1

Differential Scanning
Calorimetry (DSC)

Submitted to: Respected Teacher

Assistant Professor Muhammad Zohaib Rafay

Submitted by: Mariyam Khalid Roll no. 02

Soha Hasnain Roll no. 14 2
 Contents

• Historical Background
• Introduction
• Principle
• Technique or Working
• Instrumentation of DSC
• Types of DSC
• Sample preparation
• DSC Experiment
• DSC Calibration
• DSC Curve or Thermogram
• Factors affecting DSC curve
• Phase transitions
• Applications of DSC 3
 Historical Background

• This technique was developed by E.S. Watson & M.J.O. Neill in 1962, but it
was first introduced commercially in 1963 in Pittsburgh conference on
Analytical chemistry & Applied spectroscopy.

• 1st DSC that could be used in biochemistry was developed by P.L. Peivalor
and D.R. Moraselidze in 1964.

Pans of DSC DSC instrument

4
 Introduction
Calorimeter:
• A calorimeter measures the heat into or out of a sample.

Differential calorimeter:
• A differential calorimeter measures the heat of a sample relative to a reference.

Differential scanning calorimeter:

• A differential scanning calorimeter measures the heat of sample relative to
reference with a linear temperature.

Definition:
• “Differential Scanning Calorimetery or DSC is a thermo-analytical technique which
measures the difference in heat flow rate between a sample and inert reference
as a function of time and temperature. Both the sample and reference are
maintained at same temperature throughout the experiment.”
5
Features of DSC:

• Differential scanning calorimetry (DSC) is the most often used thermal

analysis method, primarily because of its speed, simplicity, and availability.
Its features are:

1. It is a relatively fast technique with most analyses taking less than thirty
minutes.
2. Sample preparation is easy. Solids, liquids, powders, films and fibers of
essentially any shape are encapsulated in metal pans and placed into a
temperature and atmosphere-controlled environment where the
measurement occurs.
3. The wide temperature operational range of -180 to 725oC permits the
analysis of transitions in a broad range of materials.
4. Sophisticated, easy to use software permits a quantitative analysis of
transitions as a function of temperature and time.

6
 Principle
• The sample and the reference materials are heated separately.

• The sample and the reference temperatures are monitored separately and
continuously maintained at same level.

• When the sample absorbs heat during endothermic process, more power is
required by the sample to allow it to be maintained at the same
temperature as the reference.

• Similarly, when the sample evolves heat during exothermic process, less
power is required by the sample to allow it to be maintained at the same
temperature as the reference.

• This deferential power is recorded as a function of temperature and the

peak area represents the energy of the transition.
7
• A characteristic DSC curve or a thermogram is plotted between heat flow (Cal.
Or J sec-1) and temperature (K) and is shown:

• A thermogram is a record made by varying temperature over a period of time.

Temperature is taken on x-axis and Heat flow is taken on y-axis. In this
particular thermogram, the peak and dip shows change in heat flow at a
particular temperature and represents a phase transition:

8
DSC Thermogram
 Technique or Working

• Differential Scanning Calorimetry (DSC) measures the temperature and

heat flow associated with transitions in materials as a function of time and
temperature in a controlled atmosphere.

• These measurements provide quantitative and qualitative information

about physical and chemical changes that involve endothermic or
exothermic processes, or changes in heat capacity.

The changes that take place on heating are:

• Melting
• Glass transition
• Crystallization

9
 Instrumentation of DSC
• DSC is used to study the thermal transitions of polymer sample. The
polymer is heated in a device that looks something like this;

OR

10
1. Two pans or crucibles:
• There are two pans in the DSC machine;
i. Reference pan: The reference pan is usually an empty pan or filled with
inert material and cover. The inert material used are alumina (Al2O3) and silica
(SiO2).
ii. Sample pan: The pan with sample polymer is sample pan. The sample is
sealed into a small pan. The pans hold up to about 10 mg of material.
• Both pans are made up of platinum or aluminum to allow high
temperature operation.

2. Sensors:
• Isothermal conditions TS = TR are obtained by placing a platinum resistance
thermometer in the sample with an identical sensor in the reference
holder.

