Voluntary Standard

Test Methods
For
PET Bottles
Issue Date: 10/03
Revision: 1
 INTERNATIONAL SOCIETY OF BEVERAGE TECHNOLOGISTS

Voluntary Standard Test Methods

For PET Bottles

International Society of Telephone: (352) 382-2008

Fax: (352) 382-2018
Beverage Technologists Email: [email protected]
8110 South Suncoats Boulevard
Website: http://www.bevtech.org
Homossa, FL 34446-5006, USA

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Conditions of Use and Legal Disclaimer

The contents of any website sponsored, maintained, or sanctioned by the

International Society of Beverage Technologists (ISBT) are provided for the benefit
of the beverage industry, and are to be used on a voluntary basis. Prior to the use of
any information, documentation, or specification, you should first determine whether
the use of these materials is appropriate to your particular application. You, the user,
assume all responsibility for the use and interpretation of website contents and agree
to use at your own risk.
No representations or warranties, stated or implied, are made as to the accuracy,
completeness or usefulness of the information, documentation, or specifications, or
the conformity of any product to them. You, the user, agree to indemnify and hold
harmless the ISBT, its officers, directors, employees and agents from any and all
losses, claims, or damages resulting from the use of the information on this website
including injury or death of any person or damage to any property of whatsoever
nature.

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Introduction

The following test methods were developed by an ISBT committee made up of end
users and suppliers in conjunction with the ISBT. The scope of this committee was
to review test methods relating to plastic bottles for CSD’s, NCB non-pressurized,
NCB pressurized and hot fill applications and standardize on conditions of testing
where practical.

Having gone through this exercise, this may now make it possible for the suppliers to
be more efficient in their lab facilities because they will now test bottles and closures
for all end users by the same methods.

Having completed the original mandate, it is recommended that the committee

should meet twice yearly to make revisions to test methods as technological
advances occur in test equipment and packaging in general.

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Table of Contents
Conditions of Use and Legal Disclaimer i

Introduction ii

Test Methods Grid for PET Bottles 1

Dimensional Tests:
Bottle Dimensions 3
Finish Dimensions 4
Section Weights 5
Wall Thickness 6
Weight and Capacity 7

Physical Performance Tests:

Burst 10
Crystallinity: Gradient Column 11
Drop Impact 12
Hot Fill Distortion 13
Pressure Retention 14
Top Load:
Non-Vented 16
Vented 17
Filled and Capped 18
Thermal Stability 19
Stress Cracking 20
Vacuum Retention 22

Reference Tests:
ASTM Test Methods: 23
AA – Ground Preform 23
AA – Head Space 23
Oxygen Transmission - MOCON 23
Transportation Test 23

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 Carbonation Retention:
Non-Destructive 24
MOCON 28
FTIR 33
Orbisphere 38

Oxygen Transmission: Orbisphere 40

Perpendicularity 42
Sodium Hydroxide Preparation 43

Abbreviations 47

Revision History 48

Bottle Nomenclature
Bottle Nomenclature CSD SW
Bottle Nomenclature CSD
Bottle Nomenclature NCB

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TEST CSD NCB-COLD FILL NCB-COLD FILL HOT FILL

PRESSURIZED NON-PRESSURIZED
Dimensional Tests:
Bottle Dimensions: X X X X

Finish Dimensions X X X X

Section Weights X X X X

Wall Thickness X X X X

Weight and Capacity X X X X

Physical Performance Tests:

Burst X X

Pressure Retention: X X
Zahm-Nagel

Crystallinity: Gradient Column X

Drop Impact X X X X

Hot Fill Distortion X

Top Load:
Non-Vented X X X X
Vented X X X
Filled and Capped X X

Thermal Stability X X

Stress Crack X

Vacuum Retention X

Reference Tests:
ASTM Test Methods:
AA – Ground Preform X X X X
AA – Head Space X X X X
MOCON O2 Ingress X X X
Transportation Test X X X X

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Carbonation Retention:
Non-Destructive X
MOCON X
FTIR X
Orbisphere X

O2 Transmission: Orbisphere X

Perpendicularity X X X X

Sodium Hydroxide Preparation X

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DIMENSIONAL TEST METHOD BOTTLE DIMENSIONS

PURPOSE
Evaluate the critical measurements (such as height, diameters, shoulder contour, and height to the
support ring) of the bottle to ensure compliance with the manufacturer's drawing and ease of
handling during the filling and capping operations. The purpose of this test is to determine if bottle
dimensions are within specifications.

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill.

TEST EQUIPMENT
1. Surface Plate, flat to 0.0025mm (0.0001 inch).

2. Height Gauge, accurate to 0.025mm (0.001 inch).

3. Calipers, accurate to 0.025mm (0.001 inch).

4. Bottle specification drawing showing dimensions and tolerances.

5. Non-contact methods of measurement are preferred.

6. Pi tape and optical comparator methods are also acceptable.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment. Dimensions to be measured are dependent upon application.

2. Diameter(s):
Measure actual samples and record data

3. Bottle Height and Height to Neck Support Ring:

Measure actual samples and record data.

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DIMENSIONAL TEST METHOD FINISH DIMENSIONS

PURPOSE
Various factors of package quality, including seal integrity and removal torque level, are dependent
on the quality of the neck finish. The purpose of this test is to verify that finish dimensions are
according to specifications (see www.Threadspecs.com or the appropriate supplier).

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill.

TEST EQUIPMENT
Optical comparator or other non-contact method for measurement must be used for exterior
dimensions.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment.

2. Observe and record incident of gross defects such as "blown necks" and other deformations.

3. Observe quality of sealing surfaces. Mark and note instances of short shots, nicks, dents,
molding flash, etc.

4. Dimensions to be measured are dependent upon application. Recommendation: T, E, A, C

and X, minimally. Verify with www.Threadspecs.com the nomenclature and tolerances. Each
diameter dimension should be measured at approximately 10o and 90o to the parting line.
Height and vertical dimensions should not be measured on the parting line.

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DIMENSIONAL TEST METHOD SECTION WEIGHTS

PURPOSE
A bottle has a unique material distribution profile depending on the bottle gram weight and
processing technique. Consistency of weight distribution is an important factor in bottle
performance. The purpose of bottle sectioning is to allow measurement of a specific cylindrical
segment (such as shoulder, panel and base) of a bottle.

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill

TEST EQUIPMENT
1. Laboratory scale with capacity of 100 grams minimum and an accuracy of ± 0.01 gram.

2. Bottle sectioning location guidelines, based on applicable end user's specifications drawing.

3. Equipment for cutting or sectioning bottle.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of balance.

2. Inspect for and remove any foreign matter from the bottles.

3. Cut each bottle into sections based on the container drawing.

4. Determine each section weight to nearest 0.1 gram.

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DIMENSIONAL TEST METHOD WALL THICKNESS

PURPOSE
Successful performance of a PET bottle is related to many critical properties that are dependent
on the bottle wall thickness profile consistency (e.g., CO2 permeation rate, O2 ingress, water vapor
transmission rate, volume change, top-load strength). The purpose of this test is to measure wall
thickness in distinct regions of plastic bottles in order to monitor and compare with physical
performance.

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill

TEST EQUIPMENT
1. Ultrasonic or other non-destructive thickness testers.
or
2. Micrometer with ball ends or equivalent with a resolution of 0.0025mm (0.0001 inch).

3. Height gauge with ink marking or scribe tip.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment.

2. For direct contact measurements, mark the bottle in the vertical & horizontal positions based
on bottle design and end users’ specifications.

3. Measure the thickness to 0.025mm (0.001”) at all intersecting points marked above.

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DIMENSIONAL TEST METHOD WEIGHT & CAPACITY

PURPOSE
Plastic bottles must meet the specific capacity requirements of the country(s) in which the bottles
will be used. Additionally, bottle weight can impact a number of performance attributes. The
purpose of this test is to determine the weight of a bottle along with fill point and overflow capacity.

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill.

