METHODS OF
THERMAL ANALYSIS (TA) |
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Thermal analysis includes
a group of methods by which the physical and chemical properties of a substance,
a mixture and/or reaction mixtures are determined as a function of temperature
or time, while the sample is subjected to a controlled temperature program. The
program may involve heating or cooling (dynamic), or holding the temperature
constant (isothermal), or any combination of these.
The adjective is thermoanalytical. The graphic result is the thermal
analysis curve.
See, for example, German standards DIN 51005 (nomenclature) or American
standard ASTM E 473 (nomenclature). |
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DIFFERENTIAL
THERMAL ANALYSIS (DTA)
DIFFERENTIAL SCANNING CALORIMETRY
(DSC)
DIN 51007,
DIN 53765, ASTM E 474, ASTM D 3418
These are techniques by which the difference in heat flow to or from a
sample and to or from a reference is monitored as a function of temperature
or time, while the sample is subjected to a controlled temperature program.
Applications:
characteristic temperatures
identification
glass transitions
melting and crystallization behavior
heat of melting and crystallization
purity
compatibility
polymorphism
solid-liquid ratio
specific heat capacity
reaction behavior
heat of reaction
reaction kinetics
oxidative stability
thermal stability
Instruments:
 DSC
204 Phoenix®
DSC
200-F3 Maia®
DSC 204 HP
DSC
404 C Pegasus®
DTA 404
STA
449 C Jupiter®
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
THERMOGRAVIMETRY
(TG)
DIN 51006, ASTM E 914, ASTM E 1131
This is a technique by which the mass of the sample is monitored as a function
of temperature or time, while the sample is subjected to a controlled temperature
program.
Dm = mass change
dm/dt = rate of mass change/decomposition
DTG = derivative thermogravimetry
DTG Peak = characteristic decomposition temperatures Æ identification
Tonset = thermal stability
composition = moisture content, solvent content, additives, polymer content,
filler content
dehydration
decarboxylation
oxidation
decomposition
Instruments:
TG
209 C-IRIS®
TG
439
STA
449 C Jupiter®
STA
409-PC Luxx®
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
SIMULTANEOUS
THERMAL ANALYSIS
This technique combines thermogravimetry with differential thermal
analysis or differential scanning calorimetry in one run.
- possible to consider the real sample mass at a given temperature
in Cp determination
- no temperature differences between signals of TG and DTA/DSC measurement
Instruments:
STA
449 C Jupiter®
STA
409 C
STA
409-PC Luxx®
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
THERMOMECHANICAL
ANALYSIS (TMA)
DILATOMETRY (DIL)
DIN 51045, ASTM E 831, ASTM D 696, ASTM D 3386
This is a technique by which the dimensional changes of the sample are
monitored as a function of temperature or time, while the sample may
be subjected to an additional mechanical load.
- negligible mechanical load Æ dilatometry
- constant load Æ (static) thermomechanical analysis
- oscillating force Æ dynamic mechanical analysis
DL = length change
DL / L0 = relative length change
a = coefficient of linear thermal expansion
Tg = glass transition temperature
expansion/shrinkage/penetration behavior
dimensional stability Æ design purposes
softening/curing behavior
volumetric expansion (Þ bulk density)
Instrument:
TMA
202
DIL
402 C
DIL
402 PC
DIL
402 E/7
TMA
402
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
DYNAMIC
MECHANICAL ANALYSIS (DMA)
DIN 53513, DIN 53440, ASTM D 4065, ASTM D 4092
This is a thermoanalytical method by which the mechanical behavior of
a sample subjected to a specific temperature program is investigated under
the effect of a load which changes with time.
Determination of the storage and loss moduli and the damping factor of a
sample as a function of temperature, time and frequency of an applied oscillating
load.
Instrument:
DMA
242
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
COMBINED
(HYPHENATED) TECHNIQUES
With these
thermoanalytical methods, the gases evolved from the sample during a
thermal analysis experiment are detected/analyzed.Instruments:
TG 209 - QMS Capillary (RT...1000°C)
TG
209 - FTIR (RT...1000°C)
STA 449 C Jupiter® - QMS Capillary (RT...1650°C)
STA
449 C Jupiter® - FTIR (RT...1500°C)
STA
409 - QMS Skimmer (RT...2000°C)
STA
409 - QMS Capillary (RT...2000°C)
STA
409 - FTIR (RT...1500°C)
PTA®
403/6
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
THERMAL
CONDUCTIVITY TESTING
ISO 8894, EN 993-14/15 (DIN 51046)
This thermoanalytical method allows the measurement of the thermal conductivity
of a sample (solid or powder) as a function of temperature.
Instruments:
TCT 416 (near RT)
TCT 426 (RT...1500°C)
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
THERMAL
DIFFUSIVITY MEASUREMENT (Laser
Flash Method)
This is a thermoanalytical method which measures the thermal diffusivity
of the sample (solid, liquid or powder) at constant temperatures while
monitoring the temperature increase of the sample caused by the absorbed
energy of a laser flash.
Instrument:
LFA
427 (-50...2000°C)
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
REFRACTORIES
TESTING (RUL, CIC, MOR)
Refractoriness Under Load (RUL): ISO 1893, EN 993-8 (DIN 51053)
Creep In Compression (CIC): ISO 3187, EN 993-9 (DIN 51053)
Hot Modulus of Rupture (HMOR): ISO 5013, EN 993-7 (DIN 51048)
This thermoanalytical test method is used for the determination of refractoriness
under load (RUL), creep in compression (CIC) and modulus of rupture
(MOR) of solid samples.
Instruments:
RUL
421 (RT...1700°C)
MOR
422 (RT...1500°C)
Top
DSC •
TG •
STA •
DIL •
DMA •
PTA •
TCT •
LFA •
RUL
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