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Integrity Testing
Introduction
Test description
Theoretical principles.
Among other things, a pressure
gradient that is dependent on
pore size is necessary to overcome negative capillary forces
(cohesive forces). This pressure is
generally called the "Water
Penetration Point" (WPP), the
pressure at which water is
pressed through a hydrophobic
membrane. The WPP is dependent on the hydrophobicity of the
filter material and the pore size
and is comparable to the bubble
point.
Dmax =
4 cos
k
p
D max =
p = Available upstream
differential pressure
(bar |psi)
= Correction factor
(required since
membrane filter pores
are not cylindrical
capillaries)
300
250
200
150
100
Water Penetration
50
Water Intrusion
0
0
3
4
Test Pressure (bar)
p1
V1 p
V = V2 - V1 = V1 p - 1 =
2
(p1 - p)
with:
p1: Absolute pressure at the beginning of the pressure drop
measurement [mbar]
p2: Absolute pressure at the end of the pressure drop measurement
[mbar]
p: = p1 - p2
V1: Upstream Volume at the beginning of the measurement [ml] (= Vn)
V2: Upstream Volume at the end of the measurement [ml]
The increase in Volume per time is defined as:
V
Vn p
t = (p1 p) t
This value is defined as one easily understands as the Water Flow
Value. This value is basically linked to the Water Intrusion Value by a
simple mathematical correlation:
WIT =
V
t
p1 - p
Vn p
(p1 - p)
Vn p
=
=
1000 mbar (p1 - p) t 1000 mbar 1000 mbar t
The Water Intrusion is a value that has been defined in analogy to the
diffusion. For small pressure drops (< 5% of the absolute test pressure),
the following equation holds:
Diff. =
with:
Vn:
p:
1000 mbar:
t:
Vn p
1000 mbar t
WIT =
Vn p
1000 mbar t
If one imagines the volume V that has been added to the upstream
Volume due to the Water Flow to be filled with gas, it would use a
different volume at an ambient pressure of 1000 mbar. Again, the
required volume at 1000 mbar (V10OO) can be calculated with Boyle
Mariott's law to be:
V1000 = V
Principle of WIT testing
(p1 - p)
1000 mbar
Test parameters
System set-up.
The WIT can be used in a variety
of air filtration applications that
require minimal engineering
changes, however, some times
systems may have to be reconfigured. This is where the Sartorius
Technical Support team comes to
your assistance.
The diagram to the right shows
an example of a manual WIT system. The basic construction does
not differ significantly from that
used for the diffusion test. In
principle, WIT systems can be
designed as manual, semi-automatic and fully automatic units
to suit the applications, e.g.,
sterile venting systems for autoclaves, Iyophilizers, fermenters
and tanks.
Basic requirements for the
test are:
1. The surface tensions of the
water used must be > 72
dynes/cm.
2. Minimized temperature difference between the water and
the inlet air 1k.
3. Temperature fluctuations must
be avoided during the test.
4. Filter element must be completely hydrophobic.
5. Adequate effective filter area,
i.e., > 0.1 m2.
6. The integrity tester must have
sufficient accuracy, e.g.,
Sartocheck unit.
Operating sequence:
1. Completely fill the upstream
side of the filter housing with
water.
2. Close all upstream valves.
3. Connect the integrity tester,
e.g., Sartocheck 3 unit.
4. Start the test: The unit performs the WIT automatically.
5. The test is completed and the
results are printed out.
6. Empty the filter housing
through an appropriate drain
or condensate valve.
7. Briefly vent dry using pressurized air with the inlet and
drain valves open.
8. Start operating the system.
Maximum permissible
intrusion rates
False failures and troubleshooting.
If the filter cartridge does not
pass the test, it might be that
partial hydrophilization of the
membrane has occurred. In this
case, the filter must be steamsterilized for at least 30 min. at
121C or 134C and then repeatedly blown dry with hot air.
Other false failures might be
attributable to water surface
tension and temperature fluctuations. All of these factors will
invariably cause elevated water
intrusion values (false failures).
Experience has shown that these
increased values indicate
marginal failures and do not
lead to high water flow rates or
extreme pressure drops. An
isopropanol|water test will determine whether one of these
causes is the problem or whether
the filter cartridge is out of
specification. Fault free filters
will pass the solvent test because
this test cannot detect any
hydrophilization or reduced surface tension of the water used
for the initial WIT.
After the WIT, the filter
cartridges need to reach their
original air flow rate as quickly
as possible. In other words, they
must not become blocked with
water, e.g., residual water in the
fleeces. The time that the filter
cartridge needs to achieve 100%
of the original flow rate is called
the blow-down" time.
Test pressure.
The high air pressures needed to
force water penetration of the
PTFE membranes used in the
Sartofluor filter cartridges result
in very high test pressures used
for the various pore size ratings.
This increases the tests reliability,
accuracy and precision.
Pore Size Water
WIT Test
Penetration Pressure
Pressure
bar psi
bar psi
0.20 m
4.5 65
2.5 36
0.45 m
2.8 41
1.5 22
Difference in temperature.
False failures may occur if the
temperature difference between
the test air and the water is too
great. If the water temperature
is much lower than the air temperature, great drops in pressure
and high intrusion rates can
result. If the water temperature is
much higher, the pressure drops
will be too low.
This situation can be remedied by
storing the water in a storage
tank in the room where the test
will be performed or by filling the
housing with water adjusted to
the right temperature.
Low surface tension of
the water.
This situation mostly arises when
the tanks being used are not
cleaned and rinsed thoroughly,
old ion exchange resins are used
for preparing the water, or the
water temperature is too high
(> 32C|90 F). These parameters
can be avoided by taking preventive measures or adapting the
water temperature.
Fluctuations in ambient
temperature.
Such temperature fluctuations
affect the pressure drop
measured during the test. The
same applies to the diffusion
and pressure drop test. The possibilities for the test being affected
are minimized because the area
of the housing that comes into
contact with the test air is very
small compared to that in the
diffusion test.
Moreover, the great heat
capacity of water compensates
for any fluctuations. Integrity
tests are normally performed
in airconditioned rooms. This
source of error is therefore
encountered very rarely.
Inlet volume.
Generally with large-volume
systems, the precise volume can
be easily determined, whereas
the measured pressure drop may
merely amount to a few mbar.
The results may then border
on the accuracy limits of the
integrity tester and false results
could be obtained.
Similarly, when dealing with very
low net volumes, high pressure
drops can occur, leading to
inaccurate test results.
The net inlet volume must therefore be selected so that both
parameters relevant for intrusion
measurement namely, volume
and pressure drop can be determined as accurately as possible.
Sartorius AG
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Phone +49.551.308.0
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Phone +44.1372.737159
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