TEST EQUIPMENT
1. Laboratory scale with accuracy of at least ± 0.01 gram

2. Depth Micrometer

3. Vented Bulb Syringe

4. Thermometer with accuracy to 0.50C (1° F)

5. Table for density of water per CRC Handbook of Chemistry and Physics

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment. Obtain bottles immediately after production and store at
ambient temperature for 72 hours, or per end user's requirements.

2. Record the actual temperature of the water (target 220C/720F).

3. Identify bottle samples.

4. Determine the weight to ± 0.1g of the (first) empty bottle, record the weight and tare the
weight.

5. Fill bottle with room temperature water (distilled water recommended) to the top of finish and
record this weight as over flow (g).

6. Set the depth micrometer to the fill level, referencing the bottle drawing, and adjust for the
appropriate correction factor to account for surface tension. Adjust a vented bulb syringe using
the depth micrometer.

7. Apply vented bulb syringe to surface of bottle finish and remove excess water and record this
weight as fill level capacity (g).

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WEIGHT & CAPACITY

8. Repeat procedure steps 4 through 7 for each bottle.

9. Determine the density of water at the respective temperature as derived from the water density
table in the CRC Handbook of Chemistry and Physics.

10. Covert the overflow and fill level weights to volumetric data using the following calculation:

Volume (mL) = Net Weight (g) / Water Density (g/mL)

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WEIGHT & CAPACITY

Bottle Capacity Weight/Volume Conversion Table

Apparent Density of Water in Air
Temperature, °C Density, gm/mL Temperature, °F
0 0.99873 32.0
1 0.99879 33.8
2 0.99884 35.6
3 0.99887 37.4
4 0.99888 39.2
5 0.99887 41.0
6 0.99885 42.8
7 0.99882 44.6
8 0.99877 46.4
9 0.99871 48.2
10 0.99863 50.0
11 0.99854 51.8
12 0.99843 53.6
13 0.99832 55.4
14 0.99819 57.2
15 0.99805 59.0
16 0.99790 60.8
17 0.99773 62.6
18 0.99756 64.4
19 0.99737 66.2
20 0.99717 68.0
21 0.99697 69.8
22 0.99675 71.6
23 0.99652 73.4
24 0.99628 75.2
25 0.99603 77.0
26 0.99578 78.8
27 0.99551 80.6
28 0.99523 82.4
29 0.99495 84.2
30 0.99465 86.0
31 0.99435 87.8
32 0.99404 89.6
33 0.99372 91.4
34 0.99339 93.2
35 0.99305 95.0

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PHYSICAL PERFORMANCE TEST METHOD BURST TEST

PURPOSE
Bottles are subjected to rapidly increasing pressure during the filling operation. The purpose of this
test is to determine the failure point of the PET bottle when pressurized under specific conditions.

APPLICATION
Only CSD and NCB-Cold Fill-Pressurized bottles.

TEST EQUIPMENT
Calibrated Burst Tester (AGR*TopWave Model BR 3000 type or equivalent) with fill ramp capabilities.

SAMPLE QUANTITIES
To be determined by end users’ specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment.

2. Place one bottle at a time in the burst tester. Ensure that the bottle is properly threaded into the
bottle support and close the safety chamber.

3. Initiate the burst tester using the following parameters:

a. CSD: Rapid pressurization to 9.18 bar (135 psi); hold for 13 seconds; ramp at 0.68 bar/sec
(10psi/sec) to failure or 20.41 bar (300 psi) (whichever comes first).

b. NCB-Cold Fill - Pressurized: Rapid pressurization to 2.04 bar (30 psi); hold for 13 seconds;
ramp at 0.34 bar/sec (5psi/sec) to failure or 2.72 bar (40 psi) (whichever comes first)

4. After the method has finished, remove the bottle.

5. Test each bottle to failure.

Note: There is a potential that the test will not proceed to failure due to physical limitations of
the machine (i.e., ramp pressure limit reached).

6. Record the following test results for each bottle:

a. Burst pressure or maximum pressure achieved. (mandatory)
b. Percent bottle expansion at 13 seconds and final expansion. (optional)
c. Time duration for each bottle tested. (optional)
d. Location of failure (side wall or base) and if it is a base failure, describe the location of failure:
through the gate, around gate, foot to foot, etc. (mandatory)

7. Record the water temperature for each series of tests.

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PHYSICAL PERFORMANCE TEST METHOD CRYSTALLINITY

PURPOSE
PET is a crystallizable polymer. Since the percent crystallinity is proportional to density, the
percent crystallinity of a PET sample can be determined by measuring the density. Crystallinity
level is an important variable in determining hot fill performance.

APPLICATION
Primarily for Hot Fill Bottles.

PROCEDURE
See ASTM # D1505-85 for the Density Gradient Column method and ASTM # D792-91 for the
Displacement method.

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PHYSICAL PERFORMANCE TEST METHOD DROP IMPACT

PURPOSE
An important feature of plastic bottles is their resistance to failure on drop impact. The purpose of
this test is to determine the ability of the bottle to withstand free-fall impact forces.

APPLICATION
PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill

TEST EQUIPMENT
1. Flat hot-rolled steel plate, or equivalent, with minimum dimensions of 1m by 1m by 12.7mm
(39" by 39" by 0.5") having an unpolished surface and securely attached to an industrial
concrete surface.

2. Safety glasses and/or face shield

SAMPLE QUANTITIES
To be determined by end users’ specifications and risk analysis.
Recommendation: 12 per orientation; 24 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment

2. Sample bottles must be filled as outlined below for the appropriate application
a. CSD: 4.2 GV +/-0.5 GV
b. NCB-Cold Fill-Pressurized: 2.72 bar (40psi+/-5psi)
c. NCB-Cold Fill-Non-Pressurized: Flat water (no pressure)
d. Hot Fill: Water filled under hot-fill conditions.

3. Test samples must be conditioned a minimum of 16 hours at 4 +/-1°C (40 +/- 2 °F)

4. Drop samples individually onto steel plate from the specified height: (measured from bottom of
bottle to plate)
a. CSD: 1.8 meters (6ft)
b. NCB– Cold Fill-Pressurized: bottles < 1L at 1.4 meters (55”); bottles > 1L at 1 meter (40”)
c. NCB – Cold Fill-Non-Pressurized: bottles < 1L at 1.4 meters (55”); bottles > 1L at 1 meter
(40”)
d. Hot fill: bottles < 1L at 1.4 meters (55”); bottles > 1L at 1 meter (40”)

5. Divide the samples into 2 groups and drop 12 samples, or number per end user, in the
following orientations:
a. 12 samples dropped vertically on to the bottle base.
b. 12 samples dropped horizontally onto the bottle side.
Each sample is tested once then discarded.

6. Observe effect of the initial impact as opposed to the effects of secondary impacts.

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PHYSICAL PERFORMANCE TEST METHOD HOT FILL DISTORTION

PURPOSE
Evaluate the container’s resistance to distortion resulting from liquid hot fill. Manufacturing
process, container material, levels of non-uniform biaxial orientation, crystallinity and design can all
impact on a container’s response to high temperature filling.

APPLICATION
Hot Fill Bottles.

TEST EQUIPMENT
1. Mechanical bottle diameter fixture with measuring standards or equivalent devices such as
Vernier calipers or non-contact devices.
2. Height Gauge.
3. Top Load Balance.
4. Bottle specification drawing.
5. Thermometer or thermocouples with read out devices.
6. Regulated hot water supply.
7. Quench box or sink.

SAMPLE QUANITIES
To be determined by end users‘ specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Test freshly blown bottles after a minimum of 20 minutes (preferably within an hour) after
collection.
2. Record initial values for volume, height (to support ledge), and diameters in multiple locations
(such as maximum bell, mid-label panel, and maximum base).
3. Fill bottles to finish “A” diameter with hot water and cap. Use water temperature appropriate for
condition of use. Generally, 90.6o C (195o F) water is used if bottles are less than 24 hours old
and 85o C (185o F) water is used if bottles are more than 24 hours old.
4. Allow bottle to stand for two (2) minutes.
5. Place bottle on side and hold for one (1) minute, to wet the closure.
6. Quench bottles to cool (generally, 22 o C/72 o F). Time dependent upon method of cooling and
container size.
7. While bottles are still sealed, check for visual distortion and measure height (to support ledge)
and diameter ovality.
8. Empty bottles and measure volume, height (to support ledge) and diameters.

