8. THERMAL ANALYSIS

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SEMINAR ON : 

THERMAL ANALYSIS AS A PART OF PREFORMULATION SEMINAR ON PRESENTED BY : CHINTAN M.PHARM -1 YEAR-2009-10 ROLL NO-01

List Of Contents : 

List Of Contents 1) INTRODUCTION 2) ROLE IN PREFORMULATION 3) CLASSIFICATION OF THERMAL ANALYSIS 4) DIFFERENT METHODS OF THERMAL ANALYSIS 5) GENERAL PRINCIPLES INVOLVED IN THERMAL ANALYSIS 6) INNOVATION IN THERMAL ANALYSIS 7) APPLICATIONS OF TA IN PREFORMULATION 8) FT-IR SPECTROMETER 9) X-RAY POWDER DIFFERACTION 10) LIMITATIONS 11) REFERENCES 12) STUDY QUESTION 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Thermal method of analysis are group of techniques in which changes in physical and /or chemical properties of a substance are measured as a function of temperature, while substance is subjected to controlled temperature programme. : 

Thermal method of analysis are group of techniques in which changes in physical and /or chemical properties of a substance are measured as a function of temperature, while substance is subjected to controlled temperature programme. THERMAL ANALYSIS 1) INTRODUCTION: Definition: 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Thermal analytical methods can measure the following physical properties, : 

Thermal analytical methods can measure the following physical properties, PHYSICAL PROPERTIES OPTICAL MASS GAS EVOLUTION MECHANICAL TEMPERATURE ENTHALPY MAGNETIC ELECTRICAL 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

2) ROLE OF THERMAL ANALYSIS IN PREFORMULAION : 

2) ROLE OF THERMAL ANALYSIS IN PREFORMULAION --They are unique methods in the field of polymer analysis & of high value for a solid state analysis.-- They finds wide application in a) Study of complexation b) Detection of impurity C) Study of polymorphism 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

3) CLASSIFICATION OF THERMAL ANALYTICAL TECHNIQUE : 

3) CLASSIFICATION OF THERMAL ANALYTICAL TECHNIQUE 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

4) DIFFERENT METHODS OF THERMAL ANALYSIS : 

4) DIFFERENT METHODS OF THERMAL ANALYSIS 4.1) Thermophotometry 4.2) Thermoluminescences 4.3) Thermomicroscopy 4.4) Microthermal analysis 4.5) Differential mechanical analysis 4.6) Emanation thermal analysis 4.7) Thermoparticulate analysis 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

5) GENERAL PRINCIPLES INVOLVED IN THERMAL ANALYSIS 5.1) THERMOGRAVIMETRY : 

5) GENERAL PRINCIPLES INVOLVED IN THERMAL ANALYSIS 5.1) THERMOGRAVIMETRY PRINCIPLE : Thermogravimetry is a technique in which a change in the weight of a substance is recorded as a function of temperature or time. Instrument: Instrument used for thermogravimetry is “Thermobalance”. Data recorded in form of curve known as ‘Thermogram’. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

5.2) DIFFERENTIAL THERMAL ANALYSIS (DTA) : 

5.2) DIFFERENTIAL THERMAL ANALYSIS (DTA) PRINCIPLE : A Technique in which the temperature difference between a substance & a reference material is measured as a function of temperature,while the substance & reference are subjected to a controlled temperature programme. The Difference in temperature is called as Differential temp(∆T) is plotted against temperature or a function of time. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Endothermic Peak : An endothermic peak, is a peak where the temperature of the sample falls below that of thereference material, i.e., ∆T is negative. Exothermic peak : An exothermic peak,is a peak where the temperature of the sample rises above that of the reference material,i.e. ∆T is positive. : 

Endothermic Peak : An endothermic peak, is a peak where the temperature of the sample falls below that of thereference material, i.e., ∆T is negative. Exothermic peak : An exothermic peak,is a peak where the temperature of the sample rises above that of the reference material,i.e. ∆T is positive. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

5.3) DIFFERENTIAL SCANNING CALORIMETRY : 

5.3) DIFFERENTIAL SCANNING CALORIMETRY PRINCIPLE: It is a technique in which the energy necessary to establish a zero temp. difference between the sample & reference material is measured as a function of temp. DSC is widely used to measure glass transition temp & characterization of polymer. Glass Transition temp(Tg) : Temp at which an amorphous polymer or an amorphous part of crystalline polymer goes from hard ,brittle state to soft,rubbery state. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

