DIFFERENTIAL SCANNING CALORIMETRY

DSC is a technique which is part of a group of techniques called Thermal Analysis (TA).
Thermal Analysis is based upon the detection of changes in the heat content (enthalpy) or
the specific heat of a sample with temperature. As thermal energy is supplied to the sample
its enthalpy increases and its temperature rises by an amount determined, for a given
energy input, by the specific heat of the sample. The specific heat of a material changes
slowly with temperature in a particular physical state, but alters discontinuously at a
change of state. As well as increasing the sample temperature, the supply of thermal energy
may induce physical or chemical processes in the sample, e.g. melting or decomposition,
accompanied by a change in enthalpy, the latent heat of fusion, heat of reaction etc. Such
enthalpy changes may be detected by thermal analysis and related to the processes
occurring in the sample. Thermal analysis encompasses a wide variety of techniques such
as :
• the measurement of heating curves,
• dynamic adiabatic calorimetry,
• differential thermal analysis, DTA
• differential scanning calorimetry, DSC
• thermogravimetry, TG
• thermal mechanical analysis, TMA
• dynamic mechanical thermal analysis, DMTA
Introduction
Differential scanning calorimetry is a technique we use to study what happens to polymers
when they're heated. We use it to study what we call the thermal transitions of a polymer.
And what are thermal transitions? They're the changes that take place in a polymer when
you heat it. The melting of a crystalline polymer is one example. The glass transition is also
a thermal transition.
The first step would be to heat it, obviously. And that's what we do in differential scanning
calorimetry, or DSC for short.
We heat our polymer in a device that looks something like this:
It's pretty simple, really. There are two pans. In one pan, the sample pan, you put your
polymer sample. The other one is the reference pan. You leave it empty. Each pan sits on
top of a heater. Then you tell the nifty computer to turn on the heaters. So the computer
turns on the heaters, and tells it to heat the two pans at a specific rate, usually something
like 10 oC per minute. The computer makes absolutely sure that the heating the rate stays
exactly the same throughout the experiment.
But more importantly, it makes sure that the two separate pans, with their two separate
heaters, heat at the same rate as each other.
t they will not heat at the same rate.The simple reason is that the two pans are different.
One has polymer in it, and one doesn't. The polymer sample means there is extra material
in the sample pan. Having extra material means that it will take more heat to keep the
temperature of the sample pan increasing at the same rate as the reference pan.
So the heater underneath the sample pan has to work harder than the heater underneath
the reference pan. It has to put out more heat. By measuring just how much more heat it
has to put out is what we measure in a DSC experiment.
Specifically what we do is this: We make a plot as the temperature increases. On the x-axis
we plot the temperature. On the y-axis we plot difference in heat output of the two heaters
at a given temperature.
Heat Capacity
We can learn a lot from this plot. Let's imagine we're heating a polymer. When we start
heating our two pans, the computer will plot the difference in heat output of the two
heaters against temperature. That is to say, we're plotting the heat absorbed by the
polymer against temperature. The plot will look something like this at first.
The heat flow at a given temperature can tell us something. The heat flow is going to be
shown in units of heat, q supplied per unit time, t. The heating rate is temperature increase
T per unit time, t. Got it?

Let's say now that we divide the heat flow q/t by the heating rate T/t. We end up with heat
supplied, divided by the temperature increase.

Remember from the glass transition page that when you put a certain amount of heat into
something, its temperature will go up by a certain amount, and the amount of heat it takes
to get a certain temperature increase is called the heat capacity, or Cp. We get the heat
capacity by dividing the heat supplied by the resulting temperature increase. And that's
just what we've done in that equation up there. We've figured up the heat capacity from the
DSC plot.

