F1249 - Transmisión de Vapor

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Designation: F 1249 – 06

Standard Test Method for


Water Vapor Transmission Rate Through Plastic Film and
Sheeting Using a Modulated Infrared Sensor1
This standard is issued under the fixed designation F 1249; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
Note—Paragraph 13.1.1 was editorially corrected and the year date was changed on June 22, 2006.

1. Scope E 104 Practice for Maintaining Constant Relative Humidity


1.1 This test method covers a procedure for determining the by Means of Aqueous Solutions
rate of water vapor transmission through flexible barrier E 178 Practice for Dealing With Outlying Observations
materials. The method is applicable to sheets and films up to 3 E 691 Practice for Conducting an Interlaboratory Study to
mm (0.1 in.) in thickness, consisting of single or multilayer Determine the Precision of a Test Method
synthetic or natural polymers and foils, including coated 3. Terminology
materials. It provides for the determination of (1) water vapor
transmission rate (WVTR), (2) the permeance of the film to 3.1 Definitions:
water vapor, and (3) for homogeneous materials, water vapor 3.1.1 water vapor permeability coeffıcient—the product of
permeability coefficient. the permeance and the thickness of the film. The permeability
is meaningful only for homogeneous materials, in which case
NOTE 1—Values for water vapor permeance and water vapor perme- it is a property characteristic of bulk material.
ability must be used with caution. The inverse relationship of WVTR to
3.1.1.1 Discussion—This quantity should not be used unless
thickness and the direct relationship of WVTR to the partial pressure
differential of water vapor may not always apply. the relationship between thickness and permeance has been
verified in tests using several thicknesses of the material. An
1.2 This standard does not purport to address all of the accepted unit of permeability is the metric perm centimeter, or
safety concerns, if any, associated with its use. It is the 1 g/m2 per day per mm Hg·cm of thickness. The SI unit is the
responsibility of the user of this standard to establish appro- mol/m2·s·Pa·mm. The test conditions (see 3.1) must be stated.
priate safety and health practices and determine the applica- 3.1.2 water vapor permeance—the ratio of a barrier’s
bility of regulatory limitations prior to use. WVTR to the vapor pressure difference between the two
2. Referenced Documents surfaces.
3.1.2.1 Discussion—An accepted unit of permeance is the
2.1 ASTM Standards: 2 metric perm, or 1 g/m2 per day per mm Hg. The SI unit is the
D 374 Test Methods for Thickness of Solid Electrical Insu- mol/m2·s·Pa. Since the permeance of a specimen is generally a
lation function of relative humidity and temperature, the test condi-
D 1898 Practice for Sampling of Plastics3 tions must be stated.
E 96/E 96M Test Methods for Water Vapor Transmission of 3.1.3 water vapor transmission rate (WVTR)—the time rate
Materials of water vapor flow normal to the surfaces, under steady-state
conditions, per unit area.
3.1.3.1 Discussion—An accepted unit of WVTR is g/m2 per
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This test method is under the jurisdiction of ASTM Committee F02 on Flexible day. The test conditions of relative humidity and temperature
Barrier Materials and is the direct responsibility of Subcommittee F02.10 on where the humidity is the difference in relative humidity across
Permeation.
Current edition approved June 22, 2006. Published June 2006. Originally the specimens, must be stated.
approved in 1989. Last previous edition approved in 2005 as F 1249 – 05.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4. Summary of Test Method
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
4.1 A dry chamber is separated from a wet chamber of
the ASTM website. known temperature and humidity by the barrier material to be
3
Withdrawn. tested. The dry chamber and the wet chamber make up a

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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Copyright by ASTM Int'l (all rights reserved); Wed Jul 12 13:10:16 EDT 2006
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F 1249 – 06