Platinum resistance thermometer:

A platinum resistance thermometer (PRT) is a device which determines the temperature by
measuring the electrical resistance of a piece of pure platinum wire. The piece of platinum wire
11
is referred to as a temperature sensor.
3. Heater:
• Each pan sits on heaters which are controlled by a computer.

4. Computer:
• Computer turns on heater and let them heat the two pans at a specific rate,
that is; usually 10oC per minute. Computer make absolutely sure that
heating rate stays exactly the same throughout the experiment.

5. Flow of Purge gas:

• A flow of purge gas usually nitrogen gas is maintained over the sample to
create a reproducible and dry atmosphere. The nitrogen atmosphere also
eliminates air oxidation of the samples at high temperatures. Helium gas
can also be used.

12
 Working of DSC

Note:
13
• The triangles are amplifiers that determine the difference between the two input signals.
 Types of DSC
• There are three types of DSC instruments:
1. Power-compensated DSC.
2. Heat-flux DSC.
3. Modulated DSC.

[1]. Power-compensated DSC:

• Two independent heating units are employed. Separate sensors for
reference and sample pan is used. Similarly, both the sample and reference
pan have separate furnace block.

• The sample and reference holders have separate platinum resistance

thermometers to continuously monitor the temperature of the materials.

• Both sample and reference are maintained at the programmed

temperature by applying power to the sample and reference heaters. 14
• The instrument records the power difference needed to maintain the sample and
reference at the same temperature as a function of the programmed temperature.

• Power-compensated DSC has lower sensitivity than heat-flux DSC, but its response
time is more rapid. This makes power-compensated DSC well suited for kinetics
studies in which fast equilibrations to new temperature settings are needed.
Power-compensated DSC is also capable of higher resolution than heat-flux DSC.

15
Power Compensated DSC
[2]. Heat Flux DSC:

• In heat flux DSC, sample holders are connected to single heat flow path.
Thermocouple sensors are used. Both the sample and reference pan have the
same furnace as a heating source.

• Heat flows into both the sample and reference material via an electrically heated
constantan thermoelectric disk. Small aluminum sample and reference pans sit on
raised platforms on the constantan disk.

• Heat is transferred through the disks and up into the material via the two pans.

• The differential heat flow to the sample and reference is monitored by Chromel-
constantan area thermocouples formed by the junction between the constantan
platform and Chromel disks attached to the underside of the platforms.

• The sample temperature is estimated by the Chromel-constantan junction under

the sample disk.

• An inert gas is passed through the cell at a constant flow rate of about 40 ml/min.
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 Heat-flux DSC

Constantan:
• It usually consists of 55% copper and 45% nickel.
Chromel:
• It is an alloy made of approximately 90% nickel and 10% chromium.
Thermocuple sensors:
A Thermocouple is a sensor used to measure temperature. Thermocouples consist of two wire
legs made from different metals. The wires legs are welded together at one end, creating a
junction. This junction is where the temperature is measured. When the junction experiences a
change in temperature, a voltage is created. The voltage can then be interpreted using 17
thermocouple reference tables to calculate the temperature.
[3]. Modulated DSC:
• Modulated DSC is a new technique introduced by Gill in 1993 which has been
thoroughly examined and discussed by Hohne in 1999. The heating rate of MDSC is
1-2 K/min (-272.1 to -271.1oC). So it has high resolution as compared to normal DSC
(resolution increases by decreasing temperature).

• The main advantage of this technique is the separation of overlapping events in

the DSC scan. In conventional DSC a constant linear heating or cooling rate is
applied.

• The operating principle of MDSC differs from standard DSC in that MDSC uses two
simultaneous heating rates - a linear heating rate that provides information similar
to standard DSC, and a sinusoidal or modulated heating rate that permits the
simultaneous measurement of the sample's heat capacity.

• In MDSC, a sinusoidal function is superimposed on the overall temperature

program to produce a micro heating and cooling cycle as the overall temperature is
steadily increased or decreased.
• This is shown in the figure:

• Using Fourier transform methods, the overall signal is mathematically

deconvoluted into two parts, a reversing heat flow signal and a non-reversing heat
flow signal.
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Thermogram of MDSC showing two heating rates- Linear heating rate and sinusoidal
or modulate heating rate.

