Thermal Characterization of Polymers

Thermoplastics, Thermoplastic Elastomers, Elastomers and Thermosets

Analyzing & Testing

 The World of Polymers
Polymer materials have greatly changed the world The importance of polymers
we live in – without them, the world would not be as in our daily lives has not come
we know it today. There is something innately about arbitrarily, but rather
fascinating about them, yet we've become accus- as a result of the distinct
tomed to their integral presence in our everyday advantages that they offer.
lives. And today, the possibility of recycling them These advantages include:

∙
makes them even more interesting from an
ecological and economical point of view. Low density

∙ Light weight

∙
Henri Braconnot’s work in the 1830s is perhaps the
first modern example of polymer science. He, along Good thermal and electrical
with others, developed derivatives of the natural insulation capacity
polymer cellulose, producing new, semi-synthetic
materials, such as celluloid and cellulose acetate. ∙ Resistance to corrosion
effects

∙
Since that time, eight Nobel Prizes have been
dedicated to polymer science. Chemical inertness

Just 50 years ago, materials we now take for granted ∙ High strength and dimensional
stability

∙
were non-existent. With further advances in the
understanding of polymers, and with new applica- Absorption of mechanical
tions being researched all the time, there is no reason shocks
to believe that this revolution will stop any time soon.
∙ Resistance to abrasion effects

∙ Good coloring

∙ Potential for decorative

surface effects
Films ∙ Low production costs

Adhesives Fibers ∙ Easy processability

Resins/Paints Thermoplastics ∙ Great flexibility of form

Thermosets Biopolymers
POLYMERS
Foams Composites
Rubber Thermoplastic Elastomers
Elastomers Coatings
Additives

2
Thermal Analysis

During their production, and gain information regarding With our broad product line of
processing and application, the condition or processing thermoanalytical instruments and
polymers are subjected to history of specific samples applications knowledge acquired
temperature-dependent struc- relative to reference samples. over several decades, NETZSCH
tural changes. Therefore, thermal Analyzing & Testing ranks among
analysis for characterization of This makes thermal analysis very the best as far as meeting the
polymers is widely practiced well-suited for quality control high demands associated with the
today in research and industry. and quality assurance. Incoming manufacture of reliable products
More and more applications are materials inspection as well and state-of-the-art technologies.
being backed up by national as materials selection can be
and international standards carried out safely and easily. This brochure gives an overview of
(ISO, EN, ASTM, DIN, etc.). Also for the research and devel- our various methods and corre-
opment of new materials, thermal sponding application examples
Thermal analysis techniques give analysis is an indispensable from thermoplastics to composites.
insight into the thermal properties tool for investigating a broad
of polymer materials and products range of materials properties.

The variety of thermoanalytical test methods opens

a broad application range for polymer testing, e.g.:

Specific heat capacity DSC

Thermal transitions DSC, DIL, TMA, LFA
Melting, crystallization and
DSC
reaction enthalpies

Glass transition temperatures DSC, TMA, DMA, DEA, LFA

Degree of crystallinity DSC

Thermal stability TGA, STA
Oxidation Induction Time/
Oxidation Onset Temperature DSC
(OIT, OOT)
Viscoelastic behavior DMA, TMA
Young’s modulus DMA, TMA
Kinetics of reactions DSC, TGA, DIL, TMA, DEA
Compositional analysis DSC, TGA, EGA
Thermal expansion coefficient DIL, TMA, DMA
Filler content TGA, STA
Thermal conductivity/diffusivity LFA, HFM
and many more

3
Differential Scanning Calorimetry (DSC)
Differential Scanning Calorimetry (DSC) is the most frequently employed thermal analysis method. It can be
used to analyze nearly any energetic effect occurring in a solid or liquid during thermal treatment. DSC analysis
in accordance with ISO 11357 provides the following valuable information for the development and quality
control of polymers:

Product Identification and Advanced Materials Analysis Product/Process Information

Characterization

∙ Melting/crystallization ∙ Decomposition effects

∙ Incoming goods inspection

∙
temperatures
∙ Oxidative stability (OIT, OOT)
∙ Thermomechanical history
Melting/crystallization
∙ Reaction behavior and kinetics
∙ Failure analysis

∙ ∙
enthalpies

∙ Cross-linking temperatures
∙
Predictions

∙
Competitor product analysis

∙ Cross-linking enthalpies
∙
Degree of curing Process optimization

∙ Degree of crystallinity
Purity determination for

∙
additives

∙
Glass transition temperatures
∙ Curing by UV irradiation
Specific heat capacity
∙ Stability under pressure

∙ Peak Separation

Photo-DSC 204 F1 Phoenix® with UV coupling

and ASC for up to 192 samples

4
DSC 214 Polyma

DSC Systems Made for Polymer Applications

The DSC 214 Polyma features high heating

and cooling rates, making it useful for both
research and quality assurance in production.

In complement to this, the DSC 204 F1

Phoenix® features a modular sensor design
(τ- and μ-sensor), a large automatic sample
changer and the ability to be coupled.

Thermally activated reactions can be studied

by conventional DSC, but cationic polyaddi-
tions and radical polymerizations can also be
started by UV irradiation with sufficiently high
energy. For this purpose, NETZSCH offers the DSC 3500 Sirius
Photo-DSC 204 F1 Phoenix®. The DSC 3500
Sirius is the economic entry-level model.

High-Pressure DSC

Numerous physical processes and chemical

reactions are influenced by the surrounding
gas pressure. In practice, it is therefore often
necessary to define a higher pressure under
which to conduct DSC measurements. With
the high-pressure DSC 204 HP Phoenix®,
thermal effects in a sample can be analyzed
in the pressure range from vacuum to 15 MPa
(150 bar) and at temperatures from -150°C
to 600°C, depending on the type of gas.

DSC 204 HP Phoenix®

5
Thermogravimetric Analysis (TGA)
Thermogravimetry (TG), or Thermogravimetric Various international standards describe the general
Analysis (TGA), is a well proven thermal analysis principles of thermogravimetry for polymers (ISO
method for measuring mass changes as a function 11358) or other specific applications, such as the TGA
of temperature or time. TGA is used in the research method for the compositional analysis of rubber
& development of various substances and engineer- (ASTM D6370).
ing materials – both solids and liquids – in order to
obtain knowledge about their thermal stability and Our vertical, top-loading design not only provides for
composition. easy operation and sample loading, but also allows
gases to flow naturally in an upward direction.
In recent decades, TGA has been used increasingly in Evolved gas analyzers such as mass spectrometers,
quality control and assurance for raw materials and FT-IR (Fourier Transform Infrared) spectrometers and/
incoming goods, as well as in the failure analysis of or GC-MS (gas chromatograph-mass spectrometers)
finished parts, especially in the polymer-processing can be coupled directly to the gas outlet on the top of
industry. the furnace.

The Automatic Sample Changer (ASC) can also be used

to conduct routine measurements around the clock.

TGA provides complementary and

supplementary characterization
information to DSC.

TG 209 F3 Tarsus® entry-level model with ASC

TG 209 F1 Libra® premium model with ceramic furnace

and ASC for up to 192 samples

6
Simultaneous Thermal Analysis (STA)
Simultaneous Thermal Analysis
(STA) generally refers to the
simultaneous application of
thermogravimetry (TG) and DSC
to one and the same sample in a
single instrument. Main advan-
tages are the identical test condi-
tions for the TGA and DSC signals
(same atmosphere, gas flow rate,
vapor pressure of the sample,
heating rate, thermal contact to
the sample crucible and sensor,
radiation effect, etc.). In addition,
sample throughput is improved as
more information is simultane-
ously gathered from each test run.

The DSC, TGA and STA systems all

meet the majority of the respective
instrument and application
standards, including: ISO 11357,
ISO 11358, ASTM E967, ASTM
STA 449 F1 Jupiter® E968, ASTM E793, ASTM D3895,
DIN 51004, DIN 51006, DIN 51007.

TGA Measurement DSC Measurement

Information Information

∙
Mass changes ∙ Specific heat capacity

∙
Temperature stability ∙ Melting/crystallization

∙
Estimation of product lifetime
∙
behavior

∙
Oxidation/reduction behavior
∙
Solid-solid transitions

∙
Filler content
∙
Polymorphism

∙
Moisture and volatiles content
∙
Degree of crystallinity

∙
Decomposition
Glass transition

∙
temperatures
Compositional analysis of
∙ Cross-linking reactions

∙
multi-component
materials/blends Oxidative stability

∙
Data for kinetic evaluation using
Kinetics Neo
∙ Purity determination
for additives

∙ Data for kinetic evaluation

using Kinetics Neo

7
Thermal Analysis Coupled to
Evolved Gas Analysis (EGA)
Top-level polymer research and characterization can be achieved by coupling the thermoanalytical methods of
TGA, DSC, STA, TMA and DIL to a mass spectrometer (MS), gas chromatograph/mass spectrometer (GC-MS) or
Fourier Transform Infrared (FT-IR) spectrometer. These hyphenated techniques may also include simultaneous
coupling of the MS and FT-IR or GC-MS and FT-IR to the thermal analyzer. In addition, the unique adapter allows
for coupling even when used in combination with an Automatic Sample Changer (ASC).