FIG. 2 Conditioning System

FIG. 1 Measuring System


top or bottom of the cell. A depth of approximately 6 mm
diffusion cell in which the test film is sealed. Water vapor (0.250 in.) has been found to be satisfactory for 50-cm2 cells.
diffusing through the film mixes with the gas in the dry 6.1.1.1 Diffusion Cell O–Ring—An appropriately sized
chamber and is carried to a pressure-modulated infrared sensor. groove machined into the humid chamber side of the diffusion
This sensor measures the fraction of infrared energy absorbed cell retains a neoprene O–ring. The test area is considered to be
by the water vapor and produces an electrical signal, the the area established by the inside contact diameter of the
amplitude of which is proportional to water vapor concentra- compressed O–ring when the diffusion cell is clamped shut
tion. The amplitude of the electrical signal produced by the test against the test specimen.
film is then compared to the signal produced by measurement 6.1.1.2 Diffusion Cell Sealing Surface—A flat rim around
of a calibration film of known water vapor transmission rate. the dry side of the diffusion cell. This is a critical sealing
This information is then used to calculate the rate at which surface against which the test specimen is pressed; it shall be
moisture is transmitted through the material being tested. smooth and without radial scratches.
6.1.1.3 Diffusion Cell Air Passages—Two holes in the dry
5. Significance and Use half of the diffusion cell. This is necessary only in the earlier
5.1 The purpose of this test method is to obtain reliable model WVTR instruments that have a separate conditioning
values for the WVTR of plastic film and sheeting. rack and testing chamber. These shall incorporate O–rings
5.2 WVTR is an important property of packaging materials suitable for sealing the diffusion cell to the test chamber
and can be directly related to shelf life and packaged product pneumatic fittings for the introduction and exhaust of air
stability. without significant loss or leakage.
5.3 Data from this test method is suitable as a referee NOTE 2—Use of Multiple Diffusion Cells—Experience has shown that
method of testing, provided that the purchaser and seller have arrangements using multiple diffusion cells are a practical way to increase
agreed on sampling procedures, standardization procedures, the number of measurements that can be obtained in a given time. A
test conditions, and acceptance criteria. separate conditioning rack (Fig. 2) may be used that contains a manifold
which connects the dry-chamber side of each individual diffusion cell to
6. Apparatus a dry-air source. Dry air is continually purging the dry chamber of those
cells that are connected to the conditioning rack while the humid chamber
6.1 This method utilizes water vapor transmission appara- side is held at a specific relative humidity by distilled water or a
tus4 (Fig. 1) comprised of the following: saturated-salt solution. It is desirable to thermostatically control the
6.1.1 Diffusion Cell—An assembly consisting of two metal temperature of the conditioning rack as described in 6.1.3.
halves which, when closed upon the test specimen, will 6.1.2 Test Chamber—A cavity into which the diffusion cell
accurately define a circular area. A typical acceptable diffusion is inserted. Again, this is necessary only in the earlier model
cell area is 50 cm2. The volume enclosed by each cell half, WVTR instruments that have a separate conditioning rack and
when clamped, is not critical; it should be small enough to testing chamber. The test chamber shall incorporate means for
allow for rapid gas exchange, but not so small that an clamping the diffusion cell in accurate registration with pneu-
unsupported film that happens to sag or buckle will contact the matic system openings to the dry-air source and the infrared
detector. The chamber shall also provide a thermometer well
for the measurement of temperature.
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The sole source of supply of the apparatus known to the committee at this time 6.1.3 Diffusion Cell Temperature Control—It is desirable to
is Mocon/Modern Controls, Inc., 7500 Boone Avenue North, Minneapolis, MN
55428. If you are aware of alternative suppliers, please provide this information to
thermostatically control the temperature of the diffusion cell to
ASTM International Headquarters. Your comments will receive careful consider- within 61°F. A simple resistive heater attached to the station in
ation at a meeting of the responsible technical committee,1 which you may attend. such a manner as to ensure good thermal contact is adequate