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PHYSICAL PERFORMANCE TEST METHOD PRESSURE RETENTION:

ZAHM NAGEL

PURPOSE
The shelf life of a carbonated or pressurized beverage is affected by a number of components.
One of these components is the amount of pressure loss (via permeation and creep) through the
plastic bottle. This test method quantifies the amount of pressure retention for the bottle.
APPLICATION
CSD and NCB Cold fill Pressurized Bottles.

TEST EQUIPMENT
1. A filling machine capable of filling carbonated water or product to 4.2 ± 0.1 volumes of CO2 or
pressure target listed below.
2. Method of applying plastic closures
3. A calibrated Zahm & Nagel Piercing Device with pressure gauge (capable of measuring 0-100
psi or 0-6.9 bars)
4. Digital or analog thermometer calibrated to manufacturer's specification
5. Fill-point syringe assembly
6. Safety glasses/face shield and gloves
7. Permanent black ink marking pen
8. Environmentally controlled chambers capable of maintaining a constant 22 +/- 1ºC (72 +/- 2ºF)
and 38 +/- 1ºC (100 +/- 2ºF).

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 84 bottles, minimum.

SAMPLE PREPARATION
1. Inspect a set of 84 bottles to ensure that no samples are out of perpendicularity and or have
rocker bottoms.
2. Using the marking pen, number the samples 1-84.
3. Rinse each sample with water to remove any dirt or dust before filling with water or the
product.

PROCEDURE
1. Fill samples with carbonated water or product to a level of:
CSD: 4.2 ± 0.1 volumes
NCB Cold fill Pressurized: 2.72 bar (40 ± 5psi)
2. Using the fill-point syringe assembly, syringe each bottle down to the proper fill height.
3. Apply closure to closure manufacture’s application specification.
4. Store samples in an environmental chamber at 22 + 1°C (72º + 2ºF) for the duration of the
test.

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PRESSURE RETENTION: ZAHM NAGEL

5. For high temperature (38°C/100°F) conditions, remove samples from the chamber and allow
them to stabilize at room temperature (22°C/72°F) for 24 hours.
SAMPLE TESTING
1. Using the table below as a guide, randomly select 12 samples for pressure and temperature
measurements.
2. Use the Zahm & Nagel tester, following the procedure below:
a. Calibrate Zahm Nagel thermometer (or temperature probe) and pressure gauge according to
manufacturer’s instructions.
b. Close tester vent valve.
c. Position sample in tester, directly under the piercing needle.
d. Squeeze the lock plates on both sides of the cross bar and lower the testing head assembly
so that the piercing needle rests on the top center of the closure. While squeezing the lock
plates, rapidly push down on the crossbar to pierce the closure. NOTE: A quick insertion
of the piercing needle is required to prevent carbonation loss.
e. Release the lock plates to lock the cross bar in place with the rubber seal compressed to
prevent leakage.
f. Insert the thermometer (or temperature probe) down until the tip is in contact with the bottom
of the bottle.
g. Read and record initial pressure.
h. Shake sample in tester (ultrasonic agitation or shaker table preferred) vigorously for 90
seconds.
i. Allow the samples to “relax” for an additional 60 seconds (no agitation).
j. Observe and record the pressure and temperature. Read pressure to the nearest 0.5 psi
(0.04 kg/cm2) and temperature to the nearest 0.5°C (1°F). Inspect visually for leaks during this
step. If found, discard the sample and select an alternate.
k. Open the vent valve slowly to relieve pressure and remove the thermometer (or temperature
probe).
l. While squeezing the lock plates, pull up on the cross bar to remove the sample from the tester.

CSD Intervals NCB Intervals

22°C (72°F) 38°C (100°F)* 22°C (72°F) 38°C (100°F)*
At time of fill N/A At time of fill N/A
24 hrs. 24hrs. 24hrs. 24hrs.
2 wks. (14 days) 3 days 2 wks. (14 days) 2 wks. (14 days)
4 wks. (28 days) 7 days 4 wks. (28 days) 4 wks. (28 days)
6 wks. (42 days) 14 days 6 wks. (42 days)
9 wks. (63 days)
12 wks. (84 days)
* OPTIONAL: Per end user’s requirements

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PRESSURE RETENTION: ZAHM NAGEL

DATA REPORTING REQUIREMENTS

Report Pressure, Temperature and resulting CO2 value for each sample Report Average, Standard
Deviation, and Range (both minimum and maximum) for the carbonation value at each time
interval.

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PHYSICAL PERFORMANCE TEST METHOD TOP LOAD – NON VENTED

PURPOSE
Empty bottles must be able to withstand a top load in the form of counter pressure during lift
cylinder filling and capping operations. The purpose of this test is to observe whether empty
bottles (non-vented) can sustain top load without failure.

APPLICATION
PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill

TEST EQUIPMENT
Calibrated compression tester (0-150 lb load cell) or equivalent with a non-vented, steel load plate.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment.

2. Obtain bottles that have been aged at least 72 hours after production.

3. Test at 510mm (20 inches) per minute cross-head speed. The load plate must be non-
vented.

4. Record the Newton or pound force for each bottle at 3.75mm (0.150”) deflection. If the
maximum load is prior to 3.75mm (0.150”) deflection, record the max load and the deflection at
which it occurs.

5. Record where the bottle failed (i.e. crushed foot, shoulder dent, etc.)

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PERFORMANCE TEST METHOD TOP LOAD – VENTED

PURPOSE
Empty bottles must be able to withstand a top load pressure during normal warehousing. The
purpose of this test is to observe whether empty bottles (vented) can sustain top load without
failure.

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill Non-Pressurized; Hot Fill

TEST EQUIPMENT
Calibrated compression tester (0-150 lb load cell) or equivalent with a vented, steel load plate.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Obtain bottles that have been aged at least 72 hours after production.

2. Verify calibration of equipment.

3. Test at 510mm (20 inches) per minute cross-head speed. The load plate must be vented.

4. Record the Newton or pound force for each bottle at 3.75mm (0.150”) deflection. If the
maximum load is prior to 3.75mm (0.150”) deflection, record the max load and the deflection at
which it occurs.

5. Record where the bottle failed (i.e. crushed foot, shoulder dent, etc.)

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PHYSICAL PERFORMANCE TEST METHOD TOP LOAD – FILLED & CAPPED

PURPOSE
Filled bottles must be able to withstand the compressive force of warehouse stacking. The purpose
of this test is to use the top load result to calculate the number of pallets high finished product can
be stacked during storage.

APPLICATION
PET Bottles: NCB-Cold Fill-Non-Pressurized and Hot Fill.

TEST EQUIPMENT
Calibrated compression tester (0-150 lb load cell) or equivalent with a vented or non-vented, steel
load plate.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Verify calibration of equipment.

2. Obtain bottles that have been aged at least 72 hours after production. Fill to level per end
user’s product requirements and cap with appropriate size closure.

3. Test at 510mm (20 inches) per minute cross-head speed. It does not matter whether the
load plate is vented or non-vented as the bottles are capped.

4. Record the Newton or pound force for each bottle at 6.35mm (0.250”) deflection. If the
maximum load is prior to 6.35mm (0.250”) deflection, record the max load and the deflection at
which it occurs.

5. Record where the bottle failed (i.e. crushed foot, shoulder dent, etc.)

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PHYSICAL PERFORMANCE TEST METHOD THERMAL STABILITY

PURPOSE
CO2 gas in carbonated beverages exerts a pressure on the container walls. As temperature
increases, pressure increases, causing the bottle to expand and creep (permanently deform under the
influence of an applied stress). Excessive creep will cause the beverage fill level to drop, which will
negatively affect package appearance and affect how the bottle fits into a carrier shell, sits on a shelf,
or fits into a vending machine. The purpose of this test is to measure a bottle’s resistance to creep.

APPLICATION
CSD and NCB Cold-fill Pressurized bottles.

