PET BOTTLE TESTS:

Stress Crack Test:

Purpose
This procedure evaluates the performance of bottle bases when they are exposed to a 0.2% solution of NaOH (Sodium
Hydroxide) to simulate the failure associated with Stress Cracking.
Description
Each bottle is filled to net target content with water equilibrated to 22C +/- 1C (72 +/- 2F). Bottles are pressurized with
compressed air to the equivalent internal pressure of 531 +/- 4 kilopasclals (77 +/-0.5 psi). After 5 minutes, the fill line on each of
the bottles is marked and they are placed in individual pockets of 0.2% Sodium Hydroxide solution. The containers remain in the
caustic solution until they fail by either catastrophic burst or leaking through cracks that develop in the base. The time to failure is
recorded for each container. Failed containers are removed and the location of the failure is determined and recorded.
Burst Test:
Purpose
This procedure evaluates the performance of a bottle when the container is pressurized to very high levels. Failure location
reveals weak areas of the bottle
Description
Bottles are pressurized with air and water in the AGR PPT burst testing device. Pressure is added until the bottle fails or the
testing limits are met. The PPT burst tester can be programmed to run many different pressure profiles from quick jumps to
elevated pressures with hold times. Profiles can also be created for cycle testing and step pressure increases.
Drop Test:
Dropped from 1.5 meter
AA CONTENT, PREFORM/RESIN
Equipment Used
Gas Chromatograph
Purpose
This procedure measures the amount of acetaldehyde in PET resin or a PET preform.
Description
PET resin or preform samples are ground to a small particle size. A known weight of this ground material is sealed into a glass
vial equipped with a teflon-lined rubber septum. These vials are then heated to drive the AA to the headspace of the vial. A
sample of the equilibrated headspace in the vial is removed and is injected into a gas chromatograph and the software measures
the acetaldehyde peak area. A suitable acetaldehyde standard is used to calibrate the gas chromatograph. This is then used to
calculate the amount of acetaldehyde in the samples.
AA CONTAINER HEAD SPACE
Equipment Used
Gas Chromatograph
Purpose
This procedure measures the amount of acetaldehyde in PET bottles 24 hours after blow molding.
Description
Bottles are blow molded using standard blow air and flushed with nitrogen for 30 seconds and sealed approximately one hour
after blow molding. The bottles are stored in a 72F, 50% RH environment for 24 hours and then analyzed for acetaldehyde
content in the bottle headspace at 241 hrs of age. A suitable standard is prepared and used to calibrate the gas chromatograph.
The maximum height of the AA peak for the sample is compared against the AA peak for a known standard to determine the
amount of AA within the bottle headspace.
BURST PRESSURE
Equipment Used
AGR TopWave PPT 3000 - Packaging Pressure Tester

Purpose
This procedure evaluates the performance of a bottle when the container is pressurized to very high levels. Failure location
reveals weak areas of the bottle.
Description
Bottles are pressurized with air and water in the AGR PPT burst testing device. Pressure is added until the bottle fails or the
testing limits are met. The PPT burst tester can be programmed to run many different pressure profiles from quick jumps to
elevated pressures with hold times. Profiles can also be created for cycle testing and step pressure increases.
CARBOQC METHOD
Equipment Used
CarboQC Instrument

