published values for flax fibre density, and it is by as reinforcement in bio-composite materials. Five methods
far the slowest test, requiring approximately 2 h for the were identified through a literature review. And three out
results to come out, as this method recommends testing of five were used in the present study. They are the diame-
100 fibres to determine an average diameter and 10 fibres ter and linear density, Archimedes, and helium pycometry.
to determine the average linear density. There is also a large Trials were conducted on a single sample of oilseed flax
variation in the density results compared to the other two fibres using the three methods to measure fibre density. The
test methods. This variation is caused by the variation in various methods were evaluated by referring to accuracy,
the diameter along the fibre length as well as irregularity in cost, how quick a method is to give the result, and whether
cross-sectional shape of natural fibres. it is convenient and safe to perform.
528 M. Truong et al.

As a result of the work, we are now in a position to favour ASTM-D1577–01. (2005). Standard test method for linear density
the Archimedes method (with canola oil as immersion fluid) of textile fibers. ASTM International, West Conshohocken,
and the helium pycnometry method, due to their better, com- PA.
ASTM-D2130. (2005). Standard test method for diam-
parable accuracy, and to the fact that no harmful chemicals eter of wool and other animal fibers by micropro-
are involved in them. When repeatability is considered, the jection. ASTM International, West Conshohocken,
helium pycnometry test is still more preferable because PA.
it provides a significantly lower variation between results. ASTM-D2734–94. (1994). Standard test method for void
However, the Archimedes test is less expensive in terms content of reinforced plastics. ASTM International, West
Conshohocken, PA.
of start-up costs, as indicated by requirements for capital ASTM-D3171–76. (1990). Standard test methods for fibre
equipment and worker training. Overall, while the canola oil content of resin matrix composites by matrix digestion.
Archimedes test is a simple, quick and inexpensive method ASTM International, West Conshohocken, PA.
for general use in measuring the density of natural fibres, the ASTM-D3800–99. (2005). Standard test method for den-
helium pycnometry method is capable of providing higher sity of high-modulus fibers, ASTM International, West
Conshohocken, PA.
quality results. This method would be preferred where fac-
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Collier, B.J., & Tortora, P.G. (2001). Understanding textiles.


tors such as stringent demands for accuracy or a high vol- Prentice Hall, Englewood Cliffs, NJ.
ume of testing exist to justify the additional cost. Goutianos, S., Peijs, T., Nystrom, B., & Skrifvars, M. (2006).
Development of flax fibre based textile reinforcements for
composite applications. Application of Composite Materials,
Acknowledgement 13, 199–215.
Li, Y., Mai, Y.W., & Ye, L. (2000). Sisal fibre and its composites:
We should like to indicate our gratefulness to the Department of A review of recent developments. Composite Science and
Agriculture and Agri-Food Canada, and Composite Innovation Technology, 60, 2037–2055.
Centre Manitoba Inc (CIC), for the support they provided us in Magurno, A. (1999). Vegetable fibres in automotive interior
the study. components. Die Angewandte Makromolekulare Chemie,
272, 99–107.
Mohanty, A.K., Misra, M., & Drzal, L.T. (2002). Sustainable
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Appendix

Table A1. Summary of experiments.

Ease Speed of Health


Test methods Accuracya Repeatability of use test result and safety Cost

Diameter/linear density Poor Poor Excellent Poor Excellent Good


Archimedes immersion fluid methanol Fair Fair Excellent Good Fair Good
Acetone Poor Fair Excellent Good Fair Good
Canola oil Excellent Good Excellent Good Excellent Good
Water Poor Poor Excellent Good Excellent Good
Ethanol Poor Poor Excellent Good Fair Good
Helium pycnometry Poor Excellent Good Good Excellent Fair
a The accuracy is rated according to comparison to the published results of 1.4–1.6 g/cm3 (AATCC, 2006; Arbelaiz et al., 2005; ASTM-D276, 2005;
Collier & Tortora, 2001).
The Journal of The Textile Institute 529

Table A2. Timing and costs comparisons.

Timing (minutes)
Samples Set up and
Test methods needed Test calibration Equipment Costa

Diameter/linear density 100/10 120 20 Micro projector $800.00


Balance $3,000.00
Ruler $1.00
Razor blades $0.50
Total $3,801.50
Archimedes 7 45 20 Density determination $841.55
kit
Blance $2,500.00
Vacuum desiccator $31.00
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and pump
Total $3,372.55
Helium pycnometry 10 35 35 Pycnometer $6,490.00
Gas regulator $575.00
Balance $2,500.00
Total $9,565.00
a Quoted in Canadian Dollars.

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