TGA-FT-IR
coupling via
an external
FT-IR gas cell

Coupling Possibilities Measurement Information by Means of

Evolved Gas Analysis Coupled to Thermal Analysis
∙ TGA-, DSC-, or STA-MS via
capillary coupling

∙
Compositional analysis Decomposition

∙
STA-MS via SKIMMER coupling
∙ Polymers
∙ Dehydration

∙
TGA-, or STA-GC-MS
∙ Plasticizers
∙ Stability

∙
TGA-, DSC-, or STA-FT-IR
∙ Solvents
∙ Residual solvent

∙
TMA-MS
∙ Additives
∙ Pyrolysis
DIL-MS
∙ Propellents
Solid-gas reactions

∙
Evolved gases are directed straight
to the gas analyzer via a heated Evaporation Combustion
capillary or transfer line. In
∙ Vapor pressure
∙ Oxidation

∙ ∙
addition to decomposition, such
systems can also be used for Sublimation Adsorption/desorption
investigating composition, evapo-
ration and solid-gas reactions.

PERSEUS STA 449 F1 Jupiter®

and GC-MS coupling

8
Thermomechanical Analysis (TMA)/
Dilatometry (DIL)
TMA/DIL Measurement
Thermomechanical analysis (TMA) and dilatometry (DIL) are two of
the most important characterization techniques in the field of thermal
Information
analysis. DIL determines the length change of samples under a negligible
∙
Thermal expansion

∙
load (DIN 51045). The closely related TMA method also determines the
dimensional changes of solids, liquids or pasty materials as a function Coefficient of thermal
of temperature and/or time under a defined static load (ISO 11359, expansion
DIN 51 005, ASTM E831, ASTM D696, ASTM D3386).
∙
Volumetric expansion
With the TMA 402 F1 Hyperion®, measuremens can additionally be
∙
Density change
carried out under bending, tension and penetration force, as well as
∙
Shrinkage steps

∙
under force modulation.
Glass transition
Investigations can be now realized on plastics and elastomers, paints temperatures
and dyes, composite materials, adhesives, films, fibers and composite
∙
Softening points

∙
materials.
Penetration behavior
The NETZSCH dilatometers (DIL Expedis) and TMA systems for polymers
∙
Phase transitions

∙
and composites fulfill the respective instrument and applications
standards for both and thermomechanical analysis. Creep behavior

∙
Anisotropic behavior

∙
Young’s modulus

∙
Data for kinetic evaluation
using Kinetics Neo

Variety of TMA 402

sample holders

TMA 402 F1 Hyperion®

DIL 402 Expedis Supreme

9
 Dynamic Mechanical Analysis (DMA)
Dynamic Mechanical Analysis (DMA) allows for the quantitative determination of the mechanical properties of
a sample under an oscillating force and as a function of temperature, time, frequency and strain (DIN 53513,
DIN EN ISO 6721, DIN 53440, DIN-IEC 1006, ASTM D4065, ASTM D4092, ASTM D4473, ASTM D5023, ASTM
D5024, ASTM D5026, ASTM D5418). The results portray the linear viscoelastic properties, typically depicting
them as a graphical plot of E’ (storage modulus), E” (loss modulus), and tanδ (loss factor) versus temperature.

The DMA 242 E Artemis and the high-force DMA GABO EPLEXOR® systems identify transition regions, such as
glass transitions in plastics and resins, and may be used for quality control or product development in the
temperature range from -180°C to 600°C.

Dynamic Mechanical Testing Supports DMA Measurement Information

Research and Quality Control of Polymers
∙ Design data concerning stiffness and damping
properties (modulus values and damping factor
R&D under a variety of conditions)
The DMA method is a very sensitive tool for generating
data that can help define the mechanical properties of
∙ Data on the composition and structure of
polymer blends (miscibility)
polymers and composites in order to support product
development in industries such as automotives. ∙ Glass transition of highly cross-linked,
amorphous or semi-crystalline polymers
and composites

∙
Quality Control
Curing/post-curing

∙
α and β transitions can be used to compare production
with standards and competitors' products. Aging

∙ Creep and relaxation

∙
Our DMA experts support you by finding the right
approach for specific applications and areas of interest. Stress and strain sweeps

∙ Multi-frequency tests

∙ Prediction of the material behavior using Time-

Temperature-Superposition (TTS) experiments

∙ Immersion tests

∙ Durability test

∙ Fatique test

∙ Hysteresis

High-force DMA GABO EPLEXOR® 500 DMA 242 E Artemis

10
Dielectric Analysis (DEA)
A variety of questions may arise during with the phase shift between voltage and current.
the curing process of reactive resins. These values are then used to determine the ion

∙
mobility (ion conductivity) and the alignment of
At which temperature, or after how much time, dipoles. In turn, the dielectric properties of permit-
does the resin begin to cure? tivity ε' and loss factor ε"are calculated from these

∙ How high is the reactivity?

effects. Of primary interest with regard to curing is

∙
the ion viscosity. This is the reciprocal value of the ion
When is curing completed? conductivity, which is proportional to the loss factor.

∙ Is the curing profile identical for every position

in the mold?
Use of the DEA technique is not limited to the lab

∙
environment; it can also be applied to monitor
How can the curing cycle be optimized in order in-situ curing in the mold under processing condi-
to save energy and costs? tions. For production monitoring and process

∙ Is there any potential for post-curing?

control, a specific ion viscosity value can be
programmed to trigger demolding when the
part being produced is sufficiently cured. This
For investigation of the curing behavior of reduces cycle times and increases throughput.
thermosetting resin systems, composite materials,
adhesives, paints and coatings, dielectric
analysis (DEA) in accordance with ASTM E2038 Portable Version
or E2039 has stood the test of time.
With up to seven channels, this DEA is the flexible
version for your day-to-day work. It can be easily trans-
Measurement Principle ported between different measurement locations.

DEA allows for the measurement of changes in the Rack Version for Integration into an
dielectric properties during curing. The liquid or Industrial Process
pasty resin must be placed in direct contact with
two electrodes comprising the dielectric sensor. A The 19” Rack version is designed for an electrical
sinusoidal voltage (excitation) is applied and the cabinet. It supports 8 simultaneous measuring
resulting current (response) is measured, along channels which can be extended up to 16 modules.

DEA Measurement
Information

∙ Ion viscosity

∙ Reactivity

∙ Cure monitoring

∙ Degree of cure

∙ Glass transition temperature

∙ Process control and

optimization

∙ Diffusion properties

∙ Aging and decomposition

effects
DEA 288 Ionic

11
 Laser Flash Technique (LFA)

Thermal conductivity and thermal diffusivity are the For polymer applications in the temperature range
most important thermophysical material parameters from -100°C to 500°C, the compact LFA 467
for describing the heat transport properties of a HyperFlash is available. The integrated Automatic
material or component. Sample Changer can test up to 16 samples in one run.
The LFA 467 HyperFlash is able to test thin and
During development and quality control, the extent high-conductivity materials as well as 2- and 3-layer
to which materials fulfill their performance expecta- structures – a capability which allows for such
tions is continuously scrutinized. Some of the analyses as the influence of coatings on heat transfer
questions which arise include: under real conditions.

∙ How is a particular insulation material performing? The LFA 467 HyperFlash operates in accordance with

∙ What is the ideal coating material?

national and international standards (e.g., ASTM

∙
E1461, DIN EN 821).
How can the heat transfer from an electronic
component be improved?

∙ How must a heat exchanger be designed in order

to achieve the required efficiency level, and what is
the best material to use?

For issues such as these, the Laser Flash technique

(LFA) has become a fast and reliable tool; it is an
absolute method for determining thermophysical
properties, including the specific heat capacity.
This data can then be used for:

∙ Prediction of the heat transfer and temperature

profile for description of the processing behavior

∙ Thermal diffusivity and thermal conductivity as

input data for numerical simulation

LFA 467 HyperFlash

Broad variety of LFA sample holders for liquids, powders, fibers, for studies of anisotropic behavior

12
Insulation Testing by Means of the
Heat Flow Meter (HFM)
All NETZSCH HFM and GHP instruments are based on all respective
Materials with low application and industry standards:
thermal conductivities
can be tested in ∙ ASTM C177, ASTM C335-05Ae1, ASTM C1363-05, ASTM D5470-06,
ASTM E1530-06, ASTM F433-02(2009), ASTM C1363-05
HFM or GHP.
∙ DIN EN 12667/12939, DIN EN 13163

∙ ISO 8301, ISO 8302, ISO 8894-1 (EN 993-14), ISO 8894-2 (EN 993-15)

∙ JIS A 1412

Heat Flow Meters

Heat Flow Meters are precise, fast and easy-to-operate The HFM 446 Lambda allows the operator to apply a
instruments for measuring the thermal conductivity of precise load on the specimen, enabling control over
insulations (e.g., polystyrene or polyurethane foams). the thickness, and thus density of compressible
The HFM 446 Lambda series owes its speed of materials – requirements for obtaining reproducible
measurement and precision to patented temperature thermal conductivity results.
control and heat flux measurement technology. High
stability over the course of several days provides The HFM 446 series consists of three instrument
excellent repeatability. This is valuable for conducting versions which cover the plate temperature range
aging studies or examining the long-term consistency from -20°C to 90°C.
of a product.

