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Packaging Authorization for Refillable PET Bottles
REQUIREMENTS
REFPET Bottle Authorization Matrices REFPET Bottle Specifications PK-RQ-065 PK-SP-045

TEST PROCEDURES
Materials REFPET Bottle Acetaldehyde Test24-Hour REFPET Bottle Acetaldehyde TestGround Preforms REFPET Bottle Appearance and Color Evaluation REFPET Bottle Scientific and Regulatory Affairs Process REFPET Bottle Taste Compatibility Test Dimensional REFPET Bottle Dimensions EvaluationExterior REFPET Bottle Dimensions EvaluationFinish Physical Performance REFPET Bottle Capacity Change (Shrinkage) Test REFPET Bottle Carbonation Retention Test REFPET Bottle Drop Impact Test REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing REFPET Bottle Durability TestStandard Trip-Per-Two-Day Washing REFPET Bottle Empty Weight and As-Delivered Capacity Test REFPET Bottle Fill-Point Variation Test REFPET Bottle Internal Pressure Test REFPET Bottle Perpendicularity Test REFPET Bottle Plastic Distribution Test REFPET Bottle Support Ledge Strength Test REFPET Bottle Thermal Stability Test REFPET Bottle Vertical Load TestEmpty PK-PR-218 PK-PR-219 PK-PR-220 PK-PR-221 PK-PR-222 PK-PR-223 PK-PR-224 PK-PR-225 PK-PR-270 PK-PR-226 PK-PR-227 PK-PR-228 PK-PR-229 PK-PR-207 PK-PR-208 PK-PR-215 PK-PR-216 PK-PR-217 PK-PR-205 PK-PR-206

Packaging Authorization for Refillable PET Bottles Issued: 20-Dec-2004

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Table of Contents
Packaging Authorization for Refillable PET Bottles
TEST PROCEDURES (CONTINUED)
Functional REFPET Bottle Line Trial PK-PR-055

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REFPET Bottle Authorization Matrices


Purpose Scope
To provide the requirements, specifications and test procedures needed to authorize a package. These requirements were developed for carbonated beverages. Multi-product designs that are also used for noncarbonated products must also meet these requirements. If a specific bottle design is developed exclusively for noncarbonated products, then new specifications may be developed and reviewed with Global Quality and Global Packaging. Applies to suppliers of refillable PET (REFPET) bottles for: Carbonated water and soft drinks Noncarbonated (NCB) pressurized and non-pressurized water and beverages

Contents

General ...........................................................................................................1 Filling Test Packages ....................................................................................2 Materials Authorization Matrix .....................................................................2 Packaging Authorization Matrix...................................................................3

Requirements
General
This document is an integral component of New Package Authorization, PK-RQ-020. The following Materials and Packaging Authorization Matrices summarize the requirements and tests for authorizing a RefPET bottle for a specific set of circumstances. Which evaluations are required depends on whether a specific combination of package components has been used previously. Therefore, it is important to include authorization information in the Global Packaging database. The testing requirements and procedures referenced herein do not preclude any additional testing that may be required where local regulations or business needs make practical or necessary the adaptation of more stringent requirements. To authorize additional plants or divisions to use an approved bottle design (shape, size, weight), the division may delegate authorization responsibility to the bottler for filling line and finish compatibility.

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Filling Test Packages
If carbonated water is required for a test, then all packages should be filled at the same time just prior to testing in order to utilize laboratory resources efficiently and to ensure maximum carbonation uniformity among the samples. If packages are filled in the lab, use the same carbonation or pressure targets used on the filling line. Whenever possible, target the high-end of the specification. You can use the following to simulate CO2 or nitrogen pressure in the lab:
Target CO2 4.2 vol 0.1 vol May use sodium bicarbonate or citric acid carbonated water or sodium bicarbonate To replace or simulate carbonated water

Nitrogen

40 psi 5 psi or as specified by the operating division

nitrogen pressure if a liquid nitrogen source is not available

Materials Authorization Matrix


Taste Compatibility Physical Performance Tests

Appearance

Color

New Resin from New or Existing Resin Supplier New resin or change in resin formulation (new components) Approved PET resin with approved CyclePET material Any change other than resin chemistry (for example, change in IV or decrease in component levels) New Resin Plant Approved resin New Additives Any new additive used in plastic bottles (for example, colorants and UV additives)

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SRA

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REFPET Bottle Authorization Matrices


Packaging Authorization Matrix
Dimension Tests Physical Performance Tests
Plastic Distribution Fill Point Variation Capacity Change Internal Pressure Strength Thermal Stability Perpendicularity Empty Weight / Capacity Support Ledge Strength Acetaldehyde Vertical Load

Functional Tests

Carbonation Retention Drop Impact Resistance

Line Trial Pressurized

Operational

Transport

Durability

New Supplier or LicenseePlastic Bottles or PreformsNew Plant (Bottle Blowing) Using Approved Resin
Bottles Preforms Resin or additive new to supplier New blow molds for approved design/size New injection molds New bottle design/size Decrease in weight New blow mold plant/ authorized preforms Bottles Preforms

Authorized SupplierPlastic Bottles or Preforms

New Technology, Design, or Equipment

Test is optional based on the discretion of the division.

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Warpage

Resin IV

Vending

Field

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REFPET Bottle Authorization Matrices


Revision History
Issue Date
20-Dec-2004

Summary of Change
New document.

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REFPET Bottle Specifications


Purpose
To specify the minimum requirements of materials, dimensions and physical performance of REFPET bottles from authorized suppliers. All bottles upon delivery shall meet the specifications in this document. This document is an integral component of New Package Authorization, PK-RQ-020. For the test matrices, refer to REFPET Bottle Authorization Matrices, PK-RQ-065.

Contents

Materials Specifications................................................................................2 Acetaldehyde ............................................................................................2 Appearance...............................................................................................2 Color..........................................................................................................3 Scientific and Regulatory Affairs (SRA) and Certificate of Food Law Compliance .................................................................................3 Taste Compatibility....................................................................................3 Dimensional Specifications..........................................................................5 Exterior ......................................................................................................5 Finish.........................................................................................................5 Physical Performance Specifications..........................................................6 Capacity Change.......................................................................................6 Carbonation Retention ..............................................................................6 Drop Impact Resistance............................................................................6 Durability ...................................................................................................7 Empty Weight and Capacity As-Delivered..............................................7 Fill-Point Variation .....................................................................................8 Internal Pressure Strength ........................................................................8 Perpendicularity ........................................................................................8 Plastic Distribution.....................................................................................8 Support Ledge Strength ............................................................................9 Thermal Stability .......................................................................................9 Vertical Load .............................................................................................9

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Materials Specifications
Acetaldehyde
Test Procedures: REFPET Acetaldehyde Test24-Hour, PK-PR-215 REFPET Acetaldehyde TestGround Preforms, PK-PR-216

Clear resins

The acetaldehyde concentration of freshly blown bottles made from all clear resins shall be as follows:
Measurement Method Standard 24-hour airspace analysis Ground preform Criteria The maximum in any single bottle shall not exceed 5.0 micrograms/liter The maximum in any single bottle shall not exceed 25.0 micrograms/gram

Green and amber resins

The acetaldehyde concentration of freshly blown bottles made from all green and amber resins shall be as follows:
Measurement Method Standard 24-hour airspace analysis Ground preform Criteria The maximum in any single bottle shall not exceed 15.0 micrograms/liter The maximum in any single bottle shall not exceed 25.0 micrograms/gram

Appearance

Test Procedure: REFPET Bottle Appearance and Color Evaluation, PK-PR-217 Blemishes (bubbles, unmelted resin, dirt specks, pitting, condensation marks) shall not constitute a more objectionable appearance than that of the limit samples submitted to and authorized in writing by a division of The Coca-Cola Company. Except for the exterior bottom of the base, there shall be no foreign material (dirt) on the surfaces of the containers, which would not come off in a typical rinser used for one-way PET bottles. The bottles shall not develop objectionable scuffing more severe than limit samples submitted to and authorized in writing by a division of The Coca-Cola Company when subjected to normal handling.

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Color
Test Procedure: REFPET Bottle Appearance and Color Evaluation, PK-PR-217 All new bottles shall have a color and clarity (pearlescence and transparency) falling within limits or standards previously submitted to and approved in writing by The Coca-Cola Company. Used bottles shall have a color and clarity (haze) falling within limits or standards previously submitted to and approved in writing by The Coca-Cola Company.

Scientific and Regulatory Affairs (SRA) and Certificate of Food Law Compliance

Test Procedure: REFPET Bottle Scientific and Regulatory Affairs Process, PK-PR-200 The material reviewed must meet all internal SRA requirements, as well as comply with local or FDA requirements for food contact use. The material must also meet any requirements established by the Package Development and Design Department to minimize sensory impact. New materials such as resins, additives, and colorants are approved by SRA. After SRA approval is obtained, divisions are responsible for ensuring that the material meets all applicable food laws for the intended countries of use.

Taste Compatibility

Test Procedure: REFPET Bottle Taste Compatibility Test, PK-PR-206 A test package meets the compatibility specification when it imparts no significant taste difference (at a 95% confidence level) when compared to control samples after the required intervals. Sample ballots and statistical tables for interpreting triangle tests are in the test procedure. Any taste test that reveals a significant taste difference (at a 0.05 probability level or 95% confidence level) when compared to the control after each required interval must be repeated within 10 days using extra samples from the test set. If the repeat taste test is also significant, the package fails the taste compatibility test and the subsequent taste interval is canceled. If a trend occurs at any interval, perform a subsequent interval. If a trend occurs again, the package fails the taste compatibility test. If a repeat taste test does not confirm a significant taste result, the package passes the taste compatibility test. A trend is one correct taste judgment less than the number required for a significant taste result at a 0.05 probability level or 95% confidence level. For example, 20 correct taste judgments for a 42- member triangle taste panel are significant according to the

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Triangle Difference Test Statistical Table found in PK-PR-201. Nineteen correct taste judgments would be a trend. If there is a significant taste difference and taster comments indicate there could be a preference for the test package, then a Preference Test should be performed to determine acceptance. If you are unsure of how to interpret a set of taste data, send a summary of the taste results for all intervals (degree of difference, panelist choices, and comments for both control and test beverages) to Corporate Quality Assurance for review.

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Dimensional Specifications
Exterior
Test Procedure: REFPET Bottle Dimensions EvaluationExterior, PK-PR-207 The bottle shall conform to the drawing approved in writing by The Coca-Cola Company. Dimensions shall be taken on empty bottles as delivered. Company drawings are the only specifications to be used for the bottles. Dimension tolerances are as follows for individual bottles: Height Diameter 0.3 percent 0.8 percent

Finish

Test Procedure: REFPET Bottle Dimensions EvaluationFinish, PK-PR-208 Preforms and bottles must conform to the latest revisions of the preform drawing supplied by the manufacturer and bottle drawing supplied by The Coca-Cola Company. The supplier must provide to the Company or any of its divisions, upon request, copies of the most recent drawings for each finish specified for use with the bottles it will supply. The finish shall be fully formed and free of sharp edges, flash, overhang, or any other irregularity that will adversely affect carbonation retention, removal torque, closure or finish venting, or consumer comfort when the product is consumed from the bottle. Except for damage from abuse, the finish dimensions shall remain within specified drawing tolerances for the life of the bottle. Additionally, finish changes due to age, washing, cycling, and normal use shall not adversely affect finish performance including closure application, removal torque, carbonation retention, and opening performance. Any process or post process changes performed by the manufacturer to minimize finish shrinkage, stress cracking and the like on cycled bottles shall not increase the susceptibility of the finish to damage.

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Physical Performance Specifications
Capacity Change Test Procedure: REFPET Bottle Empty Capacity Change
(Shrinkage) Test, PK-PR-218 The capacity tolerance of a random sample of used bottles ranging in trippage from 1 to 20 that have been filled at the nominal fillpoint on a normal counterpressure filler at up to 25C (77F) and 4 gas volumes carbonation shall meet the following criteria:
Average capacity 1.5% below capacity Average capacity of a large sample shall not be lower than appropriate capacity for each size, which is 500 ml, 750 ml, 1000 ml, 1500 ml, or 2000 ml at the nominal fill-point. Not more than 2 percent of all bottles shall have a capacity of less than 1.5 percent below appropriate capacity for each size, which is 500 ml, 750 ml, 1000 ml, 1500 ml, or 2000 ml at the nominal fill-point. No bottle shall have a capacity of less than 3 percent below or more than 3 percent above appropriate capacity for each size, which is 500 ml, 750 ml, 1000 ml, 1500 ml or 2000 ml at the nominal fill-point.

