Blow
Molding
Technical
Tip
tech.topic
Environmental Stress Crack Resistance
Unstressed polyethylene at room and normal index decreases); and as molecular weight
service temperatures up to 60°C (140°F) is distribution narrows. Two American Society
highly resistant to a wide variety of rather for Testing and Materials (ASTM) and one
reactive chemicals such as inorganic acids, Plastic Bottle Institute (PBI) test methods
alcohols, fatty oils, food chemicals and that rate polymers and molded parts on their
detergents. However, items made from ability to resist ESG are:
polyethylene resins can crack when exposed to
the same chemical "environment" if they are 1. ASTM D 1693: Environmental Stress
stretched or bent in several directions at once, a Cracking of Ethylene Plastics "Bent Strip
condition known as ”polyaxial stress." ESCR"
Thus, if conditions are unfavorable, various oils At the Cincinnati Technology Center and
or even common household cleaning agents may other laboratories, Igepal® CO-630, at varying
cause a polyethylene bag, pipe, tank, drum or concentrattions, is used as the standard
bottle to crack and split open after only a short cracking reagent for this test, which is
period of time. Bottles or other parts designed to carried out on molded specimens 1/8 in. or ¾
contain detergents, solvents or acids must in. thick (depending on the PE type being
therefore be manufactured from a polyethylene tested), 1½ in. long and ½ in. wide. The
resin that exhibits a high resistance to specimens are first heated in boiling water to
"environmental stress cracking" (ESC). relax "frozen-in" stresses. A surface cut of a
specified length and depth is then made on
HOW STRESS CRACKING OCCURS the sample parallel to the long axis with a
The failure of a container to resist ESC can mounted razor blade. The specimens are the
be the result of stored stresses acquired in stressed by bending them 180 degrees. The
the molding or extrusion operation. Stress specimens are then placed in a rack that is
cracking agents, such as the liquids put into a test tube containing the stress-
mentioned above, migrate into minute cracking agent. To accelerate the effect of
cracks in the crystalline areas of the the cracking agent, the test tube is placed in
polyethylene molecules forming the surface a bath at 50°C (122°F).
of the container. These microscopic cracks
Periodically, the specimens are inspected for
are a result of a breakdown of the polymer
visual cracks perpendicular to the cuts. At
chains in the case of acids and solvents, and
each inspection, the number of failures is
a “wetting out” of the surface in the case of
recorded. A polyethylene resin is considered
detergents, largely due to their surfactant
to have failed when one half of the specimens
components.
in the tube show cracks perpendicular to the
In either case, the surface tension between cuts.
the crystalline layers is reduced. What once
2. ASTM D 2561: Environmental Stress Crack
was a microscopic surface imperfection
Resistance of Polyethylene Blow Molded
propagates or "zippers open" to a full
Containers "Bottle ESCR"
fledged break in the bottle. ESC failures are
accelerated by high temperatures and The test is usually carried out on 16-oz., 25-g.,
additional external stresses such as top Boston Round bottles blow molded from
loaded storage. polyethylene resin, although a container of any
size and shape can be used. Bottle design,
HOW RESISTANCE IS DETERMINED processing conditions and the resin used are
The resistance of polyethylene to stress all variables affecting the results of this test.
cracking increases as density decreases; as
average molecular weight increases (melt
(Continued on Page 2)
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Blow
Molding
Technical
Tip
tech.topic
Environmental Stress Crack Resistance
(continued)
ASTM specifies three environments for this placed in an oven at 140°F. The bottles then
test, so it is important to know which are subjected to an internal pressure of five
procedure was used in order to compare test psi, introduced through the cap assembly,
results. It is also important to know that for the duration of the test. Inspection and
while ASTM calls for inspection to stop after reporting is carried out in the same way as
360 hours, many suppliers continue to check Procedure A.
