77

A Test Methodology for Studying Liquid Penetration of Barrier Materials

A. MILLER AND P. 1
SCHWARTZ
Department of Textiles and Apparel, Cornell University, Ithaca, New York 14853, U.S.A.

ABSTRACT
A test apparatus for determining pressure at
liquid breakthrough as a function of flow
rate isdesigned and constructed. The method reveals that as flow rate increases, the
volume of material penetrated by the liquid increases. In addition,
pressure penetration
at
does not strongly depend on flow rate and even decreases with flow rate for some
materials. Peak pressure and distance to peak increase with flow rate.
Steady-state
pressure increases with flow rate but not according to the Poiseuille equation, as would be
expected. This test method permits comparison of materials in terms of barrier perfor-
mance.

A proper understanding of liquid penetration of porous
naterials is important for applications such as protective
clothing, resin impregnation of fibers for composites, and
iltration. Liquid penetration of a material is distinct from
)ther kinds of fluid/material interactions in that it in-
volves the saturation of a material, and so many of the
equations used to describe saturated flow are not appli-
these deficiencies [16, 19], but these methods still de-
pend on the operator.
A test method developed by Miller and Clark [17] uses
a piston and cylinder
setup, where force for penetration is
measured as a function of flow rate and the force is
recorded by a pressure transducer. They found that pres-
sure dropped upon contact with the material and then

cable. In addition, it is differentiated from the saturation
)f wettable materials in which there is an attraction
between the material and the challenge liquid,
leading to
pontaneous wetting. For barrier materials, the liquid
nust be physically forced through the material because
he material repels a challenge liquid.
There has been much research on the interaction of
luids and porous media. Specifically in the case of
extiles, there have been several studies of saturated fluid
penetration of woven fabrics [6, 13, 18, 20]. Other re- TEST
earch of textile/fluid interactions involves unsaturated
low. Kissa [11] has presented a comprehensive review
of nonsaturated fluid flow in textiles.
Many instruments have been used to study fluid pen- cell
tration of fibrous systems in an effort to understand
esin impregnation during composites manufacturing [2,
, 8, 9, 12, 21, 22]. Methods have been developed to test
une penetration resistance of barrier materials
[1, 4, 5, 7, secured with four bolts between an
4, 23]. Studies have evaluated these test methods, show-
ing limitations with all of them [14,15]. Specific prob-
lems with the test methods include
difficulty in ranking through the material to escape. As the Instron crosshead
materials (most tests give a pass/fail result), limited is
ressure range, long test time, and
operator-dependence. forcing the fluid through the barrier. The load is recorded
Other test methods have been designed in response to
1
To whom all correspondence should be addressed.
rose to a peak pressure, followed
by a drop in pressure to
steady-state flow. Their apparatus did not measure the
exact point of breakthrough and
they only tested hydro-
philic materials.
In this study, we present a methodology for
studying
liquid penetration of barriers, and we investigate three
materials using this test.
Experimental
APPARATUS
We have designed and constructed a test apparatus for
measuring liquid penetration, consisting of a brass piston
and cylinder mounted on an Instron compression load
(Figure 1). The diameter of the cylinder is 37.5 mm
and the height is 150 mm. The challenge fluid is placed
inside the cylinder on top of the piston. The fabric
sample is placed over the opening of the cylinder and
O-ring and a rigid
Plexiglas® plate, which has many small holes (0.4 mm
diameter, 0.5/mm
) to allow air and water that pass
2
lowered, the cylinder is pushed down on the piston,
by a computer interfaced with the Instron and an addi-
tional computer that records data from both the Instron
and the fluid sensor. In this method, pressure depends on
flow rate.