3% above or below capacity

In addition to the above, all bottles will meet the applicable government requirements on capacity.

Carbonation Retention

Test procedure: REFPET Bottle Carbonation Retention Test, PK-PR-219 The minimum allowable carbonation level of product agitated to equilibrium pressure in an unopened bottle originally filled to the nominal fill-point at 4.0 volumes of CO2 [as read at 22.2C 1.1C (72 F 2F)] and a maximum of 3 bar (4 psig air), at any relative humidity, shall be 3.4 volumes after 24 weeks. All carbonation readings should be taken at 22.2C 1.1C (72F 2F) from the Zahm & Nagel table for CO2 dissolved in water.

Drop Impact Resistance

Test procedure: REFPET Bottle Drop Impact Test, PK-PR-229 A sealed bottle originally filled to the nominal fill-point with product at 4.0 volumes apparent carbonation (as read at any temperature between 1.7C (35F) and 23.9C (75F) from the Zahm & Nagel table for CO2 dissolved in water) and a maximum of .3 bar (4 psig) air shall not fail when dropped in any mode, except on the finish, from a height of 0.9 meters (3 feet) onto a rigidly fastened steel plate for temperatures between 1.7C (35F) and 37.8C (*100F).

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Durability
Test procedures: REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing, PK-PR-221 REFPET Bottle Durability TestStandard Trip-Per-Two-Day Washing, PK-PR-222

The filled bottle shall not exhibit sufficient stress cracking or other bottle changes that affect the ability of the bottle to function as intended under normal production, handling, and distribution conditions. The durability of the test bottles must equal or exceed the durability of the control bottles.

Empty Weight and Capacity As-Delivered


Test Procedure: REFPET Bottle Empty Weight and As-Delivered Capacity Test, PK-PR-270 The required container weight shall be clearly marked on the drawing. The actual container weight shall not vary from the approved mean by more than 1.0 gram. The as-delivered capacity tolerance of new bottles at the nominal fill-point, as measured from the top of the finish down on each bottle with 0 bar (0 psig) internal pressure, shall be as follows:
Average Capacity Individual Capacity The arithmetic average of a sample of bottles shall be within +0.4/-0 percent of the stated capacity.

The number of bottles having capacities above the tolerance shall not be greater than 2 percent of a sample. The number of bottles having capacities below the tolerance shall not be greater than 2 percent of a sample. All bottles shall be within +1.3/-0 percent of the stated capacity.

The brimful capacity tolerance of new as-delivered bottles shall not exceed 1 percent of nominal as specified on the Company drawing. In addition to the above, all bottles shall meet the applicable government requirements on capacity.

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Fill-Point Variation
Test procedure: REFPET Bottle Fill-Point Variation Test, PK-PR-229 After exposure to 4.1 bar gauge (60 psig) and 5.5 bar gauge (80 psig) at 24C (75F) for 60 seconds at each level, the difference between the pressurized fill-height and the unpressurized fillheight for individual bottles in a sample group, originally filled to the nominal fill-point with water, shall not vary more than: 1.5 mm (.060 inch) with 4.1 bar (60 psig), and 2.5 mm (.098 inch) with 5.5 bar (80 psig)

The internal pressure shall be attained by injecting carbon dioxide gas at the constant rate of .69 bar gauge per second (10 psig per second). The sample group shall be composed of a mixture of bottles ranging in age from 0 to 20 trips.

Internal Pressure Test procedure: REFPET Bottle Internal Pressure Test, PK-PR-225 Strength
The bottle shall withstand a minimum internal pressure of 10.3 bars (150 psi) at any relative humidity and any temperature between 1.6C (35F) and 60C (140F) for 60 seconds without failure.

Perpendicularity

Test Procedure: REFPET Bottle Perpendicularity Test, PK-PR-270 Deviation from the perpendicular shall be less than the appropriate numbers in the table (total indicator reading) when measured with the bottle resting on its base and rotated 360 against a centering device. 500 ml 750 ml 1 liter 2 liter 4.4 mm (0.172 inch) 5.1 mm (0.201 inch) 5.6 mm (0.220 inch) 6.5 mm (0.256 inch)

1.5 liter 6.4 mm (0.250 inch)

Plastic Distribution

Test procedure: REFPET Bottle Plastic Distribution Test Test, PK-PR-226 Supplier will use good manufacturing practices to maximize bottle properties through maintaining material distribution. Tolerance in wall thickness is 5.0 percent of nominal.

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Support Ledge Strength Thermal Stability
Test procedure: REFPET Bottle Support Ledge Test, PK-PR-227 Bottle shall maintain sufficient ledge support strength to function as intended in filling, capping, and uncapping operations. Test procedure: REFPET Bottle Thermal Stability Test, PK-PR-228 A sealed bottle originally filled to the nominal fill-point with product at 4.0 volumes apparent carbonation (as read at any temperature between 1.7C (35F) and 23.9C (75F) from the Zahm & Nagel table for CO2 dissolved in water), and a maximum of .3 bar (4 psig) air: Shall not develop a rocker bottom, and Shall not demonstrate an objectionable appearance or gross effect to the ability of the bottle to function as intended when exposed to the conditions listed below at any relative humidity

The conical label panel shall remain axially flat and not become convex or concave. The following parameters shall not exceed the listed criteria at 38C (100F) and the listed times.
Time (Days) One/Seven Parameter Diameter (%) Height (%) Perpendicularity (mm/in) Fill-point Drop (mm) 500 ml 2.5/3.0 1.5/2.0 4.7/5.2 7.0/9.6 750 ml 2.5/3.0 1.5/2.0 5.5/5.9 8.1/1 1 liter 2.5/3.0 1.5/2.0 6.2/6.7 9.0/12.4 1.5 liter 2.5/3.0 1.5/2.0 7.0/7.6 10.2/14.0 2 liter 2.5/3.0 1.5/2.0 7.1/7.7 10.4/14.0

Vertical Load

Test procedure: REFPET Bottle Vertical Load TestEmpty, PK-PR-229 The minimum vertical load that a bottle shall withstand shall be such that the bottle can be satisfactorily filled with any filler bowl pressure up to 8.3 bars (120 psig) and satisfactorily capped and filled with noncarbonated water. The bottle shall successfully withstand any stacking loads it may incur during normal handling and distribution without developing stress cracking or significant structural weakness. The minimum vertical load strength that empty bottles should exhibit in laboratory tests is 54.6 kg (120 pounds).

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Revision History
Issue Date 20-Dec-2004 Summary of Change New document.

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REFPET Bottle Acetaldehyde Test24-Hour


Purpose Corresponding Specification Contents
Use this test to ensure that the acetaldehyde concentrations in the walls of REFPET bottles do not exceed established limits. REFPET Bottle Specifications, PK-SP-045, Acetaldehyde24Hour

Test Equipment............................................................................................. 1 Procedure ...................................................................................................... 2 Preparing Sample PET Bottles ................................................................ 2 Preparing Acetaldehyde Gas Specifications............................................ 2 Analysis of Bottles ............................................................................. 3 Calculations ....................................................................................... 4 Preparation of Aqueous Acetaldehyde Solutions..................................... 4 Test Equipment and Materials........................................................... 4 Procedure .......................................................................................... 5 Standardization of Aqueous Acetaldehyde Solutions .............................. 6 Reagents ........................................................................................... 6 Test Equipment.................................................................................. 6 Preparation of Solutions .................................................................... 7 Procedure .......................................................................................... 8 Calculations ....................................................................................... 9

Test Equipment

0- to 10-ml syringe (for example, Hamilton 701) 1000-ml Pyrex vessel with closure fitted with a septum Supply of laboratory-grade compressed nitrogen for flushing bottles Bottle closures fitted with septa Standard solution of acetaldehyde in water at a concentration of approximately 1 mg/ml Vacuum pump and gauge Suitable gas chromatograph equipped with a flame ionization detector, 5.0 ml gas sampling loop, and data-processing system

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REFPET Bottle Acetaldehyde Test24-Hour


Procedure
Preparing Sample PET Bottles
1. Allow freshly blown PET bottles to cool for at least 5 to10 minutes, then purge with a steady stream of nitrogen for 20 seconds. Bottles must be flushed within six hours of blowing. 2. Immediately cap each bottle with closures fitted with a septum for gas sampling, and mark each bottle with the time and date. 3. Store the bottles in a temperature-controlled environment at 221.5C (723F) for 241 hours.

Preparing Acetaldehyde Gas Specifications

One hour before you analyze the first PET sample bottle, prepare an acetaldehyde gas standard: 1. Flush a clean 1-liter Pyrex glass bottle with nitrogen for 20 seconds and cap it with a closure fitted with a septum. 2. Inject a 5-ml gas sample from this glass bottle into the gas chromatograph. (Refer to Analysis of Bottles in the following section for details about the injection procedure.) This is a negative control air blank, and the chromatograph of its headspace should not show any peak at the retention time for acetaldehyde. 3. Using a 10-ml Hamilton syringe, inject 4 ml of a standard solution of acetaldehyde in water, at a concentration of approximately 1 mg/ml, into the 1-liter glass bottle. CAUTION: You must know the accurate concentration of the aqueous acetaldehyde solution and the volume of the glass bottle.

4. Allow the 1-liter glass bottle to stand at room temperature for 30 to 45 minutes, until the aqueous acetaldehyde solution has completely evaporated. 5. Make three replicate 5-ml gas sample injections into the chromatograph. Obtain an average acetaldehyde response signal, and determine the response factor (signal per concentration) for that series of injections.

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REFPET Bottle Acetaldehyde Test24-Hour


Analysis of Bottles
After the sample bottles have been stored for 24 hours at 22C (72F), inject a 5-ml gas sample into the gas chromatograph: 1. With the gas sample loop system in the FILL LOOP position (see Figure 1 below), close valve A, open valve B, and evacuate the loop with the vacuum pump. The level of vacuum is registered on the vacuum gauge. Close valve B. 2. Pierce the septum of the sample bottle with the syringe needle and open valve A. A 5-ml gas sample transfers from the bottle into the loop, and the reading on the vacuum gauge falls essentially to zero. Close valve A. 3. Turn the six-port sampling valve C to the INJECT position. The nitrogen carrier gas stream now diverts through the loop and flushes the sample into the column. 4. After the sample has eluted from the gas chromatographic column, return valve C to the FILL LOOP position, and repeat the process with the next sample.