Differential scanning calorimetry

 Differential Scanning Calorimeter (TA Instruments Q100)

Acronym DSC

Classification Thermal analysis

Differential scanning calorimetry or DSC is a thermoanalytical technique in which the
difference in the amount of heat required to increase the temperature of a sample and reference
are measured as a function of temperature. Both the sample and reference are maintained at
nearly the same temperature throughout the experiment. Generally, the temperature program for
a DSC analysis is designed such that the sample holder temperature increases linearly as a
function of time. The reference sample should have a well-defined heat capacity over the range
of temperatures to be scanned.
The main application of DSC is in studying phase transitions, such as melting, glass transitions,
or exothermic decompositions. These transitions involve energy changes or heat capacity
changes that can be detected by DSC with great sensitivity.
The technique was developed by E.S. Watson and M.J. O'Neill in 1960[1], and introduced
commercially at the 1963 Pittsburgh Conference on Analytical Chemistry and Applied
Spectroscopy.

INSTRUMENTATION
Most DSC instruments are of the heat-flux design, a schematic of which is shown below. There is
another type of instrument, "power-compensated DSC", which is discussed in standard texts, and for
most practical purposes gives equivalent results to good heat-flux designs. The figure most closely
resembles the TA Instruments design of cell, but the features are common to most. Small, flat samples
are contained in shallow pans, with the aim of making a good thermal contact between sample, pan and
heat flux plate. Symmetrical heating of the cell, and therefore S and R, is achieved by constructing the
furnace from a metal of high thermal conductivity - silver in the case of the TA Instruments design.
Note the provision for establishing a gas flow through the cell, to sweep away volatiles, provide the
required atmosphere, and to assist in heat transfer.
The
control of
the
furnace,
signal

acquisition, and data storage and analysis are of course handled by a computer.
The primary signals from the cell are of the order of mV for the temperature, and µV for DeltaT. Low
noise high gain amplifiers are necessary to boost these signals before data logging. Reproducible
construction results on a known variation in sensitivity to heat flow with temperature, and software
correction results in an effectively constant sensitivity over the working range, which is typically up to
700°C, and down to ca. -140°C with a liquid nitrogen cooling system.
Temperature calibration is carried out by running standard materials, usually very pure metals with
accurately known melting points. Energy calibration may be carried out by using either known heats of
fusion for metals, commonly indium, or known heat capacities. Synthetic sapphire (corundum, or
aluminium oxide) is readily available as a heat capacity standard, and the values for this have been
accurately determined over a wide temperature range. The absolute accuracy for measurements of heat
capacity and transformation enthalpies are more often limited by the lack of appropriate standards, and
difficulties in assigning a baseline construction, than by limitations of the instrument itself.
A variety of sample pans can be used for different purposes. The best quantitative results for polymers
are obtained from thin samples crimped flat between the pan and a lid. Hermetically-sealed pans
capable of holding a few atmospheres pressure are used for liquids, or when it is necessary to retain
volatiles. Very high-pressure seals can be achieved using O-ring or screw-threaded seals. For materials
that react with aluminium, or for higher temperatures, pans may be made from stainless steel, inconel,
gold, alumina, graphite, silica or platinum.
Typical purge gases are air and nitrogen, though helium is useful for efficient heat transfer and removal
of volatiles. Argon is preferred as an inert purge when examining samples that can react with nitrogen.
The experiment can also be carried out under vacuum or under high pressure using instruments of the
appropriate design.
.

Figure 3.12: DSC Experimental Arrangement.

TypicalDSC Curve.
In other words, in DSC, the measuring principle is to compare the rate of heat flow to the sample and to
an inert material which are heated or cooled at the same rate. Changes in the sample that are associated
with absorption or evolution of heat cause a change in the differential heat flow which is then recorded
as a peak. The area under the peak is directly proportional to the enthalpic change and its direction
indicates whether the thermal event is endothermic or exothermic. For proteins, the thermally induced
process detectable by DSC is the structural melting or unfolding of the molecule. The transition of
protein from a native to a denatured conformation is accompanied by the rupture of inter- and intra-
molecular bonds, and the process has to occur in a cooperative manner to be discerned by DSC .
Analysis of a DSC thermogram enables the determination of two important parameters : transition
temperature peak (Tp) or maximum (Tmax) or denaturation (Td) temperature, and enthalpy of