HFM 446 Lambda Small HFM 446 Lambda Medium HFM 446 Lambda Large
Specimen size: 203 x 203 mm Specimen size: 305 x 305 mm Specimen size: 611 x 611 mm

13
 Advanced Software Module

Kinetics Neo
can analyze any process for which
the rate depends on temperature

NETZSCH Kinetics Neo software is used to analyze kinetics of temper- All Kinds of Advantages
ature-dependent chemical processes. The result of such analysis is a
kinetics model or method correctly describing experimental data under The primary advantage of
different temperature conditions. Use of the method/model allows for Kinetics Neo is its ability to
predictions of a chemical system’s behavior under user-defined temper- analyze both heterogeneous and
ature conditions. Alternatively, such models can be used for process phase-boundary reactions – and
optimization. to analyze such reactions with
diffusion and nucleation.
The software can analyze different types of thermal curves that depict Furthermore, reactions with
the changes in a given material property measured during a process. partial diffusion control can be
Potential data sources include studies using thermogravimetry, studied; for example, processes
dilatometry, differential scanning calorimetry, Fourier-Transform infrared which change the state of a
spectroscopy, mass spectrometry and rheometry, as well as temperature substance from the glassy to the
analysis during adiabatic measurements. non-glassy state.

The unique model-based kinetic analysis is capable of determining

the number of reaction steps, and for each step the following values:

∙ Enthalpy (exo/endothermal
DSC effects) or mass loss (TGA)

∙ Reaction type

∙ Activation energy

∙ Pre-exponential factor

∙ Order of reaction

∙ Order of autocatalysis

∙ Additional kinetic parameters

14
 2

108

2
Middle Layer
107 Bottom Layer
Top Layer
5

Kinetic Analysis
127.2 min
106 124.2 min 126.0 min

50
Heat flow rate /(W/g) 100 150 200 250
Time /min
0
Kinetic analysis allows a set of kinetic parameters to be found – e.g., the number of reaction steps, the
-0.2 contribution of each step to the total effect of the process, the reaction type, the activation energy, or
10.0 K/min
the reaction order for each step. This information5.0isK/min
then used to solve prediction problems for new
-0.4 temperature/time programs or to optimize behavior for a given system.
3.0 K/min

-0.6
A–1→B–2→C–3→D–4→E

-0.8 Step 1: n-th order with autocatalysis by B

Step 2: n-th order
Step 3: n-th order
-1.0 ↓ exo Step 4: n-th order
Heat flow rate /(W/g) Curing Behavior of an
0 40 80 120 160
Temperature /°C
200 240
Epoxy Resin
-0.2
10.0 K/min
5.0 K/min
-0.4 3.0 K/min In this example, an uncured epoxy
resin was heated at rates of 3, 5
-0.6 and 10 K/min with the DSC 204 F1
A–1→B–2→C–3→D–4→E
Phoenix®. In the Kinetics Neo
-0.8 Step 1: n-th order with autocatalysis by B software program, exothermal
Step 2: n-th order
Step 3: n-th order curing was simulated. The almost
-1.0 ↓ exo Step 4: n-th order perfect fit was achieved as a formal
nth-order 4-step reaction. The start
40 80 120 160 200 240 of the actual curing was described
Temperature /°C well by a first-order reaction with
autocatalysis.
Curing of an epoxy resin at different heating rates

Conversion Rate /%

100 100 °C
80 °C
In this plot, the curing behavior is
predicted based on the simulations
80 shown above. For different
60 °C isothermal temperatures, the
conversion rate is plotted against
60
time. For example, at 100°C, the
material investigated here was
40 totally cured after 65 min (degree
of curing of 100%).
20
Conversion Rate /%

100 100 °C
0
80 °C
0 20 40 60 80 100
80 Time /min

60 °C
Prediction of the curing behavior at different isothermal temperatures
60

40 15
 APPLICATIONS
Thermoplastics
Differential Scanning Calorimetry

Crystallization Behavior of DSC /(mW/mg)

[1.22]
Semicrystalline PET 0.6 ↓ exo
249.2°C

PET
Polyethylene terephthalate (PET) 0.5
is a semi-crystalline thermoplastic
polymer with a relatively slow crystal-
lization rate. High cooling rates lead 0.4
to a high amorphous content, high
glass transition steps (Tg) and post-
0.3
crystallization during heating.

Low cooling rates allow more 0.2

crystalline parts to crystallize during
cooling, leading to a smaller glass 10 K/min
transition step and no post-crystalli- 0.1 15 K/min
zation. The material then has an 20 K/min applied cooling rates
25 K/min
increased crystallinity and therefore before heating segment
0.0 30 K/min
loses its transparency. 35 K/min
150.5°C

100 150 200 250

Temperatur /°C

PET: glass transition, cold crystallization and melting measured at a heating rate
of 10 K/min after different cooling rates – change in the crystallinity degree by
means of DSC

Flow /(ml/min)
DSC/(mW/mg) Temp./°C
↓ exo 250 200
2.0

200
1.5 150

1.0 150

100
0.5 100
Cu crucible Al crucible
16 O.I.T.:10.0 min O.I.T.:32.8 min
0.0
Gas Flow 50 50
 0.1 15 K/min
20 K/min applied cooling rates
25 K/min before heating segment
0.0 30 K/min
35 K/min
150.5°C

Oxidative Induction Time (OIT) 100 150

Temperatur /°C
200 250

Flow /(ml/min)
Factors that influence OIT include DSC/(mW/mg) Temp./°C
test temperature, sample prepa- ↓ exo 250 200
ration, sample geometry, sample 2.0
mass, particle size, crucible
material, etc. The Oxidative 1.5
200
150
Induction Time (OIT) can be
determined in standard aluminum 150
1.0
or in open copper crucibles in
Flow /(ml/min)
accordance with ASTM D3895. DSC/(mW/mg) 100
Temp./°C
0.5 100
↓ exo Cu crucible Al crucible 250 200
This plot represents OIT measure- 2.0
O.I.T.:10.0 min O.I.T.:32.8 min
0.0
ments on high-density poly- Gas Flow 50 50
ethylene (HDPE) carried out in a nitrogen 200
1.5
-0.5 150
copper and in an Al crucible (red oxygen
0
and blue curves, respectively). It 150
1.0
can clearly be seen that, under 10 20 30 40 50
Time /min
isothermal conditions at 250°C 100
0.5 100
under an oxygen atmosphere, Influence of the crucible material on the Oxidative Induction Time (OIT) of
Al crucible
oxidation of HDPE begins approxi- HDPE by DSC; sample massesCu crucible
12.21 mg and 12.11 mg
O.I.T.:10.0 min O.I.T.:32.8 min
0.0
mately 23 min earlier in the copper Gas Flow 50 50
crucible than in the Al crucible. nitrogen
-0.5
Copper works here as a catalyst oxygen
0
for the oxidation.
10 20 30 40 50
Time /min
DSC/(mW/mg)
[3.6]
↓ exo
0.8

0.7 1st Heatings

Failure Analysis of a PA6 Clip 0.6

Area: 45.17 J/g
Peak*: 215.1 °C
PA66
0.5 part with broken clip
239.2°C
0.4 Mid: 51.6°C
Failures might be due to a variety of DSC/(mW/mg)Delta Cp*: 0.079 J/(g·K)
[3.6]
causes, including selection of the 0.3
↓ exo
wrong material for the application, 0.8
0.2 Area: 53.15 J/g
manufacturing defects in the plastic 1st Heatings
Peak*: 221.3 °C
0.7 good part
raw material, production defects in 0.1 Mid: 50.9°C
Delta Cp*: 0.100J/(g·K) Area: 45.17 J/g
the plastic part, or degradation of the 0.6
0.0 Peak*: 215.1 °C
PA66
plastic by exposure to aggressive 0.5 part
50 100with broken150
clip 200 250
chemicals, contaminants, UV Temperature /°C 239.2°C
0.4 Mid: 51.6°C
radiation, etc. DSC is a convenient Delta Cp*: 0.079 J/(g·K)
method for comparing good parts 0.3
with poor ones. 0.2 Area: 53.15 J/g
Peak*: 221.3 °C
In this example, the first heating runs 0.1 Mid: 50.9°C
Delta Cp*: 0.100J/(g·K)
good part

on two PA6 clips already show that 0.0

the poor clip (blue curve) has an
50 100 150 200 250
additional melting peak at 239°C. Temperature /°C
This indicates the presence of PA66,
which is often blended with PA6. The DSC comparison of the 1st heating runs of two clips made of PA6 reinforced
presence of a second component is with glass fiber; sample masses 12.98 mg and 13.13 mg; heating rate 10 K/min
confirmed in the 2nd heating.