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REFPET Bottle Acetaldehyde Test24-Hour


Calculations
Refer to the following formula to calculate the concentration in g/l, Cs of acetaldehyde in the gas standard:
Cs =

[volume (ml ) of

AA std . injected ] [concentrat ion (mg / ml ) of AA std .] volume (liters ) of the gas sample bottle

Then use this formula to calculate the response factor, (RF):


RF = average area counts for gas standard concentrat ion of gas standard, Cs

Consequently, the concentration of acetaldehyde, Cb, in /l, in each PET sample bottle is:
Cb = area counts of sample RF

Preparation of Aqueous Acetaldehyde Solutions

Acetaldehyde is a very unstable compound. It tends to oxidize and/or polymerize, and unless you carefully prepare aqueous solutions as described below, the acetaldehyde will likely degrade, resulting in inaccurate standard solutions. Alternatively, you can purchase specifications of known concentrations. If you do, ensure that the purchased specifications come with a Certificate of Analyses (COA). Micro-distillation apparatus Analytical balance, 160 g, readable to 0.0001 g 250-ml volumetric flask De-aerated distilled water Reagent-grade acetaldehyde Ice Pasteur pipettes Boiling stones or other anti-bumping granules Laboratory-grade nitrogen Variable-wattage heating mantle

Test Equipment and Materials

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REFPET Bottle Acetaldehyde Test24-Hour


Procedure
You should complete this entire standard preparation and standardization procedure in the same day: 1. Set up the distillation equipment with chilled water running through the condenser and the receiving flask immersed in ice. Place about 50 ml of acetaldehyde in the distillation flask and heat gently to distill the acetaldehyde. 2. Discard the first 5 to 10 ml of distillate, and then collect the next 10 to 20 ml of acetaldehyde that distills over at 22C (72F). 3. Remove the receiving flask, flush with nitrogen, and seal with a ground glass stopper. 4. Fill a 250-ml volumetric flask with about 245 ml of distilled water. Bubble nitrogen through this for about an hour to remove any dissolved oxygen. 5. Determine accurately the tare weight of the flask, water, and stopper on the balance, and then quickly add about 250 mg of freshly distilled acetaldehyde to the water. This is difficult because of the volatility of acetaldehyde, and is best done using a Pasteur pipette. Seal the flask with a ground glass stopper and mix the contents well. 6. Dilute the flask to the mark with de-aerated distilled water, mix well, flush the headspace with nitrogen, and seal once more with a ground glass stopper. 7. Analyze three 2.0-ml aliquots of this solution by the standard titration test procedure to determine the exact concentration of acetaldehyde in the solution. Do this as soon as possible after you have prepared the solution. 8. Transfer portions of the solution by Pasteur pipette into 1- or 2-ml vials with Teflon-lined septum seals. Fill the vials to overflowing to eliminate headspace, and then seal with the septum seals. Mark each vial with the concentration and store refrigerated (41C) until needed for use. Again, transfer the solution to the storage vials as soon as possible. 9. Use one of the small vials of standard for only about a week (or until an air space appears) before discarding it. If you follow this procedure exactly, you can safely store unopened vials of aqueous acetaldehyde solution at 4C (38F) without deterioration for at least six months.

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REFPET Bottle Acetaldehyde Test24-Hour


Standardization of Aqueous Acetaldehyde Solutions
An aqueous solution containing approximately 1 mg/ml acetaldehyde is prepared for use as a standard to calibrate the gas chromatograph in the determination of headspace acetaldehyde in REFPET bottles. The solution is standardized volumetrically by adding sodium bisulfite to form the aldehyde-bisulfite complex, then destroying the complex with base and titrating the liberated bisulfite with standard iodine. Potassium iodide Iodine Sodium bisulfite 0.100 N standard sodium thiosulfate solution Anhydrous sodium carbonate Acetaldehyde solution in water Starch indicator solution Glacial acetic acid Burettes: 50 and 25 ml Pipettes: 50, 25, 10, and 2 ml Volumetric flasks: 1,000, 500, 250, and 100 ml Pasteur pipettes Erlenmeyer flasks: 125 ml Graduate cylinders: 50 and 10 ml Small beakers

Reagents

Test Equipment

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REFPET Bottle Acetaldehyde Test24-Hour


Preparation of Solutions
All solutions must be prepared fresh each time the procedure is used. 1. For sodium carbonate buffer: Dissolve 80 g of anhydrous sodium carbonate in approximately 500 ml of distilled water in a 1-liter volumetric flask. When all solids have dissolved, slowly add 20 ml of glacial acetic acid and then dilute to the 1liter mark with distilled water. 2. For 1% sodium bisulfite: Dissolve 1.0 g (0.1 g) of sodium bisulfite in distilled water, transfer to a 100 ml volumetric flask, and dilute to the 100 ml mark with distilled water. 3. For 0.05 N sodium thiosulfate: Pipette 50.0 mL of 0.100 N sodium thiosulfate into a 100 ml volumetric flask and dilute to the mark with distilled water. 4. For starch indicator solution: Triturate approximately 1g of arrowroot starch in 10 ml cold water. Add to 200 ml of boiling distilled water and boil to a thin liquid with translucent appearance. Let stand overnight, and use the clear supernatant liquid. 5. For 0.01 N sodium thiosulfate: Pipette 25.0 ml of standard 0.100 N sodium thiosulfate solution into a 250 ml volumetric flask and dilute to the mark with distilled water. 6. For concentrated iodine solution 0.1 N: Dissolve 25 g (0.5 g) of potassium iodide in about 25 ml of distilled water in a 1liter volumetric flask. Carefully dissolve 12.7 g of iodine in this solution and dilute to 1 liter. Label as Standard Iodine #1. 7. For 0.01 N iodine solution: Pipette 50.0 ml of the Standard Iodine #1 into a 500-ml volumetric flask and dilute to the mark with distilled water. Label as Standard Iodine #2.

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REFPET Bottle Acetaldehyde Test24-Hour


Procedure
1. Standardize the iodine solution: Pipette 25.0 ml of Standard Iodine #2 into a 125-ml Erlenmeyer flask and titrate with standard 0.01 N sodium thiosulfate until you observe a faint yellow color. Rinse down the sides of the flask with distilled water. Add a few drops of starch indicator solution and titrate with more 0.01 N sodium thiosulfate until the blue color just disappears. Repeat these steps twice more, then average the results of the three titrations, and calculate the normality of the iodine solution. 2. Standardize the acetaldehyde solution. Do the following steps. 3. Add 10 ml of one percent sodium bisulfite solution to a 125-ml Erlenmeyer flask. Add 2.0 ml of the cold aqueous acetaldehyde solution by pipette, making sure to keep the tip of the pipette under the bisulfite solution during the addition. 4. Add a few drops of starch indicator solution with a Pasteur pipette, and swirl the flask for two to three minutes to mix the contents thoroughly. 5. Add 0.1 N iodine from a burette until the solution turns a faint blue color. Destroy the excess iodine by adding 0.05 N sodium thiosulfate dropwise with a Pasteur pipette until the solution turns clear again. 6. Add 0.01 N iodine from a burette until the solution turns a faint blue color. There is no need to record the volume added. 7. Chill the Erlenmeyer flask with the solution in an ice bath for 10 to 12 minutes. 8. Add 25 ml of chilled sodium carbonate buffer. 9. Titrate the liberated bisulfite with 0.01 N iodine until a faint blue color appears. Carefully record the volume of iodine added. Repeat this procedure again, and average the volumes of the two additions. 10. Make a blank determination on 2 ml of distilled water using the same procedure.

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REFPET Bottle Acetaldehyde Test24-Hour


Calculations
0.01 N iodine is equivalent to 0.22 mg of acetaldehyde.
normality of iodine = normality of sodium thiosulfate volulme of thiosulfat e volume of iodine

Concentration of:
actetaldeh yde in =

(normailty of

iodine ) 0.22 (volume of iodine blank ) 0.01 volume of acetaldehy de used

Aqueous solution (mg/ml)

Revision History
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REFPET Bottle Acetaldehyde TestGround Preforms


Purpose Corresponding Specification Test Equipment
Use these test guidelines for performing ASTM F-2013-00. REFPET Bottle Specifications, PK-SP-040, Acetaldehyde Ground Preforms Gas chromatograph with flame ionization detector Headspace auto-sampler with 500-ml sample loop Headspace vials (22 ml) with Teflon-lined septa Aqueous acetaldehyde stock solution of 1000 ppm Calibrated precision 0- to 10-ml Syringe Course grinding mill (5- to 10-mm screen) Fine grinding mill (1.0-mm screen) Analytical balance Liquid nitrogen

Instrument Parameters
Auto Sampler
Oven Temperature Sample Loop Temperature Transfer Line Temperature Sample Equilibrium Time Transfer Line Back Pressure Vial Pressure Vial Pressurization Time Pressurization Equilibrium Time Loop Fill Time Loop Equilibrium Time Injection Time Column Type Column Dimensions Column Coating Detector Type Detector Temperature Inlet Temperature Initial Temperature Initial Time Temperature Program 1 Temperature Program 2 Data Collection Rate 150C 160C 170C 60 min. for PET 17.5 psi 1 psi 0.10 min. 0.10 min. 0.08 min. 0.10 min. 0.20 min. Fused Silica 25 m X 0.53 mm Poraplot Q FID 200C 150C 50C 1 min. 10C/min. to 150C 20C/min. to 220C, hold for 5 min. 5 Hz

Gas Chromatograph

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REFPET Bottle Acetaldehyde TestGround Preforms


Equations
Refer to the following formula to determine the necessary specifications for calibration:

volume injected (l ) =

mass of standard concentration (g/l)

If the concentration of stock solution is 1000 parts per million (ppm), then use this formula:
volume injected (ml) = mass of standard (mg )
Expected AA in Sample 10 20 30 40 50 60 70 80 90 100 Mass (ppm) of Std Required (mg) 1 2 3 4 5 6 7 8 9 10 Volume of 1000 ppm Stock Added (ml) 1 2 3 4 5 6 7 8 9 10

Preparing Samples

1. Prepare the 22-ml vials by sealing with Teflon-lined septa. 2. Using a calibrated syringe, inject the appropriate amount of stock solution into the vials. Touch the tip of the syringe needle to the sidewall of the vial to ensure complete transfer. 3. Place the specifications in the auto-sampler to enable them to bracket the samples. Blanks are distributed at the beginning, throughout, and at the end of the samples. 4. Analyze all vials within 12 hours of preparation.

Data Analysis

The acetaldehyde peak from each run is integrated to find the peak area. A calibration plot is produced from the known amounts of the specifications and their corresponding peak areas. Linear regression is applied to determine the slope and intercept of the calibration plot. You can use this information to determine the sample concentration using the equations provided in this procedure.

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REFPET Bottle Acetaldehyde TestGround Preforms


Procedure
1. Immerse the solid samples in liquid nitrogen for three minutes before grinding. 2. For preforms: Grind the frozen material in the coarse mill and immediately transfer the milled product into a sealed vial. 3. For bottles: Cut the bottle into pieces that will easily fit into the fine grinding mill. 4. Fill the fine mill with liquid nitrogen, grind the product of step 2, and immediately transfer the final product into a sealed vial. 5. While the finely ground product is cold, transfer 0.10000.0050 g into each of three 22-ml headspace vials, and tightly seal the vials. Record the exact mass of the sample. 6. Repeat steps 1 through 5 for each solid sample.

Blanks Specifications

1. Prepare blanks as needed. 2. Seal a 22-ml headspace tight with a Teflon-lined cap. Specifications are prepared in triplicate and in order to produce a calibration curve on which the expected sample concentrations will lie. This is accomplished by adding the appropriate amount of acetaldehyde stock solution to the headspace vial according to this procedure.

mass of AA in sample (g ) =

[peak area of sample (area counts)] [intercept (area counts )] slope [area counts/ mass (g )] mass of AA in sample (g ) sample concentration (g/g or ppm ) = mass of sample (g )

Revision History
Issue Date 20-Dec-2004 Summary of Change New document.

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REFPET Bottle Appearance and Color Evaluation


Purpose
The visual examination of plastic soft drink containers is, by itself, an essential first part to any testing program. This test covers all aspects of the container that may affect its overall ability to meet the standards of performance. REFPET Bottle Specifications, Appearance/Color, PK-SP-045

Corresponding Specification Test Equipment

Strong light source Plastic marking pencil Flash-O-Lens magnifier Limit samples

Procedure
1. Having set aside the necessary number of samples required for product compatibility and carbonation retention, select 109 samples for visual inspections. 2. Sort through the 109 samples to determine if all injection and blow mold numbers are included. These numbers are usually located on the finish ring and on the pinch area, respectively. Record any missing numbers and request additional containers, if necessary, to obtain adequate mold number representation. 3. Observe each sample for color and clarity, and set out those containers that do not appear to fall within established limits for these two attributes. If necessary, refer to limit samples, which should be on hand for this purpose. Record the results of these observations. 4. Observe each sample for the presence of defects which include: a. Foreign specks or particles b. Bubbles c. Surface irregularities d. Container deformation e. Scuffing or scratches

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REFPET Bottle Appearance and Color Evaluation


Revision History
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REFPET Bottle Scientific and Regulatory Affairs (SRA) Approval


Purpose
To describe the process of reviewing the components of materials that have potential for direct contact with product, determining their compliance with regulatory, sensory, and other Company requirements, and approving them for use. REFPET Bottle Specifications, PK-SP-045, SRA Approval

Corresponding Specification Procedure


PET Resin

1. For SRA approval of a new resin, the division must have one of the following: a. An MAA with the resin supplier. b. A warranty and indemnification statement from the resin supplier for each country where the resin will be used . 2. The division must: a. Obtain the MAA or warranty and indemnification statement(s) from the resin supplier. b. Enter the appropriate information into the Global Packaging database. c. Review resin sourcing needs with the Cross-Enterprise Procurement Group (CEPG) to determine if suppliers can be CEPG-certified.

d. Successfully complete a permeation test by a third-party laboratory before a new resin can be used for REFPET. Contact Corporate SRA for details on test protocol and capable laboratories.

