QC Information For Modified Bitumen Blends: Thermal Analysis

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

Thermal Analysis

QC Information Summary
Bitumen shingles are used as a common roofing material. Polymer
for Modified additives are frequently used to enhance the performance and durability
of the product. This application note will show the DMA response from
Bitumen Blends two shingles with different additives. Two relaxation events are observed
in both samples but at different temperatures. The position of the relaxations
will have an impact on the performance of the shingles when they are
exposed to various temperature profiles. The information from the PerkinElmer®
DMA 8000 can be used as a QC technique to quickly evaluate the properties
of the material.

Introduction
Dynamic Mechanical Analysis (DMA) is one of the most appropriate methods
to investigate relaxation events. In terms of a multi-component system
like bitumen shingles, individual relaxation events can be observed in the
sample as discrete events. The experimental procedure is relatively rapid,
allowing several samples to be analyzed in one day. This lends itself to
being a good quality control technique for this material.

DMA works by applying an oscillating force to the material and the resultant
displacement of the sample is measured. From this, the stiffness can be
determined and the modulus and tan δ can be calculated. Tan δ is the
ratio of the loss modulus to the storage modulus. By measuring the phase
lag in the displacement compared to the applied force it is possible to
determine the damping properties of the material. Tan δ is plotted against
temperature and glass transition is normally observed as a peak since the
material will absorb energy as it passes through the glass transition.
This application note will describe an experiment on two The second event in the tan δ is the response from the bulk
different modified bitumen samples both with a polymer bitumen. It could be due to the physical softening (partial
additive. The Tg of the polymer additive is clearly defined in melting) of the sample, relaxation events in the sample or,
both although at different temperatures. A broad relaxation/ more probably, a combination of the two. As tan δ gives
softening of the bulk bitumen is observed at a higher an indication of the mechanical damping properties of the
temperature. material, it is clear that from these two very different profiles
totally different practical properties will result as a function
Experimental of temperature. This is important information for these
materials as they are exposed to a variety of temperature
Thermal scan of bitumen sample.
profiles when applied to roofing structures.
The sample was mounted in the Single Cantilever Bending
clamps and cooled to -80 °C. The oven was removed and Although these experiments took 45 minutes to complete,
the sample reclamped (as the cooled material was now it is possible to increase the temperature scanning rate
glassy). The temperature was stabilized at -80 °C and the without too much impact on the peak positions. Cooling
thermal scan initiated. to -80 °C using the PerkinElmer DMA 8000 is very rapid,
taking only 2-3 minutes and uses a minimum of liquid
Equipment Experimental Conditions nitrogen (ca. 0.25 L). The rapid cooling makes this type of
experiment ideally suited to QC analysis of this product.
DMA 8000 Sample: Bitumen shingle with polymer
1L Dewar additives (a) and (b)
Geometry: Single Cantilever Bending
Dimensions: 5.5 (l) x 5.0 (w) x 4.5 (t) mm
Temperature: -80 °C to 100 °C at 2 °C/min-1
Frequency: 1.0 Hz

Results and conclusion


Figure 1 shows the thermal scan of the two bitumen samples.
From -60 °C the modulus decreases steadily over the
temperature range of these experiments. A similar response
in modulus is observed for both the bitumen samples. However,
the tan δ response shows marked difference between the
Figure 1. Thermal scan data from two bitumen samples.
two samples. Both display a Tg corresponding to the different
polymer additives at about -20 °C. As the additive is different
in each sample, both the magnitude and position of the Tg
differs.

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