differential thermal analysis
{{Short description|Thermoanalytic technique similar to differential scanning calorimetry}}
{{Infobox chemical analysis
|name = Differential thermal analysis
|acronym = DTA
|classification = Thermal analysis
|related = Differential scanning calorimetry
Isothermal microcalorimetry
Dynamic mechanical analysis
Thermomechanical analysis
Thermogravimetric analysis
Dielectric thermal analysis
}}
Differential thermal analysis (DTA) is a thermoanalytic technique that is similar to differential scanning calorimetry. In DTA, the material under study and an inert reference are made to undergo identical thermal cycles, (i.e., same cooling or heating programme) while recording any temperature difference between sample and reference.{{cite web|last=Bhadeshia|first=H.K.D.H.|title=Thermal analyses techniques. Differential thermal analysis|publisher=University of Cambridge, Material Science and Metallurgy|url=https://www.phase-trans.msm.cam.ac.uk/2002/Thermal1.pdf|access-date=2023-09-17}} This differential temperature is then plotted against time, or against temperature (DTA curve, or thermogram). Changes in the sample, either exothermic or endothermic, can be detected relative to the inert reference. Thus, a DTA curve provides data on the transformations that have occurred, such as glass transitions, crystallization, melting and sublimation. The area under a DTA peak is the enthalpy change and is not affected by the heat capacity of the sample.
Apparatus
A DTA consists of a sample holder, thermocouples, sample containers and a ceramic or metallic block; a furnace; a temperature programmer; and a recording system. The key feature is the existence of two thermocouples connected to a voltmeter. One thermocouple is placed in an inert material such as Al2O3, while the other is placed in a sample of the material under study. As the temperature is increased, there will be a brief deflection of the voltmeter if the sample is undergoing a phase transition. This occurs because the input of heat will raise the temperature of the inert substance, but be incorporated as latent heat in the material changing phase.{{cite book | author= Robert Bud, Deborah Jean Warner|title=Instruments of Science |year=1998 | isbn = 9780815315612| url = https://books.google.com/books?id=1AsFdUxOwu8C&pg=PA170 | pages =170–171|publisher=Taylor & Francis }} It consist of inert environment with inert gases which will not react with sample and reference. Generally helium or argon is used as inert gas.
Today's instruments
In today's market most manufacturers don't make true DTA systems but rather have incorporated this technology into thermogravimetric analysis (TGA) systems, which provide both mass loss and thermal information. With today's advancements in software, even these instruments are being replaced by true TGA-DSC instruments that can provide the temperature and heat flow of the sample, simultaneously with mass loss.
Applications
A DTA curve can be used only as a finger print for identification purposes but usually the applications of this method are the determination of phase diagrams, heat change measurements and decomposition in various atmospheres.
DTA is widely used in the pharmaceutical{{cite journal | last1=Ferrer | first1=S. | last2=Borras | first2=J. | last3=Martin-Gil | first3=J. | last4=Martin-Gil | first4=F.J. | title=Thermal studies on sulphonamide derivative complexes | journal=Thermochimica Acta | publisher=Elsevier BV | volume=147 | issue=2 | year=1989 | issn=0040-6031 | doi=10.1016/0040-6031(89)85187-1 | pages=321–330}}{{cite journal | last1=Ferrer | first1=S. | last2=Borras | first2=J. | last3=Martin-Gil | first3=J. | last4=Martin-Gil | first4=F.J. | title=Thermal decomposition of sulphonamide derivative complexes | journal=Thermochimica Acta | publisher=Elsevier BV | volume=153 | year=1989 | issn=0040-6031 | doi=10.1016/0040-6031(89)85434-6 | pages=205–220}}{{cite journal | last1=Alzuet | first1=G. | last2=Ferrer | first2=S. | last3=Borrás | first3=J. | last4=Martín-Gil | first4=J. | last5=Martín-Gil | first5=F.J. | title=Thermal studies of sulphonamide derivative complexes | journal=Thermochimica Acta | publisher=Elsevier BV | volume=185 | issue=2 | year=1991 | issn=0040-6031 | doi=10.1016/0040-6031(91)80053-l | pages=315–333}} and food industries.