DEPARTMENT OF PHARMACEUTICAL SCIENCES
RASHTRASANT TUKADOJI MAHARAJ NAGPUR
UNIVERSITY, NAGPUR - 440033
THERMOGRAVIMETRIC ANALYSIS
PRESENTED BY
TAHMINA KHAN
M. PHARM. FRIST YEAR
PHARMACEUTICAL CHEMISTRY
CONTENT
• INTRODUCTION
• TYPES OF THERMOGRAVIMETRY
• INSTRUMENTATION
• THERMAL CURVE
• FACTORS AFFECTING THE TGA
• APPLICATIONS OF TGA
• REFERENCE
INTRODUCTION
• The thermogravimetric analysis or thermal gravimetric analysis
(TGA) is method of thermal analysis in which the mass of the
sample is measured over time as the temperature change.
PRINCIPLE
• The basic principle of TGA is that as a sample is heated, its mass
change. This change can be used to determine the composition of a
material or its thermal stability up to 1000˚C
• Usually, a sample losses weight as it is heated up due to
decomposition, reduction or evaporation oxidation or absorption.
TYPES OF THERMOGRAVIMETRY
Types of
Thermogravimetry
Isothermal
Thermogravimetry
Quasistatic
Thermogravimetry
Dynamic
Thermogravimetry
• Isothermal or static Thermogravimetry :
In the technique the sample weight in recorded as function of time at
constant temperature.
• Quasistance Thermogravimetry :
In this technique the sample is heated to constant weight at each of series of
increases temperature.
• Dynamic Thermogravimetry :
In this technique the sample is heated in an environment whose temperature
is changing in predetermined manner generally linear rate , this type is
generally used.
INSTRUMENTATION
• Thermogravimetric analysis is conducted on an instrument referred
to as a thermogravimetric analyzer.
• Thermogravimetric analyzer continuously measures mass while the
temperature of a sample is changed over time.
• Mass, temperature and time considered as base measurement in
thermogravimetric analyzer.
• A typical thermogravimetric
analyzer consist of ;
1. A furnace controlled
thermobalance
2. A furnace which can be heated so
that, the temperature with time
3. Recorder
• The apparatus required for TGA analyzer are:
1. Balance
2. Sample holder
3. Furnace
4. Furnace Temperature Programmer (Thermocouple)
5. Data Recorder
BALANCE
• There are two types of balance used in TGA-
Null point type –
This uses appropriate sensing element (sensor) which detects any slightly
deviation of the balance.
Deflection type –
Based on either conventional analytical balance
consisting of -
Helical Beam
Torsion Cantilever
SAMPLE HOLDER
• This is most important in accurate thermogravimetric analysis.
• Depending upon the nature of sample, its weight and quantity to be
handled, different size and shape of sample holders known as crucibles are
employed.
• These are constructed from various materials like glass, quartz, aluminum,
stainless steel, platinum etc.
• These generally are of two types:
1. Shallow pan for holding samples which eliminates gas, vapors or
volatile matter by diffusion during heating or.
2. Deep crucible for general purpose.
FURNACE
• Must be designed in such a fashion so as to incorporate an appropriate
smooth input thereby maintaining either a fixed temp. or predetermined
linear heating program. (e.g.- 6 c/min)
• Temperature control is achieved via a thermocouple mounted very close
to the furnace-winding.
• Maximum operational temp. may be obtained using different
thermocouple
• as indicated below:
SR NO. SPECIFICATION MAX. TEP.
1 Nickel-chrome (nichrome) 1100
2 Platinum-rhodium 1450
3 Graphite-tube furnace >1500
FURNACE TEMPERATURE PROGRAMMER
• These are the controller which can provide gradual rise of
temperature at a fixed rate.
• This device has a coarse and fine control knobs through which
desired temperature with respect to ratel time can be obtained.
• This controlling is done by increasing voltage through the heated
element by motor driven variable transformer or by different
thermocouples.
THERMAL CURVE (THERMOGRAM)
(X- Axis) can be displayed as temperature and
(Y- Axis) can be displayed as weight (%).
FACTORS AFFECTING THE TGA
(1) Instrumental factors
(a) Furnace heating rate
(b) Furnace atmosphere
(2) Sample characteristics
(a) Weight of the sample
(b) Sample particle size
APPLICATIONS OF TGA
• TGA is used as a technique to characterize materials used in various
environmental, food, pharmaceutical, and petrochemical applications.
• TGA can be used to evaluate the thermal stability of a material In a desired
temperature range.
• Can determine the purity of a mineral, inorganic compound, or organic
material.
• TGA is used to study the kinetics of the reaction rate constant.
Thermogravimetric analysis(TGA) is a powerful technique for the
characterization of the decomposition or weight loss properties of
materials. The technique provides the following useful information:
I. Oxidative degradation characteristics
II. Quantitative weight losses
III. Compositional analysis
IV. Long term stabilities
V. Flammability properties
VI. Rates of degradation
VII.Decomposition temperatures
VIII.Thermal degradation properties
REFERENCE
• Instrumental method of chemical analysis B.K Sharma page
no: 308
• Pharmaceutical drug analysis Ashutosh Kar page no: 194
TGAtk.pptx

TGAtk.pptx

  • 1.