17
 Delta Cp*: 0.100J/(g·K)
0.0

50 100 150 200 250

Temperature /°C

Influence of the Thermo-

mechanical History on
Amorphous PMMA

DSC/(mW/mg)
The thermal and mechanical
[2.5] properties of polymer materials may
↓ exo vary greatly as a result of the thermal
0.40 2nd Heatings history associated with the sample.
This DSC plot depicts the second
PMMA (finished part)
heating runs of polymethyl methac-
0.35 rylate (PMMA) pellets and a finished
DSC/(mW/mg)
Glass Transition:
Mid: 105.4°C
[2.5] PMMA part. It can clearly be seen that
↓ exo
0.30
Delta Cp*: 0.332 J/(g·K) the glass transition temperature
0.40 2nd Heatings
PMMA (pellets) observed for the pellets (midpoint
Glass Transition: 111°C, red curve) is shifted to a lower
0.25 Mid: 111.1°C temperature in the finished part
PMMA (finished part)
0.35
Delta Cp*: 0.316 J/(g·K)
Glass Transition: (midpoint 105°C, black curve). Each
Mid: additional unit of thermomechanical
105.4°C
0.20 Delta Cp*: 0.332 J/(g·K)
0.30 treatment of the polymer during
40 60 80 100 120 140 thermoplastic processing may result
PMMA (pellets)
Temperature /°C in degradation ofGlass
theTransition:
molecular mass,
0.25
DSC measurement: shift of the glass transition to lower temperatures with increasing in turn leading toMid: 111.1°C
a reduction of the
Delta Cp*: 0.316 J/(g·K)
production steps; sample masses 11.54 mg and 12.5 mg; heating rate 10 K/min glass transition temperature.
0.20

40 60 80 100 120 140

Temperature /°C
DSC / (mW/mg)
↓ exo 224.5°C

Influence of Atmospheric Moisture

2.0

1.5 220.4°C
30.17 J/(g·K) DSC / (mW/mg)
Polyamides absorb atmospheric 144.2°C
moisture, which affects their ↓ exo 224.5°C

1.0
mechanical properties. 2.0
51.41 J/g
Mid: -28.3°C
The endothermic step at -28°C of the
∆Cp: 0.205 J/(g·K)
1st heating (red curve) indicates the 196.0°C
1.5 220.4°C
0.5 30.17 J/(g·K)
glass transition of the moist PA6. The
Mid: 55.1°C -2.82 J/g
144.2°C
∆Cp: 0.179 J/(g·K)
endothermic effect between 20°C
and
-50 180°C is 0 due to50
the evaporation
100 150 200
1.0 250
Temperature / °C 51.41 J/g
of water contained in the sample. In Mid: -28.3°C
the 2nd heating, the sample is dry and ∆Cp: 0.205 J/(g·K)
the glass transition temperature is 0.5
196.0°C
Mid: 55.1°C -2.82 J/g
shifted to 55°C. Water acts as a ∆Cp: 0.179 J/(g·K)
plasticizer and lowers the glass
-50 0 50 100 150 200 250
transition temperature. The peaks at Temperature / °C
225°C (1st heating) and 220°C (2nd
heating) are related to melting. The 1st and 2nd heating of moist PA6 by means of DSC;
sample mass 9.4 mg; heating rate 20 K/min
2nd heating additionally shows a cold
crystallization at 196°C.

TG /% DTG /(%/min)
100 20
18
10
 196.0°C
0.5
1.0 Mid: 55.1°C -2.82 J/g
51.41 J/g
∆Cp: 0.179 J/(g·K)
Mid: -28.3°C
∆Cp:
-500.205 J/(g·K)0 50 100 150 200 250
Temperature / °C 196.0°C
0.5

Thermogravimetric Analysis
Mid: 55.1°C -2.82 J/g
∆Cp: 0.179 J/(g·K)

-50 0 50 100 150 200 250

Temperature / °C

Detection of Added Carbon Black

Static electricity may build up in

polyethylene materials unless anti-
static additives are used. PE macro-
TG /% DTG /(%/min)
molecules are also broken down by 100 20
UV light and burns readily unless
flame retardants are applied. Carbon 10
TG
80 /% DTG /(%/min)
black is one of the best and most 20
100
economic stabilizers. 0
862.0°C
60 10
-10
The level of added carbon black 80
-98.28 %
content in PE can be easily deter- 40
0
Nitrogen -20
mined by means of a vacuum-tight 60
Air
862.0°C
TGA system. After the total decompo- -10
-30
20 -98.28 %
sition of PE in a highly pure nitrogen 481.7 °C
40 -20
atmosphere, combustion of even the Nitrogen Air%
-1.72 -40
smallest amounts of added carbon 0
-30
black can be observed in an oxidizing 20 100 200 300 400 500 600 700 800 900
481.7 °C
Temperature / °C
air atmosphere.
-1.72 % -40
0 TGA measurement on polyethylene with added carbon black;
sample
100 mass200
17.39 mg;
300Al2O3400
crucible;500
heating600
rate 10700
K/min 800 900
Temperature / °C

c-DTA® /K
Determination of Different Filler TG /%
↓ exo
DTG /(%/min)

100 -1.28 % 1.0 0

-10.34% c-DTA® /K
Fillers were previously used mostly to 90
TG /% 0.8 /(%/min)
DTG
-61.33 % -2
lower the price of finished products. ↓ exo
80
100 -1.28 % 1.0 0
TG /% 0.6
Today they are primarily used to -10.34% Additional inorganic filler: 1.5 %
improve the technical characteristics 70
90 Melting of PA 6
27.5
0.8
0.4 -4
c-DTA®: 221.2°C 27.0 -61.33 %
of polymer products. 26.5
-2
60
80 TG /% -1.54% 0.6
26.0 1098.0 °C, 25.51 % 0.2
Additional inorganic filler: 1.5 %
In this example, the determination of 50
70 Melting of PA 6
27.5
25.5
-6
1000.0 °C, 26.38 % 0.4 -4
the inorganic filler (here glassfiber) in c-DTA®: 221.2°C 27.0
25.0 0.0
26.5
a PA6 sample is carried out by means 40
60 900 950 Temperature/°C
1000
1098.0 °C, 25.51 %
1050
-1.54%
-8
26.0
1000.0 °C, 0.2
of TGA. The sample was filled with 30 26.38 %
-0.2 -6
50 25.5
25.5% glass fiber. Decomposition of Glass25.0
Fiber Content: 25.5 %
1000.0 °C, 26.38 %
0.0
1098.0 °C, 25.51 % -0.4
an additional inorganic filler can be 40 900 950 Temperature/°C
1000 1050
200 400 600 800 1000 -8
observed between 900°C and 1100°C Temperature /°C
1000.0 °C, -0.2
30 26.38 %
(see inset). Furthermore, by applying
Glass Fiber Content: 25.5 %
the c-DTA® feature of the TG 209 F1 1098.0 °C, 25.51 % -0.4

Libra® before polymer decomposition 200 400 600 800 1000

Temperature /°C
starts, an endothermic peak at 221°C
can be detected. This effect repre- 0.15 4 0.5
Determination of the melting temperature (identification) and filler content by
As a function of temperature:
sents the melting peak of PA6. TGA with c-DTA®; sample mass 12.45 mg; Al2O3 crucible; heating rate 10 K/min
0.14 Thermal Diffusivity
Thermal Conductivity
0.15 Specific Heat 4 0.5
0.13 0.4
/ W/(m·K)

As a function of temperature:
0.14
0.12
Thermal Diffusivity 19
Thermal Conductivity
m²/s

3
Specific Heat
·K)
 1000.0 °C, 26.38 % 0.6
25.0
Additional inorganic filler: 1.5 % 0.0
27.5
40
70 Melting of PA 6 900 950 Temperature/°C
1000 1050
0.4 -4
c-DTA®: 221.2°C 27.0
1000.0 °C, -8
-0.2
30 26.5 26.38 %
60 -1.54%
1098.0 °C, 25.51 % 0.2

Laser Flash Analysis

26.0
Glass Fiber Content: 25.5 % 1098.0 °C, 25.51 % -0.4 -6
50 25.5
200 400 600 800 1000.0 °C, 26.38 %
1000
25.0 0.0
Temperature /°C
40 900 950 Temperature/°C
1000 1050

1000.0 °C, -8
-0.2
Determination of the Thermophysical Behavior Even in the Molten State
30 26.38 %
Glass Fiber Content: 25.5 % 1098.0 °C, 25.51 % -0.4
200 400 600 800 1000
0.15
Temperature /°C
4 0.5 This measurement plot shows that
As a function of temperature: the thermal diffusivity of a PP sample
0.14 Thermal Diffusivity decreases significantly from 0.098 to
Thermal Conductivity
Specific Heat 0.075 mm²/s from room temperature
0.13 0.4
to the onset of melting at 150°C

Conductivity / W/(m·K)
0.15 4 0.5 (extrapolated onset of the melting
0.12
As a function of temperature:
peak from a DSC run). After melting,
Diffusivity / mm²/s

Specific Heat / J/(g·K)

0.14 Thermal Diffusivity
0.11 Thermal Conductivity 0.3 it reaches an almost constant value of
0.13
Specific Heat
0.4
0.085 mm²/s at 250°C. As expected,
the specific heat capacity increases

/ W/(m·K)
0.10

0.12 during heating: from 1.5 J/(g·K) at

/ mm²/s

0.09 3 0.2 RT to 2.2 J/(g·K) at 90°C and, during

Thermal
Specific Heat / J/(g·K)
Thermal

0.11 softening and melting, from

Thermal Conductivity
2 0.3
0.08
2.3 J/(g·K) to 2.8 J/(g·K) at 250°C.
Thermal Diffusivity

0.10
0.07 0.1
Below and above melting, the
resulting thermal conductivity shows
0.09 0.2
0.06 an increase from 0.14 W/(m·K) to
2 0.2 W/(m·K) (250°C).
0.08
0.05 1 0.0
0 80 160 240 320
0.07 Temperature /°C 0.1