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 78
FIGURE 1. Cross-sectional view of test set-up.
We have constructed a fluid sensor (Figure 2) by
inlaying a perforated brass disk into the Plexiglas plate
so that the brass rests against the fabric sample during
testing. The barrier material, challenge liquid, and any air
over the challenge liquid then form a resistor between the
cylinder and the sensor. Initially, we used direct current
(Dc) to probe sensor resistance, but the fluid passage
through the material caused spurious voltage, affecting
the resistance measurement. We then used a model 120
lock-in amplifier, manufactured by Princeton Applied
Research (Princeton, NJ) to generate 5 volts of alternat-
ing current (AC) at 5000 Hz. Because the lock-in only
measures the changes in voltage at the frequency of the
generator, the irrelevant changes in voltage cease to be a
problem. In addition, purified water conducts Ac better
-
than Dc, so the observed change in resistance with pen-
etration is more significant with AC current. Fluid pene-
FIGURE 2. Schematic of penetration sensor.
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tration is determined by looking at the changes in am
plitude of AC voltage across the barrier material whil
applying an AC voltage of constant amplitude across th
test setup and a reference resistor. Prior to fluid penetra
tion, little or no current passes through the fabric. Thu<
the resistance of the test apparatus is much higher tha
that of the resistor. With penetration, the water forms
link through the material between the two contacts, an
the resistance of the test apparatus drops. The lock-i
records the change in voltage amplitude, amplifies thi
change, and transforms it to DC voltage that can b
recorded by the data acquisition system.
Data come from both the Instron and the lock-i
connected to the fluid sensor using an analog-to-digiti
input/output bus (ADBL/0) manufactured by Beehiv
Technologies (www.bzzzzzz.com), which is connecte
to a Macintosh SE computer for this project. Because th
Instron load cell’s full scale output is 10 volts and th
maximum input of the data acquisition device is 5 volt;
a simple two-resistor voltage divider reduces the voltag
between the Instron and the data acquisition device. Th
maximum sampling rate, 32 data points per second, i
determined by the speed of the computer processor.
MATERIALS
We tested three barrier materials: materials A and
are aramids for filtration applications, provided by Pal
flex Corp. (Putnam, CT), and material C is a bilaminal
polypropylene used for protective medical garment
provided by 3M (Minneapolis, MN). Table I lists som
properties of the materials.
TABLE I. Properties of barrier materials tested.
B
Membrane layer only.
The surface contact angle was determined with tl
sessile drop method. Note that this is the macroscop
contact angle for the surface of the fabric and does ni
necessarily correlate with the microscopic contact ang
inside the material’s pores. All materials tested wen
hydrophobic (liquid beaded up on the material surface
Air permeability was determined with a simple manon
eter set-up and thickness according to ASTM D 1777-6
We took SEM images (Figure 3) of the surfaces of ;z
three materials and attempted to use these images
 79

(TR1/Princeton, Princeton, NJ). Water for penetration

testshad a surface tension of 70 (±2) mN/m. In addition,
aliquots of water taken after testing revealed that the test
did not significantly affect the surface tension of the
water. The resistivity of the water, found
using a Sybron/
Barnstead resistivity meter, was 1.6 Mfl.

FLUID PENETRATION TESTING

We tested five samples of each material at each of four
different Instron crosshead speeds (the speed that the
piston displaces the liquid~2, 10, 50, and 100 mm/
f1lin-corresponding to four different fluid flow rates.
The load at fluid penetration (as indicated by the sensor),
the peak load, and the steady-state load
(Figure 3) were
calculated by subtracting the initial load due to piston/
cylinder friction from the recorded loads at each of these
points.
We also tested the effect of progressively
decreasing
the speed, again with five samples of each material. The
piston was started at a speed of 100 mm/minute, allowed
to go to steady state, and then
progressively lowered to
50, 20, 10, 5, 2, and I mm/min. We recorded the load
created by the fluid flowing through the material at each
of these speeds.

Results and Discussion

A plot of data collected by the ADBUo is presented in
Figure 4, showing the time and load at the point of
contact between the fluid and the material, the
point of
penetration (indicated by the change in voltage), the
peak, and steady state. One unusual attribute of the data

FIGURE 3. SEM images of material surfaces: (a. top) material A, (b,

middle) material B, (c, bottom) material C.

etermine pore size distribution. However, the pore size

istributions we found with image analysis were not
insistent with the results found with air permeability
nd liquid penetration testing. This is consistent with
revious research [10, 12] showing that surface imaging
not an adequate way to describe the
pore structure of
taterials because it describes the surface rather than the
ilk of the material. An accurate pore size measurement
necessary to estimate the penetration pressure with the
aplace equation.
Purified water was provided by a Bamstead Nanopure
filtration unit. Water surface tension was determined
FIGURE 4. Typical plot of data (material C with a crosshead speed of
-ior to penetration testing using a TRI wetting balance 10 mm/min).