TEST EQUIPMENT
1. Equipment or chemicals to carbonate bottle to 4.20 +/- 0.05 GV of CO2

2. An oven or temperature controlled room set to 38°C +/-1°C (100°F +/- 2°F) at any %RH

3. Equipment to measure carbonation level.

4. Measurement tools: Pi tape, height gauge, calipers, etc.

SAMPLE QUANTITIES
To be determined by end users’ specifications and risk analysis.
Recommendation: 12 bottles plus 3 extra for carbonation check.

PROCEDURE
1. Verify calibration of equipment.

2. Mark and then measure the required bottle dimensions on empty bottles.

3. Mark the target fill level height on each bottle.

4. Fill samples with carbonated water or product to a level of:

CSD: 4.2 ± 0.1 volumes
NCB Cold fill Pressurized: 2.72 bar (40 ± 5psi)

5. Wait approximately 1 hour after the bottles have been carbonated and check and record the
carbonation level on 3 extra samples. Then place the remaining 12 bottles in the 38°C (100°F)
condition.

6. Leave the bottles in the 38°C (100°F) condition for 24 hours.

7. Remove the bottles from the 38°C (100°F) condition and measure the required bottle dimensions.
a. Measure the bottles “hot” which is 2-4 hours after the bottles have been removed.
b. Measure the fill point drop from the original mark.
c. Check the bottles for final carbonation level.

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THERMAL STABILITY - CSD

d. Note any visual abnormalities.

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PHYSICAL PERFORMANCE TEST METHOD STRESS CRACK

PURPOSE
The hydroxide ion is the main catalyst of stress cracking in PET bottles. A bottle that has more
resistance to Sodium Hydroxide attack should be more resistant to stress crack initiators that a
bottle may be exposed to during its lifetime.

APPLICATION
Only CSD bottles.

TEST EQUIPMENT
1. Individual testing stations
2. Stop watch or timer
3. Compressed air regulated to 531 +/- 4 kilopascals (77 +/-0.5 psi)
4. Distilled water
5. Bottle closures
6. Titration apparatus (to determine alkalinity of NaOH solution)
7. Carbonated water
8. pH paper
9. 0.200% NaOH (sodium hydroxide), solution prepared with distilled water and solid NaOH
(also available as a commercial solution from VRW Scientific and Fisher as 0.05N NaOH))

Safety Concerns - The following list outlines known hazardous conditions. Conduct your
own job safety analysis prior to initiating this test.

1. NaOH is a strong alkali, which is corrosive to skin and eyes. Solid NaOH is also
hygroscopic. Dilution of solid NaOH with water is an exothermic reaction. Always add
NaOH slowly to water. Do not add water to NaOH. The pH of the 0.2% solution is about
12.7.
2. Total body protection is recommended when handling the solution and the pressurized
bottles.
3. It is highly likely the bottles will explode during the test procedure. It is imperative to take
proper precautions to prevent injury.
4. NaOH solution must be disposed of according to MSDS requirements.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 30 bottles, minimum.

PROCEDURE
1. Bottles should be less than 2 weeks old, then aged at 50˚C +/- 1 ˚C (122 +/- 2 ˚F) and 50%
RH for 24 hours. After aging, the bottles should be stored at 22˚C +/- 1˚C (72 +/- 2 ˚F) for a
minimum of 16 hours.
2. Prepare the solution according to the procedure in the reference section.

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STRESS CRACK

3. Verify the NaOH solution is equilibrated to 22˚C +/- 1˚C (72 +/- 2 ˚F). The solution must be
stored in a closed container to minimize absorption of CO2. The container should be labeled
and dated and used within one week of preparation.
4. Measure the alkalinity level of the 0.200% NaOH solution. The acceptable range of alkalinity
is 2402-2602 mg/l CaCO3.
5. Label each bottle in the order the testing will occur
6. Fill each bottle with the target net contents of water. (2L bottle would contain 2000ml of water)
The water should be equilibrated to 22˚C +/- 1˚C (72 +/- 2 ˚F).
7. Pressurize each bottle with compressed air to the equivalent internal pressure of 531 +/- 4
kilopascals (77 +/-0.5 psi).
8. 5 minutes after pressurizing the bottles mark the liquid level on each bottle and then gently
place each bottle into an individual pocket of 0.200% NaOH solution at 22˚C +/- 1˚C (72 +/- 2
˚F). The solution must cover the base up to the top of the strap.
9. Record the start time as the time that the bottle was placed in the 0.200% NaOH solution.
10. The bottles should be checked on the following frequency:

0-30 minutes: Continual Monitoring

30-60 minutes: Check every 2 minutes
60-90 minutes: Check every 5 minutes
>90 minutes: Check every 10 minutes
If the Technician leaves the room, it should be noted on the data collection sheet.

11. Record the time to failure in minutes for each bottle. Failure is defined as a burst or a slow
leak. A slow leak is evidenced by a visual fill point drop.
12. After each use, carefully rinse and dry each test station.

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PHYSICAL PERFORMANCE TEST METHOD VACUUM RETENTION

PURPOSE
To determine the amount of vacuum a package can hold over a period of time, and/or note the
amount of vacuum lost over time. Many hot filled products hold a vacuum for seal security. Since
most hot filled products are not head spaced, it is hard to ascertain the amount of vacuum
generated after sealing. This test can be performed using a predetermined headspace so the
samples to be tested will generate a repeatable vacuum. The amount of vacuum in the
headspace can be measured with the appropriate gauge set up. Any loss of vacuum over time
can then be measured with reliability.

APPLICATION
Only Hot Fill Bottles.

TEST EQUIPMENT
1. Hot Filler or acceptable substitute.
2. Head space tool.
3. Cooling shower
4. Single head/Lab capper, Vibrac in application mode, or Secure Pak Spring Torque Tester for
application.
5. Gloves.
6. Canner’s gauge with appropriate neck holder set-up or Terriss CO2 tester converted to
Vacuum with the appropriate gauge and neck holder.

SAMPLE QUANTITIES
To be determined by end users’ specifications and risk analysis.
Recommendation: 12 bottles minimum

PROCEDURE
1. Hot fill bottles at required temperature, flood fill to top of finish.
2. Heat closures to required temperature.
3. Headspace to predetermined depth.
4. Immediately place closure down on finish and apply closure to required torque.
5. Cool as required in cooling shower or bath.
6. Hold 24 hours or overnight at ambient or predetermined temperature.
7. Adjust piercing head to proper height.
8. Place bottle in neck holder, turn on gauge.
9. Pierce and read gauge.
10. Record vacuum.
11. Repeat for the rest of the samples requested.
12. Store any remaining samples as requested.
13. Repeat sample readings at intervals requested.

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REFERENCE TESTS

The reference section consists of several tests that may be helpful to use
during bottle development or special troubleshooting. The Subcommittee
acknowledged that in addition to the full test methods included in this section,
that there were several ASTM methods that are commonly used. As the
methods are documented via the ASTM, it was determined that they did not
need to be repeated here. The following grid lists several ASTM test methods,
along with their corresponding ASTM numbers, to ensure that all applicable
test methods are documented in this manual.

Test Method ASTM Test Method Number

Acetaldehyde (AA) – Ground Preform F-2013-00
AA – Head Space D-4509
Oxygen Transmission : MOCON F-1307-0
Transportation Test 4169-96

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REFERENCE TEST METHOD CO2 RETENTION: NON-DESTRUCTIVE

PRINCIPLE
The carbonation level in bottles varies with time due to volume expansion, sorption and
permeation. Carbonation loss may also result from improperly applied closures. It is essential to
have the CO2 content within specified limits to assure product quality. The purpose of this test is
to determine the carbonation level in filled and capped bottles as a function of termperature,
pressure and time.

APPLICATION
Only CSD bottles.

