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Differential scanning calorimetry
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==Types== There are two main types of DSC: ''Heat-flux DSC'' which measures the difference in heat flux between the sample and a reference (which gives it the alternative name ''Multi-Cell DSC'') and ''Power differential DSC'' which measures the difference in power supplied to the sample and a reference.<ref>{{Cite journal |last1=Yurchenko |first1=Olena |last2=Pernau |first2=Hans-Fridtjof |last3=Engel |first3=Laura |last4=Wöllenstein |first4=Jürgen |date=2023-06-16 |title=Differential thermal analysis techniques as a tool for preliminary examination of catalyst for combustion |journal=Scientific Reports |language=en |volume=13 |issue=1 |pages=9792 |doi=10.1038/s41598-023-36878-8 |pmid=37328603 |issn=2045-2322|pmc=10276022 |bibcode=2023NatSR..13.9792Y }}</ref><ref>{{cite journal | vauthors = Höhne G, Breuer KH, Eysel W| title = Differential scanning calorimetry: Comparison of power compensated and heat flux instruments | journal = Thermochimica Acta | volume = 69| issue = 1–2 | pages = 145–151 | date = October 1983 |doi=10.1016/0040-6031(83)85073-4| bibcode = 1983TcAc...69..145H }}</ref> ===Heat-flux DSC=== With Heat-flux DSC, the changes in heat flow are calculated by integrating the ΔT<sub>ref</sub>- curve. For this kind of experiment, a sample and a reference crucible are placed on a sample holder with integrated temperature sensors for temperature measurement of the crucibles. This arrangement is located in a temperature-controlled oven. Unlike the traditional design, the special feature of heat-flux DSC is that it uses flat temperature sensors placed vertically around a flat heater. This setup makes it possible to have a small, light, and low-heat capacity structure while still working like a regular DSC oven.<ref>{{cite journal|vauthors=Missal W, Kita J, Wappler E, Gora F, Kipka A, Bartnitzek T, Bechtold F, Schabbel D, Pawlowski B, Moos R|publisher=Elsevier|year=2010|pages=940–943|title= Miniaturized Ceramic Differential Scanning Calorimeter with Integrated Oven and Crucible in LTCC Technology|journal=Procedia Engineering|volume=5|doi=10.1016/j.proeng.2010.09.263|issn=1877-7058|doi-access=free}}</ref> ===Power differential DSC=== For this kind of setup, also known as ''Power compensating DSC'', the sample and reference crucible are placed in thermally insulated furnaces and not next to each other in the same furnace as in heat-flux-DSC experiments.<ref>{{Cite web |last=IOM3 |title=Simultaneous thermal analysis |url=https://www.iom3.org/resource/simultaneous-thermal-analysis.html |access-date=2024-07-27 |website=www.iom3.org}}</ref> Then the temperature of both chambers is controlled so that the same temperature is always present on both sides. The electrical power that is required to obtain and maintain this state is then recorded rather than the temperature difference between the two crucibles.<ref>{{cite book|vauthors=Höhne G, Hemminger WF, Flammersheim HJ|title=Differential Scanning Calorimetry|publisher=Springer-Verlag|year=2003|pages=17 ff|isbn=978-3-540-00467-7}}</ref> ===Fast-scan DSC=== The 2000s have witnessed the rapid development of Fast-scan DSC (FSC),<ref>{{cite book|vauthors=Schick C, Mathot V |title=Fast Scanning Calorimetry |publisher=Springer |year=2016| isbn=978-3-319-31329-0}}</ref> a novel calorimetric technique that employs micromachined sensors. The key advances of this technique are the ultrahigh scanning rate, which can be as high as 10<sup>6</sup> K/s, and the ultrahigh sensitivity, with a heat capacity resolution typically better than 1 nJ/K.<ref>{{cite journal | vauthors = Poel GV, Mathot V| title = High-speed/high performance differential scanning calorimetry (HPer DSC): Temperature calibration in the heating and cooling mode and minimization of thermal lag | journal = Thermochimica Acta | volume = 446| issue = 1–2 | pages = 41–54 | date = March 2006 | doi = 10.1016/j.tca.2006.02.022| bibcode = 2006TcAc..446...41V }}</ref> Nanocalorimetry <ref>{{cite book|vauthors=Garden JL, Bourgeois O |title= Nanocalorimetry. In: Bhushan B. (eds) Encyclopedia of Nanotechnology |publisher=Springer, Dordrecht |year=2016| doi = 10.1007/978-94-017-9780-1_208}}</ref> has attracted much attention in materials science, where it is applied to perform quantitative analysis of rapid phase transitions, particularly on fast cooling. Another emerging area of application of FSC is [[physical chemistry]], with a focus on the thermophysical properties of thermally labile compounds. Quantities like [[Melting point|fusion temperature]], [[Enthalpy of fusion|fusion enthalpy]], [[Sublimation (phase transition)|sublimation]], and [[Vapor pressure|vaporization pressures]], and [[Enthalpy of vaporization|enthalpies]] of such molecules became available.<ref>{{cite journal | vauthors = Schick C, Mukhametzyanov TA, Solomonov BN | title = Fast Scanning Calorimetry of Organic Materials from Low Molecular Mass Materials to Polymers | journal = Reviews and Advances in Chemistry | volume = 11| issue = 1–2 | pages = 1–72 | date = September 2021 | doi = 10.1134/S2079978021010064| s2cid = 237539353 }}</ref> ===Temperature Modulated DSC=== When performing Temperature Modulated DSC (TMDSC, MDSC), the underlying linear heating rate is superimposed by a sinusoidal temperature variation. The benefit of this procedure is the ability to separate overlapping DSC effects by calculating the reversing and the non-reversing signals. The reversing heat flow is related to the changes in specific heat capacity (→ glass transition) while the non-reversing heat flow corresponds to time-dependent phenomena such as curing, dehydration and relaxation.
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