Purpose
This procedure determines the CO2 shelf life of a given carbonated beverage container by evaluating the CO 2 level within sample
bottles over time using a CarboQC test instrument. The CarboQC uses an automated piercing method, which improves test
repeatability as well as operator-to-operator test reproducibility relative to tests using a manual piercing method. It also corrects
for the amount of air in the package and reports both the volumes of carbon dioxide with the impact of air factored out and the
parts per million of air in the sample.
Description
Sixty bottles are carbonated to 4.2 0.1 volumes CO 2 and then stored in a constant temperature chamber at 72F, 50% RH for
the duration of the test procedure. Six bottle samples are destructively evaluated using the CarboQC to measure pressure and
temperature data to calculate volumes of CO2 at the following intervals: 0 hrs, 24 hrs, 2, 4, 6, 9, 12, 16, 20 and 24 weeks.
Packages are sampled by piercing them through the top panel of the closure with an automated sampling tube, then drawing a
fixed volume of liquid into a test cell. After the aliquot has been drawn into the cell and equilibrated by agitation, the cell is
expanded by first 10%, then by 30%, with the pressure and temperature being measured after each expansion. The pressure at
10% sample chamber expansion, the pressure at 30% sample chamber expansion, and measured temperatures are then used
to calculate the CO2 volumes contained within the bottle and the average % CO 2 loss per week is determined. The value of
CO2 volumes calculated by this method is corrected for the air content in the sample. This correction is possible because of the
differences in solubility of CO2 and air in water. As the test cell expands, the pressure contributed by CO 2 will remain the same as
more CO2 is pulled from the liquid phase, while the pressure contributed by air will drop as there is relatively minimal air
dissolved in the liquid phase that can be drawn out to further fill the expanded cell headspace. Air content is also reported as
parts per million of air. This test measures the CO2 loss from the entire package (bottle and closure) not just the bottle alone, as
does Zahm & Nagel testing.
Differences from manual Zahm & Nagel testing:
CarboQC measurements are more repeatable and reproducible because of the automated piercing and sampling.
The CarboQC reports a more accurate CO2 content as the calculations subtract the pressure contribution from air or
nitrogen.
The CarboQC reports amount of air content in ppm in addition to volumes of CO 2.
Volumes of CO2 as reported CarboQC will be nearly identical to volumes reported by Zahm & Nagel methods if the
water is effectively de-aerated prior to carbonation as it is in many production filling operations. If the water is not de-aerated
prior to carbonation, total pressure in packages measured by CarboQC to have the same volumes will be higher in package
pressure by an amount proportional to the amount of pressure in the package due to air content. This higher pressure will vary
depending on how much air is entrained in the water being used for filling, which depends on water temperature among other
variables. Use of water without effective de-aeration will typically add pressure equivalent to another 0.2 to 0.5 volumes of
CO2 content. Since this added pressure will lead to more tension stress for a package filled to a given "CarboQC volumes" than
would be experienced by a package filled to the same nominal "Zahm & Nagel volumes," it is critical that everyone who will use
the results of the testing understand the effects of this difference on testing results
COEFFICIENT OF FRICTION TESTING
Equipment Used :Instron COF Fixture
Purpose
This procedure determines the coefficient of friction between two PET film samples using an adapted version of ASTM D1894Description
Bottle samples are prepared and handled with gloves during both injection and blow molding to prevent contamination that might
affect the COF results. The bottle sidewalls are cut from the bottle and one sidewall is mounted to a metal sled while the other

sidewall is mounted to a flat plane. The COF assembly is then attached to the Instron machine and the force required to move
the sled across the plane is measured using the 10lb load cell. The data is plotted as force (lbs) vs. the sled travel (in.) and is
typically reported graphically. Our typical test usually results in a series of static COF values rather than an initial static value
followed by a kinetic value; this is because our samples usually "jump" across the sidewalls rather than pull uniformly. The COF
value is calculated by dividing the measured force by the weight of the sled.
DENSITY
Equipment Used
Techne Density Gradient Column

