Nutshells of Thermal Analysis. Heat it up! Burn it! Thermal Analysis
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1 Nutshells of Thermal Analysis Heat it up! Burn it! 1 Thermal Analysis
2 Thermal Analaysis (TA) Techniques Abbreviations Full Names Measure DSC Differential Scanning Calorimetry Heat difference DMA Dynamic Mechanical Analysis Mechanical Stiffness and Damping TMA Thermomechanical Analysis Dimension TGA Thermogravimetric Analysis Mass DTA Differential Thermal Analysis Temperature Difference DIL Dilatometry Volume DEA Dielectric Thermal Analysis Dielectric Permittivity and Loss Factor EGA Evolved Gas Analysis Gaseous Decomposition Products TOA Thermo-Optical Analysis Optical Properties Many more.
3 Thermogravimetric Analysis (TG, TGA) Principle An analytical technique used to determine a material s thermal stability and its fraction of volatile components by measuring the change of a sample mass as a function of temperature or/and time. Mass changes of solid samples occurs when Type Process Mass Physical changes Chemical changes Gas adsorption Gas desorption Phase transition - Vaporization Phase transition - Sublimation Decomposition Breakdown reaction Gas reaction Chemisorption Gain Loss Loss Loss Loss (when losing gases) Loss (when losing gases) Gain or Loss Gain
4 Thermogravimetric Analysis (TG, TGA) Experimentals Temperature vs Time Programs Constant heating Gradually isothermal Isothermal Heating/cooling rate : 1 50 o C / min (typically 5 10 o C / min ) Sample size : mg (typically 5-20 mg) Atmosphere: In air or inert gas (He, Ar, N 2 ) or slow oxidation atm (1-5 % O 2 in He, N 2 ) Run: at least three times
5 Thermogravimetric Analysis (TG, TGA) Instrument Balance types : Horizontal sample pan and reference pan Vertical sample pan (usually no reference pan - cannot perform DTA, DSC)
6 Thermogravimetric Analysis (TG, TGA) Reading Data TGA of CaC 2 O 4 H 2 O
7 Thermogravimetric Analysis (TG, TGA) Reading Data TGA of CaC 2 O 4 H 2 O TG curve DTG curve
8 Thermogravimetric Analysis (TG, TGA) Reading Data Temperature and Mass Definitions Onset temperature (T onset ) Temperature of the process - temperature of the maximum mass loss rate (T 0 ) Residual Mass (M res )
9 Thermogravimetric Analysis (TG, TGA) Reading Data TGA of CaC 2 O 4 H 2 O In inert gas In air (or inert gas) TG curve DTG curve CaC 2 O 4 H 2 O (FW: , 100%) % (-H 2 O) CaC 2 O 4 (FW: , 87.67%) % (-CO) CaCO 3 (FW: , 68.50%) % (-CO 2 ) CaO (FW:56.077, 68.50%)
10 Thermogravimetric Analysis (TG, TGA) Reading Data Common gaseous molecules originating from inorganic compounds decomposing before melting point H 2 O, CO, CO 2, SO x, NO x, Cl 2, F 2, CH 3 OH, other solvents
11 Thermogravimetric Analysis (TG, TGA) Reading Data Software: NETZSCH Proteus (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement TG /mg ~430 C: Ca(OH) 2 -> CaO + H 2 O Onset*: C [1] cemi 1A 4d.dsv TG DTG DTG /(mg/min) [1] Temperature / C [1] -0.3 jacek.chwast@ees.kuleuven.be
12 Thermogravimetric Analysis (TG, TGA) Reading Data Software: NETZSCH Proteus (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement TG /mg ~430 C: Ca(OH) 2 -> CaO + H 2 O [1] cemi 1A 4d.dsv TG [1] Temperature / C jacek.chwast@ees.kuleuven.be
13 Thermogravimetric Analysis (TG, TGA) Reading Data Software: NETZSCH Proteus (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement TG /mg ~430 C: Ca(OH) 2 -> CaO + H 2 O [1] cemi 1A 4d.dsv TG Mass Loss (Marsh): Onset: C Inflection: C Mass Change: mg [1] Temperature / C jacek.chwast@ees.kuleuven.be
14 Thermogravimetric Analysis (TG, TGA) Reading Data Software: NETZSCH Proteus (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement TG /mg ~430 C: Ca(OH) 2 -> CaO + H 2 O Onset*: C [1] cemi 1A 4d.dsv TG DTG DTG /(mg/min) [1] Temperature / C [1] -0.3
15 Thermogravimetric Analysis (TG, TGA) Reading Data Factors affecting TG curve Instrumental Heating rate Furnace atmosphere and flow-rate Geometry of pan and furnace Material of pan Sample Mass Particle size (Make fine powders) Sample history/pre-treatment Packing (Make compact solids) Thermal conductivity Heat of reaction Sample purity In N 2 In air TG of CaC 2 O 4 H 2 O