APPARATUS
1. Calibrated pressure gauge or transducer [readability to 0.03 bar (0.5 psi)] fitted with shut off
valve (Whitey ball valve) and Luer-Lok adapter (Thomas Scientific #8960-D59)

2. Closures punched, fitted with rubber septums (Thomas Scientific #1780-J07) and applied with
superglue inside and out

3. Syringe needles (Thomas Scientific #8956-B90)

4. Calibrated thermometer or thermocouple with readability to 0.25° C ( 0.5° F)

5. Constant temperature room set at 21° C ± 1° C ( 70° F ± 2°F)

6. Gas Volume Slide Rule appropriate for product being tested (diet or sugar).

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 30 bottles, minimum.

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CARBONATION RETENTION : NON-DESTRUCTIVE TEST METHOD

TEST INTERVAL CHART

Time (days) Time (weeks)

0 0
2 0.3
14 2
21 3
28 4
42 6
56 8
70 10
84 12
98 14
112 16
126 18

PROCEDURE
1. Mark and identify each bottle sample.

2. Fill the 30 random test bottles to fill point with carbonated water* 22°C (72°F) to 4.20 ± 0.05
gas volumes and apply closures fitted with rubber septums. (Note: These 30 bottles will be
used throughout the test to measure pressure of the container for gas volumes calculations,
herein referred to as Pressure Bottles.) Record capacity at fill volume.

3. Fill the 3 random bottles with carbonated water* or tap water 22°C (70°F) which is at the same
temperature as the carbonated water. Apply regular CSD closures. (Note: These 3 bottles
will be used throughout the test to measure the temperature of the water for gas volume
calculations, herein referred to as Temperature Bottles. These will not be used to measure
pressure.)

*Carbon Dioxide [C02] injection is the only acceptable form of carbonating.

4. Immediately upon filling and capping (within 1-hour), shake all pressure and temperature
bottles 5 minutes to equilibrate the pressure and temperature inside the bottles.

5. Immediately after shaking, measure and record (within 1/2-hour) the initial interval reading
(T=0):

a. Record the pressure of each Pressure Bottle using the needle-pressure gauge assembly.
(Note: The gauge must be pre-pressurized between each reading by closing the shut off
valve.)

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CARBONATION RETENTION : NON-DESTRUCTIVE TEST METHOD

b. Record the average temperature of the Temperature Bottles.

c. Determine the volumes of CO2 for each Pressure Bottle using a Gas Volume Circular Slide
Rule or equivalent chart appropriate for product being tested (diet or sugar). (Note: When
testing with carbonated water use the “Diet” side of the Circular Slide Rule.)

d. Record raw data.

6. Store all Pressure and Temperature Bottles in the constant temperature room for the duration
of the test.

7. For each subsequent test interval repeat procedure steps 4 through 6.

8. Continue the test until the test interval CO2 gas volume mean is less than 3.2 (or 0.8 gas
volumes loss). Conduct at least one more test interval past 0.8 gas volumes loss.

CALCULATIONS & REPORT

1. Calculate and report the average, minimum and maximum gas volume for each test interval.

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CARBONATION RETENTION : NON-DESTRUCTIVE TEST METHOD

Source:
Dev Tech, Inc.
15 Columbia Drive
Amherst, NH 03031
Phone: 603-889-8311
Fax: 603-889-8221

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REFERENCE TEST METHOD CARBONATION RETENTION: MOCON

PRINCIPLE
To determine carbonation loss and shelf life of PET bottles. Testing CO2 permeation with the
Mocon provides a rapid approximation of the result obtained by the Zahm Nagel method. This
method tests a single set of conditions. Actual shelf life is very dependent on external
environmental conditions, therefore common sense must be exercised in interpreting the results.
APPLICATION
Only CSD Bottles

TEST EQUIPMENT
1. Mocon Permatran C or equivalent, with suitable test fixtures
2. Carbonated beverage filling systems
3. Zahm Nagel Carbonation Tester or equivalent
4. Cadbury Beverages carbonation chart/wheel
5. Appropriate closures
6. Temperature and humidity controlled storage faciltiy.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 22 PET bottles (minimum for Refillable PET)
12 PET bottles (minimum for Non-refillable PET)

RELEVANT READING
1. Mocon Permatran Operating Instructions

PROCEDURE
1. Measure and record the following criteria on 12 of the bottles selected at random:
a. Bottle Weight
b. Wall Thickness (base, label panel, shoulder)
c. Volumetric Expansion/Creep (see Method PTP203)
d. Overflow Capacity
e. Base configuration
2. Fill all bottles to normal fill level with carbonated water or product to 4.8 +/- 0.2 volumes CO2.
3. Use a filling method capable of consistent carbonation and fill level control to +/- 0.2 volumes
CO2 and +/- 15 mil, respectively.
4. Measure off-line carbonation, using Zahm-Nagel Non-Snift test method, of every fifth bottle
filled. This measurement should be made five minutes after filling that particular bottle. If
bottle samples are in short supply, the bottles test for carbonation may be refilled, if they are
not visibly damaged.
5. Record the temperature and pressure reading for each of the samples tested. Then,
determine and record the carbonation, in volumes CO2 using the Cadbury Beverages Gas
Volume Chart or Cadbury Beverages carbonation wheel.

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CARBONATION RETENTION: MOCON

6. Store bottle in controlled environment, as follows:

Temperature: 21oC +/- 2oC (72oF +/- 2oF

Relative Humidity 50% +/- 5%

7. Determine Carbonation

a. Sample according to Table 1 below

b. Use Cadbury Beverages Test Method FPTM-014b (Non-Snift)
c. Record temperature and pressure for each bottle
d. Determine and record carbonation, in volumes CO2, using either the Cadbury Beverages
Gas Volume Chart or the Cadbury Beverages carbonation wheel.

8. Mocon Permeation Determination

a. After appropriate equilibration period (i.e., 2wks N/R PET; 6 wks. Ref/PET) conduct Mocon
testing (see discussion for further clarification).
b. Record permeation for the package in units of :

P = (cc)/()pkg.day)

CALCULATIONS & REPORT

1. To convert the Mocon reading in (cc)/(pkg-day) to (vols CO2)/(week), use the following
equation:

CO2 Loss Rate = 7 P

V
where 7 = the days/week
P = the Permeation rate in (cc)/(pkg.day)
V = the container overflow volume in (cc)

2. Detemine average, minimum and maximum carbonation values for each of samples (i.e., time
= 0, 24 hr, 2 wk, …).

3. Plot average, minimum and maximum carbonation values (in volumes CO2) vs. time (in
weeks). See Figure 1. for example.

4. Use the time = 2 wk reading* as the y-intercept and the CO2 loss (in vols CO2/week) as the
slope to plot the equation:

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CARBONATION RETENTION: MOCON

Y = mx +b

where
y= the Y-coordinate
m = the slope (CO2 Loss Rate)
x = the X-coordinate
b = the Y-intercept (time = 2 wk*)
* - 6 weeks for RefPET

5. Shelf life limit calculation:

The minimum carbonation (i.e., shelf life - 15% CO2 loss) is determined by the following
formula:

= 0.85 [(24 hr carbonation) - 0.3]

6. Overlay the minimum carbonation on the carbonation vs. time plot. The "X" coordinate of the
intersection between the CO2 loss curve and the minimum carbonation life is the shelf life for
the bottle being tested (at test conditions, of course). See Figure 1. for example.

DISCUSSION
When considering CO2 "loss" in PET containers, there are several important factors that must be
sonsidered, as follows:

Bottle Creep (expansion under the pressure of carbonation)

Although carbonation is not "lost" from the package, the CO2 is no longer in solution in the
beverage, which is really why we measure carbonation in the first place. The “creep loss" of CO2
is due to the greater volume of the bottle after expansion and the resulting equilibration of the CO2
in the headspace. Bottle creep is measured using the Topwave Creep Tester (Cadbury
Beverages Method PTP203), and the measurements can be directly related to the initial
carbonation loss observed in the first 24 hours after filling.