Purpose
This procedure determines a sample density and correlates that density to crystallinity using theoretical PET amorphous and
crystalline densities according to ASTM D1505.
Description
Five samples are prepared by cutting approximately 1/4" samples from a preform or bottle without touching the samples to
prevent oils from disturbing the testing. The entrapped air is removed from the surface of the sample and the samples are then
dropped into a density gradient column and allowed to settle for approximately 15 minutes. The height of the samples is then
carefully measured. Standard density balls are used to calibrate the density of the column. The sample density is then correlated
to the theoretical amorphous (1.3331) and crystalline (1.45234) PET densities to determine the % crystallinity.
Base Push-up
Base Thickness
Bottle Dimensions
This procedure is designed to measure the dimensions of a bottle to insure the containers meet the requirements and tolerances
specified on the bottle drawings.
Capacity Shrinkage
This procedure determines the amount of shrinkage in a blown container in the first 24 hours after blow molding by evaluating
the bottle height and diameters and overfill volume at 0.5, 5 and 24 hours.
Finish Dimensions
The Finish Dimensions test is designed to ensure that all thread finishes on bottles or preforms comply with the dimensions and
allowable tolerances specified on the respective bottle finish design drawings. In addition, there shall be no continuous or
excessive flash, and no overhang between the F and G dimensions.
Height and Diameter Shrinkage
Laser Metrology (Diameters)
Non-Carbonated Container, Package Test
Perpendicularity
Section Weights
This procedure determines the weight of specified container sections by physically cutting the container at defined locations.
Wall Thickness
This procedure determines the wall thickness at given locations on samples using a magnetic thickness gauge.
Shrinkage Blown Containers
This procedure determines the amount of shrinkage in a blown container in the first 24 hours after blow molding by evaluating
the bottle height and diameters and overfill volume at 0.5, 5 and 24 hours.
SECTION WEIGHTS
Equipment Used
PTI Bottle Cutter
Purpose
This procedure determines the weight of specified container sections by physically cutting the container at defined locations.

Description

Twelve bottles are cut at given height locations (typically found on a container drawing or specified by a project engineer) and
each section is weighed. The average and standard deviations are determined for each section. A general weight specification
range will be the target weight + / -0.5g.
Drop Testing
Whole container, non-carbonated
This procedure evaluates strength of a PET bottle when dropped.
Whole container, carbonated
This procedure evaluates the strength of a PET bottle carbonated to 4.0 0.05 volumes and then dropped from 2 meters (6.7
Ft.).
DSC THERMAL ANALYSIS
Sample Type

Required Quantity

Equipment Used

Resin Flake Preform Bottle

1 gram

Differential Scanning Calorimeter - TA

Instruments 2910

Purpose
This procedure measures the quantity of energy absorbed or released as the temperature of a plastic sample increases from
50C to 300C, is quench cooled and then reheated from 50C to 300C.
Description
10mg of a finely ground sample is weighed out into an aluminum DSC boat. This sample is then heated to 30 above the
anticipated melting temperature. It then is quickly quenched in liquid nitrogen to retain the properties of the material. At this point
it then is reheated. During both of these heating periods, the caloric values of the energy required to make the temperature
change are recorded. A graph is then produced and analyzed. From this analysis, glass transition temperature (Tg), crystallinity
temperature (Tc) and melting temperature (Tm) are determined.
Top Load

Filled
Empty
Top Load
TOP LOAD
Equipment Used
Instron 4411
Purpose
To insure that the vertical strength of PET bottles is sufficient to meet minimum performance standards for vertical loading as
might be encountered during bottle filling, capping and stacking of filled product.

Description
Twelve test samples are individually placed under the test platen on an Instron test device. The downward movement of the load
platen is initiated at a constant rate, and continues downward until the bottles resistance to loading peaks and the bottle loses
column strength and deforms. The maximum load and deflection at max load are recorded and reported by the machine, and the
failure location is added by the operator. Loads at other preset points may also be included in the recorded data.
To insure that the vertical strength of PET bottles is sufficient to meet minimum performance standards for vertical loading as
might be encountered during bottle filling, capping and stacking of filled product.
VOLUMES
Sample Type

Required Quantity

Equipment Used

Bottles

12

Top Load Balance Height Gage

Purpose

This procedure is used to determine the overfill (brimful) and fill line volume of each container in a set. This test can be used for
either statistical information like average and standard deviation numbers or can be used to obtain mold specific information. Our
typical test is either 12 samples chosen at random from a full mold round or it could be one container from each blow mold cavity.
Description
The overfill and fill line volumes are determined on twelve containers. Overfill is simply filling the container to a level equal to the
top of the finish of the container. The typical methods for measuring fill line volume are: 1. Filling the container to a specific height
and measuring the volume at that point. 2. Filling the container with a specific volume of water and measuring the height of the
liquid and comparing it to the target height. The weight of the water at these two points is used to calculate the volume of the
container by dividing the weight by the density of water at the recorded temperature.
Pateurization tolerance:
PASTEURIZATION
Sample Type

