Important

Techniques used in
Cocrystal
Analysis
Thermal Gravimetric Analysis (TGA)
Presented by:
Gurleen Kaur
Differential Scattering Calorimetry (DSC)
Date Presented:
3rd April 2023
Thermal
Gravimetric Analysis
(TGA)
Contents

• Introduction

• How TGA Works

• Types of TGA

• TGA Curve

• Advantages and Drawbacks

• Applications
 Introduction
Thermal gravimetric analysis (TGA) is a method of thermal analysis in which
changes in physical and chemical properties of materials are measured as :

Function of increasing temperature Function of time

(with constant heating rate), (with constant temperature and/or
constant mass loss).
TGA can provide information about physical and chemical
phenomena, such as second-order phase transitions including;

• vaporization
• sublimation,
• absorption and desorption
• chemisorptions,
• desolvation
• decomposition

Thermo-Balance: • The instrument used for thermo-gravity

is a programmed precision balance for
rise in temperature
How TGA Works
01 02 03
Sample Temperature Observations &
Preperation Variations Plotting

A sample is continously weighted The temperature is increased and the Many solids undergo reactions that
while heating, as an inert gas changes in the weights are recorded as evolve gaseous byproducts. In TGA,
atmosphere is passed over it. a function of temperature at different these gaseous byproducts are removed
intervals and changes in the remaining mass of
the sample are recorded

The plot of weight changed against

temperature is called
Thermogravimetric curve or
Thermogram.
Types of TGA
Three variations are commonly employed:

Dynamic TGA Static TGA Quasistatic TGA

• Temperature is held constant as the mass is • Sample is heated in multiple temperature

• Temperature continues to increase over
measured intervals, and held at those intervals for a time,
time as mass is recorded
often until the mass stabilizes
• This can be used to gain more information
on a decomposition that happens at a • This is ideal for investigating substances that
• This allows simulataneous identification of
certain temperature or to investigate a are known to decompose in various ways at
how much gas is removed and the
material’s ability to withstand a given different temperatures, and better characterizing
temperature at which it occurs
temperature the way in which they decompose
TGA Curve

• These curves are plotted with the flowing terms:

y-axis : mass change (Dm)

x-axis : Temperature or Time

• For better understanding of the graphs, let's

consider the example of TGA curve of AgNo3 :
Example of AgNo3

• The horizontal segment of the curve shows that there has been no
change in weight, while the abrupt drop in the graph line indicates
that there has been a change in weight.

• The weight of the material (AgNO3) stays constant up to a

temperature of roughly 470°C, demonstrating that AgNO3 is
thermally stable up to that degree.

• At this temperature, it begins to lose weight, indicating that the

decomposition process has begun. It degrades to NO2, O2, and Ag.
The weight loss continues until a specific higher temperature is
reached, leaving metallic Ag as the stable remnant. Above this
temperature, the sample's weight remains unchanged.
Advantages Advantages
• Accurate and precise method of Macro Quantitative
& Analysis
• Reliable Data
Limitations • Low Detection Limit ( up to 10^-7)
• capable of conducting isothermal and cooling experiment

Limitations
• Limited range of samples
• Time Consuming
• Usually not qualitative
• Mis step in procedure can lead to error in anlaysis
 Applications
Used in the study of Catalyst:
The change in the chemical states of the catalyst may be Determination of the composition of complex mixture
studied by TGA techniques. and decomposition of complex. and for studying the
(Zn-ZnCrO4) Zinc-Zinc chromate is used as the catalyst sublimation behaviour of various substances.
in the synthesis of methanol.

Determination of the bound and unbound water in the

From TGA, we can determine the purity and thermal
suspension of Milk of Magnesia (MoM), used as a
stability of both primary and secondary standard.
laxative.
Differential
Scanning Calorimetery
(DSC)
Contents

• Introduction

• How DSC Works

• Principle

• DSC Thermogram

• Advantages and Drawbacks

• Applications
 Introduction

• Differential scanning calorimetry is a specific type of calorimetry including

both a sample substance and a reference substance, residing in separate
chambers.

• While the reference chamber contains only a solvent (such as water), the
sample chamber contains an equal amount of the same solvent in addition to
the substance of interest, of which the Heat of Reation (ΔrH) is being
determined.

• Both the sample and the refernce are maintained at nearly the same temperature
throughout the experiment.
How DSC Works
01 02 03
An aluminum case is taken
and the sample is weighed The difference in
in it after tare. Not more A typical calorimeter is an temperature between
than 1-1.5 gms of sample is isolated chamber where a sample and surrounding
taken. sample is placed in a medium gives the heat
The lid is put on and wiht surrounding medium. Then capacity of the sample and
the help of a crimper, the the sample is heated with a information about heat
case is crimped only to a definite amount of heat. release and consumption of
certain level leaving some the sample.
space inside.
 Working Principle
The basic principle underlying this technique is, when the sample undergoes a physical transformation such
as phase transitions, more or less heat will be needed to flow to it than the reference to maintain both at the
same temperature.

These transitions involve energy changes or heat capacity changes that can be detected by DSC with great
sensitivity.
 DSC Thermogram
• The output yielded by differential scanning calorimetry is called a differential thermogram,
which plots the required heat flow against temperature

• This graph indicates the change in power (electrical heat) as the temperatures of the two cells
are gradually increased. A change in specific heat results in a small change in power, and can be
either positive or negative depending on the particular process

• The advent of an endothermic reaction will cause an increase in power as temperature increases,
since additional heat is required to drive the reaction and still maintain the reference temperature

• When an exothermic reaction occurs, the opposite effect is observed; power decreases because
heat is released by the reaction and less power is required to maintain equivalent temperatures in
the chambers
Advantages Advantages
• Wide range of temperatures
& • Any material in any form may be tested
• Small amount of material is required
Limitations • Time efficient
• Auto sampler and Auto Analysis

Limitations
• Interpretation of data is complex
• Quantitative analysis is not possible
• Very sensitive to any changes
 Applications
DSC is widely used in the pharmaceutical and polymer industries.
In the pharmaceutical industry it is necessary to have well- The main application is in studying phase transitions,
characterized drug compounds in order to define processing and widely used to determine temperatures and melting
parameters. For instance, if it is necessary to deliver a drug in the enthalpy, estimation of crystallization kinetics of
amorphous form, it is desirable to process the drug at temperatures polymers
below those at which crystallization can occur.

Using this technique it is possible to observe fusion and

Analysis of proteins through DSC can provide both the
crystallization events as well as glass transition
enthalpy of denaturation and information about the
temperatures Tg. DSC can also be used to study
cooperativity of the denaturation process.
oxidation, as well as other chemical reactions.