{{cite journal | last1=BERGER | first1=K. G. | last2=AKEHURST | first2=E. E. | title=Some applications of differential thermal analysis to oils and fats | journal=International Journal of Food Science & Technology | publisher=Wiley | volume=1 | issue=3 | date=2007-06-28 | issn=0950-5423 | doi=10.1111/j.1365-2621.1966.tb01810.x | pages=237–247}}{{cite journal | last1=C. Ramos-Sanchez | first1=M | last2=Rey | first2=F.J. | last3=L. Rodriguez | first3=M | last4=Martin-Gil | first4=F.J. | last5=Martin-Gil | first5=J. | title=DTG and dta studies on typical sugars | journal=Thermochimica Acta | publisher=Elsevier BV | volume=134 | year=1988 | issn=0040-6031 | doi=10.1016/0040-6031(88)85216-x | pages=55–60}}{{cite journal | last1=Rey | first1=F.J. | last2=Ramos-Sanchez | first2=M.C. | last3=Rodriguez-Mendez | first3=M.L. | last4=Martin-Gil | first4=J. | last5=Martin-Gil | first5=F.J. | title=DTG and DTA studies on sugar derivatives | journal=Thermochimica Acta | publisher=Elsevier BV | volume=134 | year=1988 | issn=0040-6031 | doi=10.1016/0040-6031(88)85218-3 | pages=67–72}}{{cite journal | last1=L. Rodriguez-Mendez | first1=Ma | last2=Rey | first2=F.J. | last3=Martin-Gil | first3=J. | last4=Martin-Gil | first4=F.J. | title=DTG and DTA studies on amino acids | journal=Thermochimica Acta | publisher=Elsevier BV | volume=134 | year=1988 | issn=0040-6031 | doi=10.1016/0040-6031(88)85219-5 | pages=73–78}}
DTA may be used in cement chemistry,Ramachandran V.S. “Applications of differential thermal analysis in cement chemistry”. Chap. V, Chemical Publishing Co., Inc., New York (1969), 92. mineralogical research{{cite journal | last=Smykatz-Kloss | first=W. | title=Application of differential thermal analysis in mineralogy | journal=Journal of Thermal Analysis | publisher=Springer Science and Business Media LLC | volume=23 | issue=1–2 | year=1982 | issn=0022-5215 | doi=10.1007/bf01908484 | pages=15–44| s2cid=93921297 }} and in environmental studies.{{cite book | last1=Smykatz-Kloss | first1=W. | last2=Heil | first2=A. | last3=Kaeding | first3=L. | last4=Roller | first4=E. | title=Thermal Analysis in the Geosciences | chapter=Thermal analysis in environmental studies | series=Lecture Notes in Earth Sciences | date=1991 | volume=38 | publisher=Springer-Verlag | publication-place=Berlin/Heidelberg | isbn=3-540-54520-4 | doi=10.1007/bfb0010275 | pages=352–367}}
DTA curves may also be used to date bone remains{{cite journal|last1=Villanueva|first1=PrE|last2=Girela |first2=F. |last3= Castellanos |first3=M. |title=The application of differential thermal analysis and thermogravimetric analysis to dating bone remains|journal=Journal of Forensic Sciences|year=1976|volume= 21|issue=4|pages=822–830|doi=10.1520/JFS10567J |pmid=184235}} or to study archaeological materials.Misiego-Tejeda J.C., Marcos-Contreras G.J., Sarabia Herrero F.J., Martín Gil J. and Martín Gil F.J. "Un horno doméstico de la primera Edad del Hierro de "El Soto de Medinilla" (Valladolid) y su análisis por ATD". BSAA (University of Valladolid) 1993, LIX, 89 111.{{cite journal | last=KINGERY | first=W. D. | title=A note on the differential thermal analysis of archaeological ceramics | journal=Archaeometry | publisher=Wiley | volume=16 | issue=1 | year=1974 | issn=0003-813X | doi=10.1111/j.1475-4754.1974.tb01099.x | pages=109–112}}
Using DTA one can obtain liquidus & solidus lines of phase diagrams.