Dta use in preformulation study copy

GUIDED BY: PRESENTED BY:
Dr.R.K.Parikh AHALGAMA JIGNESH V
DEPARTMENT OF PHARMACEUTICS AND
PHARMACEUTICAL TECHNOLOGY M.Pharm -1 (2011-12)
L.M.COLLEGE OF PHARMACY Roll no :- 09
AHMEDABAD-380009

 Thermal analysis
 Classification of thermal analysis
 Differential thermal analysis(DTA)
 Principle
 Instrumentation
Advantage and Disadvantage
 Application
 References

Ahalgama Jignesh V. , M-Pharm-1(paper code-
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910102), DTA,LMCP,GTU(2011-12))

 Thermal analysis incorporates those techniques in
which some physical parameter of the system is derived
and/or recorded as a function of temperature.

 Matter is heated it undergoes physical and chemical
changes occur.

 physical change: melting or boiling ,weight loss,gas
evolution.

 chemical change:decomposition or reaction take place.

910102), DTA,LMCP,GTU(2011-12)) 3/25

Sr no Technique Parameter Instrument Graph
measured used
1 Thermogravimetry mass thermobalance Mass vs.
temp or time
2 Derivative dm/dt thermobalance dm/dt vs.
thermogravimetry temp.
3 Differential thermal Delta T DTA apparatus Delta T vs.
analysis temp.
4 Differential dH.dt calorimeter dh/dt vs.
scanning temp.
calorimetry
5 Thermometric temperature calorimeter Temp vs.
titrimetry titrant volume
(Cont…..)
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6 Dynamic Reflectance Spectrophot %
Reflectance ometer reflectance
spectroscopy and temp
7 Evolved gas Thermal Thermal T.C vs.
detection conductivity conductivity temp.
cell
8 Thermo Volume or dilatometer Volume or
mechanical length length vs.
analysis temp.
9 Electrical Current or electrometer I or R vs.
conductivity resistance temp.
10 Emanation Radioactivity ETA E vs. temp.
thermal apparatus
analysis
910102), DTA,LMCP,GTU(2011-12)) 5/25

 Combination with
thermogravimetry

1)for better interpretation
a) TG DTA b) TG DSC

2)for identification of gas involved in
thermal analysis
a) TG MS b) TG GC MS

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TG/DTA Simultaneous
Measuring Instrument
Simultaneous
TG/DTA
improves ease
of operation,
sensitivity and
analytical
accuracy .

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Principle:

A technique in which the temperature difference
between a substance and a reference(Al2o3) material
is measured as a function of temperature while the
substance and reference are subjected to a controlled
temperature program.

 endothermic and exothermic peak.

 endothermic and exothermic reaction.
910102), DTA,LMCP,GTU(2011-12)) 8/25

Δ T vs. temperature

ΔT

Temp.
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Ahalgama Jignesh V. , M-Pharm-
1(Pharmaceutical technology & Pharmaceutics, 10/25
DTA,LMCP(2011-12))



a) METALIC : nickel,stainless steel,platinum
sharp endothermic peak.
a) NON METALIC : glass,silica,sintered alumina
sharp exothermic peak.



For heating the sample.
Material used wire or ribbon wound on refrectory
tube.
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1) SENSOR
2) CONTROL ELEMENT
3) HEATER

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1) DEFLECTION TYPE: Recording pen is
moved directly by the input signal.

2) NULL TYPE: Input signal is compared
with a reference or standard signal and
difference is amplified.

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High resolution and a robust easy to
use.

 Less satisfactory than dsc with regard to
resolution of thermal traces and quantitative data.

 Unable to measure the energy associated with
each event.

910102), DTA,LMCP,GTU(2011-12)) 15/25

1) Identification of substance: DTA curve of two
substance is not identical.

2) Identification of product:substance is react with another
substance product is identified by their specific DTA curve.

3) Melting point: It is an endothermic process in which heat
is absorbed by analyte.

4) Detection of impurity
curves could be compared with the curve of reference
standard.
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5) Studying and characterizing polymers
Thermochimica acta ,vol,4,Aug-1972,page-249-255.
thermal transition for a polymer often take place over a
extended temp. range because even a pure polymer is a
mixture of homologues and not a single chemical.
species.

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6) Detection of eutectic mixture:

 binary mixture :two endotherm

 eutectic mixture : single major endotherm.

7) generation of phase diagram and
phase transitions
In which the peak at 113 c corresponds to the
solid phase change from the rhombic to
monoclinic form.the peak at 124 c corresponds
to the melting point of the element. The peak at
446 c corresponds to the boiling point of sulfur.

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8) Application of DTA to compatibility and
stability problems in penicillin –stearic acid
mixture
journal of pharmaceutical science,vol-5,page 631-633,may-1969

Identify stearic acid as the inactivating component in
unstable formulation containing sodium dicloxacin and
other excipients.

Stearic acid + k.penicilin=incompatible

Stearic acid+ sodium dicloxacin =incompatible

Stearic acid+ ampicilin trihydrates=compatible
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(9) Comparative physical-chemical charecterization
of encapsulated lipid based ISOTRETINOIN
product by thermal behavior analysis
Thermochimica acta 505 ,(2010),73-78.

 Use in nodular acne.

 Study the three encapsulated product (1 reference and 2
generic).

 measure thermal behavior of that product no specific
change and more thermostable than isotretinoin.

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(10) Physiochemical charecterization of edaravone
with hydroxy propyl –B-cyclodextrin.
carbohydrate polymer 83(2011),1101-1105.

 novel free radical scavenger.

 that preparation for the improve solubility and stability.

 inclusion complex charecterized by DTA-TG method.

 inclusion complex more stable than edaravone.

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Remington’s Pharmaceutical Science,21st edition,2005.
 Theory and Practice of Industrial Pharmacy by Lachman &
Lieberman,third edition.
 Physical pharmacy, Alfred martin, fourth edition
 The Science of Dosage form Design M.E Aulton
 Thermochimica acta ,vol,4,Aug-1972,page-249-255.
 journal of pharmaceutical science,vol-5,page 631-633,may-1969.
 Thermochimica acta 505 ,(2010),73-78.

 carbohydrate polymer 83(2011),1101-1105.

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Principle and Instrumental analysis, skoog-hollar-nieman, 5th editio.

Chemical Abstract vol:146, No:25,June 18 :2007,507180

Instrumental methods of chemical analysis,gurdeep r.chatwal,2008.

 www.linseis.net
 www.nd.edu
www.shimadzu.lacerta-technology.com
www.wikipedia.com
 www.ijpsonline.com/article.asp

 Encyclopedia of pharmaceutical Technology ,Swarbrick & Boylan vol-06

 Encyclopedia of pharmaceutical Technology ,Swarbrick & Boylan vol-02
Ahalgama Jignesh V. , M-Pharm-1(paper code- 24/25
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Dta use in preformulation study copy

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