denaturation ( ). The denaturation temperatures are measures of the thermal stability of proteins,
although they are influenced by the heating rate and protein concentration (The extrapolated onset
temperature ( Tm ) is less influenced by protein concentration and transition temperature at zero heating

rate can be obtained by plotting peak temperatures as a function of heating rate The value,
calculated from the area under the transition peak, is correlated with the content of ordered secondary

structure of a protein The value is actually a net value from a combination of endothermic
reactions, such as the disruption of hydrogen bonds determined as 1.7kcal per mole of hydrogen bond
and exothermic processes, including protein aggregation and the breakup of hydrophobic interactions

The sharpness of the transition peak can be measured as width at half-peak height ( ), and is an
index of the cooperative nature of the transition from native to denatured state. If denaturation occurs

within a narrow temperature range (a low value), the transition is considered highly cooperative
Heat denaturation of small globular proteins is generally considered reversible in high yield, provided
that the reaction is carried out under conditions preventing aggregation., i.e. dilute solution and far from
the isoelectric point. This allows indirect thermodynamic evaluation of the process by applying
equilibrium thermodynamics and assuming a two-state model, i.e. A (native) --> B (denatured). Under
these conditions one can determine the equilibrium constant, K, of the process and subsequently the

standard enthalpy change, from the van't Hoff equation:

The standard free energy change, may be obtained from :

and the standard entropy change, , form :

If , made from calorimetric studies and obtained from equilibrium studies are equivalent, it
can be deduced that the denaturation process is a two-state, all-or-none process, with minimum
intermediate states. At high protein concentrations (5-20%) and heating rates (5-20°C/min), which
resemble actual processing conditions, denaturation becomes an irreversible process since extensive
intermolecular interactions are favoured with aggregation of the unfolded protein molecules (Biliaderis,
1983). In contrast to denaturation, which is connected with intensive heat absorption, aggregation is

generally considered as an exothermic process, therefore, it becomes more difficult to interpret

values quantitatively, since they represent the net product of a positive (denaturation) and a negative
(aggregation) contributor.
Materials and Methods
Amylum SWP was hydrated in distilled water at pH 7.0 and diluted as required.
Method
Differential scanning calorimetry studies were carried out on a Setaram microcalorimeter using a
sample mass of approx. 0.92g and a scan rate of 0.5 degrees per minute.
Results
Up to 94ºC SWP remained stable with no sign of denaturation or conformational change in its tertiary
structure (Figure 3.28).
DSC thermogram of 10% SWP at a scanning rate of 0.5ºC/min at pH 7.0
Detection of phase transitions
The basic principle underlying this technique is that, when the sample undergoes a physical
transformation such as phase transitions, more or less heat will need to flow to it than the
reference to maintain both at the same temperature. Whether more or less heat must flow to the
sample depends on whether the process is exothermic or endothermic. For example, as a solid
sample melts to a liquid it will require more heat flowing to the sample to increase its
temperature at the same rate as the reference. This is due to the absorption of heat by the sample
as it undergoes the endothermic phase transition from solid to liquid. Likewise, as the sample
undergoes exothermic processes (such as crystallization) less heat is required to raise the sample
temperature. By observing the difference in heat flow between the sample and reference,
differential scanning calorimeters are able to measure the amount of heat absorbed or released
during such transitions. DSC may also be used to observe more subtle phase changes, such as
glass transitions. DSC is widely used in industrial settings as a quality control instrument due to
its applicability in evaluating sample purity and for studying polymer curing.[2][3][4]
DTA
An alternative technique, which shares much in common with DSC, is differential thermal
analysis (DTA). In this technique it is the heat flow to the sample and reference that remains the
same rather than the temperature. When the sample and reference are heated identically phase
changes and other thermal processes cause a difference in temperature between the sample and
reference. Both DSC and DTA provide similar information; DSC is the more widely used of the
two techniques.[2][3][4]
DSC curves
The result of a DSC experiment is a curve of heat flux versus temperature or versus time. There
are two different conventions: exothermic reactions in the sample shown with a positive or
negative peak; it depends on the different kind of technology used by the instrumentation to
make the experiment. This curve can be used to calculate enthalpies of transitions. This is done
by integrating the peak corresponding to a given transition. It can be shown that the enthalpy of
transition can be expressed using the following equation:
ΔH = KA
where ΔH is the enthalpy of transition, K is the calorimetric constant, and A is the area under the
curve. The calorimetric constant will vary from instrument to instrument, and can be determined
by analyzing a well-characterized sample with known enthalpies of transition.[3]

