FREEZE-THAW STABILITY TESTING

During transportation of cosmetic products, it is not uncommon for them to encounter

extreme temperature conditions such as freezing and overheating. It is necessary for cosmetic
products to be able to withstand a certain degree of temperature changes in transport.
Freeze-thaw cycle testing is a part of stability testing that allows you to determine if your
formula will remain stable under various conditions. This type of test puts your sample
through a series of extreme, rapid temperature changes that it may encounter during normal
shipping and handling processes. Freeze-thaw stability testing is highly recommended,
especially for liquid-based cosmetics. These products may experience phase separation that
can negatively affect the intended function.
Freeze-thaw testing is conducted by exposing the product to freezing temperatures
(approximately -10C) for 24 hours, then allowing to thaw at room temperature for 24 hours.
The sample is then placed in a higher temperature (approximately 45C) for 24 hours, and
then placed at room temperature again for 24 hours. The sample is analyzed for significant
changes. This completes one cycle. If, after three cycles of freeze-thaw testing, no significant
changes are observed, you can be confident that the stability of your product is sufficient for
transport.

Cosmetic Stability Test Freeze Thaw Cycles

by Perry Romanowski
What is Freeze Thaw testing

Freeze thaw testing is a type of stability test in which you freeze your formula, then thaw it
out, and test to see what effect the process has on your product. To do a thorough freeze-thaw
test you will repeat the cycle a few times.
Why do Freeze thaw testing?

Freeze thaw testing gives you information that regular stability testing cant. Namely, it will
show you whether your formula will remain stable under varied conditions that it might
experience during the shipping and storage phases of the product life cycle.
Its likely that your product will be shipped via trucks or rail cars. These vehicles are rarely
equipped with temperature controls so it is likely that your product may freeze one day and
be in hot temperatures another. It is crucial that your formula is able to withstand extreme,
rapid temperature changes.

How to conduct a freeze-thaw test

While there is no right way to do a freeze-thaw test, the following method is standard in the
industry and will give you the information you need if you follow it.
Step 1 Prepare samples. (3 test, 1 control)
Step 2 Take initial readings.
Step 3 Put test samples in the freezer for 24 hours
Step 4 Remove samples and allow to thaw at room temperature
Step 5 - Put samples in 50C oven for 24 hours
Step 6 Remove samples & allow to equilibrate at room temperature.
Step 7 Take end of the cycle readings
You should repeat this test through 3 cycles. If done correctly it can be completed in 3 weeks.
What to look for

While the specific tests will depend on the type of formula you are testing, generally youll
want to take readings for Appearance, Odor, Viscosity and pH. Make particular note of
whether there is any separating at the top or the bottom of samples. This is the most common
form of instability.
You may also test the products for performance characteristics just to ensure that the formulas
still work as expected.
following temperatures. 4C, RT, 37C, 45C.
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