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24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Ideal DSC curve: : 

Ideal DSC curve: 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

5.4) THERMO MECHANICAL ANALYSIS : 

5.4) THERMO MECHANICAL ANALYSIS PRINCIPLE: A Technique in which changes in dimension of substance are measured as a Function of temp. TMA is useful for the measurement of changes in shape(volume or dimension),penetration characteristic & viscoelastic properties of different material as a function of controlled temp elevation. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

5.5) THERMOMICROSCOPY : 

5.5) THERMOMICROSCOPY This Technique also known as Hot stage microscopy. This Technique essentially involves the observation of a sample through a microscope fitted with a stage that can be heated or cooled at a controlled rate. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

5.6) MICROCALORIMETRY : 

5.6) MICROCALORIMETRY PRINCIPLE: Calorimetric technique deals with the measurement of heat evolved or absorbed by chemical or physical process. ISOTHERMAL ADIABATIC 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

6) INNOVATION IN THERMAL ANALYSIS : 

6) INNOVATION IN THERMAL ANALYSIS 6.1) MULTIELEMENTAL SCANNING THERMAL ANALYSIS (MESTA) 6.2) MICROTHERMAL ANALYSIS 6.3) MODULATED DSC 6.4) ROBOTIC SYSTEM 6.5) FAST SCAN DSC 6.6) DYNAMIC MECHANICAL ANALYSIS 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7) APPLICATION OF THERMAL ANALYSIS IN PREFORMULATION : 

7) APPLICATION OF THERMAL ANALYSIS IN PREFORMULATION 7.1) Characterization of hydrates and solvates Preformulation studies is to identify the ability of drug to take up water and characterize the state of this water. TGA is useful for characterization of hydrates & solvates. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.2) Study of polymer : 

7.2) Study of polymer Qualitative information: Thermogram provides information about Decomposition mechanism for various polymeric preparation. In addition,the Decomposition patterns are characteristic for each kind of polymer & in some case can be used for identification purpose. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Thermogram Of Various Polymer: : 

Thermogram Of Various Polymer: 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Quantitative information: : 

Quantitative information: Thermogram is also used for quantitative analysis of a polymeric material. Example:Polyethylene mixed with fine carbon black. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.3) Detection of impurity : 

7.3) Detection of impurity Basics of any calorimetric purity method: A sharp melting endotherm indicates the relative purity where as broad asymmetric curve suggest impurity. The presence of minute amount of substance broadens its melting range & lowers its mp. Compare to other thermal methods , DSC is best method for detection of impurity. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

eg. DSC of Phenacetin. (Checking purity of Phenacetin) : 

eg. DSC of Phenacetin. (Checking purity of Phenacetin) 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.4) Drug excipient compatibility study : 

7.4) Drug excipient compatibility study The potential compatibilities of several commonly used pharmaceutical excipients with any drug is evaluated using DSC. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

e.g DRUG EXCIPIENT COMPATIBILITY STUDY : 

e.g DRUG EXCIPIENT COMPATIBILITY STUDY a) DSC of Captopril b) DSC of PVP C) DSC of 1:1 physical mixture of Drug:PVP Conclusion: Incompatibility Reason: Absence of melting endotherm & exotherm is broad. (Ref: C.A.,Volume-148,No:20, May 19,2008 ) 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.5) Study of polymorphism e.g:-DSC Curves of two mannitol polymorphs : 

7.5) Study of polymorphism e.g:-DSC Curves of two mannitol polymorphs 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

e.g: Analysis of polymorphic form of Naloxane hydrochloride - FTIR,TGA & X-RAY POWDER DIFFRACTION were used to research the various polymorphic form of Naloxane hydrochloride.(Ref: C.A.,Volume-149,No:3,July 21,2008 ) : 

e.g: Analysis of polymorphic form of Naloxane hydrochloride - FTIR,TGA & X-RAY POWDER DIFFRACTION were used to research the various polymorphic form of Naloxane hydrochloride.(Ref: C.A.,Volume-149,No:3,July 21,2008 ) 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.6) Prediction of stability of drug : 

7.6) Prediction of stability of drug STABILITY TEST Required longest time in development of Drug Thermal analysis is ideal technique to solve this problem. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