Applications of Differential Scanning

Calorimetry

The Glass Transition Temperature

Of course, we can learn a lot more than just a polymer's heat capacity with DSC. Let's see
what happens when we heat the polymer a little more. After a certain temperature, our plot
will shift upward suddenly, like this:
This means we're now getting more heat flow. This means we've also got an increase in the
heat capacity of our polymer. This happens because the polymer has just gone through the
glass transition. And as you learned on the glass transition page, polymers have a higher
heat capacity above the glass transition temperature than they do below it. Because of this
change in heat capacity that occurs at the glass transition, we can use DSC to measure a
polymer's glass transition temperature. You may notice that the change doesn't occur
suddenly, but takes place over a temperature range. This makes picking one discreet Tg
kind of tricky, but we usually just take the middle of the incline to be the Tg.

Crystallization
But wait there is more, so much more. Above the glass transition, the
polymers have a lot of mobility. They wiggle and squirm, and never stay in
one position for very long. They're kind of like passengers trying to get
comfortable in airline seats, and never quite succeeding, because they can
move around more. When they reach the right temperature, they will have
gained enough energy to move into very ordered arrangements, which we
call crystals, of course.

When polymers fall into these crystalline arrangements, they give off heat. When this heat
is dumped out, it makes the little computer-controlled heater under the sample pan really
happy. It's happy because it doesn't have to put out much heat to keep the temperature of
the sample pan rising. You can see this drop in the heat flow as a big dip in the plot of heat
flow versus temperature:
This dip tells us a lot of things. The temperature at the lowest point of the dip is usually
considered to be the polymer's crystallization temperature, or Tc. Also, we can measure the
area of the dip, and that will tell us the latent energy of crystallization for the polymer. But
most importantly, this dip tells us that the polymer can in fact crystallize. If you analyzed a
100% amorphous polymer, like atactic polystyrene, you wouldn't get one of these dips,
because such materials don't crystallize.
Also, because the polymer gives off heat when it crystallizes, we call crystallization an
exothermic transition.
Melting
Heat may allow crystals to form in a polymer, but too much of it can be
their undoing. If we keep heating our polymer past its Tc, eventually we'll
reach another thermal transition, one called melting. When we reach the
polymer's melting temperature, or Tm, those polymer crystals begin to fall
apart, that is they melt. The chains come out of their ordered
arrangements, and begin to move around freely. And in case you were
wondering, we can spot this happening on a DSC plot.

Remember that heat that the polymer gave off when it crystallized? Well when we reach
the Tm, it's payback time. There is a latent heat of melting as well as a latent heat of
crystallization. When the polymer crystals melt, they must absorb heat in order to do so.
Remember melting is a first order transition. This means that when you reach the melting
temperature, the polymer's temperature won't rise until all the crystals have melted. This
means that the little heater under the sample pan is going to have to put a lot of heat into
the polymer in order to both melt the crystals and keep the temperature rising at the same
rate as that of the reference pan. This extra heat flow during melting shows up as a big
peak on our DSC plot, like this:
We can measure the latent heat of melting by measuring the area of this peak. And of
course, we usually take the temperature at the top of the peak to be the polymer's melting
temperature, Tm. Because we have to add energy to the polymer to make it melt, we call
melting an endothermic transition.
Putting It All Together
So let's review now: we saw a step in the plot when the polymer was
heated past its glass transition temperature. Then we saw a big dip when
the polymer reached its crystallization temperature. Then finally we saw a
big peak when the polymer reached its melting temperature. To put them
all together, a whole plot will often look something like this:
Of course, not everything you see here will be on every DSC plot. The
crystallization dip and the melting peak will only show up for polymers
that can form crystals. Completely amorphous polymers won't show any
crystallization, or any melting either. But polymers with both crystalline
and amorphous domains, will show all the features you see above.