0.06 LFA measurement on PP between 20°C and 300°C; sample thickness 1.05 mm, Ø 11.0 mm

0.05 1 0.0
0 80 160 240 320
2.0 Thermal Diffusivity
Temperature /°C thru plane 2.0 2.0
ThermalConductivity thru plane
1.8 Specific Heat 1.8

Thermal Diffusivity and Thermal Conductivity of PA46 Filled with Al2O3 by Means of LFA
Thermal Diffusivity in-plane
1.6 Thermal Conductivity in-plane
1.6 1.6
Conductivity /W/(m·K)
Diffusivitiy /mm²/s

Specific Heat /J/(g·K)

1.4 1.4
2.0 Thermal Diffusivity thru plane 2.0 2.0 The use of glass fiber and other
ThermalConductivity thru plane
1.2
1.8 Specific Heat 1.2
1.8
1.2 reinforcements such as Al2O3 in
Thermal Diffusivity in-plane highly crystalline PA types improve
1.0 Thermal Conductivity in-plane 1.0
1.6 1.6 1.6 the mechanical properties (modulus,
/W/(m·K)
/mm²/s

0.8 0.8 0.8 strength). These fillers also influence

Specific Heat /J/(g·K)

1.4 1.4
Thermal

the thermophysical properties (TPP,

Thermal

0.6 0.6
1.2 1.2 1.2 thermal diffusivity/conductivity and
Thermal Diffusivitiy

Thermal Conductivity

0.4
1.0
0.4
1.0
0.4 specific heat capacity), which can
be tested by means of LFA. Tests
0.2 0.2
0.8 0.8 0.8 can be carried out in the thru-plane
0.0
0.6
0.0
0.6
0.0 and the in-plane directions. For
0 10 20 30 40 50 60 70 the in-plane tests, a special sample
Alumina content /%
0.4 0.4 0.4 holder for laminates is available.
0.2 0.2
In the case of nylons, only PA46
has a very low thermal conduc-
0.0 0.0 0.0 tivity. With an increasing filler
0 10 20 30 40 50 60 70
dL/Lo/% Alumina content /%
content (here Al2O3), the specific
heat capacity decreases while
30.00
Thermophysical properties of filled PA46 depending on the alumina the thermal diffusivity and
25.00 content at room temperature thermal conductivity increase.
20.00 Temp./°C Techn. Alpha/(1/K)
dL/Lo/% 20, 50 : 48.4653E-06
15.00 50mN
30.00 Temp./°C Techn.Alpha/(1/K)
10.00 20, 50 : 50.4183E-06
25.00 Temp./°C Techn. Alpha/(1/K)
5.00
20, 50: 51.7761E-06
20
20.00 Temp./°C Techn. Alpha/(1/K)
0.00 20 mN
20, 50 : 48.4653E-06
15.00 50mN
 4000
0.04

2000
0.02

0 0.00
0 50 100 150 200
Temperature /°C

Thermal Conductivity by Heat Flow Meter

0.045

0.044

0.043
Thermal Conductivity / W/(m·K)

0.042

0.041
Test at 24°C, average 0.03992 ±0.00020 W/(m·K)

0.040

0.039

0.038 Test at 10°C, average 0.03742 ±0.00013 W/(m·K)

0.037

0.036 Deviation Lit./Average: < 0.2%

Maximum Deviation from mean: < 1%
0.035
0 1 2 3 4 5 6 7 8 9 10 11
Sample Number

Quality control of 10 EPS samples from the same batch between 10°C and 24°C;
thickness 50 mm, HFM Lambda measurements, NIST 1450c callibration standard

0.0017

Thermal Conductivity of Expanded Polystyrene Foam (EPS)

Thermal Diffusivity/ cm2/s

0.0016
The tests shown here were of the typical quality control purpose types
conducted on ten EPS samples from the same batch, to determine the
thermal conductivity in accordance with DIN EN12667.
0.0015
It can be seen that the thermal conductivity does not vary significantly
from sample to sample. The values measured are around 0.04 W/(m·K),
which is exactly the value specified for insulating materials in the
datasheet.
0.0014

The high test speed of the HFM allows for a large throughput to be tested.
This becomes important if an insulating foam needs to be analyzed in
accordance
0.0013 with DIN EN13163. In that procedure, the number of samples
18
influences 20
the λ90/90 22
value which 24
is determined 26
from the test28results. 30
Carbon Black Content / %

21
 1.6 Thermal Conductivity in-plane 1.6 1.6

Thermal Conductivity /W/(m·K)

Thermal

S
Ther
0.6 0.6

Thermal Diffusivitiy /mm²/s

Specific Heat /J/(g·K)

1.4 1.4
0.4 0.4 0.4
1.2 1.2 1.2
0.2 0.2
1.0 1.0

Thermomechanical and Dynamic Mechanical Analysis

0.0
0 10 20 30 40 0.8
Alumina content /%
50 60 70
0.0 0.0
0.8 0.8

0.6 0.6

0.4 0.4 0.4

0.2 0.2

Tension Test on a70 Shrink

dL/Lo/%
0.0 0.0 0.0
30.00 0 10 20 30 40 50 60

25.00
Alumina content /% Film of PC
20.00 Temp./°C Techn. Alpha/(1/K)
20, 50 : 48.4653E-06 Orientation effects, stretch
15.00 50mN
Temp./°C Techn.Alpha/(1/K) condition and shrinkage are
10.00 20, 50 : 50.4183E-06dL/Lo/% measured under load for films
5.00
Temp./°C Techn. Alpha/(1/K)
30.00
with the TMA 402 F1 Hyperion®.
20, 50: 51.7761E-06
In these examples, the expansion
0.00 25.00 20 mN and contraction of a 40-μm-thick
-5.00 20.00 film of polycarbonate (PC) were
Temp./°C Techn. Alpha/(1/K)
-10.00 15.00
5 mN20, 50 : 48.4653E-06tested under tensile50mN
load.
The results vary significantly
Temp./°C Techn.Alpha/(1/K)
-15.00 10.00 20, 50 : 50.4183E-06
depending on the applied load.
Temp./°C Techn. Alpha/(1/K)
0 50 100
5.00 150
20, 50: 51.7761E-06
Under low amounts of force
Temperature /°C (5 mN), the film contracts at higher
0.00 20 mN
Orientation effects of a PC shrink film measured with the TMA 402 F1 Hyperion®; temperatures; however, it expands
-5.00
sample thickness 40 µm; length ≈ 5 mm; heating rate 5 K/min if a higher force (50 mN) is applied.
-10.00 5 mN

-15.00
E´/Mpa tanδ
0 50 100 150
1000
42.9°C 8910.8 Temperature /°C
(65.7°C, 0.103) (106.6°C, 0.103)

Anisotropic
8000 Behavior of a Glass Fiber-Reinforced (PBT) by Means
0.10 of DMA
0.08
6000 (65.2°C, 0.068)
High mechanical stiffness due
(36.1°C, 4232.2)
E´/Mpa
1000 0.06
tanδ

to glass fiber reinforcement

4000
42.9°C 8910.8
(106.6°C, 0.103)
(65.7°C, 0.103)
0.04 0.10
8000
2000
The DMA measure­ments of a 0.02 0.08
finished part made of glass fiber- 6000 (65.2°C, 0.068)
reinforced
0 PBT were carried (36.1°C, 4232.2) 0.00 0.06
out on samples0 taken parallel
50 100 150 200
4000/°C
or perpendicular to the cavity Temperature
0.04
filling direction in order to inves-
tigate the anisotropic behavior. 2000
0.02

The viscoelastic properties parallel

to the fiber orientation (solid lines) 0 0.00
indicate a significantly higher 0 50 100 150 200
Temperature /°C
stiffness
0.045 (E') and a lower damping
(tanδ level). In the perpendic- Polybutylene Terephthalate: DMA measurements on PBT/30%GF parallel
ularly-oriented
0.044 fiber direction to the fiber direction (solid curves) and perpendicular to it (dotted curves);
(dotted lines), on the other hand, 3-point bending; heating rate 2 K/min; frequency 1 Hz
0.043
damping is higher and stiffness
l Conductivity / W/(m·K)

is0.042
correspondingly lower.

