LABORATORY OF CALORIMETRY
New building, B-block, 5th floor, Lab No. img, Department of Inorganic Chemistry, Faculty of Chemical and Food Technology STU
Head: doc. Ing. Blažena Papánková, PhD.
Differential Scanning Calorimetry (DSC)
DSC measures the amount of energy absorbed or released by a sample as it is heated, cooled or held at a constant temperature. DSC also performs precise temperature measurements.
There are two types of DSCs:
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Heat flux DSC
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Power Compensation DSC
The heat flux DSC
In this design, both sample and reference pans are heated by a single furnace, which is much larger in mass than the furnaces used in a power compensation DSC. The temperature vs. time profile through a phase transition in a heat flux instrument is not linear. At a phase transition, there is a large change in the heat capacity of the sample, and this leads to a difference in temperatures between the sample and reference pan. Mathematical equations convert the signal into heat flow information.
The power compensation principle
When an event occurs in the sample material, sensitive Platinum Resistance Thermometers (PRTs) detect the change in the sample, and power (energy) is applied to or removed from the sample furnace to compensate for the change in heat flow to or from the sample. As a result, the system is maintained at a “thermal null” state at all times. The amount of power required to maintain system equilibrium is directly proportional to the energy changes occurring in the sample. No complex heat flux equations are necessary with a power compensation DSC because the system directly measures energy flow to and from the sample.
Additionally, power compensation DSC benefits include enhanced modulated temperature DSC (StepScan) technique and fast scan DSC (HyperDSC) for dramatic improvements in productivity, as well as greater sensitivity.
Advanteges over heat flux DSC are rapid heating and cooling rates up to 500 C/min. It increases your lab's productivity. Power compensation DSC provides the best possible
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resolution
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sensitivity
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fast scan DSC using HyperDSC
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modulated temperature DSC using StepScan
DSC is used to analyze melting, crystallization, glass transition, oxidative induction time (OIT), polymorphism, purity, specific heat, kinetic studies, curing reactions, denaturation, etc. Here are some practical applications:
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Characterization of Single Fibers for Forensic Applications Using High Speed DSC
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High Resolution Characterization of Pharma Polymorphs Using Power Compensation DSC
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DSC Isothermal Crystallization Studies for Better Injection Molding of Polymers
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High Sensitivity Measurement of Magnetic Coatings Using StepScan DSC
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Characterization of Fats in Cookies Using Power Compensation DSC
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High Sensitivity Characterization of Transparency Films Using High Speed DSC
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Better DSC Isothermal Cure Kinetics Studies Using Power Compensation DSC
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Better Characterization of Hot Melt Adhesives Using the PYRIS Power Compensation DSC
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Determination of Rigid and Mobile Amorphous Content of Semicrystalline Polymers Using DSC
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Importance of DSC Rapid Cooling for the Analysis of Plastic Microwave Food Trays
Instrumental equipment of the Laboratory of Calorimetry
Instrument specifications
Features/Benefits include:
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Unique power compensation design
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HyperDSC, the leading fast scan DSC technique
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StepScan, for modulated temperature DSC
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Superior signal resolution and sensitivity
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Highest caloric accuracy
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Multiple cooling options for a temperature range of –170 °C to 730 °C
DSC Type
Power compensation temperature null principle. Measures temperature and energy directly, rather than differential temperature (DT).
DSC Cell
Independent dual furnaces constructed of platinum-iridium alloy with independent platinum resistance heaters and temperature sensors with furnace mass less than 1g.
Temperature Sensors
Distributed, Platinum Resistance Thermometers for best linearity.
Atmosphere
Static or dynamic, including nitrogen, argon, helium, carbon dioxide, air, oxygen or other inert or active gases, over full temperature range. Oxygen can be used up to 730 °C which allows easy cleaning.
Temperature
Range -170 °C to 730 °C
Accuracy / Precision ±0.1 °C / ±0.01 °C
Calorimetry
Accuracy / Precision < ±1% / < ±0.1%
Scanning Rates
Heating/Cooling 0.01 °C to 500 °C/min
Temperature Overshoot
100 °C/min < 0.1 °C
Cooling Times
Ambient Coolant 725 °C to 100 °C (under 4 minutes)
Liquid Nitrogen Coolant 200 °C to -150 °C (under 2 minutes)
Cooling Options
Ice Water 25 °C to 730 °C
Circulating Liquid -10 °C to 730 °C
Refrigerator (Intracooler) -70 °C to 730 °C
Automatic Liquid N2 (CryoFill) -170 °C to 300 °C
Autosampler
The Diamond DSC Autosampler can run up to 44 sample positions unattended. It has the ability to be customized through Pyris Player to meet your analysis needs and increase productivity.
High Pressure Cell
Extends the capabilities of the power compensation Diamond DSC design to elevated pressure measurements. Pressure range is up to 42 bar (600 psi).
Quality Assurance
Developed under ISO 9001