- 1.GUIDED BY:PRESENTED BY:Dr.R.K.Parikh AHALGAMA JIGNESH VDEPARTMENT OF PHARMACEUTICS ANDPHARMACEUTICAL TECHNOLOGY M.Pharm -1 (2011-12)L.M.COLLEGE OF PHARMACY Roll no :- 09AHMEDABAD-380009
2. Thermal analysis Classification of thermal analysis Differential thermal analysis(DTA) Principle InstrumentationAdvantage and Disadvantage Application References Ahalgama Jignesh V. , M-Pharm-1(paper code- 2/25 910102), DTA,LMCP,GTU(2011-12)) 3. Thermal analysis incorporates those techniques inwhich some physical parameter of the system is derivedand/or recorded as a function of temperature. Matter is heated it undergoes physical and chemicalchanges occur. physical change: melting or boiling ,weight loss,gasevolution. chemical change:decomposition or reaction take place. Ahalgama Jignesh V. , M-Pharm-1(paper code- 910102), DTA,LMCP,GTU(2011-12))3/25 4. Sr no TechniqueParameterInstrumentGraph measured used1 Thermogravimetry mass thermobalance Mass vs.temp or time2 Derivative dm/dtthermobalance dm/dt vs.thermogravimetrytemp.3 Differential thermal Delta TDTA apparatus Delta T vs.analysistemp.4 Differential dH.dtcalorimeter dh/dt vs.scanningtemp.calorimetry5 Thermometric temperaturecalorimeter Temp vs.titrimetrytitrant volume(Cont..)Ahalgama Jignesh V. , M-Pharm-1(paper code-4/25910102), DTA,LMCP,GTU(2011-12)) 5. 6 DynamicReflectanceSpectrophot%Reflectance ometer reflectancespectroscopy and temp7 Evolved gas Thermal ThermalT.C vs.detectionconductivity conductivity temp.cell8 ThermoVolume or dilatometerVolume ormechanicallength length vs.analysis temp.9 ElectricalCurrent orelectrometer I or R vs.conductivityresistance temp.10 EmanationRadioactivity ETAE vs. temp. thermalapparatus analysisAhalgama Jignesh V. , M-Pharm-1(paper code-910102), DTA,LMCP,GTU(2011-12)) 5/25 6. Combination withthermogravimetry 1)for better interpretation a) TG DTAb) TG DSC 2)for identification of gas involved inthermal analysisa) TG MS b) TG GC MSAhalgama Jignesh V. , M-Pharm-1(paper code-6/25910102), DTA,LMCP,GTU(2011-12)) 7. TG/DTA Simultaneous Measuring InstrumentSimultaneousTG/DTAimproves easeof operation,sensitivity andanalyticalaccuracy . Ahalgama Jignesh V. , M-Pharm-1(paper code- 910102), DTA,LMCP,GTU(2011-12)) 7/25 8. Principle:A technique in which the temperature differencebetween a substance and a reference(Al2o3) materialis measured as a function of temperature while thesubstance and reference are subjected to a controlledtemperature program. endothermic and exothermic peak. endothermic and exothermic reaction.Ahalgama Jignesh V. , M-Pharm-1(paper code-910102), DTA,LMCP,GTU(2011-12)) 8/25 9. T vs. temperatureT Temp.Ahalgama Jignesh V. , M-Pharm-1(paper code-9/25910102), DTA,LMCP,GTU(2011-12)) 10. Ahalgama Jignesh V. , M-Pharm-1(Pharmaceutical technology & Pharmaceutics, 10/25DTA,LMCP(2011-12)) 11. 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 refrectorytube. Ahalgama Jignesh V. , M-Pharm-1(paper code- 11/25 910102), DTA,LMCP,GTU(2011-12)) 12. 1) SENSOR2) CONTROL ELEMENT3) HEATERAhalgama Jignesh V. , M-Pharm-1(paper code-12/25910102), DTA,LMCP,GTU(2011-12)) 13. 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.Ahalgama Jignesh V. , M-Pharm-1(paper code-13/25910102), DTA,LMCP,GTU(2011-12)) 14. Ahalgama Jignesh V. , M-Pharm-1(paper code-14/25910102), DTA,LMCP,GTU(2011-12)) 15. 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.Ahalgama Jignesh V. , M-Pharm-1(paper code-910102), DTA,LMCP,GTU(2011-12))15/25 16. 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 impuritycurves could be compared with the curve of referencestandard. Ahalgama Jignesh V. , M-Pharm-1(paper code- 16/25 910102), DTA,LMCP,GTU(2011-12)) 17. 5) Studying and characterizing polymersThermochimica 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. Ahalgama Jignesh V. , M-Pharm-1(paper code- 17/25 910102), DTA,LMCP,GTU(2011-12)) 18. 6) Detection of eutectic mixture: binary mixture :two endotherm eutectic mixture : single major endotherm.7) generation of phase diagram andphase 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.Ahalgama Jignesh V. , M-Pharm-1(paper code- 18/25910102), DTA,LMCP,GTU(2011-12)) 19. Ahalgama Jignesh V. , M-Pharm-1(paper code-19/25910102), DTA,LMCP,GTU(2011-12)) 20. 8) Application of DTA to compatibility and stability problems in penicillin stearic acid mixturejournal 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=compatibleAhalgama Jignesh V. , M-Pharm-1(paper code-20/25910102), DTA,LMCP,GTU(2011-12)) 21. (9) Comparative physical-chemical charecterizationof encapsulated lipid based ISOTRETINOINproduct by thermal behavior analysisThermochimica acta 505 ,(2010),73-78. Use in nodular acne. Study the three encapsulated product (1 reference and 2generic).measure thermal behavior of that product no specificchange and more thermostable than isotretinoin.Ahalgama Jignesh V. , M-Pharm-1(paper code-21/25910102), DTA,LMCP,GTU(2011-12)) 22. (10) Physiochemical charecterization of edaravonewith 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. Ahalgama Jignesh V. , M-Pharm-1(paper code- 22/25 910102), DTA,LMCP,GTU(2011-12)) 23. Remingtons 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.Ahalgama Jignesh V. , M-Pharm-1(paper code- 23/25910102), DTA,LMCP,GTU(2011-12)) 24. Principle and Instrumental analysis, skoog-hollar-nieman, 5th editio.Chemical Abstract vol:146, No:25,June 18 :2007,507180Instrumental methods of chemical analysis,gurdeep r.chatwal,2008. www.linseis.net www.nd.eduwww.shimadzu.lacerta-technology.comwww.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 910102), DTA,LMCP,GTU(2011-12)) 25. Ahalgama Jignesh V. , M-Pharm-1(paper code-25/25910102), DTA,LMCP,GTU(2011-12))