Derivative of Linear heating

rate

Derivative of modulated
heating rate

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The reversing heat flow signal is associated with the pure thermodynamic component:
• Heat capacity
• Glass transitions temperature Note:
Resolution is the ability to
• Melting point separate close-lying effects.

The non reversing heat flow is related to kinetic processes.

• Crystallization
• Dehydration/Oxidation
• Evaporation.

• A plot showing the decomposition of the total heat flow signal into reversing and non-
reversing components is shown.

• Note that the transition near 60°C appears in the reversing heat flow component
associated with the heat capacity part of the total heat flow. The endothermic process
near 250°C also appears in the reversing component, and the exothermic event near
150oC appears in the non-reversing component.

Fourier transform:
Fourier transforms (FT) take a signal and express it in terms of the frequencies of the waves that
20
make up that signal. A complicated signal can be broken down into simple waves.
 Crystal
Crystallization
Perfection

Glass
Transition

Melting

MDSC
thermogram

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 For Your Concept
Resolution Sensitivity

Definition Resolution is the ability to Sensitivity is the ability to

separate close-lying effects. reliably detect weak effects.

How to improve • Use lower heating rates. • Use higher heating rate.
• Use lighter crucibles. • Use a larger sample mass.
• Use a smaller sample mass.
• Improve the contact
between the sample and
crucible.

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 Heat Flow in DSC

• In DSC, we can write the total heat flow dH/dt as:

Where;
• H is the enthalpy in J mol-1
• Cp is the specific heat capacity (heat capacity per mole) in J K -1 mol-1
• and f (T, t) is the kinetic response of the sample in J mol –1
• T is temperature (K)
• t is time (sec)

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 Sample Preparation
1. Selection of Sample size:
• The recommended sample amounts for DSC
measurements are:

2. Selection of crucible or pan:

• The reference crucible or pan should be of the same type as the sample crucible or pan.
• Crucible requirements:
1. The crucible material must be inert and not show any effects in the measured
temperature range.
2. The melting point of the crucible must be higher than the effects that you want to
observe in the sample.
3. Crucibles must be inert to the sample and its end products in the applied temperature
range

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Al Pt alumina Ni Cu quartz
3. Filling of crucible or pan:
• The best way to insert different types of samples into DSC crucibles
are:

Filling of powder

Filling of liquid
4. Weighing of Sample and reference crucible or pan:
•Accurately weigh the sample. The sample is weighed in a Micro
Balance.

•Measurements of sample pan or crucible is taken as compared to

the reference crucible. For good measurement result, the crucible
and lid combination weighed with sample and reference should not
differ more than 0.2 mg.
Weighing of
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sample
4. Sealing of crucible or pan:

• After weighing, sample pan is sealed by crucible

sealing press.

Important precautionary measures:

• For performing measurements above 150 °C, make
sure to punch a small hole in the crucible lid to prevent
the crucible from exploding due to sample
evaporation.

Sealing of pan
• The bottom of the crucible should remain flat when
the crucible is sealed in the crucible press (do not
overfill). A flat bottom guarantees good thermal
contact between the crucible and the sensor and
results in an optimum signal.

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 DSC Experiment
• A typical DSC experiment begins by weighing an empty sample pan. The pans are
most often made of aluminum, although gold, stainless steel, and glass ampoules
can be used. Hermetic pans are often used.

• A small portion of the sample is then transferred to the pan so as to provide a

uniform layer at the bottom of the pan. The pan is hermetically sealed and then
weighed again. When the sample and reference pans are in position, the purge gas
is applied.

• Some DSC units have auto-samplers that allow multiple sample pans placed in a
holder to be run sequentially.

• Helium or nitrogen is the usual purge gas, although occasionally air or oxygen is
employed to study oxidation processes. The purge gas helps to rid the sample of
moisture and oxygen and aids in transferring heat to the sample pan.