the bottles to 500 or 1,000 hours after the
test begins. Successful results from these 3. PBI 11: Recommended Practice for
lengthier tests are reported as >500 or Determining Top Load Stress Crack
>1,000 hours. Resistance of Blow Molded Polyolefin
Bottles
Procedure A: A minimum of 15 containers is
filled to nominal capacity with the chosen The purpose of this test is to simulate the
test liquid, usually a proprietary liquid conditions a container undergoes during
product or an aqueous solution of shipment or storage. A minimum of 15
polyoxyethylated nonylphenol (a surfactant). bottles is filled to nominal capacity and heat-
The containers are heat sealed and placed in sealed as in ASTM D 2561. The bottles are
an oven at 140°F. then placed in a jig that applies a constant
top load for the duration of the test. Bottles
Inspection takes place hourly for the first and jig are placed in an oven at 1220°F.
eight hours and at least once every 24 hours Inspection and reporting occurs in the same
thereafter. Results are reported as the way as ASTM D 2561, Procedure A. Data
number of hours elapsed before 50 percent from this test appears to reproduce reality
of the specimens failed (F50). more closely than ASTM D 2561 or ASTM D
1693.
Procedure B: A minimum of 15 containers is
filled to one-third of their overflow capacity All of the test procedures described
with the same stress cracking solution used generate valuable data that provides insight
in Procedure A. The containers are heat into the phenomenon of ESCR. However,
sealed and placed in beakers vertically with these methods are very sensitive to testing
the finish up. The beakers are then filled error; the data must be used with caution.
with a sufficient amount of stress cracking As an example, some testing errors can
agent to cover the chime area of the occur during the ASTM D 1693 "Bent Strip
container and placed in an oven at 140°F ESCR" test because of:
Inspection and reporting occurs in the same
way as Procedure A. Surface imperfection on the test specimens
Defective method of fabricating the test
Procedure C: A minimum of 15 containers is
specimens
filled to one-fourth of their overflow capacity
Different rates of cooling of test specimens
with the same stress cracking solution used
in Procedure A, The containers are then Incorrect or inconsistent concentration of
sealed with a special cap assembly and the reagent
(Continued on Page 3)
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Blow
Molding
Technical
Tip
tech.topic
Environmental Stress Crack Resistance
(continued)
are very important. Differences in ESCR
Defects in the specimen holder
performance of various products could actually
Temperature variations within the water
be attributed to varying degrees to test error. In
bath
addition, test method guidelines permitting
Inconsistent depth, length or width of the different surfactants and container styles add to
notch cut in the specimen the confusion. Additionally, some resin
Inconsistent rates at which the specimens manufacturers may make minor modifications to
are bent the test procedures to suit their own needs.
Defective condition of the die, if the
specimens are cut from a sheet When considering ESCR, it is important for the
Inconsistent data reporting resin customer to compare "apples to apples. "
Find out test conditions such as temperature,
With such a large number of variables, it is not surfactant used, bottle type and weight, among
surprising ASTM has found the precision of D other variables. For best comparison, the
1693, when performed at different laboratories, polymers in question should be subjected to side-
to be 2.9, which is expressed as two standard by- side testing, using the same equipment,
deviation limits on the 50-percent failure point. operator and environment. These conditions
This number means that if one laboratory were to minimize much of the test variation and give the
test a material and find that the 50-percent fairest comparison.
failure point (F50) occurred at 10 hours, other
laboratories, testing the same material, could be Equistar technical service representatives are
expected to generate data that varies between 3.4 available to assist you in understanding ESCR
hours and 29 hours. data. In certain cases, they may even be able to
coordinate a test program to evaluate ESCR
ASTM has determined the precision of D 2561 to properties of several different resins of your
be 1.8 and PBI reports the precision of PBI 11 is choice. For further information, please your
approximately 1.5, which means these two tests Equistar sales or technical service
are more reproducible than D 1693. However, representative.
the ramifications of all these precision numbers
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