Colorants and Materials other than PET

1. For SRA approval of new colorants and additives, suppliers must: a. Meet the materials requirements found in REFPET Bottle Authorization Matrices, PK-RQ-065. b. Contact the division to initiate the approval process. c. Complete and submit the Material Formulation Approval Request Form, RF-PK-110, to Corporate Quality.

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REFPET Bottle Scientific and Regulatory Affairs (SRA) Approval


2. The submitted request form must list all qualitative components of the material and their regulatory status, including Food Law Compliance, as follows. Refer to RF-PK-111 and RF-PK-112 for examples of what to submit. a. The common name of each component b. The CAS number of each component c. The regulatory body (for example, FDA or EU) that governs the use of the component

3. If an Extraction test is required according to PK-RQ-060, then the instructions below must be followed. Typically, third-party laboratories perform extraction testing.
Promotional Inks Food Grade Approved Not Food Grade Approved Tests Required Taste test Extraction test Taste test Special Instructions Division reviews all test results SRA reviews all test results Division reviews all test results

4. Whether the material is food grade approved or not, all information required by step 2 must be submitted to SRA. 5. Corporate SRA will review the information provided, approve the material, or request additional information. 6. When Corporate SRA gives initial approval of the material: a. The division is responsible for authorizing the material for use in additional countries or by additional closure suppliers. b. The supplier must provide the division with Certificates of Food Law Compliance for the additional countries of use. 7. SRA, Package Development and Design, or Corporate Quality will determine whether further testing is needed, for example, taste compatibility or thermal desorption. 8. Corporate Quality will maintain a list of SRA-approved materials and regularly update it with current information.

Revision History
Issue Date 20-Dec-2004 Summary of Change New document.

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RefPET Bottle Taste Compatibility Test


Purpose
To ensure that RefPET bottles are capable of containing the products of The Coca-Cola Company without causing a significant taste difference in any of those products or otherwise imparting any significant off-taste or off-odor to them. This test applies to the following package types: Carbonated Water and Soft Drinks NCB Pressurized NCB Non-pressurized

Scope

Corresponding Specification Test Equipment

REFPET Bottle Specifications, PK-SP-045, Taste Compatibility

This is a general list. There may be equipment requirements that are specific to the product under test. For both carbonated and noncarbonated product: Source for treated water that has been filtered through a 0.2micron filter or a carbonated water source Closures known to perform properly in taste compatibility tests Capping machinery capable of applying the closure to the RefPET bottles and the glass control bottles Stainless steel 10-liter (2.5-gallon) product tanks, properly passivated and rinsed Large glass container (4-liter jug) for treated filtered water Digital thermometer Coded 60-ml taste-test glasses Safety equipment, including safety glasses, gloves, hair restraint, and so forth Source of CO2 for recarbonating test and control samples Carbonation pressure gauge Carbonation Computer Dial

For carbonated product only:

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RefPET Bottle Taste Compatibility Test


Procedure
Preparing Samples
1. The package should be filled with the product specified and tested according to the intervals in the table below. Add additional intervals for retests. If any interval is significant, and the retest is not significant, then the interval is considered satisfactory. In addition to the acceptance criteria in the table, the lab manager may accept results with one or two significant intervals based on a review of data, such as taster comments.
Interval (weeks) 2 2, 4, 10 2, 4, 10 3, 6, 9, 12, 16, 24 2, 4, 8, 12 2, 4, 6, 9, 12, 16, 24 Number of Intervals 1 interval + 1 retest = 2 3 intervals + 2 retest = 5 3 intervals + 2 retest = 5 6 intervals + 2 retest = 8 4 intervals + 2 retest = 6 7 intervals + 2 retest = 9

Package type All CB, except recycled content CB, Recycled content: colorless CB, Recycled content: green All NCB except water and recycled content NCB water NCB recycled content

Fill Product Treated filtered or carbonated water Coca-Cola Sprite Refer to #2 below Refer to #2 below Refer to #2 below

Acceptence Criteria No significant difference No significant difference at any interval No significant difference at any interval No more than 2 intervals may be significant No more than 1 interval may be significant No more than 1 interval may be significant

2. All bottles must be filled within fourteen days of bottle production. Bottles intended for NCB must be filled with the product that is normally put into the package being tested, unless a more sensitive or representative product has been identified. Bottles intended for ozonated water must be filled with ozonated water. Bottles intended for non-ozonated water can be tested with treated filtered water. 3. If treated water is used, it must not contain chlorine and must also meet the following specifications:
Attribute TDS Alkalinity Specification <500 mg/l < 85 mg/l

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RefPET Bottle Taste Compatibility Test


4. To calculate the number of bottles needed for the test, find the bottle size in the table below and then multiply the number of bottles by the number of intervals. Always use the smallest size bottle the supplier produces.
Size 390 ml 500 ml 360 ml (12 oz) 480 ml (16 oz) 600 ml (20 oz) 720 ml (24 oz) 1.5 liter 2 liter Number of bottles needed for test 11 x number of intervals 8 x number of intervals 11 x number of intervals 8 x number of intervals 7 x number of intervals 6 x number of intervals 3 x number of intervals 3 x number of intervals

5. RefPET bottles must impart no significant taste difference at the 95% confidence level when compared to control samples under controlled environmental conditions (212C) after the intervals defined above.

Testing Samples

1. For test bottles of size 1 liter or larger, select a separate subgroup of 20 sample bottles from the main group of samples. For test bottles of size less than 1 liter, select 30 samples; the testing protocol requires a minimum or 4 liters of product per test interval. Ensure that all injection and blowmold cavities are represented uniformly in this subgroup sample set. For bottle submissions from molds with more than 32 or 64 cavities, ensure that no cavity is repeated in the subgroup. 2. Obtain the same number of clean, dry glass control bottles of similar size as the test bottles. Rinse all bottles thoroughly with treated filtered water or carbonated water and drain well. Fill all bottles with carbonated or treated filtered water. If using carbonated water, ensure that volumes are within 3.75 0.25. 3. Store at 211C for the duration of the test. 4. At the end of the storage interval(s), randomly select enough test and control bottles to enable sampling 4-liter portions of test product and glass control product. With liter or larger bottles, take the product from at least four different bottles. Pour the portions into a clean, dry and labeled stainless steel product tank or large glass jug or bottle, and seal the lid.

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RefPET Bottle Taste Compatibility Test


5. Filling with carbonated water: Because carbonation is lost more rapidly from the RefPET bottles than from the glass controls during the course of the test, both test and control water must be recarbonated prior to taste testing: a. Measure the temperature of the water, and then use a Carbonation Computer Dial to determine the required equilibrium CO2 pressure for 3.8 volumes carbonation. b. Set the regulator gauge of the CO2 source to 14 kPa (2 psig) higher than this equilibrium pressure and connect the CO2 source to the tank. c. Add CO2 gas to the tank until the established pressure is reached, then open the tank valve to the atmosphere and release the headspace contents. This will flush out much of the initial air content of the tank headspace.

d. Close the tank again and bubble more CO2 gas into the tank, with vigorous shaking, until no further gas will bubble into the water. e. Disconnect the gas line, draw samples from each tank and determine that the water tastes acceptable. f. Refrigerate the tank to prepare the contents for taste testing.

6. Bring the temperature of test and control tanks to within a range of 9 to 12C (48 to 54F) and dispense samples into clean, dry coded taste-test glasses and test the beverages with the Triangle method described as follows.

Taste Testing CSD, NCB, or Water Samples


1. Use a panel of testers to taste test the samples. A minimum of 18 tasters is strongly recommended. An optimal panel size is 30 to 42 tasters. It is best if the panel can be divided in multiples of 6 to ensure a balanced presentation. Refer to Triangle Taste Test on page 6. 2. Dispense all beverages from the containers into the taste test cups as follows: a. Noncarbonated beverages or water: without any cooling or other treatment. b. All carbonated beverages and water: refrigerate the samples for three hours and use a cooling plate when dispensing the water to the taste panel.

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RefPET Bottle Taste Compatibility Test


3. Taste test the beverage exposed to the test bottles using the beverage exposed to the control bottles as a reference. 4. Record all results. Forms and statistical tables for interpreting taste tests begin with Triangle Taste Test on page 6.

Test Methodology

Prepare three samples. Make two of the samples the same product and one sample a different product. Ask the panelists to taste the three samples in order from left to right. Then ask the panelists to select the sample they think is different from the other two samples. Present each panelist with three coded samples. Always present the samples simultaneously. Present both products in the test as the odd sample an equal number of times throughout the test. This methodology is typically called a balanced reference design. To ensure reliability in your test data, conduct several practice tests with your panel to familiarize the panelists with taking the Triangle test. A panel size of 30 to 42 tasters is optimal; a minimum of 18 tasters is strongly recommended.

Analysis of the Data

To analyze the Triangle test data, you need to know the following: The number of panelists that tasted, The number of panelists that were correct, and The level of significance to use (for plastic bottle approvals, this is typically a probability of 0.05 or the 95% confidence level).

Using the information, reference the Triangle Difference Test Statistical Table on page 7 to determine if there is a significant difference between the samples in the test. For example, if you had 30 panelists taste and 15 were correct, the test would be significant at the 95% confidence level; therefore, you could conclude that a difference exists between the two products.

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RefPET Bottle Taste Compatibility Test


Triangle Taste Test
Name: Date:

Taste the samples presented to you from ______ (e.g., Left) to ______ (e.g., Right). Two of the samples are the same and one is different. Select the sample you think is the ______ (e.g., Odd) or ______ (e.g., Different) sample by circling the code of the odd sample.

Sample:

Sample:

Sample:

Please describe how the odd sample is different from the like samples.

Test Number:

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RefPET Bottle Taste Compatibility Test


Triangle Difference Test Statistical Table
Minimum numbers of correct judgment to establish significance at various probability levels for triangle (p = 1/3). Panel size is n. Use a taste panel size of 30 to 42 tasters for optimal statistical sensitivity. At a minimum, use an 18-member taste panel.

Significance level (%) n trend 5 18 10 10 19 10 11 20 10 11 21 11 12 22 11 12 23 12 12 24 12 13 25 12 13 26 13 14 27 13 14 28 14 15 29 14 15 30 14 15

1 12 12 13 13 14 14 15 15 15 16 16 17 17

.01 13 14 14 15 15 16 16 17 17 18 18 19 19

Significance level (%) n trend 5 31 15 16 32 15 16 33 15 17 34 16 17 35 16 17 36 17 18 37 17 18 38 18 19 39 18 19 40 18 19 41 19 20 42 19 20

1 18 18 18 19 19 20 20 21 21 21 22 22

.01 20 20 21 21 22 22 22 23 23 24 24 25

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RefPET Bottle Taste Compatibility Test


Triangle Taste Test Results Report Form
Test Number: Test Date: Project Name: Product: Product Age: Description Samples Presented: Control:

Experimental:

Number of Tasters: Statistic Significance:

Number Correct:

Tasters Comments:

Control

Experimental

Interpretation:

Approved:

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RefPET Bottle Taste Compatibility Test


Revision History
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REFPET Bottle Dimensions EvaluationExterior


Purpose
Use this test to ensure that packages comply with the dimensions and allowable tolerances specified on the respective bottle design drawings. Refer to the Global Packaging database to obtain the number of the drawing. REFPET Bottle Specifications, PK-SP-045, Exterior

Corresponding Specification Test Equipment

Dial calipers, complete with base Digital height gauge Vernier diameter measurement tape Pi tape Optical comparator Electronic measuring device

Procedure

1. Randomly select the number of filled and capped samples as shown in the table below:
Test Samples Control Samples Total Number of Samples Needed

108

108

2. Select a sub-group of 12 Exterior Dimension samples. 3. Measure the maximum and minimum neck diameters of each bottle using any of the measurement devices listed in the preceding Test Equipment section. Measure at points on the neck immediately below the neck support ring, before the bottle wall begins to flare out toward the shoulder area. 4. Measure the maximum overall height of each bottle. 5. Measure the nominal shoulder diameter of each bottle. When using an optical comparator, make a minimum of two diameter measurements 90 apart. 6. Measure the sidewall diameter of each bottle. When using an optical comparator, make a minimum of two diameter measurements 90 apart.