• Modern DSC instruments are computer controlled so that the experiment is

performed automatically after the user enters parameters such as the temperature
program and various calibration parameters. 27
 DSC Calibration

Baseline calibration:
• Baseline calibration is done for the evaluation of the thermal resistance of sample
and reference sensors.
• The DSC system is usually calibrated in several ways. Baseline calibration is
performed with no pans in place. The temperature difference of two empty
cubicles is measured.

• The calibration measures the baseline

slope and offset over the temperature
range of interest.
• The computer system controlling the
DSC, stores these values and subtracts
baseline slope and offset from
subsequent sample runs to minimize
their effects.

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Heat flow calibration:
• After baseline calibration is performed, heat flow calibration is done by melting a
known quantity of a material with a well-known heat of fusion. Indium is the most
often used standard. Indium is placed in the sample pan and scanned against an
empty reference pan. The area of the melting peak or heat of fusion in related to
the reference value. If the values lie within the allowed limits, then the message
‘The DSC module is within specifications’ is displayed. The instrument displays the
appropriate message if an adjustment of the instrument is required.

• This procedure also

calibrates the
temperature axis from
the known melting
temperature of indium.

• Temperature calibration
should also be performed
over a wider temperature
range, by measuring the
melting points of several
well-known standards.
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Heat capacity calibration:
• Heat capacity calibration is performed by scanning a heat capacity
standard, such as sapphire with a known heat capacity at a specific
temperature of interest. Calibration is typically done at a heating or
cooling rate of 10 to 20 °C/min. The heat capacity is measured and
compared with the known heat capacity value of sapphire. This
calibrates the system for Cp values and is used in separating the heat
capacity component from the total heat flow.

Characteristics of Calibrants:
• High purity
• Accurately known enthalpies
• Thermally stable
• Light stable
• Non-hygroscopic
• Un-reactive (pan, atmosphere) 30
 DSC Curve or Thermogram
• The result of DSC experiment is a curve or thermogram of heat flux
(differential heat flow) verses temperature or time. The curve can be used
to calculate the enthalpy of transitions. This is done by evaluating peak
corresponding to each transition. Enthalpy of transition can be expressed
by following equation;
∆𝐻 = 𝐾𝐴
Where,
• ∆H = Enthalpy of transition
• K = Calorimetric constant
• A = Area of Curve

• Calorimetric constant (K) varies from instrument to instrument. Area under

the peak is directly proportional to heat absorbed or evolved by reaction.

• While, Height of the peak is directly proportional to rate of reaction.

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• The DSC curves are;

• Typical DSC curves A showing exothermic peak and B showing endothermic peak.

• The deviation observed above the base (zero) line is called exothermic transition and
below is called endothermic transition. The area under the peak is directly
proportional to the heat evolved or absorbed by the reaction, and the height of the
curve is directly proportional to the rate of reaction.
For your concept:
• Which way do you plot your DSC thermograph of the heat flow signal? Do you plot “exo
up” or “exo down?
• There are two conventions:
1. If we were used to DSC instrument of power compensation design, we are most likely
to see our DSC plot as “exo down”.
2. If we were to use DSC instrument designed with heat flux principal, however, we are
more likely to see our DSC thermographs plotted as “exo up”. 32
 Factors affecting DSC Curve
• 2 types of factors affects DSC curves majorly;
[A]. Instrumental factors
[B]. Sample characteristics

[A]. Instrumental factors:

• The instrumental factors includes;
1. Composition of sample containers
2. Sensitivity of recording system
3. Recording speed
4. Furnace heating rate
5. Heating rates of pan
[B]. Sample characteristics:
• The sample factors includes;
1. Amount of sample
2. Nature of sample
3. Particle size
4. Heat of reaction
5. Thermal conductivity
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 Phase Transitions

• During a DSC experiment, sample goes through many phase

transitions. Each phase transition is represented by its peak or dip in
the thermogram.

• These phase transitions are:

1. Heat Capacity
2. Glass Transition
3. Crystallization
4. Melting

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[1]. Heat capacity:
• “When a certain amount of heat is transferred to the sample, its
temperature increases by a certain amount, and the amount of heat it
takes to get a certain increase in temperature is called the heat capacity”.

• It is denoted by Cp and is measured in J/ mole.

Complete Thermogram of DSC 35

Determination of Heat Capacity:

• DSC plot can be used to determine Heat Capacity.