2
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Reproduction authorized per License Agreement with YSABEL M PASTOR (OPPFILM S.A.);
F 1249 – 06
for this purpose. A thermistor sensor and an appropriate control
circuit will serve to regulate the temperature unless measure-
ments are being made close to ambient temperature. In that
case it may be necessary to provide cooling coils to remove
some of the heat.
6.1.4 Flowmeter—A means for regulating the flow of dry
air within an operating range of 5 to 100 cc/min is required.
6.1.5 Flow-Switching Valves, for the switching of dry-gas
flow streams of the water vapor transmission apparatus.
6.1.6 Infrared Sensor—A water vapor detector capable of
sensing 1 µg/L of water, or, in other terms, 1 ppm by volume,
or 0.002 % relative humidity at 37.8°C. FIG. 3 Film Diffusion Cell
6.1.7 Recording Device—A multirange strip chart recorder
or other appropriate instrument for measuring the voltage
developed by the signal amplifier. 9. System Calibration With Reference Film
6.1.8 Desiccant Drying System, shall be capable of reducing 9.1 Follow the manufacturer’s instructions for calibrating
the concentration of water vapor in the gas source down to less the WVTR instrument with a reference film.
than 0.5 ppm by volume or 0.001 % relative humidity at
37.8°C. In earlier model WVTR equipment, a separate desic- 10. Test Procedure
cant drying system is needed for the conditioning rack and test 10.1 Preparation of Apparatus (Fig. 1)—If preceding tests
chamber. have exposed the apparatus to high moisture levels, outgas the
6.1.9 Flow-Metering Valve—A fine-metering valve capable system to desorb residual moisture.
of controlling the dry-gas flow rate to the test cell when the 10.2 Number of Specimens Tested—Test enough specimens
apparatus is in the “measure’’ mode of operation. to characterize package permeation rates but never less than
three per sample.
7. Reagents and Materials 10.3 Preparation of Test Samples:
7.1 Desiccant,4,5 for drying gas stream. 10.3.1 Cut the test specimen to approximately 10 cm by 10
7.2 Absorbent Pads (not critical), such as filter pads of 30 cm (4 in. by 4 in.).
to 75 mm in diameter. Necessary only in earlier model WVTR 10.3.2 Measure specimen thickness at four equally spaced
equipment that utilizes distilled water or saturated salt solu- points within the test area and at the center in accordance with
tions to generate the desired relative humidity. guidelines described in Test Method D 374.
7.3 Distilled Water, for producing 100 % relative humidity, 10.3.3 Lightly grease the cell sealing surface and the cell
or various saturated salt solutions to produce other relative O–ring.
humidities as described in Practice E 104. Newer WVTR 10.3.4 For earlier model WVTR systems that require the use
equipment does not require saturated salt solutions. Refer to of distilled water or saturated salt solutions, insert one to three
the manufacturer’s instructions for generating relative humid- absorbent pads into the lower half-cell and dampen with
ity. distilled water or a desired salt solution. Otherwise, for newer
7.4 Reference Film, known WVTR material for system WVTR instruments, follow the manufacturer’s instructions for
calibration. generating the desired relative humidity.
7.5 Sealing Grease, a high-viscosity, silicone stopcock 10.3.5 Affix the test film to the diffusion cell following the
grease or other suitable high-vacuum grease is required for manufacturer’s instructions. Fig. 3 shows the type of diffusion
lubrication of O–rings and to seal the specimen film in the cell used in earlier model WVTR equipment that consisted of
diffusion cell. a separate conditioning rack and testing chamber. Diffusion
7.6 Nitrogen Gas, shall be dry and contain not less than cells in newer WVTR equipment are similar to the lower half
99.5 % nitrogen. Needed only with certain WVTR instruments. of the cell displayed in Fig. 3.
10.3.6 If using a separate conditioning rack, clamp the
8. Sampling assembled cell in the conditioning rack. Allow the film to
condition in the diffusion cell until steady state has been
8.1 Select material for testing in accordance with standard attained. If unfamiliar with the material being tested, the
methods of sampling applicable to the material under test. operator should investigate the effect of conditioning time to be
Sampling may be done in accordance with Practice D 1898. certain that sufficient time has been allowed for the material to
Select samples considered representative of the material to be equilibrate under the test conditions (see Note 3).
tested. If the material is of nonsymmetrical construction, the
10.4 Measure the WVTR of the film specimen following the
orientation should be noted.
manufacturer’s instructions.
NOTE 3—When testing materials for which the operator has no previous
history, additional time must be allowed to assure that true equilibrium has
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Linde Molecular Sieve, Type 4A or Type 5A, in the form of 1⁄8 in. pellets as may been reached. When in doubt, retest after an additional conditioning
be obtained from the Union Carbide Co., Linde Division, Danbury, CT 06817-0001. interval of several hours.

