THERMAL ANALYSIS AND CALORIMETRY “Josep Carilla”
Scientific Supervisor: Josep LLuis Torres
The Thermal Analysis and Calorimetry laboratory (ATC) offers its services to IQAC groups, other CSIC institutes and university research groups, as well as R + D departments of the chemical-pharmaceutical, plastic, cosmetic and food industries. The service is mainly used for quality control, optimization of lyophilisation processes, storage temperature, drying isotherms, compatibilities active-excipient principle, polymorphism, obtaining isotherms of sorption-desorption, determination of the glass transition (Tg), compositional analysis of fibres, dilatometry studies, thermoporometry, coefficients of thermal expansion and studies of useful average life of materials.
Josep Lluis Torres
Scientific Supervisor
joseplluis.torres@iqac.csic.es
Sonia Pérez
Technical Supervisor
sonia.perez@iqac.csic.es
The ATC offers services through the following equipment:
- Differential Scanning Calorimetry, DSC & micro DSC
- Thermogravimetric Analysis, TGA
- Thermomechanical Analysis, TMA
- Dynamic vapour sorption, DVS
DSC calorimeters (heat flow)
The change of the difference in the heat flow to the sample and to a reference is analysed while they are subjected to a T alteration.
- DSC (821e, Mettler Toledo):
T range: -150 to 500 ⁰C
- DSC (823e, Mettler Toledo):
T range: 30 to 500 ⁰C
Applications: The technique is widely used across a range of applications, both as a routine quality test and as a research tool. DSC is widely used in pharmaceutical, polymer, cosmetic, textile and food industries. The DSC technique can be utilised in the following determinations:
- Phase transitions: determination of melting and crystallization points
- Study of polymorphism and pseudopolymorphism
- Determinations of glass transition temperature (Tg)
- Determinations of Cp
- Determinations of purities
- Measurement of thermal/oxidative stability
- Kinetic studies
- Study of polymers: curing, glass transitions, melting, crystallinity degree.
- Compatibility studies (API/excipients)
DSC microcalorimeter (heat flow)
The change of the difference in the heat flow to the sample and to a reference is analysed while they are subjected to a T alteration.
microDSC III (Setaram):
T range: -20 to 120 ⁰C
Applications: suited for low energy events (solid samples or dilute solutions):
- Proteins: denaturation, aggregation
- Fusion and gelification processes
- Phase transitions: liquid crystals, lipids
- Thermoporometry determinations
Thermogravimetric Analysis (TGA)
The change in weight of a sample is measured while it is heated or held at a constant temperature. Mass changes are used to detect the chemical or physical processes.
Applications: It is usually used to study the thermal stability of a material or its composition. Application areas include: medicine/pharmaceuticals, environment/recycling, chemistry/plastics, agriculture, food, glass/ceramics. The TGA technique can be utilised in the following determinations:
- Thermal/oxidative stability
- Decomposition kinetics
- Quantitative content analysis
- Quantitation of volatiles/moisture
- Pseudopolymorphism (determination of hydrates and solvates)
- Carbon black and ash content
Dynamic Vapour Sorption (DVS)
The change in weight of a sample is measured at a given temperature while it is subjected to varying conditions of humidity. Water vapour is most commonly used, but it’s also possible with organic solvents.
DVS analyser
- Q5000 SA(TA Instruments): T range: 5 to 85 ⁰C
HR control range: 0 to 98%
Applications: Determining the effect of exposure to controlled conditions of T and humidity is a valued tool in a wide range of materials: pharmaceuticals, fine chemicals, polymers, fibres, food, agricultural products, building materials and porous materials. The DVS technique can be utilised in the following determinations:
- Sorption/desorption isotherms → stability studies (scale-up, production and storage conditions).
- Quantification of amorphous content
- Polymorphism and pseudopolymorphism (hydrate and solvate formation)
Thermomechanical Analysis (TMA)
TMA determines the dimensional changes of a sample as a function of temperature and applied force.
TMA analyser
- TMA/SDTA (840, Mettler Toledo): T range: r.t. to 1100 ⁰C
Deformation modes
Different accessories enable you to perform measurements on solid samples, foams, films and fibres. The TMA supports the following measurement modes:
Probes and sample holders made of quartz glass
The following measuring probes are available:
- Probe with ball-point (3.0 mm)
The sample holder used depends on the type of sample and the application:
- Standard sample holder
- Film attachment device
- Fibber attachment device
- Bending device
It is an excellent tool for studying the behaviour of various materials such as thermoplastics, thermosets, elastomers, adhesives and coatings, films and fibres, metals, ceramics and composites. Application areas include: plastics, coatings and adhesives, electronic industry, pharmaceutical products or textile industry. The TMA technique can be utilised in the following determinations:
- Coefficient of thermal expansion
- Glass transition temperature (Tg)
- Creep behavior
- Delamination
- Softening point
- Expansion and shrinkage behavior
- Solid-solid transitions
- Melting, swelling and elastic behavior