If you look at the DSC plot you can see a big difference between the glass transition and the
other two thermal transitions, crystallization and melting. For the glass transition, there is
no dip, and there's no peak, either. This is because there is no latent heat given off, or
absorbed, by the polymer during the glass transition. Both melting and crystallization
involve giving off or absorbing heat. The only thing we do see at the glass transition
temperature is a change in the heat capacity of the polymer.
Because there is a change in heat capacity, but there is no latent heat involved with the
glass transition, we call the glass transition a second order transition. Transitions like
melting and crystallization, which do have latent heats, are called first order transitions.
Measurement of crystallinity of polymers
DSC can also tell us how much of a polymer is crystalline and how much is
amorphous. If you read the page dealing with polymer crystallinity, you
know that many polymers contain both amorphous and crystalline
material. But how much of each? DSC can tell us. If we know the latent
heat of melting, ΔHm, we can figure out the answer.

The first thing we have to do is measure the area of that big peak we have for the melting of
the polymer. Now our plot is a plot of heat flow per gram of material, versus temperature.
Heat flow is heat given off per second, so the area of the peak is given is units of heat x
temperature x time-1 x mass-1. We usually would put this in units such as joules x kelvins x
(seconds)-1 x (grams)-1:

Got that? Don't worry. It gets simpler. We usually divide the area by the
heating rate of our dsc experiment. The heating rate is in units of K/s. So
the expression becomes simpler:
Now we have a number of joules per gram. But because we know the mass
of the sample, we can make it simpler. We just multiply this by the mass of
the sample:

Now we just calculated the total heat given off when the polymer melted.
Neat, huh? Now if we do the same calculation for our dip that we got on
the DSC plot for the crystallization of the polymer, we can get the total
heat absorbed during the crystallization. We'll call the heat total heat
given off during melting Hm, total, and we'll call the heat of the
crystallization Hc, total.

Now we're going to subtract the two:

Why did we just do that? And what does that number H' mean? H' is the
heat given off by that part of the polymer sample which was already in the
crystalline state before we heated the polymer above the Tc. We want to
know how much of the polymer was crystalline before we induced more of
it to become crystalline. That's why we subtract the heat given off at
crystallization. Is everyone following me?

Now with our magic number H' we can figure up the percent crystallinity. We're going to
divide it by the specific heat of melting, Hc*. The specific heat of melting? That's the
amount of heat given off by a certain amount, usually one gram, of a polymer. H' is in
joules, and the specific heat of melting is usually given in joules per gram, so we're going to
get an answer in grams, which we'll call mc.

This is the total amount of grams of polymer that were crystalline below
the Tc. Now if we divide this number by the weight of our sample, mtotal, we
get the fraction of the sample that was crystalline, and then of course, the
percent crystallinity:
And that's how we use DSC to get percent crystallinity.

Properties of sample
Differential scanning calorimetry can be used to measure a number of characteristic properties of
a sample. Using this technique it is possible to observe fusion and crystallization events as well
as glass transition temperatures (Tg). DSC can also be used to study oxidation, as well as other
chemical reactions.[5][2][3][4]
Glass transitions may occur as the temperature of an amorphous solid is increased. These
transitions appear as a step in the baseline of the recorded DSC signal. This is due to the sample
undergoing a change in heat capacity; no formal phase change occurs.[2][4]
As the temperature increases, an amorphous solid will become less viscous. At some point the
molecules may obtain enough freedom of motion to spontaneously arrange themselves into a
crystalline form. This is known as the crystallization temperature (Tc). This transition from
amorphous solid to crystalline solid is an exothermic process, and results in a peak in the DSC
signal. As the temperature increases the sample eventually reaches its melting temperature (Tm).
The melting process results in an endothermic peak in the DSC curve. The ability to determine
transition temperatures

DSC is the most widely used of all thermoanalytical techniques. It is used primarily to
characterize polymers and organic materials, as well as metals, ceramics, and composites.