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 80

is the initial decune in sensor voltage and then the increase equal to the Laplace pressure for that pore and the forr~

in sensor voltage after reaching a minimum. These anom- to flow through a pore (FllmB) as being eclual to thi
alies are due to two factors. First. alternating current is Poiseuille pressure for that pore. Thus. the total forci
sensitive to water vapor (DC is not). Part of the initial (Fy) for the illustrated steps is as t~ollows:
decrease in voltage may be due to water vapor contact with
the sensor. Second, the resistivity of the material changes
with compression, and this causes most of the initial drop in
voltage as well as the increase in voltage as the material
recovers after minimum.
reaching a

The peak in the load data is interesting. Miller and

Clark [ 17] saw a similar peak, and they explained that
peak as corresponding with fluid penetration. In our the
work, the peak does not correspond with fluid penetra- And at steady state. the total force is equal to sum c

tion (which occurs consistently before this peak). After
the peak, the load decreases to a steady-state load cor-
responding with saturated flow.
Fluid penetration through materials is commonly de-
scribed by a capillary bundle model using the Laplace
equation (Equation 1 ) to describe penetration into the
material and the Poiseuille equation (Equation 2) to
describe flow through the material:
’
the Poiseuille force for every tilled pore (E F&dquo;&dquo;&dquo;,
, I
Given mconsecutive pores, if F&dquo;&dquo;&dquo;&dquo;, < there wi
be a drop in force equal to Flilllll - F,~&dquo;~&dquo;&dquo;. Thus. th
drop in load from the peak to the equilibrium stat
represents a transition from the force to wet the niateril
to the force to continue flowing through the material (F,
-

F,,,,,), where the wetting force is greater than th

continuous flow force.
Figure 6 shows the distance the cylinder traverst
from first contact of the liquid with the fabric to pen(
tration versus flow rate (in all graphs. the error bai
.

and
represent the standard deviation). It. is difficult to gai
any quantitative information from the distance at pen<
tration since the variability increases with flow rate. Th
is because the data acquisition device is limited in tt
where L = pore length, t = time. r = pore radius, y
amount of points taken per second. At a faster flow rat
=
liquid liquid/material contact
surface tension, 0 =

fewer points are taken, leading to more variation. We c;

angle, ~ liquid viscosity,
=
and Q liquid flow rate.
=

Expanding on the capillary bundle model, the peak in the
load (Figure 4) can be explained (Figure 5). Each rect-
angle (labeled a, b, c, and d) represents the same set of
four connected pores (numbered) and shows the progres-
sion of fluid being forced into the material.
,
explain a possible increase in distance: As flow ra
increases, it is more likely that the fluid will fill mo
pores due to the added pressure created by viscous dn
between the fluid and the material. Thus. it is possib
that fluid would actually take a longer path at higher flo
rates because more pores would be filled in the beginnir

of the test.

FIGURE 5. Simplitied illustration of fluid filling four connected pores.

Usingthe Laplace equation to describe fluid filling a

pore and the Poiseuille equation to describe flow through
a pore, we have the force to fill a pore (F till) as being FIGl~I&OElig; 6. Distance to penetration versus l:ro~~hc:~’.i speed.

