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Differential Thermal Analysis (Dta)

Differential thermal analysis (DTA) measures the temperature difference between a sample and an inert reference material as both are subjected to identical temperature programs in a controlled atmosphere. It can detect endothermic or exothermic reactions in a sample as they cause the sample's temperature to lag or exceed the reference's temperature. DTA provides information about phase transitions, dehydration reactions, and other thermal events through the shape and size of peaks in the recorded thermogram. It has applications in pharmaceutical analysis, materials characterization, and determining thermodynamic properties of reactions.

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0% found this document useful (0 votes)
1K views11 pages

Differential Thermal Analysis (Dta)

Differential thermal analysis (DTA) measures the temperature difference between a sample and an inert reference material as both are subjected to identical temperature programs in a controlled atmosphere. It can detect endothermic or exothermic reactions in a sample as they cause the sample's temperature to lag or exceed the reference's temperature. DTA provides information about phase transitions, dehydration reactions, and other thermal events through the shape and size of peaks in the recorded thermogram. It has applications in pharmaceutical analysis, materials characterization, and determining thermodynamic properties of reactions.

Uploaded by

Naveen Kumar
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PPTX, PDF, TXT or read online on Scribd

Differential thermal

analysis (dta)

Presented By:
Mohd Nayeem Uddin Qureshi,
Roll no. 2568-20-887-005
m.Pharm Ist Year
DIFFERENTIAL THERMAL ANALYSIS
(DTA)
Principle:
The basic principle involved in DTA is the temperature
difference (∆T) between the test sample and an inert
reference sample under controlled and identical conditions
of heating or cooling is recorded continuously as a
function of temperature or time, thus the heat absorbed or
emitted by a chemical system is determined.
DIFFERENTIAL THERMAL
ANALYSIS (DTA)
If any reaction takes place in the sample, then the
temperature difference will occur between the sample and
the reference material.
In an endothermic change (such as melting or dehydration
of the sample) the temperature of the sample is lower than
that of the reference material (i.e) ∆T = ve (for
endothermic process)‒
In an exothermic change or process the sample
temperature is higher than that of the reference material.
(i.e) ∆T = + ve (exothermic process)
The shape and the size of the peak give information about
the nature of the test sample.
(1)Sharp endothermic peaks indicate phase changes (such as
melting, fusion etc.) transition from one crystalline form
to another crystalline form.
(2) Broad endothermic peaks are obtained from dehydration
reactions
(3)Chemical reactions like oxidative reactions are
exothermic reactions.
INSTRUMENTATION FOR DTA
BLOCK DIAGRAM
The DTA apparatus consists of the following components
Furnace sample and reference holder with thermocouple
assembly.
Sample holder furnace(To heat the sample)
Furnace temperature controller(to increase the furnace
temperature steadily)
Furnace atmospheric control system(To maintain a suitable
atmosphere in the furnace and sample holder)
Low level DC amplifier
Recording device(Recorder)
Differential temperature sensor (to measure the temperature
difference between the sample and reference material) the
sample and reference holder are kept inside the furnace and the
temperature of the furnace and sample holder is controlled by
using furnace controller.
DTA OF CALCIUM OXALATE
MONOHYDRATE
• The DTA curve for the decomposition of calcium oxalate monohydrate
(CaC2O4.H2O) is shown in the diagram.

The thermogram shows the decomposition in CO2 atmosphere and in air


atmosphere.
DTA OF CALCIUM OXALATE
MONOHYDRATE
The thermogram of calcium oxalate monohydrate has three
peaks corresponding to the successive elimination of H2O,
CO and CO2.
These three points of weight loss corresponds to the three
endothermic process.
Curve (b) represents the DTA diagram for the same
compound in air. The second peak in this curve is sharply
exothermic, but corresponds to the same weight loss as in
carbon dioxide atmosphere.
This peak represents the exothermic burning of carbon
monoxide in air at the temperature of the furnace.
FACTORS AFFECTING THE DTA
CURVE
Instrumental Factors:
Size and shape of the sample and furnace holder. •
Material from which sample holder is made and its
corrosive attack.
Heating rate(furnace heating rate)
Sample characteristics:
Amount of the sample(sample weight)
Particle size of the sample
APPLICATIONS OF DTA
DTA curves for two substances are not identical. Hence they
serve as finger prints for various substances.
Used to study the characteristic of polymeric material.
This technique is used for testing the purity of the drug sample
and also to test the quality control of number of substances like
cement, soil, glass,etc.
Used for the determination of heat of reaction, specific heat
and energy change occurring during melting etc.
Trend in ligand stability (thermal stability of the ligands) gives
the information about the ligands in the coordination sphere.

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