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4
 In Differential Thermal Analysis, the
  temperature difference that develops
  between a sample and an inert reference
  material is measured, when both are subjected
  to identical heat - treatments.
 The related technique of Differential Scanning
  Calorimetry relies on differences in energy
  required to maintain the sample and reference
  at an identical temperature.
Most read
14
 Heart of the analysis  heating block
 Identical pair of cavities for the sample, ref.
  material
 Whole unit is set in an oven- control pressure
 Thermocouple is place directly in contact with
  the sample and another in contact with the
  reference
 Temp.of the block is raised, the temperature of
  the sample & reference follow
 Zero temp. difference  no physical or chemical
  change
 If any reaction  difference in T
Most read
20
Applications

 Quantitative identification and purity
  assessment of materials are accomplished by
  comparing the DTA curve of sample to that of
  a reference curve
 Impurities may be detected by depression of
  the M.P
Most read
DIFFERENTIAL
   THERMAL
ANALYSIS (DTA)

   Prepared by:-
   Mr. Jiten B. Patel
   M.pharm(1st sem)


                        B.M.C.P.
Thermal Analysis Techniques
 When a material is heated its structural and
  chemical composition can undergo changes
  such as fusion, melting, crystallization,
  oxidation, decomposition, transition,
  expansion and sintering.

 Using Thermal Analysis such changes can be
  monitored in every atmosphere of interest. The
  obtained information is very useful in both
  quality control and problem solving.
Types of thermal analysis
 TG (Thermogravimetric) analysis:
  weight

 DTA (Differential Thermal Analysis): temperature

 DSC (Differential ScanningCalorimetry):
  temperature
 In Differential Thermal Analysis, the
  temperature difference that develops
  between a sample and an inert reference
  material is measured, when both are subjected
  to identical heat - treatments.
 The related technique of Differential Scanning
  Calorimetry relies on differences in energy
  required to maintain the sample and reference
  at an identical temperature.
Thermogravimetry (TG)

 Thermogravimetry is the measurement of the
  mass of a sample as the temperature increases.
  This method is useful for determining sample
  purity and water, carbonate, and organic
  content; and for studying decomposition
  reactions.
INTRODUCTION

 This is a comparison method

 Analytical method for recording the
  difference in temperature (T) b/w a
  substance and an inert reference material as
  a function of temperature or time
 Any transformation  change in specific heat
  or an enthaply of transition can be detected
  by DTA
 In DTA both test sample & an inert reference
  material (alumina)  controlled heating or
  cooling programming
 If zero temperature difference b/w sample &
  reference material  sample does not
  undergo any chemical or physical change.
 If any reaction takes place temperature
  difference (T) will occur b/w sample &
  reference material
 A DTA curve can be used as a finger print for
  identification purposes, for example,
 in the study of clays where the structural
  similarity of different forms renders diffraction
  experiments difficult to interpret.
T VS Temp.
Sharp Endothermic  changes in crystallanity or fusion
Broad endotherms - dehydration reaction
Physical changes usually result in endothermic curves
Chemical reactions are exothermic
Apparatus

 The key features of a differential thermal analysis
  kit are as follows

  1. Sample holder comprising thermocouples,
  sample containers and a ceramic or metallic
  block.
  2. Furnace.
  3. Temperature programmer.
  4. Recording system.
DTA
DTA
DTA
 Heart of the analysis  heating block
 Identical pair of cavities for the sample, ref.
  material
 Whole unit is set in an oven- control pressure
 Thermocouple is place directly in contact with
  the sample and another in contact with the
  reference
 Temp.of the block is raised, the temperature of
  the sample & reference follow
 Zero temp. difference  no physical or chemical
  change
 If any reaction  difference in T
DTA
DTA
Differential Thermal Analysis
Advantages:

 instruments can be used at very high
  temperatures

 instruments are highly sensitive

 characteristic   transition or reaction
  temperatures       can    be  accurately
  determined

Disadvantages:                                     DTA

 uncertainty of heats of fusion, transition,
  or reaction estimations is 20-50%
Factors affect results in DTA

   Sample weight
   Particle size
   Heating rate
   Atmospheric conditions
   Conditions of sample packing into dishes
DTA
Applications

 Quantitative identification and purity
  assessment of materials are accomplished by
  comparing the DTA curve of sample to that of
  a reference curve
 Impurities may be detected by depression of
  the M.P
THANK YOU

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Ad

DTA

  • 1. DIFFERENTIAL THERMAL ANALYSIS (DTA) Prepared by:- Mr. Jiten B. Patel M.pharm(1st sem) B.M.C.P.
  • 2. Thermal Analysis Techniques When a material is heated its structural and chemical composition can undergo changes such as fusion, melting, crystallization, oxidation, decomposition, transition, expansion and sintering. Using Thermal Analysis such changes can be monitored in every atmosphere of interest. The obtained information is very useful in both quality control and problem solving.
  • 3. Types of thermal analysis TG (Thermogravimetric) analysis: weight DTA (Differential Thermal Analysis): temperature DSC (Differential ScanningCalorimetry): temperature
  • 4. In Differential Thermal Analysis, the temperature difference that develops between a sample and an inert reference material is measured, when both are subjected to identical heat - treatments. The related technique of Differential Scanning Calorimetry relies on differences in energy required to maintain the sample and reference at an identical temperature.
  • 5. Thermogravimetry (TG) Thermogravimetry is the measurement of the mass of a sample as the temperature increases. This method is useful for determining sample purity and water, carbonate, and organic content; and for studying decomposition reactions.
  • 6. INTRODUCTION This is a comparison method Analytical method for recording the difference in temperature (T) b/w a substance and an inert reference material as a function of temperature or time Any transformation change in specific heat or an enthaply of transition can be detected by DTA
  • 7. In DTA both test sample & an inert reference material (alumina) controlled heating or cooling programming If zero temperature difference b/w sample & reference material sample does not undergo any chemical or physical change. If any reaction takes place temperature difference (T) will occur b/w sample & reference material
  • 8. A DTA curve can be used as a finger print for identification purposes, for example, in the study of clays where the structural similarity of different forms renders diffraction experiments difficult to interpret.
  • 9. T VS Temp. Sharp Endothermic changes in crystallanity or fusion Broad endotherms - dehydration reaction Physical changes usually result in endothermic curves Chemical reactions are exothermic
  • 10. Apparatus The key features of a differential thermal analysis kit are as follows 1. Sample holder comprising thermocouples, sample containers and a ceramic or metallic block. 2. Furnace. 3. Temperature programmer. 4. Recording system.
  • 14. Heart of the analysis heating block Identical pair of cavities for the sample, ref. material Whole unit is set in an oven- control pressure Thermocouple is place directly in contact with the sample and another in contact with the reference Temp.of the block is raised, the temperature of the sample & reference follow Zero temp. difference no physical or chemical change If any reaction difference in T
  • 17. Differential Thermal Analysis Advantages: instruments can be used at very high temperatures instruments are highly sensitive characteristic transition or reaction temperatures can be accurately determined Disadvantages: DTA uncertainty of heats of fusion, transition, or reaction estimations is 20-50%
  • 18. Factors affect results in DTA Sample weight Particle size Heating rate Atmospheric conditions Conditions of sample packing into dishes
  • 20. Applications Quantitative identification and purity assessment of materials are accomplished by comparing the DTA curve of sample to that of a reference curve Impurities may be detected by depression of the M.P