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CARBONATION RETENTION: MOCON

Absorption of Carbon Dioxide (by the PET)

Table 1 -- Pull Schedule

Test Interval Zahm Nagel Mocon Test

Sample Number (from time of filling) No. of Bottles No. of Bottles
0 At filling As required
1 24 Hours 5
2 2 Weeks 5 2 N/R PET
3 4 Weeks 5
4 6 Weeks 5 2 RefPET
TOTAL BOTTLES 12 (NR PET)
22 (RefPET))

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CARBONATION RETENTION: MOCON

Figure 1 -- Example CO2 vs. Time Plot

5
AVG
4.5
MAX
CO2 (volumes)

4 MIN
SPEC
3.5

2.5
0 5 10 15 20
Time (weeks)

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REFERENCE TEST METHOD CARBONATION RETENTION: FTIR

PRINCIPLE
The FT IR method for carbonation retention testing is designed to accurately assess the
carbonation loss-rate of a plastic beverage bottle and to extrapolate shelf-life to 17.5% loss. The
amount of CO2 is evaluated in a sample size of 12 test bottles over a 49 day period for non-
refillable or a 70 day period for refillable plastic bottles, using an infrared light beam. Based on the
calculated loss rate determined from this test, a shelf life can then be accurately calculated.

APPLICATION
Only CSD Bottles.

TEST EQUIPMENT
1. A calibrated Zahm & Nagel Piercing Device with pressure gauge (capable of measuring 0-100
psi or 0-690 bar).
2. A supply of "bone dry" CO2 (moisture level not to exceed 15ppm and CO2 must be at least
99.8% pure).
Safety Note: Use protective gloves when handling frozen CO2. Ensure the area is well
ventilated.
3. Approved plastic closures that properly fit the test bottles.
4. Analytical gram balance accurate to +/-0.1 grams.
5. Approved device to measure bottle diameters accurate to +/-0.1mm, such as:
• Optical comparator with a minimum magnification of 20X or,
• Laser measuring device.
6. Approved properly calibrated FTIR instrument, such as:
Perkin-Elmer FTIR Spectrometer with supporting hardware fixtures and software patented by
The Coca−Cola Company are recommended.
7. Safety glasses/face shield and gloves.
8. Torque meter to properly apply approved plastic closures.
9. Permanent ink marking pen.
10. Environmentally controlled chamber or room capable of maintaining a constant 22º +/-1ºC and
50% relative humidity (RH).

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

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CARBONATION RETENTION: FTIR

PROCEDURE
Sample Preparation
Marking Samples
1. Pre-inspect the 12 non-refillable plastic bottles to be tested to ensure that no bottles are out of
perpendicularity or have rocker bottoms.
a. Two extra bottles will be required for validating initial carbonation level.
2. Mark each sample with an individual number for identification purposes.
3. Mark all 12 sample bottles with an indexing line, on the heel or foot that runs through the
center of base. This line is used to ensure that the bottles can always be properly and
consistently aligned on the FTIR.
a. The indexing line must not fall on a dimple, flute or bottle parting line, or other irregular
surface area of the bottle.
Determining Sample Volume and Dry Ice Weight
It is necessary to first determine the bottle volume so that the proper amount of dry ice is used to
achieve the correct internal pressure. To determine the proper amount of dry ice, do the following
steps:
1. Place one sample bottle on an analytical balance and tare the scale to zero.
2. Fill the sample bottle to the brim-full capacity (to top of bottle finish) with water of known
temperature.
3. Record the weight of the water in grams.
4. Convert the water weight (g) to bottle volume (mL). Use the following conversion table:
Water Temperature H2O specific volume
(mL/g)
19ºC 66.2ºF 1.002637
20ºC 68.0ºF 1.002838
21ºC 69.8ºF 1.003039
22ºC 71.6ºF 1.003261
23ºC 73.4ºF 1.003492
5. Convert the bottle volume (mL) to weight of dry ice (grams) by using the following formula:
(Bottle volume in mL) x (0.0077) = weight of dry ice (grams)
a. This weight of dry ice should yield an internal bottle pressure of 3.81 +/- 0.14bar (56 +/- 2
psi) at 22ºC, which is the equilibrium pressure of 4.0 volumes of CO2 at 22ºC.

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CARBONATION RETENTION: FTIR

Filling Samples with Dry Ice

Safety glasses should be worn while the sample bottles are being filled with dry ice. Gloves should
be worn to prevent skin burns when handling dry ice.
1. Place one empty bottle and closure on the balance and then tare their combined weight.
2. Continue to add small pieces of dry ice to the bottle until the weight exceeds the previously
calculated weight (refer to Step 5) by approximately 0.3g.
3. Put an approved plastic closure on the bottle finish and screw down loosely without completely
sealing the bottle. Observe the balance reading. As the dry ice sublimates, the weight of the
bottle/sample will decrease. Once the balance reading is approximately 0.1 grams greater
than the calculated dry ice weight (3.2.5), quickly tighten the closure on the bottle. The plastic
closure should be tightened by hand to the application torque recommended by the closure
manufacturer.
4. By hand, gently swirl the bottle at ambient temperature (approximately 22ºC) until all the dry
ice evaporates inside the bottle. Do not hit the bottles on tables, or on any other rigid objects
to break up the dry ice. This may affect the physical characteristics of the bottle.
5. After all of the dry ice has evaporated in the capped bottle, check the internal pressure of the
sample using a Zahm and Nagel piercing device. The pressure should 3.81+/- 0.14bar ( 56 +/-
2 psi) at a temperature of 22ºC +/- 1ºC (72 ºF +/- 2ºF). .
6. If necessary, use an additional bottle to adjust the amount of dry ice until the correct pressure
is obtained. Once the correct pressure has been confirmed, fill 12 test bottles with the
confirmed amount of dry ice per the procedure described in Steps 1 − 3.
Measuring Initial Bottle Diameters
1. After the samples have been filled and capped, and all of the dry ice has sublimated, measure
the bottle diameters. The initial diameter measurements must be made within 10 to 30 minutes
after the dry ice has sublimated.
2. Measure each bottle at 86mm up from the base of the bottle. This corresponds to the exact
point where the FTIR beam passes through the bottle. Ensure that all bottles are aligned
consistent with their heel mark (refer to Step 3 in the “Marking Samples” section included
previously in this document). Record this as the initial diameter for each sample.
a. All diameters need to be measured at the same distance from the base for each interval.

IR CALIBRATION
Calibrate the IR instrument according to the manufacturers recommended procedure.

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CARBONATION RETENTION: FTIR

SAMPLE TESTING
1. After the 12 test bottles have been pressurized and the initial diameters measured, they will be
evaluated on the FTIR to establish the initial CO2 concentration.
2. After all 12 test bottles have been measure for CO2 concentration, store the samples in a
conditioned environmental chamber (22ºC +/- 1ºC or 72ºF +/- 2ºF at 50% RH).
3. At each interval shown in the table below, the CO2 level will need to be measured on the FTIR.
You do not need to measure the diameters at every interval. To see a suggested frequency for
diameter measuring refer to “Sample Measurement Schedule” section later in this document.

SAMPLE STORAGE
Store all test bottle samples in an environmentally controlled room or chamber at 22ºC +/- 1ºC or
72ºF +/- 2ºF, 50% relative humidity (RH), between each test interval throughout the entire test
period.

SCHEDULE FOR MEASURING SAMPLES

Measure the CO2 level for each test bottle according to one of the following schedules:
NON-REFILLABLE BOTTLES
Test Interval Days Diameter Measurement
1 (initial) 0 (10 to 30 minutes after filling) X
2 1 X
3 10 X
4 14 optional*
5 18 optional*
6 25 X
7 33 optional*
8 40 optional*
9 44 optional*
10 (final) 49 X

1. The schedule should be followed as closely as possible so as not to miss a measurement

interval, otherwise the final results may be affected.
2. The initial (#1) and the 1 day (#2) interval measurements cannot be missed or delayed. The
initial measurement will be used as the baseline from which the subsequent CO2 loss and
shelf life will be calculated. The 1 day (#2) is not used in the CO2 loss calculation. It can be
used to characterize the CO2 loss within the first 24-hour period if necessary.

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CARBONATION RETENTION: FTIR

3. If a measurement cannot be performed at the scheduled time (in case of a holiday or

weekend), it may be performed up to three days later (except interval 1 and 2). A late or
delayed measurement will result in a longer test period, but there is no negative influence on
the accuracy of final test results. A measurement should never be performed prior to its
scheduled interval.

