Standard Test Method for Determining the Carbon Dioxide Loss of Beverage Containers

SIGNIFICANCE AND USE
Two procedures, A and B, are outlined in this test method. Procedure A is used most often for development of various beverage container designs to determine the functional characteristics of the package in regard to shelf life. Procedure B is recommended for use in beverage filling operations as a quality control tool in maintaining the desired CO2 fill pressure. A loss of CO2 will affect product taste.
Procedure A involves the use of sensitive pressure and temperature monitoring equipment where a high degree of accuracy is essential, for example, a micro-pressure transducer and thermocouple for measuring pressure and temperature of the package in a closed system. Alternatively, this procedure may also use bottles closed with roll-on aluminum caps containing rubber septums. The septum is pierced with a hypodermic needle attached to a pressure transducer to obtain pressure readings. This procedure should be confined to laboratories that are practiced in this type of analytical testing.
Procedure B is more widely used when measuring the carbonation level of the package due to the simplicity of the technique. A simple Zahm-Nagle pressure assembly or Terris CO2 Analyzer is utilized.
SCOPE
1.1 The objective of this test method is to determine the carbon dioxide (CO2) loss from plastic beverage containers after a specified period of storage time.
1.2 Factors contributing to this pressure loss are volume expansion and the gas transport characteristics of the package including permeation and leakage.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
31-Jan-2008
Drafting Committee
Current Stage
Ref Project

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ASTM F1115-95(2008)e1 - Standard Test Method for Determining the Carbon Dioxide Loss of Beverage Containers
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: F1115 − 95(Reapproved 2008)
Standard Test Method for
Determining the Carbon Dioxide Loss of Beverage
Containers
This standard is issued under the fixed designation F1115; 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 (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial corrections were made throughout in March 2008.
1. Scope ation volumes should be made using a carbonation volumes
table.Atable for carbonated water would not necessarily apply
1.1 The objective of this test method is to determine the
to liquids containing additional substances, such as carbonated
carbon dioxide (CO ) loss from plastic beverage containers
beverages containing sugar.
after a specified period of storage time.
3.2.2 initial pressure—the equilibrium pressure in the test
1.2 Factors contributing to this pressure loss are volume
bottles as measured at 24 h after filling with carbonated water.
expansion and the gas transport characteristics of the package
(The filled bottles are allowed to stand for 24 h to obtain
including permeation and leakage.
temperatureequilibriumwiththetestenvironmentandtoallow
1.3 This standard does not purport to address all of the
time for pressure adjustment and equilibration of the CO in
safety concerns, if any, associated with its use. It is the
the headspace and liquid.)
responsibility of the user of this standard to establish appro-
3.2.3 sample—a set of bottles produced on the same equip-
priate safety and health practices and determine the applica-
ment in a single run and using the same material and process
bility of regulatory limitations prior to use.
conditions. Bottles should represent normal thickness distribu-
tion.
2. Referenced Documents
2.1 ASTM Standards: 3.2.4 shelf life—the number of weeks a sample set of bottles
D1129 Terminology Relating to Water
retain a specified carbonation level, or a percent of the initial
D1193 Specification for Reagent Water level.
E380 Practice for Use of the International System of Units
3.2.5 pressure monitoring device—a pressure gage or trans-
(SI) (the Modernized Metric System) (Withdrawn 1997)
ducer assembly with support electronics for indicating internal
pressure level of the bottle. This device is used with brass
3. Terminology
closure fitting-equipped bottles.
3.1 Units, symbols, and abbreviations used in this test
3.2.5.1 temperature monitoring device—a thermocouple
method are those recommended by Practice E380.
with support electronics (same equipment as described in
3.2 Definitions of Terms Specific to This Standard:
7.2.2). A precision glass thermometer may be used provided a
3.2.1 carbonation volume—the volume of CO (at 0°C, 1
bottle filled with noncarbonated water is used as a control in
atm pressure) that is dissolved in the carbonated water, divided
each sample set (Procedure A).
by the volume of the liquid (based on water volume at 3.98°C
3.2.6 Terriss CO Analyzer—an electronic unit that will
equals 1.000 g/cm ). The conversion of pressure to carbon-
pierce the roll-on closure and automatically read pressure and
temperature and calculate volume of gas (Procedure B).
1 3.2.7 Zahm-Nagle Pressure Tester—a unit that manually
This test method is under the jurisdiction ofASTM Committee F02 on Flexible
Barrier Packaging and is the direct responsibility of Subcommittee F02.10 on pierces the closure and measures container pressure; an at-
Permeation.
tached thermometer is then used to measure temperature
Current edition approved Feb. 1, 2008. Published March 2008. Originally
(Procedure B).
approved in 1987. Last previous edition approved in 2001 as F1115 – 95 (2001).
DOI: 10.1520/F1115-95R08E01.
3.2.8 support ring—a protrusion below the bottle finish
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
which is used to support or stabilize the bottle during filling
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on and capping.
the ASTM website.
3.2.9 finish—the threaded part of the bottle which receives
The last approved version of this historical standard is referenced on
www.astm.org. the cap.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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F1115 − 95 (2008)
3.3 For other terms used in this test method, refer to 7.1.3 Top Loading Balance, capable of weighing to 2500 g
Terminology D1129. with an accuracy of 60.01 g (optional).
7.1.4 Outside Diameter Measuring Device, π tape or similar
4. Summary of Test Method
device (optional).
4.1 Test bottles are filled with carbonated water or beverage 7.1.5 Carbonated Water or Beverage Dispensing Equip-
and, after closure application, are exposed to test environments
ment.
forspecifiedtimeperiods.Byperiodicallymeasuringtheinitial 7.1.6 Micrometer or Ultrasonic Thickness Gage, capable of
and final carbonation levels in the container, the carbonation
measuring to within 0.001 in. or less (optional).
loss and carbonation transfer rate can be calculated.
