NETZSCH Methods of Thermal Analysis

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METHODS OF THERMAL ANALYSIS (TA)

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).

TA Methods

Differential Thermal Analysis (DTA)
Differential Scanning Calorimetry (DSC)
Thermogravimetry (TG)
Simultaneous Thermal Analysis (STA)
Thermomechanical Analysis (TMA)
Dilatometry (DIL)
Dynamic Mechanical Analysis (DMA)
Combined (Hyphenated) Techniques
(TA-MS, TA-FTIR, PTA)
Thermal Conductivity Testing (TCT)
Thermal Diffusivity Measurement (LFA)
Refractories Testing (RUL, CIC, MOR)

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^®

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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
T_onset = 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^®

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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 C_p determination
- no temperature differences between signals of TG and DTA/DSC measurement

Instruments:
STA 449 C Jupiter^®
STA 409 C
STA 409-PC Luxx^®

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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
T_g = 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

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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

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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

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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)

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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)

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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)

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DSC • TG • STA • DIL • DMA • PTA • TCT • LFA • RUL

NETZSCH offers instruments for thermal analysis, thermal properties measurement, thermal hazard screening, and contract testing services. Our portfolio is the world's broadest, including a full range of dilatometers to measure high accuracy thermal expansion, classical DSC & TGA, high temperature DSC to 1650°C for specific heat, very high temperature STA (TGA-DSC/DTA) from sub-ambient to 2400°, thermal / evolved gas analysis with fully-integrated FTIR & MS, high resolution TMA and DMA, plus DEA - dielectric analysis for thermoset cure monitoring. We also feature leading-edge technology for thermal conductivity by guarded hot plate and heat flow meters, laser flash thermal diffusivity measurement, thermal hazard screening via adiabatic reaction calorimetry, as well as refractories testing including HMOR, CIC, and RUL. Finally, we offer advanced software packages including thermokinetics for process modeling and development.

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