0.041
Test at 24°C, average 0.03992 ±0.000200.045
W/(m·K)

0.040 0.044
22
0.039 0.043
)
 Therm
Con
0.038 Test at 10°C, average 0.03742 ±0.00013 W/(m·K)
0.039

Thermal
0.037 Test at 10°C, average 0.03742 ±0.00013 W/(m·K)
0.038

Elastomers
0.036 Deviation Lit./Average: < 0.2%
0.037
Maximum Deviation from mean: < 1%
0.035
0.036 Deviation Lit./Average: < 0.2%
0 1 2 3 4 5 6 7 8 9 10 11
Maximum Deviation from mean: < 1%
Sample Number

Laser Flash Analysis

0.035
0 1 2 3 4 5 6 7 8 9 10 11
Sample Number

Influence of Carbon Black on Thermal Diffusivity in a Rubber Compound

0.0017
The flash method also offers a fast
solution for determination of the 0.0017
effect of the filler content on the cm2/s cm2/s
thermal conductivity of a polymer. 0.0016
This example on NR shows the
Diffusivity/

linear correlation of the thermal 0.0016

diffusivity, measured at room
Diffusivity/

temperature, and the carbon black 0.0015

content of a rubber mixture.
Thermal

With an increasing carbon black 0.0015

content, the thermal diffusivity rises.
Thermal

0.0014

0.0014

0.0013
18 20 22 24 26 28 30
Carbon Black Content / %
0.0013
18 20 22 24 26 28 30
LFA measurement: thermal Carbon
diffusivity
BlackofContent
rubber/ mixtures
% filled with different
quantities of carbon black at room temperature

Differential Scanning Calorimetry DSC /(mW/mg)

0.7 ↓ exo
Brittleness Point DSC /(mW/mg)
Area: 22.44 J/g
0.7 ↓ exo
0.6 Peak*: 155.4 °C

Area: 22.44 J/g

This DSC measurement was 0.6
0.5 Peak*: 155.4 °C
carried out on an SEBS+PP blend
at a heating rate of 10 K/min. The 0.5
0.4 Area: 16.51 J/g
SEBS component shows the glass Peak*: -15.7 °C

transition temperature of the soft 0.4

0.3 Area: 16.51 J/g
segments at -67°C. Melting of the Peak*: -15.7 °C

hard segments occurs at -16°C. 0.3

0.2
These effects are followed by Mid: -67.2°C
melting of the PP component at 0.2
0.1
Delta Cp*: 0.234 J/(g·K)

155°C. The glass transition temper- -100 Mid: -50 -67.2°C 0 50 100 150
ature correlates with the brittleness 0.1
Delta Cp*: 0.234 J/(g·K)
Temperature /°C
point (DIN EN ISO 11357). This is a -100 -50 0 50 100 150
material property that is required Temperature /°C
by the automotive industry.
DSC measurement of the thermoplastic elastomer SEBS+PP

23
 0.5

0.4 Area: 16.51 J/g

Peak*: -15.7 °C

0.3

0.2
Mid: -67.2°C

0.1
-100
Differential Scanning Calorimetry,
Delta Cp*: 0.234 J/(g·K)

-50 0 50 100 150

Thermogravimetry and Gas Analysis

Temperature /°C

Plasticizer Influence on the Cold Flexibility

DSC /(mW/mg)
Plasticizers or dispersants are
0.90 ↓ exo
sample A: 11% standard: 5.5% sample B: 0% additives which increase the
Glass Transition: Glass Transition: Glass Transition: plasticity or fluidity of a material.
0.80 Mid: - 13.5°C Mid: -10.1 °C Mid: - 6.8°C
Inflection: -11.7 °C Inflection: - 8.4 °C Inflection: -5.3 °C
When cooled below the glass
Delta Cp*: 0.419 J/(g·K) Delta Cp*: 0.438 J/(g·K) Delta Cp*: 0.446/(g·K) transition temperature, the viscous
0.70 chain segments "freeze" into fixed
geometries and the rubber abruptly
0.60 loses its high elasticity, although
the process is reversible. The DSC
0.50 method offers fast and reliable tests
for investigating the influence of
0.40 the plasticizer content in rubbers.
-60 -40 -20 0 20 40

Temperature /°C These measurements were carried

out on three NBR samples differing
DSC measurements on NBR. With increasing plasticizer in their plasticizer content. It can be
contents, the glass temperature is shifted to lower values;
sample masses ≈ 10 mg; heating rate 20 K/min
observed that modification of the
NBR plasticizer content yields different
glass transition temperatures. The
cold flexibility can be improved by
Temp./°C increasing the plasticizer content.
TG /% DTG /(%/min)

refill with 2 900

vacuum nitrogen oxygen
100 1 800
-20.04 % 0 700

80 -1 600

-2 500
342.0°C
60 152.1°C rubber -42.86 % 647.7°C
volatiles compound 1 -3 400
combustion of
carbon black -4 300
40
-9.08 % -5 200
429.0°C
rubber compound 2 ash content -6 100
20 Residual Mass: 28.02 % (102.5 min)
0 20 40 60 80 100
Time /min

24
TG /% Ion Current *10-11 /A
 sample A: 11% Temperature
standard: 5.5%/°C sample B: 0%
Glass Transition: Glass Transition: Glass Transition:
0.80 Mid: - 13.5°C Mid: -10.1 °C Mid: - 6.8°C
Inflection: -11.7 °C Inflection: - 8.4 °C Inflection: -5.3 °C
Delta Cp*: 0.419 J/(g·K) Delta Cp*: 0.438 J/(g·K) Delta Cp*: 0.446/(g·K)
0.70
Comprehensive Rubber Characterization
0.60

Temp./°C
Clear separation and precise identifi- TG /%
0.50 DTG /(%/min)
cation of rubber compounds can be 900
refill with 2
achieved by using the vacuum 0.40
vacuum nitrogen oxygen
1 800
capability of the TG 209 F1 Libra®. 100
-60 -40 -20 0 20 40
Under vacuum, the boiling point of -20.04 % 0 700
Temperature /°C
the volatiles is reduced, which leads 80 -1 600
to their release at lower temperatures
-2 500
while the decomposition of the 152.1°C
342.0°C
60 rubber -42.86 % 647.7°C
rubber components is shifted by an volatiles compound 1 -3 400
combustion of
insignificant amount. carbon black -4 300
40
-9.08 % -5 200
In the first measurement segment of 429.0°C
rubber compound 2 ash content -6Temp./°C
the plasticizer release (152°C, DTG TG /%
20 Residual Mass: 28.02 % (102.5DTG
min)/(%/min)
100

peak) is clearly separated from the 900

0 20 40 60
refill with 80 100 2
decomposition of the two rubber vacuum
Time /minnitrogen oxygen
1 800
components at 342°C and 429°C 100
(DTG peaks). After decomposition of TGA measurement on a%rubber mixture under vacuum and back-filling with
-20.04 0 700
nitrogen followed by combustion of carbon black in oxygen; sample mass
the rubber components at 600°C, the 80 10.05 mg; heating rate 10 K/min; Al2O3 crucible -1 600
TGA system is refilled with nitrogen
-2 500
under isothermal conditions. In the 152.1°C
342.0°C
60 rubber -42.86 % 647.7°C
following step, the atmosphere is volatiles compound 1 -3 400
combustion of
changed to oxygen, which leads to carbon black -4 300
the immediate combustion of carbon 40
-9.08 % -5 200
black (9%) under increasing tempera- TG /% 429.0°C Ion Current *10-11 /A
rubber compound 2 ash content -6 100
tures (remaining ash content 28%). 20 Residual Mass: 28.02 % (102.5 min) 1.4

100 0 20 40 60 80 100
1.2
Time /min
1.0
80 -42.52 %
amu 67
0.8

Classification of the Gases Evolved During Rubber Decomposition:

60
0.6

Plasticizer and PAHs by Means of Gas Analysis

40 Coupledamu
to TGA
55
-24.73 %
0.4

amu 81
0.2
20 amu 78
amu 57
Coupling of gas analyzers such as TG /% Ion Current *10 0/A
-11

amu 136 amu 92 amu 104

mass spectrometers to TA methods 1.4
0 -0.2
allows for the chemical identification 100
100 200 300 400 500 600 700 1.2
of the evolved gases. An example of a Temperature /°C
question here would be whether the 1.0
80 -42.52 %
rubber releases potentially carcino- amu 67
genic polycyclic highly aromatic 0.8

hydrocarbons (PAHs). 60
0.6
-24.73 %
During heating of the rubber sample 40 amu 55 0.4
to 800°C, two mass-loss steps of amu 81
0.2
42.5% and 24.7% were observed. 20 amu 78
amu 57
From the MS signals (only a few 0
amu 136 amu 92 amu 104
exemplary mass numbers are shown),
0 -0.2
conclusions can be drawn as to which E´/ MPa E“ / MPa 500
tanδ
100 200 300 400 600 700
organic molecules evolved at which 4000 600 (-21.9°C,
Temperature /°C 0.53)
0.6

temperature. For example, at 3500 (-29.0°C, 508.0)

500 STA-MS measurement detects evolved gases during decomposition 0.5
350°C, mass number 67 (most of a tire sample
3000 Onset
probably due to C5H7) indicates the (-36.1°C, 3009.5)
400 0.4
release of the plasticizer. 2500

2000 300 0.3

20 Hz
10 Hz
1500
200 5 Hz 25
0.2
2 Hz
1000
 0 700

80 -1 600

-2 500
342.0°C
60 152.1°C rubber -42.86 % 647.7°C
volatiles compound 1 -3 400
combustion of
carbon black -4 300
40
-9.08 % -5 200
429.0°C
rubber compound 2 ash content -6 100
20 Residual Mass: 28.02 % (102.5 min)
0 20 40 60 80 100
Time /min

TG /% Ion Current *10-11 /A

Dynamic Mechanical Analysis

1.4

100
1.2

1.0
80 -42.52 %
amu 67
Influence of the Frequency on the Glass Transition Temperature of an SBR Rubber
0.8

Mixture by Means of DMA

60
0.6
-24.73 %
40 amu 55 0.4
The modulus and damping factor are the main viscoelastic properties of polymers measured by DMA. The
storage modulus, E’, is a measure of the stiffness amu 81and is temperature-dependent. The mechanical damping
0.2
(tanδ, internal friction) of20filled rubbers is highly78relevant for such amu
amu functions
57 as the wet grip behavior of a tire
0
or the seal behavior of an O-ring. amu 136 amu 92 amu 104
0 -0.2
This example of an SBR (styrene
100 butadiene
200 rubber)
300 mixture
400 shows 500that at600
low temperatures
700 (-70°C to -45°C),
the loss factor tanδ is also very low, because there isTemperature
so little free
/°C volume in the polymer that polymer segments

are not able to move at all. This results in a low energy dissipation and the polymer transitions into the glassy
state with a high storage modulus (high elasticity and high stiffness).