DATA/REPORT REQUIREMENTS
1. All data should be reported in a standardized format. The data should include the projected
shelf life and the % CO2 loss per week.

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REFERENCE TEST METHOD CARBONATION RETENTION:

ORBISPHERE

PURPOSE
To accurately assess the carbonation loss-rate of plastic beverage bottles and closures filled with
carbonated water or product. The amount of CO2 will be evaluated using the Orbisphere Beverage
Package Analyzer (or comparable instrument) using a sensor to measure dissolved CO2 in the
product.
APPLICATION
CSD and other CO2 Pressurized Bottles.

TEST EQUIPMENT
1. A filling machine capable of filling carbonated water or product to 4.2 ± 0.1 volumes of CO2
2. Capping machine to apply approved closures that properly fit the test bottles
3. A calibrated Orbisphere Beverage Package Analyzer with a model 31460 CO2 sensor
4. A pure pressurized N2 gas supply
5. Digital or analog thermometer calibrated to manufacturer's specification
6. Safety glasses/face shield and gloves
7. Permanent ink marking pen
8. Environmentally controlled chamber or room capable of maintaining a constant 22º + 1ºC (72
+ 2°F) and 50% relative humidity (RH), or other conditions if specified.
9. Horizontal bottle shaker
10. Water bath for bring bottles to room temperature for testing {capable of maintaining a constant
22º + 1ºC (72 + 2°F)}.

Other Applicable Methods

Chemical carbonation or carbonator

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 64 bottles, minimum.

SAMPLE PREPARATION
1. Inspect a set of 64 bottles to ensure that no samples are out of perpendicularity and or have
rocker bottoms.
2. Using the marking pen, number the samples 1-64.

PROCEDURE
1. Fill samples with carbonated water or product to recommended fill level and carbonation level
of:
CSD: 4.2 ± 0.1 volumes
2. Apply closures with specified torque and conditions.

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PRESSURE RETENTION: ORBISPHERE

3. Store samples in an environmental chamber at 22 + 1°C and 50% RH for the duration of the
test.
4. If other storage conditions are required, make note of them, and bring bottles to room
temperature for testing. Variations of more than 1-2°C will introduce noticeable scatter to the
results.

SAMPLE TESTING
1. Submerge 8 randomly selected bottles in the water bath to warm them to 22 + 1°C (72 + 2°F).
Confirm product temperature with a “dummy” bottle.
2. Using a horizontal shaker, agitate for a minimum of 3 minutes to assure that equilibrium has
been established between the liquid and headspace.
3. Test the bottle on the Orbisphere by piercing the closure and lowering the sampling tube when
requested by the software. (1 hour after filling).
4. Record the “CO2 Sensor” value (v/v). This is the actual dissolved CO2 concentration in the
liquid, and will be the initial measurement used in calculations. The software also records a
“CO2 Pressure” value, which is analogous to the Zahm & Nagel measurement, and is based
on measured temperature and pressure. The amount of N2 in the product is also calculated by
the software.
5. Continue to perform and record 8 measurements from the remaining samples at:

CSD Intervals
At time of fill
24 hours
1 week
2 weeks
4 weeks
6 weeks
9 weeks
12 weeks

DATA REPORTING REQUIREMENTS

1. Determine average, minimum and maximum carbonation value at each time interval.
2. Carbonation loss is defined as:
% Carbonation Loss = [initial carbonation (v/v) – current carbonation (v/v)]*100
[initial carbonation (v/v)]
3. Determine best linear fit of daily average carbonation loss (omitting data <1 week) vs. storage
days, and extrapolate to the specified maximum allowable carbonation loss to determine shelf
life. Confirm that points included in the fit are outside the nonlinear portion of the curve.

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REFERENCE TEST METHOD OXYGEN TRANSMISSION: ORBISPHERE

PURPOSE
The objective of this test is to determine the oxygen transmission through the bottle and closure
during the shelf life of the product. This method can also be used to determine the affect of various
environmental conditions on the oxygen transmission rate of the package.

The oxygen barrier properties of plastics and oxygen scavengers used in packaging are greatly
affected by manufacturing, filling, and storage conditions. By measuring the total package oxygen
over time the oxygen ingress can be determined under conditions that closely resemble the actual
life of the package. This method also allows the identification of the activation and consumption of
oxygen scavengers.

APPLICATION
PET Bottles: NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill:
The transmission rate for bottles is determined by using a foil barrier lined closure to eliminate
transmission through the closure during the test.

Plastic Closures: NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill.

The transmission rate of the closure and gasket is determined by using a non-scavenger bottle
and subtracting the transmission rate for the bottle only (using a barrier foil lined closure) from the
transmission rate for the total package.

TEST EQUIPMENT
1. Sealed water preparation tank
2. Tank heater for hot-fill applications
3. Regulated carbon dioxide or other inert gas supply
4. Counter-pressure bottle filler
5. Appropriate closing equipment
6. Bottle shaker
7. Orbisphere Package Analyzer capable of measuring dissolved oxygen at 1 ppb.
8. Environmental chambers

SAMPLE QUANTITIES
Six samples per variable per test period are recommended. Initial and final test periods are
required, additional data points are suggested to identify activation and consumption of
scavengers, and affect of package abuse.

SAMPLE PREPARATION
Bottles or closures are labeled to identify type and series number. Samples should be filled, stored
and tested in a manner to not allow any bias.

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Oxygen Transmission: Orbisphere

PROCEDURE
1. Deoxygenating Water: Water is deoxygenated by bubbling inert gas through it for 24 hours or
by boiling for 15 minutes and cooling to desired fill temperature under inert atmosphere.
2. Filling: Using a counter-pressure filler, bottles are flushed with inert gas, and then filled to the
appropriate level from the bottom to minimize incorporation of air in the liquid. The headspace
is flushed with inert gas before applying the closure.
3. Processing: If additional processing such as cooling or pasteurization is carried out in
production, the test samples are treated the same way.
4. Storage: Samples are stored at 22+/-1°C (72+/-2°F) for standard test. Additional samples can
be stored at 100 F, in an oxygen atmosphere for 5X acceleration, or abused with a headload
or transportation test.

SAMPLE TESTING
1. Samples to be tested are stored at 22+/-1°C (72+/-2°F) for 24 hours
2. Samples are shaken for 30 minutes.
3. Each bottle is measured for total package oxygen with the Orbisphere Package Analyzer

ANALYSIS OF DATA
1. In order for the test to be valid, the initial total package oxygen values should be below 400
ppb and have a standard deviation of less that 15 % of the average.
2. The Total Package Oxygen values for each type of package are plotted versus time. The
slope of the best-fit line is the overall oxygen transmission rate for the package.
3. A reduction in the slope towards the beginning of the test indicates the activation of an oxygen
scavenger.
4. An increase in the slope either indicates the consumption of an oxygen scavenger or the loss
of sealing integrity.
The range of the Total Package Oxygen values at the various time intervals is an indication of
consistency of the oxygen barrier properties

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 INTERNATIONAL SOCIETY OF BEVERAGE TECHNOLOGISTS

REFERENCE TEST METHOD PERPENDICULARITY

PURPOSE
The perpendicularity test is designed to ensure that non-refillable plastic bottles stand upright in an
orientation that is completely perpendicular to the bearing surface on which they stand.

APPLICATION
All PET Bottles: CSD; NCB-Cold Fill Pressurized; NCB-Cold Fill-Non-Pressurized; Hot Fill.

TEST EQUIPMENT
1. Perpendicularity gauge assembly or equivalent.

SAMPLE QUANTITIES
To be determined by end users' specifications and risk analysis.
Recommendation: 12 bottles, minimum.

PROCEDURE
1. Using 108 randomly selected sample bottles as a source, select a sub-group of 12
perpendicularity samples.
2. Fill each sample bottle approximately half full with tap water and place it in the measuring
apparatus. Be sure that the base of each bottle is held securely in the support fixture.
3. Adjust the dial indicator contact so that it rests on the locking ring of the bottle finish. Set the
dial indicator on "0."
4. Rotate the bottle through at least 360° and note the maximum and minimum deviation on the
gauge on either side of vertical. Set the zero mark of the gauge at that position.
5. Repeat steps 3 and 4 for remaining samples.
6. Record all measurements.

