ICT Prague > Central Laboratories > Laboratory of Thermal Analysis

Laboratory of Thermal Analysis

Laboratory | Principles of methods | Instrumental equipment | Usage of TG, DTA and DSC applications | Samples requirements | Contact

Laboratory

In Laboratory of Thermal Analysis is carried on the thermal analysis of organic and inorganic samples using these methods:

·   Thermogravimetric analysis (TGA)

·   Differential thermal analysis (DTA)

·   Differential scanning calorimetry (DSC)

Principles of methods

Thermogravimetric analysis (TGA)

Method is based on the measurement of the weight loss (resp. weight gain) of the material as a function of temperature and time. Sample of analyzed substance is heated (constant heating rate or in isothermal mode) during continuous weighting. Results are displayed on thermogravimetric graph - thermogram.

Differential thermal analysis (DTA)

Sample of analyzed substance and reference sample (thermal stable sample) are heated by controlled heating rate. Temperature difference between sample and reference is measured by thermocouple. This difference describes heat affected and heat production processes in time.

Differential scanning calorimetry (DSC)

Differential scanning calorimetry (DSC) is based on same principles as DTA. Differences between sample temperature and reference temperature are measured and convert by software to energy units. After mathematic conversion the value is called Heat Flow.

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Instrumental equipment

Simultaneous instrument for TG a DTA Setsys Evolution (in the middle) designed by Setaram. Maximum furnace temperature is 1600 °C, type of measurements: DTA-MS or TG-MS = DTA (TGA) + mass spectroscopy analysis of combustion products. Mass spectroscopy is carried out on mass-spectroscopy analyzer OmniStarTM designed by Pfeiffer Vakuum (on the left). Mass spectrometer is based on principles quadrupole mass analyzer (mass-to-charge ratio m/z), operating range: 300 amu. Type of operating gas: air, nitrogen or argon; operating temperature range: 30-1600°C

http://www.vscht.cz/clab/lta/obrazky/tg_dta.jpg

Differential scanning calorimetry carried on DSC 131 by Setaram (right side in the picture). Operating temperature range: 25°C (in case of liquid nitrogen cooling (-150°C)) or normal range 25-700°C; supplied external cooling device: range -50 - +400°C.

Thermogravimetric AnalyserPyris 1 TGA by Perkin ElmerTM Instruments; maximum furnace temperature is 1000°C, associated with FT-IR spectrometer Spectrum 100 by Perkin ElmerTM Instruments used for analysis of compunction product connected to gaseous output. FT-IR analyzer’s wavenumber range is 7 800–350 cm–1. Operating gas: air or nitrogen; operating temperature range: 30-1000°C.

http://www.vscht.cz/clab/lta/obrazky/tg_1000.jpg

 

 

 

Thermobalance Stanton Redcroft TG 750 (Tmax = 900 °C), Temperature range: ambient to 900°C

Heating rates: 1, 2, 3, 10, 15, 20, 30, 50, 100°C.min-1, Programme modes: Heat-Hold; Heat.Off; Cool-Hold; Cool-Off; Isothermal

Sample size: 0.1mg - 100mg

Balance ranges: 1 - 200mg

Atmosphere: flowing air or inert gas

Data collection and acquisition additionally installed

 

http://www.vscht.cz/clab/lta/obrazky/tg_900.jpg

 

Two devices for DTA (self-made in our laboratory) temperature operating range: 25 - 1000 °C or 25 - 1300 °C

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Usage of TG, DTA a DSC applications

·   Thermal decomposition of inorganic and organic substances

·   Dehydratation of hydrates and minerals

·   Thermal stability of materials

·   Pyrolysis of coal, petroleum and wood

·   Roasting and calcining minerals

·   Determination of moisture, volatiles and ash contents

·   Degradation of polymeric materials

·   Corrosion of metals

·   Solid-state reaction

·   Evaporation of liquids

·   Infrared spectroscopy analysis of gaseous products (TGA-IR)

·   Mass spectroscopy of gaseous products (TG+DTA-MS)

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Samples requirements

·   Samples should be prepared suitable for selected analyses – no any special preparation of samples will take place in our laboratory

·   Samples for analysis have to be in liquid or solid phase

·   Solid samples – preferably in powder state or little pieces

·   Samples amount: 1 mg – 100 mg - depends on technique type  (consultation recommended)

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Contact

Ing. (MSc) Anežka Veselá
Head of laboratory

Phone: +420 220 443 839
E-mail: Anezka.Vesela

RNDr. (MSc) Jana Ederová, CSc. (PhD)
Phone: +420 220 443 834
E-mail: Jana.Ederova

Ing. (MSc) Jiří Endrýs, CSc. (PhD)
Phone: +420 220 443 258
E-mail: Jiri.Endrys

Michaela Tomková
Phone: +420 220 443 834
E-mail: Michaela.Tomkova

Ing. (MSc) Přemysl Janík
Phone:+420 220 443 258
E-mail: Premysl.Janik

Location

ICT Prague
Building B

Basement, door n. S28
Technická 3, 166 28 Praha 6

Czech Republic

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