As temperature increases, the polymer segments also exhibit increased movement, thus yielding high values for
loss modulus (E”) and tanδ with a maximum at the glass transition. Increasing frequencies shift these peak
temperatures for the glass transition to higher temperatures. Additionally, higher E’ values are obtained with
increasing frequencies.

E´/ MPa E“ / MPa tanδ

4000 600 0.6
(-21.9°C, 0.53)
3500 (-29.0°C, 508.0)
500 0.5
3000 Onset
400 (-36.1°C, 3009.5) 0.4
2500

2000 300 0.3

20 Hz
10 Hz
1500
200 5 Hz 0.2
2 Hz
1000 1 Hz
100 0.1
500

0 0 0.0
-70 -60 -50 -40 -30 -20 -10 0 10 20
Temperature /°C

DMA measurement of the viscoelastic properties of an SBR rubber mixture: storage modulus (E‘, green),
loss modulus (E“, blue) and damping factor (tanδ, red) as a function of frequency; heating rate 2 K/min

26
E´/MPa tanδ E“ / MPa
1500
200 5 Hz 0.2
2 Hz
1000 1 Hz
100 0.1
500

0 0 0.0
-70 -60 -50 -40 -30 -20 -10 0 10 20
Temperature /°C

E´/MPa tanδ E“ / MPa

Onset: -63 °C
10³ Peak: -51 °C 10³
0.18
Peak: 2 °C
5 0.16 5

2 Onset: -19 °C 0.14

2
Peak: -56 °C 0.12
10² 10²
0.10

5 5
0.08
Onset: -5 °C

2 0.06
2

0.04
101 101
0.02
5 5
0.00
-60 -40 -20 0 20 40 60
Temperature /°C

DMA measurement of the thermoplastic elastomer EPDM+PP

Viscoelastic Properties of a TPE

68 u *106a.u.
TG /% 144 u *104 /a.u.
TG
100 DMA is a valuable tool for determining
-42.23 % the viscoelastic properties of TPE
materials.
DTGThe plot exhibits a DMA measurement on Santoprene®.
6
8
80
This TPE is a blend of EPDM rubber and the semi-crystalline poly-propylene
(PP) thermoplastic. The DMA measurement was carried out between 4
60 -80°C and 80°C at a frequency of 1454 Hz.°CDepicted in the plot are the6 storage
modulus (E’), loss modulus394 °C(E”) and loss factor (tanδ). The glass transition
405 °C
of the EPDM component can be observed in E'
-28.67 % at -63°C (E’, onset),
2 again
40 in E” at -56°C (peak) and finally in tanδ at -51°C (peak). Subsequently, 4
the
glass transition of the PP component can be also observed in E' at -19°C
m/z 68
0
(onset), again in E" at -5°C (also onset), 486and
°C finally in tanδ at 2°C (peak).
2
20

m/z 144 -2
0 0
100 200 300 400 500 600 700 800
Temperature /°C

DSC /(mW/mg)
[reversing]

0.11 ↓ exo
27
0.10
 0.04 4
101 101 454 °C 6
60
0.02 394 °C
5 5 °C
405 2
0.00 -28.67 %
40 4
-60 -40 -20 0 20 40 60

Evolved Gas Analysis

Temperature /°C m/z 68
0
20 486 °C 2

m/z 144 -2
TGA-GC-MS Measurement for Significantly
0
Improved Interpretation of Organic Vapors 0
100 200 300 400 500 600 700 800
Temperature /°C

The very high-sensitivity TGA-GC-MS

68 u *106a.u.
TG /%
coupling yields information on
144 u *104 /a.u.
TG the composition of evolved gases.
100 -42.23 %
Separation of the volatiles is made
DTG
6 possible by use of the GC column.
8
80 DSC /(mW/mg)
[reversing] The plot depicts a measurement
0.11 ↓ exo 4 on NR/SBR rubber. The GC-MS was
60 454 °C 6
0.10
operated with a fixed column
394 °C
405 °C temperature (250°C) and short
-28.67 2
0.90% injection intervals of 1 min. The
40 4
0.80 TGA and DTG curves indicate an
m/z 68 DSC (reversing)
0 overlapping decomposition
Glass Transition: of the
DSC (non-reversing)
20 486 °C 0.70 2
Mid: 61.5 °C
individual rubber components.
DSC (total)
Delta Cp*: 0.170 J/(g·K)
0.60 However, the evolved gases can be
Complex Peak:
m/z 144
0.50 Area: 5.99 J/g
-2 identified inComplex
good Peak:
temperature and
0 Area: -8.79 J/g
Peak*: 55.2 °C 0 time correlation Peak*: 133.2 °Che TGA and
with
100 200 300 400 500 600
0.40 700 800 DTG results. The DTG peak at 394°C
Temperature /°C is due to the release of isoprene
0.03
0
Identification of the gases evolving during decomposition of a rubber mixture;
50 (1,3-butadiene,
100 2-methyl,
150 m/z 68)
Temperature /°C
sample mass 5.28 mg; heating rate 20 K/min; 1 min injection intervals which is typical for NR. The DTG peak
at 454°C corresponds to the release
of C11H12 (1-cyclopentene-1-1yl-
benzene, m/z 144) which is repre-
DSC /(mW/mg) sentative of the SBR component.

Dielectric Analysis
[reversing]

0.11 ↓ exo

0.10

0.90 Cure Monitoring of EVA Ionenvisc. /Ohm cm Temperature / °C

0.80
DSC (reversing)
The EVA copolymer is used Glass Transition:
DSC (non-reversing)
0.70 Mid: 61.5 °C 3 140
for encapsulation of electricDelta Cp*: 0.170 J/(g·K)
DSC (total)
0.60 devices. As the polymerization . cm
151.3°C, 18.9E+0.9 Ohm
Complex Peak: 2 Peak:
reaction is irreversible, the
Area: 5.99 J/g
Complex
. cm
End: 150.9°C, 15.7E+0.9 Ohm
120
0.50 Area: -8.79 J/g
thermal
Peak*:treatment
55.2 °C is crucial in Peak*: 133.2 °C
0.40 the encapsulation process. 100
0.03 10
9
The
0 plot presents50 the sample 100
8
150
80
Temperature /°C
behavior of the ion viscosity at 7
6
1 Hz. The cross-linking reaction
5 60
from using peroxide was observed
under isothermal conditions at 4
Peak: 150.7°C, 3.88E+0.9 Ohm. cm Ion visc. (1,000 Hz)
150°C. The subsequent increase 3 Temperature
40

in ion viscosity correlates with the

increase in the degree of cure. 10 20 30 40 50 60
Time / min
After 60 min, the ion viscosity
remains nearly constant, which Multi-frequency test on EVA was carried out at frequencies between 1 Hz
indicates that the cross-linking and 10000 Hz while monitoring the ion viscosity (Ωcm). The plot shows the
Ionenvisc. /Ohm cm Temperature / °C
reaction has practically terminated. measurement at 1 Hz at 150°C.

3 140

28 . cm
151.3°C, 18.9E+0.9 Ohm
2 120
. cm
End: 150.9°C, 15.7E+0.9 Ohm
 60 454J/(g·K)
°C DSC (total) 6
Delta Cp*: 0.170
0.60 394 °C
Complex Peak: 405 °C Complex Peak:
-28.67 % 2
0.50 Area: 5.99 J/g Area: -8.79 J/g
40 4
Peak*: 55.2 °C Peak*: 133.2 °C
0.40 m/z 68

Thermosets and Composites

0
0.03
20 486 °C 2
0 50 100 150
Temperature /°C
m/z 144 -2
0 0
100 200 300 400 500
Temperature /°C
600
Differential Scanning Calorimetry
700 800

Glass Transition and Curing

of a PUR Resin
Ionenvisc. /Ohm cm
DSC /(mW/mg) Temperature / °C
[reversing] Temperature-Modulated Differ-
0.11 ↓ exo ential Scanning Calorimetry
3 140
(TM-DSC) is a DSC technique in
0.10
. cm
151.3°C, 18.9E+0.9 Ohm which the sample is subjected to
2 120
0.90 . cm
End: 150.9°C, 15.7E+0.9 Ohm a superposition of a linear and a
periodic temperature program.
0.80
Glass Transition:
DSC (reversing) 100 With TM-DSC, it is possible to
DSC (non-reversing)
0.70
10 Mid: 61.5 °C
DSC (total) separate overlapping DSC signals
9 Delta Cp*: 0.170 J/(g·K)
0.608 80 by calculating the reversing and
7 Complex Peak: Complex Peak: the non-reversing part. Glass transi-
0.506 Area: 5.99 J/g Area: -8.79 J/g
Peak*: 55.2 °C Peak*: 133.2 °C
tions can therefore be well separated
5 60
0.40 from other effects such as relaxation,
4
Peak: 150.7°C, 3.88E+0.9 Ohm. cm curing, decomposition, evaporation
0.03 Ion visc. (1,000 Hz) 40
3 0 50 100 150
Temperature or cold-crystallization processes.
Temperature /°C
10 20 30 40 50 60
TM-DSC measurement of a polyurethane resin The overlapping relaxation in the
Time / min
total DSC curve can be clearly
separated from the endothermic glass
transition (reversing) and exothermic
curing (non-reversing) in a single run.