7.2 Procedure A:
7.2.1 Machined Metal Cap (see Fig. 1).
5. Significance and Use
7.2.2 Temperature-Measuring Device, capable of accurately
5.1 Two procedures, A and B, are outlined in this test
measuring temperature in increments of 0.1°C or less in a
method. Procedure A is used most often for development of
range from 18 to 32°C (65 to 100°F).
various beverage container designs to determine the functional
7.2.3 Pressure-Monitoring Device.
characteristics of the package in regard to shelf life. Procedure
7.2.4 Fillpoint-Level Syringe Assembly (see Fig. 2).
B is recommended for use in beverage filling operations as a
7.3 Procedure B:
quality control tool in maintaining the desired CO fill pres-
7.3.1 Pressure- and Temperature-Measuring Device.
sure. A loss of CO will affect product taste.
5.1.1 ProcedureAinvolves the use of sensitive pressure and
8. Reagents and Materials
temperature monitoring equipment where a high degree of
8.1 Water carbonated to a level sufficient to ensure a
accuracy is essential, for example, a micro-pressure transducer
minimum carbonation level of 4.5 volumes in the filled bottles.
and thermocouple for measuring pressure and temperature of
the package in a closed system. Alternatively, this procedure
may also use bottles closed with roll-on aluminum caps
The sole sources of supply of the apparatus (Terriss Unit or Zahm-Nagel
containing rubber septums. The septum is pierced with a
apparatus) known to the committee at this time is Terriss-Consolidated Industries,
hypodermic needle attached to a pressure transducer to obtain
Box 110B,Asbury Park, NJ 07712, and Zahm and Nagel Co., Inc., 74 HewettAve.,
pressure readings. This procedure should be confined to
Buffalo, NY 14214. If you are aware of alternative suppliers, please provide this
information to ASTM International Headquarters. Your comments will receive
laboratories that are practiced in this type of analytical testing.
careful consideration at a meeting of the responsible technical committee, which
5.1.2 Procedure B is more widely used when measuring the
you may attend.
carbonation level of the package due to the simplicity of the
technique. A simple Zahm-Nagle pressure assembly or Terris
CO Analyzer is utilized.
6. Interferences
6.1 The following conditions can interfere with the test
results:
6.1.1 CO leakageatclosureduetodefectivebottlefinishor
improper sealing of closure apparatus,
6.1.2 CO leakage due to improper equipment set-up,
6.1.3 Change in ambient temperature, upsetting the equilib-
rium of the headspace and dissolved CO gas,
6.1.4 Measurement of pressure before the bottle and liquid
have reached ambient temperature,
6.1.5 Inaccurate thermocouple device used for measuring
the liquid temperature,
6.1.6 Excessive air in the bottle headspace or dissolved in
the liquid,
6.1.7 Inaccurate or erratic pressure monitoring device,
6.1.8 Ambient humidity in the test area,
6.1.9 Age of bottles, and
6.1.10 Excessive bottle-to-bottle variation in the material
distribution,whichmayresultinawidevariationfrombottleto
bottle within the sample population.
7. Apparatus
NOTE 1—Break sharp edges. All dimensions are inches unless other-
7.1 Procedures A and B:
wise stated. If conversion of dimension is desired, use standard equiva-
7.1.1 Bottle Stand, optional.
lence table.
7.1.2 Height Measuring Device, capable of measuring to
Material: Brass.
within 0.001 in. (optional). FIG. 1 Machined Metal Cap for PET Beverage Bottle Testing
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F1115 − 95 (2008)
NOTE 1—Dimensions are in inches and millimetres. Other styles of suction bulbs may be used, including an in-line bulb for use with flexible tubing
attached to the gage. The assembly must be adjusted for the specified fill point (from the top down) for the specific bottle size and style being evaluated.
The gage may be adjusted using a preset syringe adjusting device or other measuring devices such as the vertical height gage (see 7.1.2).The gage should
be set 0.050 in. (1.27 mm) less than the specified value to compensate for the extra liquid withdrawn due to the effect of surface tension.
FIG. 2 Fillpoint Level Adjustment Syringe
Reagent water conforming to Type IV of Specification D1193 8.2 Carbon Dioxide, compressed (CO ).
or better shall be used.
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F1115 − 95 (2008)
8.3 Leak-Detecting Solution. shaking or mechanical agitation to ensure proper equilibration
ofheadspaceanddissolvedCO .ShiftpressureoraddCO gas
2 2
9. Conditioning
as required to adjust the carbonation level to 4.0 volumes
60.05 volumes according to a carbonation volumes table. The
9.1 Testbottlesmustbeconditionedat23°C(73.4°F) 62°C
starting CO level is critical.
and 50 6 5 % relative humidity for at least 72 h and tested at
10.4.3 After a total of 24-h equilibration, again agitate the
the same conditions unless other conditions are agreed upon by
test bottles and determine their carbonation level. If any bottle
the parties involved.
has a carbonation level of 3.95 volumes or less, discontinue
9.2 Bottles may be tested with or without base cup attached.
testing of that bottle.
10.5 Measurements:
10. Procedure A
10.5.1 Before filling bottles for the carbonation level test,
10.1 Apparatus Preparation:
measure wall thickness profile using suitable equipment to
10.1.1 Assemble and calibrate pressure- and temperature-
determine the quality of the material distribution (optional).
monitoring equipment.
10.5.2 Twenty-four hours after filling, agitate each test
10.1.2 Pressure test assembly at 60 psi using leak detecting
bottle to equilibrium pressure for at least 1 min to o
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