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REFPET Bottle Dimensions EvaluationExterior


7. For contour bottles, measure the pinch diameter at its minimum point. 8. Measure the heel diameter of each bottle. 9. Record all observations. These measurements also may be used as the initial data set for the procedure described in REFPET Bottle Thermal Stability Test, PK-PR-228. 10. Return the 12 sample bottles to the original group of 108 for use in subsequent testing. Alternatively, transfer the set of bottles to the Thermal Stability test for continued analysis.

Revision History
Issue Date 20-Dec-2004 Summary of Change New document.

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REFPET Bottle Dimensions EvaluationFinish


Purpose
Use this test to ensure that all thread finishes comply with the dimensions and allowable tolerances specified on the respective bottle finish design drawings. This test also reveals any defects that could hinder the performance of the finish/closure interface. NOTE: Finish drawings are available at http://www.threadspecs.com. This website is hosted by the International Society of Beverage Technology (ISBT) and sponsored by the ISBT Thread Finish Review Sub-Committee. For other finishes, the closure supplier will specify appropriate drawings.

Scope

This procedure applies to preforms and bottles. The following table lists the measurements that you must collect for each package type.
Package Type Preforms Bottles Required Measurements to Be Collected All applicable attributes (See step 3 below.) Diameters T, E, F, G, A, C (See step 4 below.)

Corresponding Specification Test Equipment

REFPET Bottle Specifications, PK-SP-045, Finish

Profile projection machine such as an optical comparator or other suitable measuring device (vision system, coordinate measuring machine, and so forth) Pin gauge set for 1690, 1716, and BPF finishes Two sets of each cavity number for preforms and twelve samples for bottles Anti-static brush to remove dirt or dust

Procedure

1. Visually inspect preforms for defects, such as air bubbles or handling damage, and place them in numerical order in a sequentially numbered rack. 2. Take all measurements 90 apart, but not at the parting line.

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REFPET Bottle Dimensions EvaluationFinish


3. For preforms, measure the following attributes:
Code T F G E S D P A LRA LRR TTW SR TR TPI TP VSD VSW C Overhang Flash Deformed Threads Weld Lines Sealing Land Uniformity Description of Attribute Thread diameter Core pin seal diameter (upper ring diameter) Thread split seal diameter (lower ring diameter) Thread root diameter Height from top of finish (TOF) to start of full depth thread Height from TOF to tamper evident bead gauge point Thread pitch Tamper evident bead diameter Locking ring angle Locking ring radius Thread tip width Seal radius Thread radius Thread per inch Thread projection Vent slot depth Vent slot width Control internal diameter at TOF F may not protrude past G Not continuous; minimum allowable -0.12 mm Key pull Hair line crack in TOF over a vent slot, flow lines on TOF, or short shot (mold not completely filled) Pull-up mark (hot fill packages)

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REFPET Bottle Dimensions EvaluationFinish


4. For bottles, measure the following dimensions:
Code Description of Diameter Thread Thread root Core pin seal Thread split seal Tamper evident bead Control internal at top of finish (TOF) Height from TOF to start of full depth of thread Height from TOF to bottom of support ledge

T E F G A C S X

5. Record all measurements. If any of the dimensions are out of specifications for a bottle from a particular injection mold cavity, measure the second preform with the same cavity number to confirm whether the problem is consistent or isolated.

Revision History
Issue Date 20-Dec-2004 Summary of Change New document. Added S and X dimensions to bottle finish measurements.

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REFPET Bottle Capacity Change (Shrinkage) Test


Purpose
This test measures the ability of a plastic container to maintain correct volume without overfilling as the bottle expands and contracts during cycling. The conditions here relate to field performance. REFPET Bottle Specifications, Capacity Change, PK-SP-045

Corresponding Specification Test Equipment

Caustic tank and safety equipment Dial caliper with base Pi-Tape or equivalent circumferential tape Mettler PC4000 scale or equivalent Fill-height syringe assembly Rinse basin

Procedure
1. Determine as-delivered capacity for 10 bottles, as described in REFPET Bottle Empty Weight and As-Delivered Capacity Test, PK-PR-223. Then measure bottle diameter and height dimensions as in REFPET Bottle Dimensions Evaluation Exterior, PK-PR-207. 2. Condition bottles as follows: a. Bottles numbered 1 through 5 store empty at 72F, 50% relative humidity for 7 to 9 days. b. Bottles numbered 6 through 10 store submerged under water at 72F for 7 to 9 days. 3. One day before submerging bottles in caustic, measure bottle height and diameter dimensions along with fill-point capacity. Then, put bottles back in same conditioning environment, described in step 2, overnight. 4. Immerse the bottles in 3.0% +0.5 -0% caustic solution for five continuous hours continuously at 59.5C 1C (139F 1.8F). Measure and record caustic concentration and temperature. 5. Remove the bottles, rinse thoroughly, and repeat the capacity and dimension measurements taken in step 1 above.

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REFPET Bottle Capacity Change (Shrinkage) Test


6. Refer to the Density Conversion Table in document Weight to Volume Conversion Table for Capacity Testing, RF-PK-108, to report the weight of the water, temperature of the water, and milliliters for each bottle along with the maximum, average, minimum, and standard deviation for the samples.

Revision History
Issue Date 20-Dec-2004 Summary of Change New document.

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REFPET Bottle Carbonation Retention TestFT IR Method


Purpose
Use this test to assess accurately the carbonation loss rate of a REFPET beverage bottle and to extrapolate shelf life to a 17.5% loss for bottles initially carbonated to 4.0 volumes. REFPET Bottle Specifications, PK-SP-045, Carbonation Retention

Corresponding Specification Test Equipment

Calibrated Zahm and Nagel piercing device with pressure gauge (capable of measuring 0 to 100 psi or 689.5 KPa) Supply of bone-dry CO2 (moisture level not to exceed 15 ppm and CO2 must be at least 99.8% pure)

WARNING: Use protective gloves when handling frozen CO2, and ensure that the area is well ventilated. Approved plastic closures that properly fit the test bottles Analytical gram balance accurate to 0.1 g Approved device to measure bottle diameters accurate to 0.1 mm Optical comparator with a minimum magnification of 20X, or Laser measuring device Approved properly calibrated FT IR instrument (We recommend the Perkin-Elmer FT IR Spectrometer with supporting hardware fixtures and software patented by The Coca Cola Company.) Safety glasses/face shield and gloves Torque meter to properly apply approved plastic closures Permanent black ink marking pen Environmentally controlled chamber or room capable of maintaining a constant 22 1C (72 2F) and 50% relative humidity (RH)

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REFPET Bottle Carbonation Retention TestFT IR Method


Procedure
Sample Preparation
1. Pre-inspect the 12 bottles to be tested to ensure that no bottles are out of perpendicularity or have rocker bottoms.

NOTE:

Two extra bottles will be required for validating the 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 always can be aligned properly and consistently on the FT IR. NOTE: 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

You must determine the bottle volume first so that you can use the proper amount of dry ice to achieve the correct internal pressure. To determine the proper amount of dry ice: 1. Place one sample bottle on an analytical balance and tare the scale to zero. 2. Fill the sample bottle to the brimful capacity (that is, to top of the bottle finish) with water of a known temperature. 3. Record the weight of the water in grams. 4. Convert the water weight (g) to bottle volume (ml) using the following conversion table:
Water Temperature 19C or 66.2F 20C or 68.0F 21C or 69.8F 22C or 71.6F 23C or 73.4F Water Density (g/ml) 1.002637 1.002838 1.003039 1.003261 1.003492

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REFPET Bottle Carbonation Retention TestFT IR Method


5. Convert the bottle volume (ml) to the weight of dry ice (g) using the following formula:

(bottle volume in ml) (0.0077 ) = weight of dry ice in g


This weight of dry ice should yield an internal bottle pressure of 56 2 psi at 22C, which is the equilibrium pressure of 4.0 volumes of CO2 at 22C, or 60 2 psi at 22C which is the equilibrium pressure of 4.2 volumes of CO2 at 22C. It is preferred to fill the bottles to an equivalent of 4.2 volumes, but if the FTIR software is pre-set to calculate CO2 loss based on 4.0 volumes, then the shelf-life based on 4.2 volumes can be extrapolated after the test is completed. For RefPET, it is acceptable to calculate the shelf-life based on 4.0 volumes. WARNING: While filling the sample bottles with dry ice, wear safety glasses and gloves to prevent skin burns.

Filling Samples with 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 0.3 g. 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 sample bottle will decrease. When the balance reading is approximately 0.1 g greater than the calculated dry ice weight (from step 5 above), quickly tighten the closure on the bottle. Tighten the plastic closure by hand to the application torque recommended by the closure manufacturer. 4. By hand, gently swirl the bottle at ambient temperature (approximately 22C) 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 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 56 2 psi at a temperature of 221C (or alternatively, 60 2 psi).

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REFPET Bottle Carbonation Retention TestFT IR Method


6. If necessary, use an additional bottle to adjust the amount of dry ice until the correct pressure is obtained. When the correct pressure has been confirmed, fill 12 test bottles with the confirmed amount of dry ice according to the procedure described in steps 1 through 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 86 mm up from the base of the bottle. This corresponds to the exact point where the FT IR beam passes through the bottle. Ensure that all bottles are aligned consistent with their heel mark (refer to step 3 in the Sample Preparation section). Record this as the initial diameter for each sample. NOTE: All diameters need to be measured at the same distance from the base for each interval.

IR Calibration Sample Testing

Calibrate the IR instrument according to the manufacturers recommended procedure. 1. After you have pressurized the 12 test bottles and measured the initial diameters, evaluate the test bottles on the FT IR to establish the initial CO2 concentration. 2. After have measured all 12 test bottles for CO2 concentration, store the samples in a conditioned environmental chamber (221C or 722F at 50% RH). 3. At each interval shown in the table below, the CO2 level will need to be measured on the FT IR. You do not need to measure the diameters at every interval. To see a suggested frequency for diameter measuring, refer to Schedule for Measuring Samples below.

Sample Storage

Store all test bottle samples in an environmentally controlled room or chamber at 221C or 722F, 50% RH, between each test interval throughout the entire test period.

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REFPET Bottle Carbonation Retention TestFT IR Method


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

*Measure diameter at every interval if performing an accelerated test. For a standard test, the software does not use the diameter measurement at these intervals to calculate shelf-life.

CAUTION:

Follow the schedule as closely as possible so you do not miss a measurement interval; otherwise, the final results may be affected. You can neither miss nor delay the initial (#1) or the 1 day (#2) interval measurements. 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. However, it can be used to characterize the CO2 loss within the first 24-hour period, if necessary.

If you cannot perform a measurement at the scheduled time (in case of a holiday or weekend), you may perform the measurement up to three days later (except intervals 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. Never perform a measurement before its scheduled interval.

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REFPET Bottle Carbonation Retention TestFT IR Method


Data/Report Requirements
1. Report all data in a standardized format. The data should include the projected shelf life and the percentage of CO2 loss per week. 2. If the data is to be submitted to Packaging Design and Development for approval, you must report the shelf life data in the Carbonation Shelf Life and Standard Lab Conditions fields of the Submission Data Form (SDF). The SDF is located in the Global Packaging database.