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F 1249 – 06
10.5 Record temperature of each test with reference to a 12.1.1 A description of the test specimen. If the material is
thermometer or thermocouple installed in the test chamber nonsymmetrical (two sides different), include a statement as to
thermometer well. Temperature is a critical parameter affecting which side was facing the high humidity,
the measurement of WVTR. During testing, monitor the 12.1.2 The humidity environment on each side of the test
temperature, periodically, to the nearest 0.5°C. Report the film and means by which it was obtained,
average temperature and the range of temperatures observed 12.1.3 The test temperature (to nearest 0.5°C),
during the test. 12.1.4 The values of WVTR and, if desired, values of
10.6 Standby and Shutoff Procedures: permeance and permeability. These entries should be rounded
10.6.1 Follow the manufacturer’s instructions for putting off to three significant figures or less, as may be consistent with
the instrument in standby when not being used. the operator’s estimate of precision or bias,
10.6.2 When the system is not to be used for an extended 12.1.5 A statement of the means used to obtain the calibra-
period and there are no films that require conditioning, the tion factor,
electrical power may be turned off.
12.1.6 The effective area exposed to permeation and a
11. Calculation description of how it was defined,
11.1 WVTR—If using a recorder, calculate water vapor 12.1.7 The time to reach steady-state after introduction of
transmission rate using the formula: the diffusion cell into the test chamber, and
12.1.8 A description of the conditioning procedure.
WVTR 5 C ~ES 2 EO!

where: 13. Precision and Bias


C = a calibration factor expressing rate as a function of 13.1 Precision:
voltage (or mV). The value of C is derived from tests 13.1.1 Four different film materials cut and distributed in
of a known reference film (Section 9), accordance with Practice E 691 were evaluated by eight
EO = permeation system zero level voltage, and
laboratories. The number of laboratories and materials in this
ES = equilibrium voltage obtained with the test specimen.
study does not meet the minimum requirements for determin-
ing precision prescribed in Practice E 691. Of the total eight
Newer computer-controlled systems will automatically cal-
laboratories that participated in this round robin, one did not
culate the WVTR.
report results for the PET sample. Due to equipment limita-
11.2 Permeance—Calculate sample permeance (if required)
tions, only five laboratories were able to measure the water
using the following relationship:
vapor transmission rate of the EVOH material. Of these five
WVTR 2 labs, the data from two laboratories were determined to be
Metric Perms 5 Pw 5 g/m · day · mm Hg outliers in accordance with Practice E 178. In addition, due to
where: the type of equipment used, two of the laboratories participat-
WVTR = Specimen water vapor transmission rate, g/m2·d, ing in the round robin actually measured all of the samples at
and 90 % RH and converted the results to 100 % RH driving force
Pw = Water vapor partial pressure gradient across the by multiplying by 1.11.
test specimen, mmHg. Precision, characterized by repeatability Sr and r, and repro-
11.3 Permeability Coeffıcient—Calculate the water vapor ducibility SR and R, has been determined for the following
permeability coefficient (if required) using the following rela- materials to be:
tionship: Materials No. of Labs Average† Sr SR r R
PET 7 14.0 0.3 2.0 0.8 5.7
Permeability 5 metric perms · t PE 8 29.8 2.3 4.6 6.3 12.9
EVOH 3 239.6 26.7 177.6 74.7 497.3
where: PP 8 4.1 0.2 0.6 0.5 1.7
t = the average thickness of the specimen, mm. Note:
† Editorially corrected.
Permeability calculations are meaningful only in cases
where materials have been determined to be homoge- 13.2 Bias—Measured values are derived from comparisons
neous. with known-value reference films. The accuracy of this method
is therefore dependent upon the validity of the values assigned
12. Report to these reference films. This information should be available
12.1 Report the following information: from the manufacturer of the reference films.

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Reproduction authorized per License Agreement with YSABEL M PASTOR (OPPFILM S.A.);
F 1249 – 06
APPENDIX

(Nonmandatory Information)

X1. TESTING POOR BARRIERS

X1.1 Normal procedures as described for the modulated X1.2.2 By reducing the area of the test film.
infrared permeation system are considered suitable for testing
barrier materials having rates up to 100 g/m2–day. Above that X1.3 Alternatively, apply foil masks with die-cut apertures.
level, a different approach may be required in order to keep the These may be applied to both sides of a barrier to reduce the
sensor output within design limits. sample area. Metal masks utilizing a neoprene O-ring are yet
another alternative.
X1.2 In general, the testing of a “high transmitter’’ requires X1.4 Each of these methods, when used alone or in
that means be employed to reduce the concentration of water combination, serves to reduce the vapor concentration of the
vapor in the sensor. This may be accomplished in two ways: air stream.
X1.2.1 By increasing the flow of dry gas (possible in earlier NOTE X1.1—The precision and bias of results obtained with reduced-
model WVTR equipment), or area masked samples has not been established.

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