16 Thermogravimetric Analysis (TG, TGA) Reading Data Backward TG curve (when combustion occurs)
17 Thermogravimetric Analysis (TG, TGA) Reading Data (i) no decomposition with loss of volatile products (ii) The rapid initial mass loss is characteristic of desorption or drying (dry the sample, redo the experiment) (iii) Single stage decomposition, (iv) Multi-stage decomposition with relatively stable intermediates (v) Multi-stage decomposition with no stable intermediate product. However heating-rate effect must be considered. At low heating rate, type (v) resemble type (iv) (vi) Gain in mass due to reaction with atmosphere, e.g. oxidation of metals. (vii) Oxidation product decomposes again at higher temperature; this is not often encountered.
18 Thermogravimetric Analysis (TG, TGA) Errors Mass Classical buoyancy Effect temp. on balance Convection and/or turbulence Viscous drag on suspension Noise / Erratic records Static Vibration Pressure pulses in lab. Uneven gas flow
19 Differential Thermal Analysis (DTA) Principle An analytical technique used to determine a material s phase diagram, heat change, and decompositions by measuring the any temperature difference between sample and reference (usually Al 2 O 3 ) as a function of time or temperature. Type Process Heat process Physical changes Chemical changes Adsorption Desorption Change in crystal structure Crystallization Melting, Vaporization, Sublimation Oxidation Reduction Breakdown reaction Chemisorption Solid state reaction Exothermic Endothermic Endo- or Exothermic Exothermic Endothermic Exothermic Endothermic Endo- or Exothermic Exothermic Endo- or Exothermic
20 Differential Thermal Analysis (DTA) Principle * Constant Heating Rate * DTA Temperature of sample minus temperature of reference vs Time (Temp.) DTA curve endothermic process
21 Differential Thermal Analysis (DTA) Reading data exothermic endothermic *Depending on instruments Measuring Onset temp Endset temp Integral enthalpy change Peak temp Peak height Peak width * Peak temperature is affected by heating rate & sample mass, but not by ΔH and T onset
22 Differential Scanning Calorimetry (DSC) Principle An analytical technique used to determine a material s phase diagram, heat change, and decompositions by measuring the difference in the amount of heat required to increase the temperature of a sample and reference. Type Process Heat process Physical changes Chemical changes Adsorption Desorption Change in crystal structure Crystallization Melting, Vaporization, Sublimation Oxidation Reduction Breakdown reaction Chemisorption Solid state reaction Exothermic Endothermic Endo- or Exothermic Exothermic Endothermic Exothermic Endothermic Endo- or Exothermic Exothermic Endo- or Exothermic
23 Differential Scanning Calorimetry (DSC) Principle
24 Differential Scanning Calorimetry (DSC) Principle * Constant Heating Rate * DSC - Heat flow to sample minus Heat flow to reference vs Time (Temp.)
25 Differential Scanning Calorimetry (DSC) Reading Data Offset C p *Directions of endo- and exo- depends on instruments
26 Differential Scanning Calorimetry (DSC) Reading Data C p DSC Curve of a Thermoplastic Polymer *Directions of endo- and exo- depends on instruments
27 TGA-DSC Reading Data TGA reveals changes of a sample due to weight, whereas DTA and DSC reveal changes not related to the weight (mainly due to phase transitions) A pharmaceutical sample C p of crystalline > C p of liquid Crystalline melt Decomposition temperature
28 TGA - DTA Reading Data
 2 ) 0.125 O w0.75 FW: 794.33 Wt% (calc. C 36.29, H 1.55, N 0) (exp. C 36.61, H 1.742, N 0.](/docs-images/79/80308397/images/29-0.jpg "034) activated SUMOF-3 Crystal: C 75 H 50 NO 31.7 Zn 8 => [Zn 4 O(NDC) 3 ] 2 (DMF)(H 2 O) 3.5 O w1.2 FW: 1995.52 Wt% (calc. C 45.14, H 2.53, N 0.71) (exp. C 46.36, H 2.24, N 0.")