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REFERENCE TEST METHOD SODIUM HYDROXIDE PREPARATION

PURPOSE
The purpose of this document is to outline the multiple procedures to prepare the 0.200% sodium
hydroxide (NaOH) solution from sodium Hydroxide bead or powder for use in the Stress Crack
Test Method.

METHOD 1: 0.200% NaOH Solution Preparation from Sodium Hydroxide Bead or Powder

Caution: Sodium Hydroxide is corrosive to skin and eyes. Use appropriate personal protective
equipment. See the test methods and MSDS for safety precautions.

Caution: The reaction of water with sodium hydroxide is exothermic. Use care with all mixing.

Note: Sodium Hydroxide absorbs moisture and carbon dioxide from the atmosphere. Since the
sodium hydroxide concentration is critical to the outcome of this test, either buy new sodium
hydroxide for each test or be certain that the sodium hydroxide has been stored in a tightly sealed
container and the beads (or powder) are free flowing.

PROCEDURE
1. Weigh the distilled water and pour it slowly into the mixing vessel.
2. Weigh the sodium hydroxide (100% active) and add slowly, with stirring, to the distilled water
in the mixing vessel.
3. Stir until the sodium hydroxide is well dissolved and the solution is homogeneous.
4. Titrate the solution to confirm total alkalinity of 2502 {100 ppm (mg/L) as CaCO3}.
5. Transfer prepared sodium hydroxide solution to a closed container.
6. Store solution in a tightly closed container with minimal headspace for up to one week.

Batch Size
1000 gm 10,000 gm 18945 gm (~ 5 gal)

Bead / Powdered Sodium Hydroxide 2.00 gm 20.0 gm 37.9 gm

Distilled Water 998 gm 9980 gm 18907 gm

Alkalinity Test Kit Selection

Target range 2400-2600 ppm (mg/L) as CaCO3
Accuracy (50 ppm (mg/L) CaCO3

Example Test Kit:

Hach Alkalinity Test Kit with Digital Titrator 20637-00 AL-DT
10-4000 mg/L sampling range
10 mg/L smallest increment

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 INTERNATIONAL SOCIETY OF BEVERAGE TECHNOLOGISTS

REFERENCE TEST METHOD SODIUM HYDROXIDE PREPARATION

METHOD 2: 0.200% NaOH Solution Preparation from 50% Sodium Hydroxide Solution

Note: It is difficult to determine whether sodium hydroxide solutions have absorbed carbon dioxide
and formed carbonate, or become more concentrated due to evaporation. Since the sodium
hydroxide concentration is critical to the outcome of this test, the preferred method involves
preparing a solution from solid sodium hydroxide. If a stock solution must be used, check for any
precipitate in the bottom of the container, or any white crust formation on the mouth of the
container. If possible, titrate a known dilution of the sodium hydroxide solution, and confirm that
the total alkalinity is equal to the phenolphthalein (or ìactiveî) alkalinity. If precipitate or crusting
is present, or if the total alkalinity does not equal the active alkalinity, replace the stock solution
with freshly purchased sodium hydroxide.

Caution: Sodium Hydroxide is corrosive to skin and eyes. Use appropriate personal protective
equipment. See the test methods and MSDS for safety precautions.

Caution: The reaction of water with sodium hydroxide is exothermic. Use care with all mixing.

PROCEDURE
1. Weigh the distilled water and pour it into the mixing vessel.
2. Weigh the 50% sodium hydroxide solution and add slowly, with stirring, to the mixing vessel.
3. Stir until the solution is homogeneous.
4. Titrate the solution to confirm total alkalinity of 2502 (100 ppm (mg/L) as CaCO3.
5. Transfer prepared sodium hydroxide solution to a closed container.
6. Store in a tightly closed container with minimal headspace for up to one week.

Batch Size
1000 gm 10,000 gm 18945 gm (~ 5 gal)

50% NaOH Solution 4.00 gm 40.0 gm 75.8 gm

Distilled Water 996 gm 9960 gm 18869.2 gm

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REFERENCE TEST METHOD SODIUM HYDROXIDE PREPARATION

METHOD 3: 0.200% NaOH Solution Preparation from 1N Sodium Hydroxide

Caution: Sodium Hydroxide is corrosive to skin and eyes. Use appropriate personal protective
equipment. See the test methods and MSDS for safety precautions.

Caution: The reaction of water with sodium hydroxide is exothermic. Use care with all mixing.

PROCEDURE
1. Weigh the distilled water and pour it into the mixing vessel.
2. Weigh the 1N (normal) sodium hydroxide solution and add slowly, with stirring, to the water in
the mixing vessel.
3. Stir until the solution is homogeneous.
4. Titrate the solution to confirm total alkalinity of 2502 (100 ppm (mg/L) as CACO3.
5. Transfer the prepared sodium hydroxide solution to a closed container.
6. Store in a tightly closed container with minimal headspace for up to one week.

Batch Size
1000 gm 10,000 gm 18945 gm (~ 5 gal)

1N NaOH Solution 50.0 gm 500 gm 947 gm

Distilled Water 950 gm 9500 gm 17998 gm

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REFERENCE TEST METHOD SODIUM HYDROXIDE PREPARATION

Total Alkalinity Calculations

(0.200 gm NaOH) x (1 mole NaOH) x (1 mole equiv CaCO3) x (100.1 gm CaCO3) = (0.250 gm CaCO3)
(40.01 gm NAOH) (2 mole equiv NaOH) (1 mole CaCO3) (0.250% CaCO3) = (0.250% CaCO3)
= (2502 ppm (mg/L) CaCO3)
= 147.2 gpg

Error Limits (4% maximum)

Alkalinity Expression Lower Limit Desired Value Upper Limit
% CaCO3 0.2400 0.2500 0.260
ppm (mg/L) CaCO3 2402 2502 2602
gpg 141.3 147.2 153.1

Error Limit Calculations (4%)

Percent CaCO3
(0.250% CaCO3) ( (1.04) = 0.260%
(0.250% CaCO3) ( (0.96) = 0.240%

ppm (mg/L)
(2502 ppm CaCO3) ( (1.04) = 2602 ppm
(2502 ppm CaCO3) ( (0.96) = 2402 ppm

gpg
(147.2 gpg CaCO3) ( (1.04) = 153.1 gpg
(147.2 gpg CaCO3) ( (0.96) = 141.3 gpg

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Abbreviations
oC; oF Degrees, either in Celsius or Fahrenheit
ASTM American Standard Test Method
Bar unit of pressure
cc cubic centimeter
CO2 Carbon Dioxide
CRC Chemical Rubber Company
CSD Carbonated Soft Drink
D Diffusion
ft feet
FTIR Fourier Transform Infrared
g grams
GV Gas Volume
Hg mercury
H2 Hydrogen
H2O water
HPLC High Performance Liquid Chromatography
hr hour
in inch
ISBT International Society of Beverage Technologists
IV Intrinsic Viscosity
k solubility
kPa Kilo Pascal
lb pounds
mg milligram
mm millimeter
mL milliliter
MSDS Material Safety Data Sheet
N2 nitrogen
N Normal
NCB Non Carbonated Beverage
NPB Non Pressurized Beverage
N/R Non Refillable
O2 Oxygen
Ρ density
P permeation rate
PET Polyethylene Terephthalate
pkg package
PP Polypropylene
ppm parts per million

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PPT Plastic Pressure Tester

PSI pounds per square inch
RH Relative Humidity
s second
SST Secure Seal Tester
T time
TM Test Method
V volume
Vc volume percent crystallinity
wk week

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Bottle Test Procedures Manual

Issued: October 2003

Revision History
The table below chronologically lists revisions made to documents in this manual and a
summary of the change that was made.

Revision Date Details

June 2004 Header and footers where changed to meet
new ISBT Spec.

ISBT 2004