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REFPET Bottle Drop Impact Test


Purpose Corresponding Specification Test Equipment
The drop impact resistance test simulates abuse that plastic soft drink containers may be subjected to in its normal life cycle. REFPET Bottle Specifications, Drop Impact Resistance, PK-SP-045 Carbonator Cold storage facility Drop area/concrete floor Safety glasses or face shield

Procedure
1. Select at random 23 samples previously inspected for visual defects. Mark each sample with an identification number in a continuous sequence. Fill and cap these containers to achieve 4.0 0.2 volumes of carbonated water when measured at 22.2C (72F). 2. Store all samples for 24 hours at the following temperatures: a. 2 - 11 at 4.4C (40F) b. 1 and 12 - 23 at 22.2C (72F) 3. Check and record pressure, temperature and CO2 level of samples 1, 12, and 23. 4. In a suitable test area, mark a door or wall to a height of 1 meter above a smooth concrete floor. The person performing the drop should wear either safety glasses or a protective face guard, and be instructed to tip the sample away from his or her line of vision. 5. Hold each sample at an approximately 30 angle from the vertical at a height of 1 meter. 6. Release each sample uniformly so that it falls freely, impacting the bearing surface of the container. After dropping each sample, inspect the container for breakage, excessive deformation, or separation. In addition, place the tested container upright on the floor. If it will not stand unassisted, note the sample as a failure. Record all findings.

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REFPET Bottle Drop Impact Test


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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


Purpose
The durability of a filled plastic bottle is critical to allow it to function. The conditions tested include a minimum of three months with an abbreviated sample size and relate to field performance. REFPET Bottle Specifications, Durability, PK-SP-045

Corresponding Specification Test Equipment

Caustic tank and safety equipment Filler Fill-height syringe Capper Environmental control chamber Rinse area Mettler PC 4000 scale or equivalent Dial caliper with base Pi-Tape or circumferential tape Depth gauge Optical comparator

Procedure
1. Randomly select a 24-bottle sample. On each bottle, put the test request (TR) number and number the bottles sequentially. Also, always include a control group for comparison. 2. Select samples 1 through 5. Measure fill-point capacity on each of these bottles at completion of 0 and 25 washes. 3. On the same samples and at the same frequency as in step 2, measure and record the following if checked: a. Overall height b. Pinch diameter c. Upper label diameter d. Base push-up height e. Finish dimensions E1, E2, E3, E4, T1, T2 and A (see Finish Measurements)

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4. Precondition bottles by immersing in water at 41C 3C (105.8F 5.4F) then empty and immerse the bottles completely in 3.0% +0.5% -0% caustic and 0.15% +0.05% -0% Henkel P3 stabilon Al Fluessig additive at 59.5C 1.0C (139F 1.8F) for 15 minutes 1 minute. (If this chemically aggressive Henkel additive is not available, then use an approved additive at nominal field use concentration but increase contact time). 5. Measure and record on Data Form I Wash Conditions in this document the caustic concentration, additive concentration, temperature, and soak time at each washing. We recommend installing an alarm system and setting at 61C (141.8F) to monitor maximum temperature. 6. Remove the emptied bottles and immediately rinse them thoroughly with potable (fresh tap) water by completely immersing in water, completely filling bottles and emptying 2 times, followed by a fresh water spray rinse as follows.
First rinse Second rinse Third rinse Water immersion at 41C 3C (105.8F 5.4F) Immersion at ambient Ambient using jetting for 15 seconds at 30 psi with an inside stream type 2 mm (5/64 inch) nozzle and external dispersion type nozzle on an inverted bottle

7. As it is extremely important that there is no caustic carryover, check for caustic carryover each cycle by allowing 3 drops of phenolphthalein to run down both the base exterior and the inside of the bottle. No color indicates no caustic. If pink color develops, add 10 ml of distilled water. If pink color persists, caustic is present and more thorough rinsing is necessary. 8. Fill bottles 15 through 24 three-fourths full of water and counterpressure to 5.5 bars (80 psi) for 20 seconds, then empty. 9. Wipe a thin layer of Diversey SUPERPET C line lubricant or equivalent diluted at 1 part line lubricant to 100 parts water (1.0 percent 0.1 percent) on the entire bottom and to a height of 3 mm up the heel on each bottle. Store the one percent lube moisture in a sealed container when not in use or make a new batch daily. This is necessary to ensure that evaporation does not cause the ratio to drift outside of the stated tolerance.

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


10. Fill all of the bottles with carbonated water to achieve 4.2 volumes 0.2 volumes carbonation at 22.2C (72F) after 24 hours and apply new plastic closures. Use only Metal Closures, MCA finial plastic closures applied at 10-12 inchpounds, or other approved plastic closure for REFPET bottle. 11. Measure and record pressure and temperature of one extra bottle at beginning and end of filling operation on Data Form II Filling and Storage Conditions in this document. 12. Store at 37.8C 1C (100F 1.8F) and 40% 10% relative humidity for 24 hours 1 hours. 13. At every wash cycle, record on Data Form II the exact number of hours bottles are stored at 37.8C (100F). All bottles are to achieve 36.8C 1C (98.2F 1.8F) at the end of 24 hours. NOTE Bottles can be stored full over weekend and/or holidays at 35.6C 1C (96F 1.8F) in order to obtain one or more extra cycles per week. Under no conditions should bottles exceed 25 hours at 37.8C 1C (100F 1.8F).

14. Measure and record on Data Form II temperature and relative humidity of the chamber, then remove the bottles from storage. Immediately measure and record the unshaken pressure and temperature of one bottle from each case or at the following storage locations: a. Top stack corner b. Middle stack center c. Bottom stack opposite corner The target average unshaken opening pressures are:
Weekend/holiday storage 24-hour storage 67 3 psi for at 35.6C 1C (96F 1.8F) 70 3 psi at 36.8C 1C (98.2F 1.8F)

15. Open and two-thirds empty remaining bottles, leaving bottles one-third full of water and uncapped during empty bottle storage. Upon opening bottles, look for lack of venting which could indicate improper sealing or small stress crack leakage. On the 24-hour cycle only, remove all closures by hand at normal opening speed and note any closure releases or unusual closure performance.

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


16. Pour out remaining water immediately prior to wash. The internal bottle moisture is necessary to simulate stress crack patterns for this shortened cycle time. NOTE Achieving target opening temperatures for all bottles may require the addition of significantly more airflow around bottles. To achieve target opening unshaken pressure may require placing a nucleation particle in bottle just before cap is applied to speed-up CO2 equilibration time for 24-hour storage.

17. After every 5th cycle, record the condition of each bottle with respect to breaking, cloudiness, stress cracking, or any other noticeable change in appearance. Record the severity of stress cracks at each location on the bottle using the stress crack reference photographs in the Appendix or this scale:
Stress crack Severity A = Minor, very shallow cracks B = Moderate, shallow cracks C = Major, moderately deep cracks D = Major, deep cracks Quantity = 1 to 10 = 11 to 100 = 101 to 500 = 500+

18. Record on Data Form III Stress Crack Severity in this document the stress crack severity and quantity of cracks at: a. bottom bearing surface b. inside radius of the bottom bearing surface c. sprue d. area between the sprue and the inside radius e. finish f. neck g. top flute h. bottom flute i. heel

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


19. Record all bottle failures by bottle location and cycle. Save all bottles. If bottle has two different conditions of stress cracking at any location, then note both, for example, B4, D1 on bearing surface. 20. Return empty bottles to the environmental chamber at 37.8C 1C (100F 1.8F) and 40% RH +10% until the next filling (about 20 hours) unless the test is interrupted, then store at 72F. 21. Repeat steps 4 through 20 for 24 complete cycles. At every tenth cycle, pull one typical reference sample from bottles 6 through 14. Mark test request number and cycle pulled on the bottle. 22. Repeat steps 4 and 5 for one more cycle (cycle 25), then measure as in step 3. 23. Continue testing until at least 10% of bottles fail. NOTE To better understand stress crack results on wash test, evaluate the material distribution in the base as outlined in REFPET Bottle Plastic Distribution Test, PK-PR-226.

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


Test Figure. Finish Measurements

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


DATA FORM IWASH CONDITIONS
Test Request Number:
Date of Wash No. of Bottles Time Wash Started Time Wash Compl. Total Wash Time (Mins.) Time Rinse Compl. Total Rinse Time (Mins.) % Caustic % Additive Conc. Conc. C (F) Caustic Temp. Caustic Carry-over

Cycle

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DATA FORM IIFILLING AND STORAGE CONDITIONS
Test Request Number:
Date of Filling Bottle Order Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Filling Temp., C (F) Storage Filling Chamber Pressure, Vols. Temp., C Bars (psig) Carbonation (F) Time Storage Started Total Time Bottle Storage Storage Time (Hrs./ Storage Completed Mins.) Location* T M S T M S T M S T M S T M S T M S T M S T M S T M S T M S Product Temp.**

Cycle

*T = Top stack corner M = Middle stack corner S = Bottom stack opposite corner to top

**Measure temperature is 1 bottle for each location from storage chamber

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


DATA FORM IIISTRESS CRACK SEVERITY
T. R. #: Manuf.: Package: Test Type: Bottom Lube: Sample Size: Cycle 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 Bottle Broken Finish Neck Top Flute Bottom Flute Stress crack Severity A = Minor, very shallow cracks B = Moderate, shallow cracks C = Major, moderate deep cracks D = Major, deep cracks Top Heel Middle Heel Bearing Surface Inside Radius Quantity 1 = 1-10 2 = 10-100 3 = 100-500 4 = 500+

Push-Up

Sprue

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Appendix. Stress Crack Photographs

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REFPET Bottle Durability TestAbbreviated Trip-Per-Two-Day Washing


Revision History
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REFPET Bottle Durability TestStandard Trip-Per-Two-Day Washing


Purpose
The durability of a filled plastic bottle is critical to allow it to function. The test conditions specified here relate to field performance in a minimum of nine weeks. REFPET Bottle Specifications, Durability, PK-SP-045

Corresponding Specification Test Equipment

Caustic tank and safety equipment Filler Fill-height syringe Capper Environmental control chamber Rinse area Mettler PC 4000 scale or equivalent Dial caliper with base Pi-Tape or equivalent circumferential tape Depth gauge Optical comparator

Procedure
1. Randomly select a 154-bottle sample. On each bottle, put the test request (TR) number and number the bottles sequentially. Also, always include a control group for comparison. 2. Set aside bottles numbered 145 to 154 and retain as controls for the foaming test in step 25. 3. Select samples numbered 1 through 10. Measure fill-point capacity on each of these bottles at completion of 0, 5, 15, and 25 washes. 4. On the same samples and the same frequency as in step 3, measure and record the following if checked: a. Overall height b. Base push-up height c. Pinch diameter d. Finish dimensions, E1, E2, E3, E4 (see drawing) e. Perpendicularity, T1, T2, and A f. Upper label diameter

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REFPET Bottle Durability TestStandard Trip-Per-Two-Day Washing


5. Precondition bottles by immersing in water at 41C 3C (105.8F 5.4F), then empty and immerse the bottles completely in 3.0% +0.5% -0% caustic and 0.15% +0.05% -0% Henkel P3 stabilon Al Fluessig additive at 59.5C 1.0C (139F 1.8F) for 15 minutes 1 minutes. (If this chemically aggressive Henkel additive is not available, then use an approved additive at nominal field use concentration but increase contact time.) 6. Measure and record on Form I Wash Conditions in this document, the caustic concentration, additive concentration, temperature and soak time at each washing. We recommend installing an alarm system and setting at 61C (141.8F) to monitor maximum temperature. 7. Remove the emptied bottles and immediately rinse them thoroughly with potable (fresh tap) water by immersing in water, completely filling bottles and emptying 2 times, followed by a fresh water spray rinse as follows.
First rinse Second rinse Third rinse Water immersion at 41C 3C (105.8F 5.4F) Immersion at ambient Ambient using jetting for 15 seconds at 30 psi with an inside stream type 2 mm (5/64 inch) nozzle and external dispersion type nozzle on an inverted bottle

8. As it is extremely important that there is no caustic carryover, check for caustic carryover each cycle by allowing 3 drops of phenolphthalein to run down both the base exterior and the inside of the bottle. No color indicates no caustic. If pink color develops, add 10 ml of distilled water. If pink color persists, caustic is present and more thorough rinsing is necessary. 9. Fill the bottles numbered 124 through 144 about three-fourths full of water and counterpressure to 5.5 bars (80 psi) for 20 seconds and then empty. 10. Wipe a thin layer of Diversey SUPERPET C line lubricant or equivalent line lubricant diluted at 1 part line lubricant to 100 parts water (1.0 percent 0.1 percent) on the entire bottom and to a height of 3 mm up the heel on each bottle. Store the one percent lube mixture in a sealed container when not in use or make a new batch daily. This is necessary to insure that evaporation does not cause the ratio to drift outside of the stated tolerance.

