a p p l i c at i o n N o t e

Thermal Analysis

Authors
Peng Ye
Boon-Chun Tan
PerkinElmer, Inc.
Shelton, CT USA

How to Optimize Introduction

OIT is the abbreviation for oxidative induction
OIT Tests? time. It provides information about the oxidative
stability of mainly polymer materials. This
information is important because plastic parts
age throughout their lifetime due to exposure to
environmental elements such as heat, oxygen, light and radiation. Aging causes
the degradation of the physical properties of the polymers and will lead to their
failure. Antioxidants are often added during the plastics formulation to hinder
the aging caused by oxygen and to increase their lifetime. Because the reaction
between polymers and oxygen (O2) is exothermic, OIT determination using
Differential Scanning Calorimetry (DSC) is an ideal solution to study this process.

In the OIT test method, the test specimen is heated to a specific temperature
in an open pan under an inert atmosphere. After a short period of time, at the
isothermal temperature, the gas is switched from inert purge to O2, or air purge.
The time taken from the O2 gas switching to the onset of oxidation reaction
is defined as OIT. OIT is an accelerated test used as a qualitative evaluation
of the oxidative stability of a material. This time can be used as criteria of the
thermal stability of polyolefins in an oxidative atmosphere. The OIT method is
standardized in ASTM® D 3895 and DIN EN 728 for polyolefins. The OIT test is of
great interest to companies who produce or utilize polyolefins, which are used at
elevated temperatures under an oxygen atmosphere such as tubes or pipelines,
cable or wire insulation, geomembranes or vapor-barrier-films. It can be used
to compare the aging resistance of different plastics, to detect the impact of
antioxidant concentration and to assess the effectiveness of antioxidants.
 In this application note, we will review several influential location on the part also has an impact on the OIT result
factors for the OIT method. They are: because various locations of the sample may have different
• Isothermal measurement temperature concentrations of antioxidant additives. For example, in the
case of a water pipe, the sample taken from the outside of
• Sample selection the pipe may have a lower OIT than the sample taken from
• Sample geometry the center of the pipe because the antioxidant additive at
the surface can be extracted by water.
• Pan material

The data was generated on the PerkinElmer® Jade DSC. The Sample geometry
Jade DSC has been designed to be both rugged and reliable. Sample geometry is another important influential factor in
The system utilizes a precisely-machined disc of hardened OIT measurements. Since oxidation happens between sample
nickel chromium and a low-mass aluminum coated furnace and oxygen, the surface area relative to the sample volume
to give the instrument high resistance against contamination is important. Different sample geometries have different
or aggressive gases, and to provide accurate, reproducible surface-to-volume ratios. Figure 3 illustrates the effect of
results. The integrated gas flow control and switching device sample geometry on the onset time and rate of oxidation.
assures high stability and best control over purge gases. In this example, the standard sample was a compact disk.

Figure 1. DSC 6000.

Experiments and discussions

Figure 2. Influence of isothermal temperature on OIT for LLDPE.
Isothermal temperature
The crucial parameter in OIT determination is the isothermal
temperature. This temperature is usually above the melting
temperature for crystalline polymers. Low temperature will
make the experiment too long and may not be acceptable
economically, while high temperature can cause fast oxidation
and lead to poor reproducibility and resolution. As shown in
Figure 2, increasing the isothermal temperature from 205 °C
to 215 °C resulted in decreased OIT. Usually an OIT between
5 and 60 minutes is desired. So in this case, isothermal
measurements at 205 °C are the preferred choice.

Sample selection
For sample selection, the storage time (the time interval
between when the part is made and when the actual
OIT measurement takes place) should be taken into Figure 3. The effect of sample geometry on OIT measurement of LLDPE at
consideration because the oxidation starts as soon as the 205 °C.
plastic part is manufactured. The antioxidant additive may
be consumed during processing and storage, which can lead
to a lower OIT compared with a virgin part. The sampling

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The thin disk and small pieces had the same mass as the In the calculation window you can find the analysis for OIT
standard sample. The thick disk mass was about 3 times that (Figure 5). The standard package of the PerkinElmer Pyris
of the standard sample. To ensure a good measurement of software also includes the Pyris Player. The Player software
onset oxidation time, the thin disk is preferred because of is useful in many cases. It allows you to automate the
its good contact with the sample pan and its large surface work routine. Not only can this software be used with an
area relative to the volume. The thick disk has a smaller autosampler, this package offers the user to option to set up
surface-to-volume ratio and less sharp onset than a thin a sequence that will automatically calculate the OIT at the
disk. The small pieces sample has a very large surface-to- end of a single sample run.
volume ratio, however the thermal contact with the pan and
the heat transfer within the sample is poor. In addition, the
surface-to-volume ratio of small pieces is very irreproducible.
In order to get highly reproducible results for OIT tests, a
constant and thin disk sample geometry is favorable.

Pan material
The curves in Figure 4 show a big difference in the stability
of the sample with respect to the pan material. The sample
with the copper pan has a significantly lower OIT than
the sample with the aluminum pan. The reason for this is
because copper catalyzes the oxidation reaction. In some
application areas this must be taken into account. When
products come in contact with copper during their usage it
is obvious that their lifetime decreases. This is very important Figure 5. The OIT calculation window in the Pyris software.
for the cable industry.
Another valuable feature is the tolerance test. The customer
determines the criteria for pass or failure of the test. The
OIT criterion can be within a range, greater than or less than
a defined value. When using an autosampler the customer
can specify the action upon failure. The action can be to
either stop, continue, skip to the next sample or block the
sequence.

One final example of OIT application is given in Figure 6. It

is the measurement of a HDPE pipe piece. The temperature
was ramped from 30 °C to 200 °C at 20 °C/minute and held
isothermally. The gas switched from N2 to O2 at 2 minutes
on the isothermal hold. The onset, at about 95 minutes,
defines the time interval from time zero (switch to O2) to the
onset of the oxidation reaction. The tolerance test feature
Figure 4. The influence of sample pan material.
confirms that this material passed the test.

Data analysis
The OIT determination with Pyris™ software is easy and
offers many beneficial features. The user can select criteria
in the method set-up for the OIT measurement that, for
example, stops the measurement after the start of the
oxidation, but before the sample completely decomposes.

Figure 6. OIT test for HDPE pipe.

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Summary
In order to get good, reproducible OIT data, you need to
assure a:
• Stable isothermal temperature
• Constant sample morphology, geometry and weight
• Reliable and consistent purge gas flow rate
• Similar pan material is used

The Jade DSC with integrated mass flow controller and Pyris
software is a great combination to perform OIT tests. It is an
ideal, cost-effective solution for reliable tests in QA/QC labs
or as part of product development.

Reference
Gottfried W. Ehrenstein, Gabriela Riedel and Pia Trawiel,
Thermal Analysis of Plastics, 2004.

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