    DEPARTMENT OF PHARMACEUTICALSCIENCES RASHTRASANT TUKADOJI MAHARAJ NAGPUR UNIVERSITY, NAGPUR - 440033 THERMOGRAVIMETRIC ANALYSIS PRESENTED BY TAHMINA KHAN M. PHARM. FRIST YEAR PHARMACEUTICAL CHEMISTRY
  • 2.
    CONTENT • INTRODUCTION • TYPESOF THERMOGRAVIMETRY • INSTRUMENTATION • THERMAL CURVE • FACTORS AFFECTING THE TGA • APPLICATIONS OF TGA • REFERENCE
  • 3.
    INTRODUCTION • The thermogravimetricanalysis or thermal gravimetric analysis (TGA) is method of thermal analysis in which the mass of the sample is measured over time as the temperature change.
  • 4.
    PRINCIPLE • The basicprinciple of TGA is that as a sample is heated, its mass change. This change can be used to determine the composition of a material or its thermal stability up to 1000˚C • Usually, a sample losses weight as it is heated up due to decomposition, reduction or evaporation oxidation or absorption.
  • 5.
    TYPES OF THERMOGRAVIMETRY Typesof Thermogravimetry Isothermal Thermogravimetry Quasistatic Thermogravimetry Dynamic Thermogravimetry
  • 6.
    • Isothermal orstatic Thermogravimetry : In the technique the sample weight in recorded as function of time at constant temperature. • Quasistance Thermogravimetry : In this technique the sample is heated to constant weight at each of series of increases temperature. • Dynamic Thermogravimetry : In this technique the sample is heated in an environment whose temperature is changing in predetermined manner generally linear rate , this type is generally used.
  • 7.
    INSTRUMENTATION • Thermogravimetric analysisis conducted on an instrument referred to as a thermogravimetric analyzer. • Thermogravimetric analyzer continuously measures mass while the temperature of a sample is changed over time. • Mass, temperature and time considered as base measurement in thermogravimetric analyzer.
  • 8.
    • A typicalthermogravimetric analyzer consist of ; 1. A furnace controlled thermobalance 2. A furnace which can be heated so that, the temperature with time 3. Recorder
  • 9.
    • The apparatusrequired for TGA analyzer are: 1. Balance 2. Sample holder 3. Furnace 4. Furnace Temperature Programmer (Thermocouple) 5. Data Recorder
  • 10.
    BALANCE • There aretwo types of balance used in TGA- Null point type – This uses appropriate sensing element (sensor) which detects any slightly deviation of the balance. Deflection type – Based on either conventional analytical balance consisting of - Helical Beam Torsion Cantilever
  • 11.
    SAMPLE HOLDER • Thisis most important in accurate thermogravimetric analysis. • Depending upon the nature of sample, its weight and quantity to be handled, different size and shape of sample holders known as crucibles are employed. • These are constructed from various materials like glass, quartz, aluminum, stainless steel, platinum etc. • These generally are of two types: 1. Shallow pan for holding samples which eliminates gas, vapors or volatile matter by diffusion during heating or. 2. Deep crucible for general purpose.
  • 12.
    FURNACE • Must bedesigned in such a fashion so as to incorporate an appropriate smooth input thereby maintaining either a fixed temp. or predetermined linear heating program. (e.g.- 6 c/min) • Temperature control is achieved via a thermocouple mounted very close to the furnace-winding. • Maximum operational temp. may be obtained using different thermocouple • as indicated below: SR NO. SPECIFICATION MAX. TEP. 1 Nickel-chrome (nichrome) 1100 2 Platinum-rhodium 1450 3 Graphite-tube furnace >1500
  • 13.
    FURNACE TEMPERATURE PROGRAMMER •These are the controller which can provide gradual rise of temperature at a fixed rate. • This device has a coarse and fine control knobs through which desired temperature with respect to ratel time can be obtained. • This controlling is done by increasing voltage through the heated element by motor driven variable transformer or by different thermocouples.
  • 14.
    THERMAL CURVE (THERMOGRAM) (X-Axis) can be displayed as temperature and (Y- Axis) can be displayed as weight (%).
  • 15.
    FACTORS AFFECTING THETGA (1) Instrumental factors (a) Furnace heating rate (b) Furnace atmosphere (2) Sample characteristics (a) Weight of the sample (b) Sample particle size
  • 16.
    APPLICATIONS OF TGA •TGA is used as a technique to characterize materials used in various environmental, food, pharmaceutical, and petrochemical applications. • TGA can be used to evaluate the thermal stability of a material In a desired temperature range. • Can determine the purity of a mineral, inorganic compound, or organic material. • TGA is used to study the kinetics of the reaction rate constant.
  • 17.
    Thermogravimetric analysis(TGA) isa powerful technique for the characterization of the decomposition or weight loss properties of materials. The technique provides the following useful information: I. Oxidative degradation characteristics II. Quantitative weight losses III. Compositional analysis IV. Long term stabilities V. Flammability properties VI. Rates of degradation VII.Decomposition temperatures VIII.Thermal degradation properties
  • 18.
    REFERENCE • Instrumental methodof chemical analysis B.K Sharma page no: 308 • Pharmaceutical drug analysis Ashutosh Kar page no: 194