29 Example SUMOF-2 Crystal: C 24 H O 14 Zn => [Zn 4 O(BDC) 3 ](Zn(OH) 2 ) O w0.75 FW: Wt% (calc. C 36.29, H 1.55, N 0) (exp. C 36.61, H 1.742, N 0.034) activated SUMOF-3 Crystal: C 75 H 50 NO 31.7 Zn 8 => [Zn 4 O(NDC) 3 ] 2 (DMF)(H 2 O) 3.5 O w1.2 FW: Wt% (calc. C 45.14, H 2.53, N 0.71) (exp. C 46.36, H 2.24, N 0.051) activated SUMOF-4 Crystal: C 33 H 24 NO 15 Zn 4 => [Zn 4 O(BDC) 2 (BPDC)](H 2 O)(DMF)(OH) FW: Wt% (calc. C 42.34, H 2.58, N 1.50) (exp. C 41.24, H 2.205, N 0.029) activated J. Mater. Chem., 2012, 22, 10345
30 Example SUMOF-2 (MOF-5) Crystal: C 24 H O 14 Zn => [Zn 4 O(BDC) 3 ](Zn(OH) 2 ) O w0.75 FW: Wt% (calc. C 36.29, H 1.55, N 0) (exp. C 36.61, H 1.742, N 0.034) activated SUMOF-3 (IRMOF-8) Crystal: C 75 H 50 NO 31.7 Zn 8 => [Zn 4 O(NDC) 3 ] 2 (DMF)(H 2 O) 3.5 O w1.2 FW: Wt% (calc. C 45.14, H 2.53, N 0.71) (exp. C 46.36, H 2.24, N 0.051) activated SUMOF-4 Crystal: C 33 H 24 NO 15 Zn 4 => [Zn 4 O(BDC) 2 (BPDC)](H 2 O)(DMF)(OH) FW: Wt% (calc. C 42.34, H 2.58, N 1.50) (exp. C 41.24, H 2.205, N 0.029) activated J. Mater. Chem., 2012, 22, 10345
31 Example SUMOF-2 (MOF-5) Crystal: C 24 H O 14 Zn => [Zn 4 O(BDC) 3 ](Zn(OH) 2 ) O w0.75 FW: Wt% (calc. C 36.29, H 1.55, N 0) (exp. C 36.61, H 1.742, N 0.034) activated [Zn 4 O(BDC) 3 ](ZnO) C 24 H 12 O Zn FW: Wt% (calc. C 36.95, H 1.55, N 0) (exp. C 36.61, H 1.742, N 0.034) activated (ZnO) FW: / = /74.2 = J. Mater. Chem., 2012, 22, 10345
32 Example SUMOF-3 (IRMOF-8) Crystal: C 75 H 50 NO 31.7 Zn 8 => [Zn 4 O(NDC) 3 ] 2 (DMF)(H 2 O) 3.5 O w1.2 FW: Wt% (calc. C 45.14, H 2.53, N 0.71) (exp. C 46.36, H 2.24, N 0.051) activated [Zn 4 O(NDC) 3 ] C 36 H 18 O 13 Zn 4 FW: Wt% (calc. C 47.00, H 1.92, N 0) (exp. C 46.36, H 2.24, N 0.051) activated (ZnO) 4 FW: / = /66.0 = J. Mater. Chem., 2012, 22, 10345
33 Example SUMOF-4 Crystal: C 33 H 24 NO 15 Zn 4 => [Zn 4 O(BDC) 2 (BPDC)](H 2 O)(DMF)(OH) FW: Wt% (calc. C 42.34, H 2.58, N 1.50) (exp. C 41.24, H 2.205, N 0.029) activated [Zn 4 O(BDC) 2 (BPDC)(H 2 O)] C 30 H 18 O 14 Zn 4 FW: Wt% (calc. C 41.70, H 2.10, N 0) (exp. C 41.24, H 2.205, N 0.029) activated (ZnO) 4 FW: / = /68.2 = J. Mater. Chem., 2012, 22, 10345
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