Required Quantity

Equipment Used

Bottles

10

Pasteurizer

Purpose
This procedure tests the performance of bottles as they are pasteurized.
Description
Eight (8) bottles are measured to determine the bottle diameters at several locations, the base material distribution, the push-up
height, the overfill volume and the perpendicularity. The bottles are then carbonated to 2.95-3.13 volumes of CO 2, and allowed to
equilibrate. The bottles are placed into a pasteurization spray chamber and sprayed with controlled hot water until the internal
water temperature reaches the targeted temperature at the coldest spot in the container. The temperature is then maintained for

a predetermined amount of time. The bottles are then sprayed with cold water until the internal water temperature decreases to
40C. The bottles are then removed and remeasured.
SOLUTION INTRINSIC VISCOSITY
Equipment Used
Rheotek Viscometer
Purpose
This procedure is used to determine the intrinsic viscosity (IV) of the material. IV is a measure of the Molecular Weight (MW) of
PET. The properties of PET are better at higher MW (higher IV) and worse at lower MW (lower IV). Comparing the SIV results
from resin and molded parts can provide an understanding of the drying and process conditions.
Description
The test procedure used is ASTM D4603. The solvent system used is 60% phenol/ 40% tetrachloroethane. The PET
concentration is 0.50% and samples are analyzed at 30C. The test can be run on resin, film, preforms and bottles. Corrections
are made for samples if they contain >1.% additives or colorants. It is important to know the level of additives present when
submitting a sample for analysis. PTI uses Rheotek equipment to measure IV . SIV data reported to the customer will be
measured at a single concentration to obtain the inherent viscosity. The intrinsic viscosity is mathematically calculated from the
inherent viscosity using the Billmeyer Equation.
Hot Fill Distortion
This procedure evaluates the performance of a heat set bottle when filled with heated water. The methodology used simulates
filling and capping as found in production.
PREFORM/BOTTLE HAZINESS
Equipment Used
Minolta Spectrophotometer
Purpose
This procedure is used to determine the amount of haze and the degree of color exhibited by a preform or container sidewall.
This is an indication of how effectively the material was processed and/or the materials ability to be processed.
Description
The samples are measured in terms of L*, a*, b*, DE* and Haze: L* (100=white; 0=black), a* (positive=red; negative=green;
0=gray), b* (positive=yellow; negative=blue; 0=gray), DE is a mathematical equation which takes into account the values of L*, a*
and b*. Haze measures the scattering of light through the sample; the higher the number the more haze. The haze can be used
as an indicator of the presence of crystallinity in the sample.
FLAKE/RESIN HAZINESS:
Equipment Used
Minolta Spectrophotometer
Purpose

This procedure is used to determine the amount of haze and the degree of color exhibited by the resin or flake. This is an
indication of how effectively the material was processed and/or the materials ability to be processed.
Description
The samples are measured in terms of L*, a*, and b*, DE*: L* (100=white; 0=black), a* (positive=red; negative=green; 0=gray),
b* (positive=yellow; negative=blue; 0=gray), DE is a mathematical equation which takes into account the values of L*, a* and b*.
TILT TEST
Sample Type

Required Quantity

Equipment Used

Bottles

12

TMI Tilt Tester

Purpose
This procedure determines the angle at which a bottle will tip and fall once the center of gravity has been overcome on tilting.

Description
A tilt test device is fitted with the appropriate surface. The test device is then tipped until a test bottle breaks the plane of contact
because the center of gravity of the bottle has been overcome. The angle at which this tipping occurs is considered the tilt angle.
Typically, twelve bottles are tested and the average tilt angle is determined for the set of bottles.
Difference between cappers and closures?