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11. Fill all of the bottles with carbonated water to achieve 4.2 0.2 volumes carbonation at 22.2C (72F) after 24 hours and apply new plastic closures. Use only Metal Closures, MCA finial plastic closures at 10-12 inch-pounds application torque, or other approved plastic closure for REFPET bottle. 12. On Form II Filling and Storage Conditions for steps 12, 13, and 14, measure and record pressure and temperature of one extra bottle at beginning, middle, and end of filling operation. 13. Store at 37.8C 1C (100F 1.8F) and 40% 10% relative humidity for 24 hours 1 hours. At every wash cycle, record exact number of hours bottles are stored at 37.8C (100F). All bottles are to achieve 36.8C 1C (98.2F 1.8F) at end of 24 hours. NOTE Bottles can be stored full over weekend and/or holidays at 35.6C 1C (96F 1.8F) in order to obtain one or more extra cycle per week. Under no condition should bottles exceed 25 hours at 37.8C 1C (100F 1.8F).

14. Measure and record temperature and relative humidity of the chamber then remove the bottles from storage. Immediately measure and record temperature of one bottle from each of the following storage locations: a. Top stack corner b. Top stack center c. Middle stack corner d. Middle stack center e. Bottom stack corner f. Bottom stack center The target average unshaken opening pressures are:
Weekend/holiday storage 24-hour storage 67 3 psi for at 35.6C 1C (96F 1.8F) 70 3 psi at 36.8C 1C (98.2F 1.8F)

15. Open and two-thirds empty remaining bottles, leaving bottles one-third full of water and uncapped during empty bottle storage. Upon opening bottles, look for lack of venting which could indicate improper sealing or small stress crack leakage. On the 24-hour cycle only, remove all closures by hand at normal opening speed and note any closure releases or unusual closure performance.

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16. Pour out remaining water immediately prior to wash. Moisture in the bottle is necessary to simulate stress crack patterns of this shortened cycle time. NOTE To achieve target opening temperatures for all bottles may require addition of significantly more air flow around bottles. To achieve target opening unshaken pressure may require placing nucleation particle in bottle just before cap is applied to speedup CO2 equilibration time for 24-hour storage.

17. At the completion of every fifth cycle, record the condition of each bottle with respect to breaking, cloudiness, stress cracking, or any other noticeable changes in appearance. Record the severity of stress cracks at each location on the bottle using the stress crack reference photographs in the Appendix or the following scale:
Stress crack Severity A = Minor, very shallow cracks B = Moderate, shallow cracks C = Major, moderately deep cracks D = Major, deep cracks Quantity = 1 to 10 = 11 to 100 = 101 to 500 = 500+

18. Record on Data Form III Stress Crack Severity the stress crack severity and quantity of cracks at the following: a. bottom bearing surface b. inside radius of the bottom bearing surface c. sprue d. area between the sprue and the inside radius e. finish f. neck g. top flute h. bottom flute i. heel 19. Record all bottle failures by bottle location and cycle. Save all bottles. If bottle has two different conditions of stress cracking at any location, then note both, for example B4, D1 on bearing surface.

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20. Return empty bottles to the environmental chamber at 37.8C 1C (100F 1.8F) and 40% +10% until the next filling (typically about 20 hours), unless the test is interrupted, then store at 72F. 21. Repeat steps 5 through 20 for 24 complete cycles. At every fifth cycle, pull one typical reference sample from bottles numbered 11 through 123. Mark test request number and cycle pulled on the bottle. 22. Repeat steps 5 through 8 for one more cycle (cycle 25). 23. After 25 washings (not complete cycles) choose 18 cycled bottles and six new bottles (for air and temperature checks) for conducting carbonation retention testing using REFPET Bottle Carbonation Retention Test, PK-PR-219. 24. After 25 washings conduct the following tests: a. PK-PR-247, Appearance and Color Evaluation b. PK-PR-207, Dimensions EvaluationExterior c. PK-PR-270, Perpendicularity Test d. PK-PR-223, Empty Weight and As-Delivered Capacity Test e. PK-PR-218, Capacity Change (Shrinkage) Test f. PK-PR-225, Internal Pressure Test g. PK-PR-229, Vertical Load TestEmpty h. PK-PR-228, Thermal Stability Test i. j. k. PK-PR-224, Fill Point Variation Test PK-PR-220, Drop Impact Test PK-PR-227, Support Ledge Test

25. Conduct foaming tests using control samples numbered 145 to 154 from step 2 and select 10 samples after 25 washings. Control samples should be washed once prior to filling. All samples should be wet before filling. a. Fill all samples with Coca-Cola and note foaming/snift characteristics. Store filled and capped overnight. b. Open bottles and note foaming characteristics by measuring distance from top of finish to top of foam or amount of foam-over. Empty the bottles and rinse thoroughly. Repeat foaming procedure using diet Coke.

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26. In addition, after 25 washes, conduct a storage test on remaining bottles. Fill these with 4.2 volumes 0.2 volumes carbonated water and store at 37.8C (100F) and 30% relative humidity for one week. Each day check each bottle and note any bottle failures, such as leakers, and note location and other details concerning the failure. NOTE To better understand stress crack results on wash test, evaluate the material distribution in the base as outlined in REFPET Bottle Plastic Distribution Test, PK-PR-226.

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Test Figure. Finish Measurements

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FORM IWASH CONDITIONS
Test Request Number:
Date of Wash No. of Bottles Time Wash Started Time Wash Compl. Total Wash Time (Mins.) Time Rinse Compl. Total Rinse Time (Mins.) % Caustic % Additive Conc. Conc. C (F) Caustic Temp. Caustic Carry-over

Cycle

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FORM IIFILLING AND STORAGE CONDITIONS
Test Request Number:
Date of Filling Bottle Order Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Start Middle Last Filling Temp., C (F) Storage Filling Chamber Pressure, Temp., C Vols. Bars (psig) Carbonation (F) Time Storage Started Total Time Storage Bottle Storage Time (Hrs./ Storage Completed Location* Mins.) T M S T M S T M S T M S T M S T M S T M S T M S T M S T M S Product Temp.**

Cycle

*T = Top stack corner M = Middle stack corner S = Bottom stack opposite corner to top

**Measure temperature is 1 bottle for each location from storage chamber

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FORM IIISTRESS CRACK SEVERITY
T. R. #: Manuf.: Package: Test Type: Bottom Lube: Sample Size: Cycle 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 Bottle Broken Finish Neck Top Flute Bottom Flute Stress crack Severity A = Minor, very shallow cracks B = Moderate, shallow cracks C = Major, moderate deep cracks D = Major, deep cracks Top Heel Middle Heel Bearing Surface Inside Radius Quantity 1 = 1-10 2 = 10-100 3 = 100-500 4 = 500+

Push-Up

Sprue

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Appendix. Stress Crack Photographs

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REFPET Bottle Empty Weight and As-Delivered Capacity Test


Purpose
Controlling empty bottle weight at manufacture is the first step in achieving consistent container properties. Bottle capacity affects the containers ability to meet correct volume requirements without overfilling. REFPET Bottle Specifications, Empty Weight and Capacity AsDelivered, PK-SP-045 Mettler PC4000 scale or equivalent Fill-height syringe assembly

Corresponding Specification Test Equipment Procedure

1. Select at random 10 samples previously inspected for visual defects. Mark each sample with an identification number in a continuous sequence. 2. Weigh each bottle and record the weight to the nearest 0.1 grams. Report each bottle weight and the maximum, average, minimum, and standard deviation for the sample group. 3. Place each bottle on a digital scale and tare the weight so that the readout is at 0.0. 4. Fill the bottle with water at a known temperature to a level above the fill-point. 5. With a preset fill-height syringe, remove the excess water down to the proper fill-point. 6. Record the weight and water temperature. 7. Use the Density Conversion Table found in RF-PK-108 to adjust to milliliters. 8. With the bottle still on the scale, add water until the level is just above the finish. 9. Record the weight and water temperature. 10. Use the Density Conversion Table found in RF-PK-108 to convert to milliliters. 11. Report the weight of the water, temperature of the water, and milliliters for each bottle and the maximum, average, minimum, and standard deviation for the sample group.

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REFPET Bottle Fill-Point Variation Test


Purpose
These test procedures address the ability of a plastic container to maintain adequate fill-height variation, under pressure, between containers in the same lot. REFPET Bottle Specifications, Fill-Point Variation, PK-SP-045

Corresponding Specification Test Equipment

Carbon dioxide source Hypodermic needle/pressure transducer assembly Height gauge Fill-height syringe assembly Thomas septums (fitted) Capper

Procedure
1. Select 10 samples which provide the best representation of all mold numbers that have previously been inspected for visual defects. 2. Fill each container with tap water at 22.2C (72F) and syringe each to the proper fill-point. Cap each sample with a closure that has been fitted with a septum. 3. Measure the liquid fill height from the top of each container to the bottom of the meniscus. Record this value. 4. Inject carbon dioxide gas through the septum at a rate of 4.1 bar gauge (10 psig) per second to a level of 4.1 bar gauge (60 psig). Hold this pressure for one minute and then remove the hypodermic needle/pressure transducer from the septum. 5. Repeat step 3. 6. Increase the pressure in the same manner as in step 4 to a level of 5.5 bar gauge (80 psig). Hold this pressure for one minute and then remove the hypodermic needle/pressure transducer from the septum. 7. Repeat step 3. 8. The fill-point variation is the difference between the minimum and maximum fill-points for each pressure.

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REFPET Bottle Internal Pressure Test


Purpose
The internal pressure strength of a plastic container varies due to its method of manufacture and conditions it may encounter in its normal life cycle. This test presents a means of measuring internal pressure strength to determine whether it meets minimum performance requirements. REFPET Bottle Specifications, Internal Pressure, PK-SP-045

Corresponding Specification Test Equipment Procedure

AGR internal pressure tester or equivalent

1. Select at random 10 samples previously inspected for visual defects. Mark each sample with an identification number in a continuous sequence. 2. Fill each bottle completely with water. 3. Place in a suitable apparatus that will build internal pressure hydraulically. Pressure should be increased steadily until bottle failure. 4. Record the pressure at which the bottle failed, along with the location of failure. 5. Report each failing pressure and location of failure, maximum, average, minimum, and standard deviation for the sample group.

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REFPET Bottle Perpendicularity Test


Purpose
Use this test to ensure that REFPET plastic bottles stand upright in an orientation that is completely perpendicular to the bearing surface on which they stand. REFPET Bottle Specifications, PK-SP-045, Perpendicularity Empty and Filled Uncapped Bottles Perpendicularity gauge assembly or equivalent

Corresponding Specification Test Equipment Procedure

1. Using 108 randomly-selected sample bottles as a source, select a subgroup 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 to zero. 4. Rotate the bottle through at least 360 degrees 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 the remaining samples. 6. Record all measurements.