Basically the DSC measurement is a function of differential heat flow with temperature for
compounds that exhibit thermal transitions. These transitions are typically melting,
crystallization, and the glass transition, Tg.. Such measurements provide quantitative and
qualitative information about physical and chemical changes that involve endothermic or
exothermic processes.

Examples

Detection of Polymorph

The figure to the right is an example of a low temperature DSC scan on a newly synthesized
polymer containing carbon, silicon, and oxygen. The glass transition occurs between –130° and –
123°C, followed by an exotherm that is thermally-induced crystallization. The crystalline
polymer component is stable up to -50°C,
where it then melts in a bi-phasic pattern.
The detection of this behavior via DSC was
the first evidence that the polymer
exhibited two distinct crystalline forms.

Crystallization and
Supercooling
Accurate recordings of crystallization of a
polymer from the melt were desired for an
injection-molding application. Previous
experience with the polymer showed a tendency to supercool in an unpredictable manner. DSC
pans were surfaced etched to provide nucleation sites for crystallization. Subsequent experiments
carried out in a programmed heat-cool mode showed conclusively that this phenomenon could be
controlled with minimal supercooling.

Differential Scanning Calorimetry (DSC) is a thermal analysis technique used to measure

changes in heat flows associated with material transitions. DSC measurements provide
both qualitative and quantitative data on endothermic (heat absorbing) and exothermic
(heat evolving) processes. DSC is commonly used to determine the glass transition
temperature and crystalline melting point of polymeric materials.

A simplified explanation of a DSC sample evaluation may be described as follows. A

material specimen is weighed and placed into a DSC sample pan. The sample pan and an
empty reference pan are placed within the DSC apparatus. The DSC cell is heated or
cooled at some controlled rate while continuously monitoring the differential heat flow
between the sample and reference pans. The heat flow profile so obtained during the
DSC heating or cooling run is subsequently analyzed for any of several endothermic
and/or exothermic transitions.

Examples
• The DSC technique can be used to
make qualitative statements about
whether or not polymer blend
 systems are miscible or immiscible, provided the inherent homopolymer
transition temperatures of the blend components are sufficiently well separated. A
description of the glass transition temperature characteristics of two different
polymer blend systems evaluated by DSC will illustrate this point. Polymer
blends based on polystyrene (Tg = 100°C) and poly(dimethylphenylene oxide)
(Tg = 210°C) are miscible in all proportions. DSC thermal profiles of various
PS/PDMPO blend compositions show only a single glass transition temperature,
located somewhere between 100°C and 210°C, dependent upon the relative
weight fractions of the homopolymer components within the blend. In contrast,
polymer blends based on polystyrene and polyisoprene (Tg = -70°C) are
immiscible. PS/PI blends exhibit distinct phase separated domains and show two
characteristic glass transition temperatures in the same temperature ranges as
their respective homopolymer blend components. In summary, polymer blend
systems which show two Tgs by DSC are recognized as being immiscible; those
which show only a single Tg may or may not be miscible.
• TeflonTM samples are manufactured using different processing conditions, which
directly influence the extent of crystallinity in the finished parts. Using the heat of
fusion of an ideal, 100% crystalline sample, the percent crystallinity of
manufactured samples may be determined by DSC. Specifically, a TeflonTM
sample was heated in a DSC cell and showed a characteristic endothermic
melting peak. The peak area was normalized and integrated to quantify the
experimental heat associated with the crystalline melting process. By comparing
the experimental heat value to that of a theoretical, 100% crystalline sample, the
percent crystallinity of the sample was determined.
Examples
The technique is widely used across a range of applications, both as a routine quality test and as
a research tool. The equipment is easy to calibrate, using low melting indium for example, and is
a rapid and reliable method of thermal analysis.
Liquid crystals
DSC is used in the study of liquid crystals. As some forms of matter go from solid to liquid they
go through a third state, which displays properties of both phases. This anisotropic liquid is
known as a liquid crystalline or mesomorphous state. Using DSC, it is possible to observe the
small energy changes that occur as matter transitions from a solid to a liquid crystal and from a
liquid crystal to an isotropic liquid.[3]