Ionenvisc. /Ohm cm Temperature / °C

Ion
3 visc. /Ohm cm 140
Fast UV Curing of an
. cm
151.3°C, 18.9E+0.9 Ohm
Epoxy Resin
2
1010 End: 128.5 s, 4659E+06 Ohm.cm 120
. cm
End: 150.9°C, 15.7E+0.9 Ohm
The fast curing of this epoxy
10 9
100
adhesive can be observed with the
10
DEA by using an IDEX sensor and
9
1088
applying a frequency of 1000 Hz.
80
7 The UV light exposure (intensity
6
107
55 mW/cm2 to 60 mW/cm2) was
5 60 applied for 60 s on the sample
4 layer, which was approx. 200 μm
106 Peak: 150.7°C, 3.88E+0.9 Ohm. cm
3
17.0 s, 1.2E+06 Ohm.cm Ion visc. (1,000 Hz) 40 thick, at room temperature.
Temperature
After 17 s of light exposure,
105 curing began. This was evidenced
10 20 30 40 50 60
0 100 200 300
Time / min 400 500 600 by the increase in ion viscosity.
Time / s
The adhesive was completely
UV curing of a cationic epoxy resin at room temperature with the DEA at 1000 Hz cured after approx. 350 s.

29
 24.0
0
107
22.0

106
-5000 17.0 s, 1.2E+06 Ohm.cm 20.0

Heat Flow Meter

400 420 440 460 480 500
105 Time/min

0 100 200 300 400 500 600

Time / s

Specific Heat Capacity of a PU Foam

The plot compares the specific heat Specific Heat/J/(g·K)

results of a PU foam between 10°C and 1.5
30°C (10 K steps) measured by DSC and
HFM. The sample mass for the DSC test 1.4
amounted to 10 mg; for the HFM tests,
1.3
the sample masses were 38 g and 51 g,
respectively. 1.2

0.04
1.1
The differences between the DSC and
HFM results are less than 3%, which is 1
Thermal Conductivity / W/(m·K)

DSC
within the stated uncertainty for the 0.9
GHP
HFM – PU Foam – 3cm
instruments and homogeneity of the HFM HFM – PU Foam – 2cm
material. 0.8
0.03 +3%
-3%
0.7
These tests show that the HFM
446 Lambda is capable of deter- 0.6
5 10 15 20 25 30 35
mining the specific heat capacity of Temperature/°C
0.02
large-volume and inhomogeneous
materials typical for applications in the Comparison of the cp test results on a PU foam obtained by the DSC 204 F1
building and insulation industries. Phoenix® and HFM 446 Lambda. Sample thicknesses for the HFM tests were
2 cm and 3 cm, respectively.

0.01
-175 -150 -125 -100 -75 -50 -25 0 25 50

High-Pressure DSC
Temperature /°C

Polycondensation of Phenolic Resin

The curing reaction of phenolic DSC /(mW/mg)

resins is caused by polyconden- 0.80 ↓ exo
150.8°C
sation. The endothermal release
of the polycondensation products 0.60

overlaps the exothermal curing. In -137.3 J/g 236.6°C

0.40 201.9°C, 67.12%
such cases, curing can only be inves- 140.5°C 282.3°C, 100%
tigated with standard DSC measure-
0.2
ments using autoclaves, or with
high-pressure DSC measurements.
0 -144.2 J/g
162.5°C 191.3°C, 61.84% 235.6°C
This test example shows two 280.3°C, 100%
-0.2
phenolic resins measured with
the DSC 204 HP Phoenix® under 157.5°C
-0.40
a practical pressure of 9 MPa 120 140 160 180 200 220 240 260 280
(90 bar). The differences between Temperature /°C
these resins can be seen in the fact
DSC 204 HP: exothermal curing behavior of two phenolic resins under high
that curing begins at 141°C and pressure; sample mass 10.5 mg; heating rate 10 K/min; pressure 9 MPa;
151°C (extrapolated onsets), respec- atmosphere inert
tively, as well as in the different
results of the partial area evaluation.

E‘ /MPa tan δ E‘‘ /MPa

30 16000 18000
180.01 °C 188.0°C
 GHP

Thermal Conductivity / W/(

HFM
0.03

0.02

0.01
-175 -150 -125 -100 -75 -50 -25 0 25 50
Temperature /°C

DSC /(mW/mg)
0.80 ↓ exo
150.8°C

Dynamic Mechanical Analysis 0.60

-137.3 J/g 236.6°C

0.40 201.9°C, 67.12%
140.5°C 282.3°C, 100%
Stiffness Determination
0.2

0 -144.2 J/g
This example depicts the storage modulus
162.5°C E’ (green),
191.3°C, loss 235.6°C
modulus
61.84% E” (red) and loss factor tanδ (blue) of a
280.3°C, 100%
carbon fiber-reinforced
-0.2 epoxy resin. The sample was measured in the bending mode at a frequency of 10 Hz
and a heating rate of 3 K/min using the DMA. Prior to reaching 120°C, the material is even stiffer than titanium,
157.5°C
at a value of 140,000
-0.40 MPa.
120 140 160 180 200 220 240 260 280
Temperature /°C
At 158°C (extrapolated onset temperature of E’), the modulus drops due to the glass transition of the epoxy
matrix. The corresponding peaks for E” and tanδ are at 180°C and 188°C, respectively.

E‘ /MPa tan δ E‘‘ /MPa

16000 18000
180.01 °C 188.0°C

157.6°C 16000
14000 0.20
14000
12000
12000
0.15
10000
10000

8000 0.10 8000

6000 6000

0.05 4000
4000
2000

0 50 100 150 200 250

Temperature /°C

DMA measurement on a high-modulus carbon fiber-reinforced epoxy resin

Ion visc. /Ohm*cm Temp. /°C

End*: 170.8 min, 130E+09 Ohm*cm

109

2 31
8
 Dielectric Analysis E‘ /MPa
16000
180.01 °C 188.0°C
tan δ E‘‘ /MPa

18000

157.6°C 16000
14000
Cure Monitoring of a CF-Reinforced Epoxy Resin
0.20
14000
12000
12000
0.15
After what 10000
amount of time or at what temperature ion viscosity initially decreased10000
due to the temper-
does a curing reaction start? Is the thermosetting ature increase. It then increased during the first
8000 0.10 8000
resin already fully cured? Such or similar questions isothermal segment, due to the start of curing. While
are those that resin producers and thermoset
6000
heating to 180°C, the temperature 6000 increase counter-
processors would like to answer comprehensively. acted with the curing so0.05 that the ion viscosity first
4000
4000 decreased before curing began to dominate. There-
The plot depicts the curing of a carbon fiber- after, the ion viscosity was recorded
2000 with a rising
reinforced epoxy resin (DEA measurement) during degree of cure. As soon as the curing was completed,
0 50 100 150 200 250
Resin Transfer Molding (RTM) for aircraft applications. the ion viscosity reached a constant value (here
Temperature /°C
During a two-step temperature curing program, the evaluated as extrapolated onset at 1.3 x 109 Ωcm).

Ion visc. /Ohm*cm Temp. /°C

End*: 170.8 min, 130E+09 Ohm*cm

109

108

2
Middle Layer
107 Bottom Layer
Top Layer
5

2
127.2 min
106 124.2 min 126.0 min

50 100 150 200 250

Time /min

Dielectric analysis (DEA) with different IDEX sensor positions

Heat flow rate /(W/g)

-0.2
10.0 K/min
5.0 K/min
-0.4 3.0 K/min

-0.6
A–1→B–2→C–3→D–4→E

-0.8 Step 1: n-th order with autocatalysis by B

Step 2: n-th order
Step 3: n-th order
-1.0 ↓ exo Step 4: n-th order

32 40 80 120 160 200 240

Temperature /°C
Conversion Rate /%

100 100 °C
80 °C

80
60 °C

60

40

20
In-Process Cure Monitoring
0
The NETZSCH DEA 288 Ionic can be applied as a sensor for online cure
0 20 40 60
monitoring during thermoset injection
Time /min molding. 80 100

The upper pictures show the DEA sensor (blue area) integrated in a
test mold applied at a injection molding machine.

The lower picture shows the ion viscosity signals for the four subse-
quent shots as a function of time. All shots show excellent agreement
thus depicting perfect reproducibility of the process conditions used.

Log (Ionenvisk.) /Ohm*cm Temp. /°C

7.6
182.8

7.4 182.6

182.4
7.2
182.2
7.0
182.0

6.8
181.8

6.6 181.6

181.4
6.4
181.2
0.0 0.5 1.0 1.5 2.0 2.5 3.0
Time /min

Curing Behavior of a thermoset during molding process; mold temperatures are

represented in solid lines, ion viscosity in dotted curves

33
34
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35
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