• Suppose a polymer is being heated. When we start heating two pans, the
computer will plot the difference in heat output of the two heaters against
temperature i.e. plot of heat absorbed by the polymer against temperature.

• Plot will look like this at first;

• After some time, when certain amount of heat

is transferred to the sample, the temperature
of sample increases.

• By measuring the Heat flow and Heating rate,

heat capacity can be calculated. DSC curve at the beginning

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• The heat flow is heat (q) supplied per unit time (t), whereas,

• The heating rate is increase in temperature (ΔT) per unit time (t).

• By dividing heat flow (q/t) by the heating rate (ΔT/t), we get heat
supplied divided by the temperature increase, which is called heat
capacity.

37
[2]. Glass Transition Temperature (Tg):

• “Glass transition temperature is the temperature at which amorphous

(noncrystalline) polymers are converted from a brittle, glass like form to a
rubbery, flexible form.”

• Above the glass transition temperature certain segmental motions of the

polymer are comparatively unhindered by the interaction with neighboring
chains. Below the glass transition temperature, such motions are hindered
greatly.

• The operative definition of glass transition temperature is that at this

temperature, or within a few degrees, the specific heat, the coefficient of
thermal expansion, the free volume, and the dielectric constant (in the
case of a polar polymer) all change rapidly.

• Since the mechanical behavior of polymers changes markedly at the glass

transition temperature, it is an important characteristic of every polymer.
38
• In the DSC experiment, Tg is manifested by a drastic change in the base line,
indicating a change in the heat capacity of the polymer.

• No enthalpy is associated with such transition; therefore, the effect in a

DSC curve is slight and is observable only if the instrument is sensitive
enough.

• 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.

Latent heat:
The heat required to convert a solid into a liquid or vapour, or a liquid into a vapour, without
change of temperature.
First order transition Second order transition
• Transitions which have latent heat are • Transitions which have no latent heat are
called first order transition. called second order transition.

• e.g. Melting, crystallization, evaporation, • e.g. Glass transition. 39

condensation etc.
Measurement of Tg of Polymethyl methacrylate
(PMMA) by DSC

Tg

40
[3]. Crystallization:
• Above the glass transition, the polymers have a lot of mobility.

• When they reach the right temperature, they will have gained enough
energy to move into very ordered arrangements called crystals.

• When polymers fall into these crystalline arrangements, they give off heat.
When this heat is evolved, the computer do not have to put out much heat
to keep the temperature of the sample pan rising.

Endo Tc in DSC
• You can see this drop in the heat flow
as a big dip in the plot of heat flow
versus temperature:

Exo
41
• This dip gives us three kinds of information:

1) The temperature at the lowest point of the dip is usually considered to be

the polymer's crystallization temperature, or Tc.
2) Also, we can measure the area of the dip, and that will tell us the latent
energy of crystallization for the polymer.
3) But most importantly, this dip tells us that whether the polymer can
crystallize or not.

Example: If you analyze a 100% amorphous polymer, like 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.

• Transitions like crystallization, which have latent heats, are called first order
transitions.
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Calculation of Percentage Crystallinity:

• First, measure the area of peak for the melting of the polymer. As the
thermogram of DSC is a plot of heat flow per gram of material, versus
temperature, so:

• Heat flow is heat given off per second, so the area of the peak is given as:

• Than we divide the area by the heating rate of DSC which is temperature
over time:

43
• By multiplying this by the mass of the sample:

• This is the total heat absorbed during the melting of polymer.

• Now if we do the same calculation for the crystallization of the polymer, we

can get the total heat evolved during the crystallization.

• We'll express the total heat absorbed during melting as Hm, total, and we'll
express the total heat evolved during crystallization as Hc, total.

• By subtracting the both we get:

44
• Whereas H' is the heat given off by that portion 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.

• This can be done by dividing H’ by the specific heat of melting, Hm*.

“Specific heat of melting Hm* is the amount of heat evolved 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:

45
• This mc 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 percent crystallinity:

46
[4]. Melting:
• Heat may allow crystals to form in a polymer, but too much of heat can
degrade them.