Oxidative stability
Using differential scanning calorimetry to study the stability to oxidation of samples generally
requires an airtight sample chamber. Usually, such tests are done isothermally (at constant
temperature) by changing the atmosphere of the sample. First, the sample is brought to the
desired test temperature under an inert atmosphere, usually nitrogen. Then, oxygen is added to
the system. Any oxidation that occurs is observed as a deviation in the baseline. Such analysis
can be used to determine the stability and optimum storage conditions for a material or
compound.[2]
Safety Screening
DSC makes a reasonable initial safety screening tool. In this mode the sample will be housed in a
non-reactive crucible (often Gold, or Gold plated steel), and which will be able to withstand
pressure (typically up to 100 bar). The presence of an exothermic event can then be used to
assess the stability of a substance to heat. However, due to a combination of relatively poor
sensitivity, slower than normal scan rates (typically 2-3°/min - due to much heavier crucible) and
unknown activation energy, it is necessary to deduct about 75-100°C from the initial start of the
observed exotherm to suggest a maximum temperature for the material. A much more accurate
data set can be obtained from an adiabatic calorimeter, but such a test may take 2-3 days from
ambient at a rate of a 3°C increment per half hour.
Drug analysis
DSC is widely used in the pharmaceutical and polymer industries. For the polymer chemist, DSC
is a handy tool for studying curing processes, which allows the fine tuning of polymer properties.
The cross-linking of polymer molecules that occurs in the curing process is exothermic, resulting
in a positive peak in the DSC curve that usually appears soon after the glass transition.[2][3][4]
In the pharmaceutical industry it is necessary to have well-characterized drug compounds in
order to define processing parameters. For instance, if it is necessary to deliver a drug in the
amorphous form, it is desirable to process the drug at temperatures below those at which
crystallization can occur.[3]
General chemical analysis
Freezing-point depression can also be used as a purity analysis tool when analysed by
Differential scanning calorimetry.[6] The results obtained are in mol%, but the method has its
place, where other methods of analysis fail.
Food science
In food science research, DSC is used in conjunction with other thermal analytical techniques to
determine water dynamics. Changes in water distribution may be correlated with changes in
texture. Similar to material science studies, the effects of curing on confectionery products can
also be analyzed.
Polymers
DSC is used widely for examining polymers to check their composition. Melting points and glass
transition temperatures for most polymers are available from standard compilations, and the
method can show up possible polymer degradation by the lowering of the expected melting
point, Tm, for example. Tm depends on the molecular weight of the polymer, so lower grades will
have lower melting points than expected. It may also be used to evaluate drug and polymer
purities. This is possible because the temperature range over which a mixture of compounds
melts is dependent on their relative amounts. This effect is due to a phenomenon known as
freezing point depression, which occurs when a foreign solute is added to a solution. (Freezing
point depression is what allows salt to de-ice sidewalks and antifreeze to keep your car running
in the winter.) Consequently, less pure compounds will exhibit a broadened melting peak that
begins at lower temperature than a pure compound.[3][4]
Metals
In the last few years this technology has been involved in metallic material study. The
characterization of this kind of material with DSC is not easy yet because of the low quantity of
literature about it. It is known that it is possible to use DSC to find solidus and liquidus
temperature of a metal alloy, but the widest application is, by now, the study of precipitations,
Guiner Preston zones, phase transitions, dislocations movement, grain growth etc.The DSC can
also be used to find out the percentage crystallinity of the sample using the heat absorbed by the
sample .