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REFPET Bottle Plastic Distribution Test


Purpose
Controlling plastic distribution is a basic requirement for maintaining properties of all plastic containers. This test provides a means to judge this aspect of bottle manufacture. REFPET Bottle Specifications, Plastic Distribution, PK-SP-045

Corresponding Specification Test Equipment Procedure

Electronic sensing probe Mettler PC4000 scale or equivalent

1. Select 10 samples previously inspected for visual defects. 2. Measure the plastic sidewall thickness every 30 around the bottle at the specified heights. 3. Report the maximum height for each bottle, and then the maximum, average, minimum, and standard deviation height for the sample. 4. Measure the neck thickness every 90 around the bottle at 10 mm, 20 mm, 30 mm, and 40 mm down from the support ring for all bottles. For bottles larger than 1 liter, also measure at 50 mm. 5. Report each reading for each bottle along with the maximum average, minimum, and standard deviation for each location for the sample. 6. Measure bottom thickness around the base at five locations according to the test figure. Rotate the bottle 360 to obtain the minimum and maximum thickness for each location. 7. Report the individual measurements for each bottle. Indicate where the mold seam is in relation to the thickness measurements. Report the maximum, average, minimum, and standard deviation for each location. 8. Conduct sectional weight evaluation of the bottle as follows: a. entire bottle b. neck weight (50 mm from top) c. base weight (25 mm from bottom) d. panel weight (remaining midsection)

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Test Figure. Measuring Bottom Thickness

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REFPET Bottle Support Ledge Strength Test


Purpose
The topload strength of a plastic container support ledge varies to the profile design and load conditions encountered during its normal cycle life. This test presents a means of measuring support ledge strength to determine whether it meets minimum requirements. This testing is normally conducted only in conjunction with a retest after caustic wash cycling.

Corresponding Specification Test Equipment Procedure

REFPET Bottle Specifications, Support Ledge Strength, PK-SP-045 Tensile/compression tester Fixture (to represent support ledges in capper)

1. Select 10 samples that provide the best representation of all preform mold numbers that have previously been inspected for visual defects. 2. Cut off the finish of the container about 6.3 mm (1/4 inch) below the ledge support. Place each finish into the fixture in the compression test apparatus at room temperature. 3. Position the load platen approximately 50 mm (2 inches) above the top of the container and zero the load gauge readout if necessary. 4. Apply the load at a rate of 5 cm (0.2 inches) per minute and record the resulting curve. 5. Report the first failure peak of the ledge support in pounds or kilograms of force. Also, report the maximum, average, minimum, and standard deviation for the peak loads.

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REFPET Bottle Thermal Stability Test


Purpose
The thermal stability of a plastic container varies due to its method of manufacture and the environmental conditions it may have to withstand in its normal life cycle. This test presents a means of measuring its axial and hoop strength to determine whether it meets minimum performance requirements. REFPET Bottle Specifications, Thermal Stability, PK-SP-045

Corresponding Specification Test Equipment

Tensile/compression tester Carbonator Capper Environmental control chamber Perpendicularity gauge assembly Fill-height syringe assembly Pi-Tape or equivalent circumferential tape Dial caliper with base Depth gauge

Procedure
1. Use the same 10 bottles previously tested for empty dimensions and perpendicularity. Randomly select 2 new additional samples. Mark the additional samples as 11 and 12 (the first 10 bottles are already marked 1 through 10). 2. Rinse each sample prior to filling to eliminate dust or dirt particles from the inside surface of the bottle. 3. Fill all samples and controls on Meyer filler, or equivalent, to the proper fill-point with carbonated water to achieve 4.0 0.2 volumes apparent carbonation when measured at 22.2C (72F). Deaerated water should be used if possible to minimize air content in headspace of the bottle. High air content can significantly affect the test results. Samples should be immediately capped after filling. 4. After completion of step 3, immediately measure and record the fill height of samples 1 through 10 within one minute of capping. Measure fill-point from top of closure to bottom of liquid meniscus.

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5. Store all samples at 22.2C (72F) for 24 hours. Measure and record carbonation level and oxygen content of samples 11 and 12. Maximum allowable air is 4 psi. Now measure and record the following for samples 1 through 10: a. Overall height b. Diameters c. Perpendicularity d. Fill height e. Dome depth NOTE Any rocker bottoms, burst samples or any objectionable appearance (stress, whitening, localized expansion and the like).

6. Reclose bottles 11 and 12, then store all 12 samples at 37.8C 1C (100F 1.8F) and 40% 10% relative humidity for 24 hours 1 hour. All bottles are to achieve 36.7C 1C (98F 1.8F). Measure temperature of samples 11 and 12 then recap. Measure samples 1 through 10 as in part 5. Record all findings. 7. Place the samples that havent burst or developed rocker bottoms back into the oven at 37.8C (100F) and store them for six more days. Continue to measure and record temperature of controls and relative humidity daily. 8. Test as per 5 above. In addition, measure and record temperature in samples numbered 11 and 12. All bottles are to achieve 37.8C 1C (100F 1.8F). 9. Randomly divide the remaining intact samples into two groups and designate them as groups I and II. 10. Perform a drop impact test (PK-PR-220) at 37.8C (100F) on group I (drop from one meter or approximately three feet onto a smooth concrete floor and note any failures). 11. Store group II at 22.2C (72F) for 24 hours. Test as per 5 above. 12. Perform a drop impact test on group II (drop from one meter or approximately three feet onto a smooth concrete floor at a 30 angle) and note any failures.

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13. Report all measurements and observations along with the bottle numbers. Report the maximum, average, minimum, and standard deviation for each measurement location, fill-point, and perpendicularity. Compare the averages and report the percent increase or decrease for each measurement location.

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REFPET Bottle Vertical Load TestEmpty


Purpose
The topload strength of a plastic container varies due to its method of manufacture and the load conditions it may have to withstand in its normal life cycle. This test presents a means of measuring column strength to determine whether it meets minimum performance requirements. REFPET Bottle Specifications, Vertical Load, PK-SP-045

Corresponding Specification Test Equipment Procedure

Tensile/compression tester

1. Select 10 samples which provide the best representation of all mold numbers that have previously been inspected for visual defects. 2. Place each empty container in the compression test apparatus at room temperature (approximately 22C or 72F). 3. Position the load platen approximately 50 mm ( 2 inches) above the top of the container and zero the load gauge readout if necessary. 4. Apply the load at the rate of 51 cm per minute and record the resulting curve. 5. The compression tester readout should be capable of indicating the minimum load between 1.59 mm and 4.76 mm (1/16 inch and 3/16 inch) bottle deflection, the peak load, and the bottle deflection at peak load. 6. Report the minimum load between 1.59 and 4.76 mm bottle deflection for each bottle in pounds or kilograms of force. Also, report the maximum, average, minimum, and standard deviation for these minimum loads. 7. Report the peak load in kilograms (pounds) of force and the bottle deflection at the peak load for each bottle. Also, report the maximum, average, minimum, and standard deviation for the peak loads.

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REFPET Bottle Vertical Load TestEmpty


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REFPET Bottle Line Trial


Purpose
As part of New Package Authorization, PK-RQ-020, use this procedure as a general guide to performing a Line Trial for REFPET bottles. The line trail identifies areas within bottle handling, production and distribution that may contribute to scuffing. This document describes the procedure for performing a line trial and suggests corrective actions. REFPET Bottle Specifications, PK-SP-045

Corresponding Specification Procedure


Bottling Line Test
Preparation

1. Obtain ten new REFPET bottles 2. Mark them with a caustic-proof adhesive tap around the bottle neck

Operation

1. Select a pallet of REFPET bottle returns identified for immediate production 2. Place the ten new, marked bottles at locations within the pallet. 3. Pass the pallet through the bottling line. 4. Retrieve the ten bottles from the cases after the caser. 5. Empty the contents of the bottles 6. Record the line speed, stoppage information, amount of time bottles are in washer. 7. Repeat for a total of 25 cycles or until bottles reach a scuff level #4, whichever happens first. NOTE To make sure no bottles are misplaced, gather the group of test bottles at the entrance to the washer and manually place the bottles in one row of washer pockets so that all the bottles in the sample come out at the same time and are easier to find. In addition, it may help to gather them after the filler and mark the closure top with black in felt marker. This makes collection mush easier after the caser.

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Data Handling
Record results. No action is necessary if 25 cycles are completed without bottles reaching scuff standard #4. Otherwise, isolate the source of abuse by the Bottling Machine Test, Route Truck Test, and Remote Sorting Test in this document, and take appropriate corrective action.

Bottling Machine Test


Preparation
Obtain five new bottles for each piece of equipment: combiner, sniffer, decapper, washer and the like. Mark them with an adhesive tape and identify each bottle with a code for each machine. Pass each group of five bottles through the respective machines 25 times. See Loop Trial Desired Performance and Scuffing Scores section of this document for interpretation of results.

Operation

Route Truck Test


Preparation
1. Remove two cases from the line prior to the caser. 2. On only one of these cases, clean thoroughly all the inside bottle contact surfaces. Put new filled REFPET bottles in each pocket, and wrap the case so it will keep clean through the test. 3. Put new filled bottles in the other case. 4. In a like manner two cases should be selected, one cleaned, both filled with new, empty REFPET bottles, and the cleaned case should be wrapped to keep it clean.

Operation

Place the four cases on a route truck in the normal manner in which they are handled, and leave on the truck for ten days of deliveries. Compare the condition of bottles in the wrapped cases with the bottles in the unwrapped cases. If the bottles in the unwrapped cases are noticeably different, take appropriate action. For example, if the bottles are noticeably dirtier, then the covering for the truck is probably not adequate, or the truck bays might need cleaning. If the unwrapped bottles are more scuffed, the case washer is probably inadequate.

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Remote Sorting Test
If sorting is done at a location other than the bottling plant, then carry out this test.

Preparation Operation

Obtain ten new bottles, mark and code them for easy identification. 1. Select a pallet to be sorted and replace ten bottles at random with the new marked bottles. 2. Retrieve the bottles after sorting. 3. Repeat for a total of 25 cycles.

Observations

While the bottles are running, inspect conveyor guide rails, infeed screws, star wheels, washer guides, washer pockets, and other bottle contact surfaces for sand, grit, and dirt. Where appropriate, use photographs and video tape to illustrate handling and storage conditions. Record the visual appearance of the test bottles after every five cycles. It may be found that on some pieces of equipment, the scuffing does not change markedly after reaching a certain level.

After 25 trips the bottles should: Loop Trial Desired show no stress cracks Performance and each have a scuff level 3 or less Scuffing Scores Calculate scuffing scores for each machine by adding the scuff level number for each bottle in the five bottle group after completing five additional cycles. These scores allow comparison of different machines scuffing action, or of the filling process VS distribution.

Corrective Action

1. Thoroughly clean all the bottle contact surfaces of the conveyors, guide rails, and individual pieces of equipment between the uncaser and the washer. Remove all accumulated dirt, sand, oil, or foreign substance of any kind. 2. Lightly rub guide, starwheels, and infeed screw body with a fine sandpaper and wipe off. Replace or repair any part to eliminate all rough spots, nicks, burns, and sharp edges.

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3. Adjust top guides so they do not touch the upper part of the REFPET bottles. 4. Adjust conveyor speeds leading into combiners to avoid excessive bottle-to-bottle pressure. 5. Adjust infeed conveyor speeds at each piece of equipment slightly above the pitch speed to allow the infeed screw to merely separate the bottles rather than to accelerate them. The goal is to minimize the pressure between the infeed screws and bottles. 6. Adjust bottle handling parts of each piece of equipment to obtain smooth handling of bottles through the equipment from infeed to discharge. 7. Make sure there is at least 5 mm clearance between the bottles, the infeed screws and the back guides that are opposite the screws. 8. The conveyor guides leading in the infeed screw must be placed ahead of the solid bodies of the screws to avoid each bottle hitting the screw body instead of moving smoothly inside the screw pockets. 9. If after making all adjustments the plastic infeed screws still damage the bottles, replace them with screws made with stainless steel or cast in brass, polished and then chrome plated. 10. Replace roller belts and powered roller combinations, and adjust so that: a. only rollers are in contact with the bottle b. rollers are lubricated and cleaned with a water spray mist c. rollers do not touch the bottle pinches, and contact only the major diameters at the bottle heels.

11. Install water sprays to provide bottle cleaning and lubrication. a. in-case bottle pre-rinsing with high pressure water sprays prior to the uncaserMinimize introduction of water spray into the uncapped bottles. b. high-volume, low pressure spray on both sides of the single file conveyor after the uncaser, minimize introduction of water into the container.

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c. low volume, high pressure water spray on the infeed screws of the machines between the uncaser and the washer. It should keep the screw as clean as possible while providing lubrication between the bottle and the screw.

d. low volume, high pressure water spray on the roller of powered roller combiners. e. If after the changes there is still scuffing from the infeed screws, replace the plastic infeed screw with a stainless steel screw, or with brass cast screw, polished and chrome plated.

Revision History
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