• If we keep heating our polymer past its Tc, eventually we'll reach another
thermal transition, 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 this can be detected on a DSC plot.

• 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 as
melting is a first order transition.
47
• This means that when the melting temperature is reached, the
polymer's temperature won't rise until all the crystals have melted.

• As a result the 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.

Endo Tm in DSC
• This extra heat flow during melting shows
up as a big peak on DSC plot, like this:

Exo

48
• The latent heat of melting can be measured by the area of the peak.

• And the temperature at the top of the peak represents the polymer's
melting temperature, Tm.

• Because the sample absorbs heat during melting, melting is

an endothermic transition.

• Transitions like melting which have latent heats, are called first order
transitions.

49
50
Summary of Phase Transitions:
• To put all the phase transitions together, a DSC plot will look
something like this:

Complete Thermogram of DSC

51
DSC thermogram of Polyethylene terephthalate (PET)

52
 Applications of DSC
[1]. Qualitative and Quantitative analysis:

Qualitative applications:
• Glass transition temperatures and melting points are useful for qualitative
classification of materials, although thermal methods cannot be used alone
for identification.

• Melting points are also very useful in establishing the purity of various
preparations. Hence, thermal methods are often used in quality control
applications.

• It is also used for finger printing of minerals, clays, polymers etc.

Geochemical Finger printing:

Geochemical fingerprint is a chemical signal that provides information about the origin, the 53
formation and/or the environment of a geological sample.
Quantitative applications:
• Quantitative applications include the determination of heats of fusion and
the extent of crystallization for crystalline materials and heat capacity
determination.

DSC can be used to measure the following:

1. Glass transitions
2. Crystallization time and temperature
3. Melting and boiling points
4. Heat of Fusion
5. Heat capacity
6. Percentage crystallinity
7. Reaction kinetics
8. Purity

54
2. Oxidative stability:

• DSC can be used to study the stability to oxidation of samples.

• 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.
55
3. Liquid Crystals:

• DSC is used in the study of liquid crystals.

• Some materials when convert from solid to liquid, they go through a

third state, which displays properties of both the phases.

• This anisotropic liquid is known as a liquid crystalline state 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 anisotropic liquid.
Difference between isotropic and anisotropic liquids:
A true liquid is isotropic , meaning that its properties are uniform in all directions—
the result of its molecules being in constant random motion. Crystalline solids, in
contrast, are anisotropic ; optical- and other properties such as thermal and electrical
56
conductivity vary with direction.
4. Drug Analysis:
• DSC is widely used in the pharmaceutical and polymer industries.

(a). Polymer industries:

• For polymers, 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 peak in DSC curve that usually appears soon after the glass transition.

(b). Pharmaceutical industries:

• 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 which crystallization can occur.

Curing process:
Curing is a term in polymer chemistry
and process engineering that refers to the
toughening or hardening of a polymer material
by cross-linking of polymer chains, brought
about by electron beams, heat, or chemical
additives.
Pre-existing data
Pre-existing data is the already present data
in the DSC computer. After each analysis of a
compound, the computer automatically
matches the results with the pre-existing
57
data.
5. General Chemical Analysis:

• Melting-point can be used as a purity analysis tool when analyzed by Differential

Scanning Calorimetry.

• This is possible because the temperature range over which a mixture of

compounds melts is dependent on their relative amounts.

• Consequently, less pure compounds will exhibit a broadened melting dip that
begins at lower temperature than a pure compound.

6. Food Sciences:

• Differential scanning calorimetry (DSC) is the most widely used thermal analytical
technique in food research and it has a great utility in quality assurance of food.

• Proteins are the most studied food components by thermal analysis including
studies on conformation changes of food proteins as affected by various
environmental factors, thermal denaturation of tissue proteins, food enzymes and
enzyme preparations for the food industry, as well as effects of various additives on
their thermal properties. 58
References:

1. Pharmaceutical Analysis by P. Parimoo.

2. Principles of instrumental analysis 6th edition by Skoog, Holler and
Crouch.
3. Pharmaceutical analysis Sheffield analytical series.
4. Thermal analysis in practice volume 2 by Metler Toledo.
5. Internet.

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