Differential scanning calorimetry (DSC) is a destructive technique to study thermal transitions in materials over a wide range of temperatures. This thermoanalytical tool is used to monitor changes in heat capacity of a material as a function of temperature. In this technique, heat flow through a known weight of sample is measured upon heating or cooling the sample over time against a reference material having a clearly defined heat capacity. Read more about Differential Scanning Calorimetry (DSC) Analysis below.
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Introduction to Differential Scanning Calorimetry
Differential scanning calorimetry is a powerful and sensitive thermoanalytical technique. In this destructive technique, the difference in the amount of heat required to increase the temperature of a sample and a reference is measured as a function of temperature. DSC is used to measure the energy transferred to or from a sample undergoing a physical or chemical change, hence it determines alterations in structural properties of a sample as a function of time and temperature.
DSC is widely used in several industries such as polymers and composites, nanomaterials, membranes and films, biological materials, pharmaceuticals, food industry and research, electronics, drug delivery and interactions.
Figure 1: SC thermogram of bisphenol A/aniline benzoxazine monomer.
Figure 2: Schematic of the combined DSC/SAXS/WAXS experiment
Types of Differential Scanning Calorimetry
There are two types of DSCs based on the mechanism of operation.
Heat-flux DSC. In this type, the sample and empty reference pans are placed on a thermoelectric disk enclosed in a furnace. The furnace is heated at a linear rate, transferring heat to the pans through the disk. The temperature difference between both the pans is measured by thermocouples and is converted into a heat flow signal via a calibration procedure.
Power-compensated DSC: In this type, separate furnaces house the sample and reference pans while maintaining them at the same temperature. Temperature is changed according to a predetermined programme. The difference in thermal power needed to keep them at the same temperature is determined and plotted as a function of time or temperature.
Uses of Differential Scanning Calorimetry
This versatile technique is operated in a dry state and is quite useful in characterizing the crystals between size range 1–100 nm. DSC provides information about the wide range of structural aspects such as arrangement of the crystal components, and macroscopic information like mean shape and size of crystalline samples. DSC is also used to phase transition temperatures (Tg, Tm) and heat capacities (Cp) of analytes.
Other uses involve determination of heat of fusion and extent of crystallization for the crystalline materials, the cure behavior of thermoset monomers or oligomers oxidative stability, thermal degradation, and water loss in a sample.
DSC is also used to evaluate thermal reversibility of protein degradation; eutectic point and construction of phase diagrams; effect of hardeners on the thermal properties of cured materials; heat and degree of curing reaction, and residual cure.
Other uses of DSC involves determination of drug–lipid interactions, the status of the lipid, and melting and recrystallization behaviors of the nanostructured lipid carriers (NLCs), determination of thermodynamics of nucleic acid-folding transitions (DNA and RNA), analysis of physicochemical transformation during starch gelatinization process,prediction of the storage life of food products and determination of glass transition temperature (Tg) to determine the miscibility of biopolymer blends.
Strengths and Limitations of Differential Scanning Calorimetry
DSC is a convenient and low cost method of studying thermal transitions in various materials. It can be used for a wide range of temperatures (−90 to 550°C) and utilizes a low amount of sample. This is quite a sensitive method where the slightest phase transitions are captured.
On the other hand, DSC is a destructive analysis technique, so analysis of heterogeneous materials is difficult. This does not detect generation of gases and cannot be used for elemental analysis purposes. Sensitivity of the methods reduces in the instances of overlapping in some phase transitions. Samples that might sublime or evaporate during the procedure are most likely to give inaccurate results as a constant mass of the sample is required throughout the test.
Key elements of Differential Scanning Calorimetry (DSC) Analysis
Characterizes thermal phase transitions (e.g. melting, crystallization, Tg) and measuring heat of fusion and heat of crystallization. The information can be used to determine best processing temperatures, obtaining thermal fingerprints of the materials; comparing thermal properties of the materials with different performance (ASTM E 793-06; ASTM E 794-06)
Determines specific heat capacity (ASTM E1269-11) of pure compounds or mixtures
Determines purity of relatively pure substances (ASTM E 928-08)
Determines phase separation of polymer blend, copolymers
Characterizes cure process, glass transition temperature of the cured sample and residue cure
Performs Oxidation Induction Time (OIT) (ASTM D 3895)
Modulates DSC to determine weak subtle transitions and to separate overlapping thermal events
Assesses thermal stability (ASTM E 537-12)
Prepares kinetic study of chemical reaction or decomposition (ASTM E 698-11)
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The turnaround time for types and uses of dsc test methodology depends upon the test procedure mentioned in the standard test document. However, we at MaTestLab understand your research requirements and hence try to get your test completed within the least possible time.
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You can share your types and uses of dsc testing requirements with MaTestLab. MaTestLab has a vast network of material testing laboratories, spread across the USA and Canada. We support your all material testing needs ranging from specific types and uses of dsc test to various testing techniques.
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