ADVANTAGE OF THERMAL ANALYSIS IN PREDICTION OF STABILITY : 

ADVANTAGE OF THERMAL ANALYSIS IN PREDICTION OF STABILITY 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.7) Degree of crystallinity : 

7.7) Degree of crystallinity Partial crystallinity is also a type of polymorphism. The degree of crystallinity was determined by solution calorimetry. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

The Disappearance of the DSC peak of the drug is the proof of Complexation in solid state. Figure shows , that no complexation was obtained for a drug with ß-cyclodextrin. 7.8) Study of complexes & inclusion compound 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.9) Study of Thermal behaviour of Sugar esters:- : 

7.9) Study of Thermal behaviour of Sugar esters:- They have wide range of HLB value so they can be used as surfactant or penetration enhancer. Aim of this study, to measure thermal properties of Sugarester & to differentiate sugarester with HLB. Thermal properties are measured with modulated DSC,& combined with HOT STAGE MICROSCOPY to visualised changes in sample during heating. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

7.10)Defining phase transitions & electrical behavior of D & L Amino acid by thermal analytical method. : 

7.10)Defining phase transitions & electrical behavior of D & L Amino acid by thermal analytical method. The chiral difference in the D & L Amino acid has been clearly revealed by Dielectrical analysis ( DEA ) Powder X-ray diffraction of three sets of D & L Amino acid further illustrated the chiral differences. ( Ref: C.A.,Volume-148,No: 25,June 23, 2008 ) 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

8) FT-IR SPECTROMETER : 

8) FT-IR SPECTROMETER New technique in preformulation. Generally used in combination with other techniques. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

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ADVANTAGE: 1) Simple 2) Sensitive 3) Accurate 4) Speedy DISADVANTAGE: 1) Generally not used alone. 2) Gives peak at same wave number, e.g so can not differentiate polymorph. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

9) X-RAY POWDER DIFFRACTION : 

9) X-RAY POWDER DIFFRACTION Why only x-ray are used? Because x-rays have wavelengths of about the same magnitude as the distance between the atoms or molecules of crystal. PRINCIPLE: X-ray are Diffracted & order of this diffraction is measured in form of graph. Diffraction occur as a result of the interaction of radiation with electron of atom. 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

Applications of x-ray diffraction:- : 

Applications of x-ray diffraction:- 1) For structure determination 2) Identification of Impurity 3) Characterization of polymorphism 4) Characterize spray dried & crystalline material 5) For particle size & shape analysis e.g. Accurate determination of oxide nano particle size & shape based on X-ray powder diffraction pattern. ( Ref: C.A.,Volume-149,No: 1,July 7,2008 ) 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

10) Limitations of Thermal analysis:- : 

10) Limitations of Thermal analysis:- 1)low sensitivity for transitions involving small energies. 2)Impurity consisting of molecules of same size,shape,& character as those of the major component are not detected by DSC. 3)TGA used to studies hydrates & moisture study are not always reliable. 4)Thermal analysis are affected by number of factors . 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

11)REFERENCES : 

11)REFERENCES 1) The science of dosage form Design m.e Aulton 2) Physical pharmacy,Alfard martin,fourth edition. 3) The science & practice of pharmacy,remington,20th edition. 4) Instrumental methods of analysis ,willard ,7th edition 5) Encyclopedia of pharmaceutical technology ,swarbrick & boylan vol-15 6) Chemical abstract, Volume-149,No: 3,July 21, 2008 7) Chemical abstract,Volume-148,No: 25,June 23,2008 8) Chemical abstract,Volume-149,No: 1, July 7,2008 9) Chemical abstract,Volume-148,No: 20, May 19,2008 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

12)Study Questions :- : 

12)Study Questions :- 1) Explain the role of thermal analysis in preformulation (Guj. Uni. 2006) 2) Explain the application of any one technique based on thermal analysis? (Guj. Uni. 2005) 3) Enlist the modern technique and explain any one combined technique based on thermal analysis. (First internal 2006) 4) What do you mean by thermal analytical method?(first internal 2006) 5) What are the limitation of these method? 6) Application of thermal analysis in Preformulation. (Guj UNI.2007) 24/09/2008 PAPER 411/JIGNESH B.GAVIT(M.Pharm-1 2008-09)/LMCP

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THANK YOU