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 81
Also of interest is that the travel distance is
greater
than the thickness of the material. The excess distance is
likely due to air that is not forced through the material
until after the liquid comes in contact with the material
and the small change in cylinder diameter at the
O-ring.
Because the material is so thin, this leads to a large error
in the distance measured.
The data show an increase in pressure at penetration from
materials A to B and from B to C, indicating that material
C has the smallest pores. Materials A and B
may have pores
that are just as small as those in material C, but the fluid will
preferentially fill larger pores, meaning that materials A and
B have a larger maximum pore size than material C.
All materials show a significant decrease in
pressure at
penetration at test speeds between 10 and 50 mm/min
(Figure 7). This is consistent with the explanation above
and again is most likely due to the number of data
points
taken per unit, time remaining constant. The
penetration
point is taken as the point at which the slope of voltage
is greatest. Actually, the point
may be anywhere between
this point and the next point recorded. The distance the
piston travels between data points increases with flow
rate, leading to a perceived drop in pressure with in-
creased flow rate. In addition, we have found some
evidence that the pores are enlarged at higher flow rates,
but this is not conclusive.
FIGURE 9. Peak pressure versus crosshead speed.

with the higher permeability materials. At penetration,

there are only a limited number of paths open through the
material. At higher flow rates, more fluid is
being pushed
through these paths. If more pores are being filled at
higher flow rates, then smaller pores are being filled at
higher flow rates and more fluid is passing through the
material. This increases the pressure in two ways.
Smaller pores lead to higher pressures as predicted by the
Laplace equation, because more fluid flow leads to
higher pressures as predicted by the Poiseuille equation.
At the flow rates tested for this study, it is
typical that
the steady-state pressure (Figure 10) is lower than the
FIGURE 7. Pressure at penetration versus crosshead speed. peak pressure. We also observed that the difference
between peak and steady-state pressures decreases as
There is flow rate increases. Once the material is penetrated, the
asignificant increase in the distance between fluid can pass through this opening or fill more of the
vater contact with the material and
peak force with material. Whether the fluid passes through the material or
rosshead speed (Figure 8). Studies have shown that a
fills a new pore depends on the pressure each requires.
iigher flow rate leads to more capillaries being filled [9,
0]. Thus, this increased distance is consistent with these Following Newtonian physics, we would expect the
force on the system to be minimized. After fluid pene-
Ither studies. As flow rate increases, more material is
tration, it is likely that if all the fluid passed through this
illed and the distance to reach the peak force increases.
one opening, it would cause a
Similar to the increase in time to peak, there is a greater force than filling
more of the material. As more
passages are opened
ignificant increase in peak pressure with flow rate (Fig- through the material, this passage force decreases, mak-
re 9). The slope of peak
pressure versus flow rate is less ing filling the material the higher load-inducing option.

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Downloaded from trj.sagepub.com at SONA COLG TECH on July 24, 2015

rates and then using the Leplace
equation, we can get a
reasonable estimate of the largest pore size present in the
material. We can then calculate the
largest pore size
penetrated at each of the speeds using the Laplace equa-
tion with the peak pressure at each of the
speeds to get an
idea of the range of pore sizes in the material. We can
estimate the smallest pore present in the material
by
calculating the pore size using the Laplace equation at
the point when the material follows Poiseuille behavior
(thereby indicating that all available pores in the material
have been filled).
,
Conclusions
We have presented a test methodology for
determining
pressure at penetration as a function of flow rate. The test
differentiates between materials, is independent of an
operator, and is fast, making this a good method for
research of barrier materials. Our tests of materials with
this method have shown that flow rate increases the
amount material that is penetrated
by fluid, pressure at
penetration does not strongly depend on flow rate and
even decreases with flow rate for some
materials, peak
pressure and distance to peak increase with flow rate, and
steady-state pressure increases with flow rate but not
according the Poiseuille equation. This further supports
the theory that more pores are filled at higher flow rates.
This test method also offers some
insight into the pore
size distribution of materials and could be
.
adapted to
investigate fluid penetration of other porous systems
such as resin impregnation of fibers for
composites.
ACKNOWLEDGMENTS
This research was supported by a grant from the Cor-
nell College of Human Ecology and Agricultural
Exper-
iment Station grant 329-424. Dr. Adiletta of the Pallflex
Corp. and the 3M Corp. donated the materials. Professors
F. Rodriguez and P. Baveye provided
many ideas for the
experiments.
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