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generally refers to the simulta-
neous application of Thermogra- Melting/crystallization Mass changes
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vimetry (TGA) and Differential behavior Temperature stability
Scanning Calorimetry (DSC) to Solid-solid transitions Oxidation/reduction
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one and the same sample in a Polymorphism behavior
single instrument. The advan- Degree of crystallinity Decomposition
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tages are obvious: The test condi- Glass transitions Corrosion studies
tions are perfectly identical for Cross-linking reactions Compositional analysis
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the TGA and DSC signals (same Oxidative stability Thermokinetics
atmosphere, gas flow rate, Purity Determination
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vapor pressure on the sample, Specific heat capacity
heating rate, thermal contact to Thermokinetics
the sample crucible and sensor,
radiation effect, etc.). Furthermore,
sample throughput is improved Standard* Description
as more information can be
gathered from each test run. ISO 11358 Plastics – Thermogravimetry (TG) of Polymers
Standard Test Method for Enthalpies of Fusion and
ASTM E793
Crystallization by Differential Scanning Calorimetry
Thermal Analysis; Determination of Melting Temperatures
DIN 51004
of Crystalline Materials by Differential Thermal Analysis
DIN 51006 Thermal analysis (TA); Thermogravimetry (TG); Principles
DIN 51007 Thermal Analysis; Differential Thermal Analysis; Principles
2
The NETZSCH STA Eco-Line
70% LESS ENERGY AND COST.
NO EXTERNAL TEMPERATURE CONTROL NEEDED.
To obtain exact Thermogravimetric results with low drift behavior, most manufacturers
have to resort to thermostatic control using a water cycle. Having to run the thermostat
continuously requires a lot of energy and produces waste heat, which subsequently
needs to be regulated by air conditioning.
NETZSCH has succeeded in removing the external thermostat. The weighing chamber’s
temperature is now regulated electronically, while maintaining excellent temperature
stability. By removing the thermostat, the energy consumption of an STA 449 F3 Jupiter®
will decrease by 70% for an average user.*
* When using the instrument 3 times a day on 250 days a year
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Saves space
Less maintenance
Best performance
3
World-Leading Flexibility for
Your Applications hrough
c h m arks t n
n io
n g N ew Be & Innovat
i
Sett perience
Ex
The STA 449 F3 Jupiter® combines
a high-performance Heat-Flux DSC
with a submicrogram-resolution
thermobalance, thereby offering
an unmatched sample load and
measurement range. The Simulta-
neous Thermal Analyzer can easily
be adjusted to nearly any possible
application by selecting the
optimum furnace, installing the
most appropriate sensor and using
the proper accessories.
The robust system setup, user-
friendly software and flexible
design along with the wide range
of different options make the
system an ideal tool for quality
control and research for material
characterization.
4
Top-Loading – The Standard Stability, Low Drift and Defined Atmosphere
for Balance Systems High Sample Loads Conditions – Vacuum-Tight
Design
The STA 449 F3 Jupiter® is a The balance system of the The STA 449 F3 Jupiter® is
top-loading system using a STA 449 F3 Jupiter® offers high vacuum-tight by design. Several
balance design that has been sample loads (up to 35 grams) and pump systems can be connected
standard for a long time in other measurement range (35 grams) as to the STA which allow evacuation
types of scales – in laboratories well as high resolution (0.1 μg) down to 10-4 mbar* and back-filling
and even in the kitchen at home or and low drift (in the microgram with well-defined atmospheres.
in a supermarket, most balances range over hours). The unique OTS® (oxygen
have been top-loading for Another outstanding feature of trapping system) accessory can
decades. The reasons are simple: the balance section of the STA is be used to reduce the oxygen
These systems combine ideal its high accuracy. partial pressure at the sample.
performance with easy handling.
S–
YEAR
– 5 0 er of
n u factur
a e
ing M manc
Lead h-Perfor Systems
Hig nalys
is
m a l A
Ther
Trend-Setting
Technology
5
Select the Appropriate
Ten interchangeable furnaces are available to accommodate different application areas across the entire
temperature range (-150°C to 2400°C). A double furnace hoist allows the simultaneous installation of two
different furnaces for improved sample throughput or for low- and high-temperature tests with the same
instrument. The furnaces can easily be changed by the operator. Therefore, the system is adaptable to any
future application range.
For standard STA measurements, The silver and steel furnaces allow
the silicon carbide furnace (SiC) is for measurements in the subam-
the robust workhorse in your bient temperature range by using
laboratory, operating from devices for controlled cooling.
ambient temperature to 1600°C. Whereas the silver furnace is
For measurements under corrosive ideally suited for the determi-
atmosphere, the SiC furnace can nation of the specific heat
be equipped with a protected capacity, the steel furnace offers a
TGA-DTA sensor, guaranteeing broad temperature range from
instrument-safe conditions. -150°C to 1000°C.
The platinum and the rhodium The high-speed furnace allows for
furnaces in combination with the simulation of realistic heating
dedicated DSC sensors are specifi- processes with linear heating rates
cally suited for determination of up to 1000 K/min. Additionally, the
the specific heat capacity in the high heating rates are useful when
higher temperature range. implementing kinetic studies.
6
Furnace
for Your Application!
The tungsten heating element The copper furnace is ideal for measurements under relative humidity
allows for measurements under between room temperature and 100°C. For this purpose, a humidity
helium atmosphere from room generator is available which offers a maximum dewpoint of 80°C corre-
temperature to 2400°C. sponding to 47% molar concentration. In addition, the copper furnace
can be used for conventional STA measurements including determi-
nation of the specific heat capacity up to 500°C.
The water-vapor furnace covers the broad temperature range from room
temperature to 1250°C. The furnace can be connected to the aforemen-
tioned humidity generator, or to a vapor generator which produces
steam by evaporating water. A molar concentration of up to 100% can
be achieved.
7
The Right Sensor for Your Demands
Various Sensors
The STA 449 F3 Jupiter® can be equipped with different sensor types. TGA sensors with slip-on
plates or large crucibles (up to 5 ml) allow tests on large sample volumes and masses. TGA-DTA
sensors can be used for applications such as routine tests or measurements on aggressive
sample substances. For special applications such as tests under corrosive atmospheres, the
protected sensors can be employed. The TGA-DSC and TGA-DSC-cp sensors are used for
most tests and allow quantitative DSC testing simultaneously to the TGA results. The cp
versions additionally allow determination of the specific heat capacity with high accuracy.
Sensor
Temperature range Sensor types Atmospheres
thermocouple
Type E -150°C to 700°C* TGA-DTA, TGA-DSC (cp) inert, red., oxid., vac.
Type K -150°C to 800°C* TGA-DTA, TGA-DSC (cp) inert, red., oxid., vac.
Type S RT to 1650°C TGA, TGA-DTA, TGA-DSC (cp) inert, red., oxid., vac.
Type S protected RT to 1650°C TGA, TGA-DTA inert, red., oxid., vac., corr.
Type P -150°C to 1000°C TGA, TGA-DSC, TGA-DSC (cp) inert, red., oxid., vac.
Type B RT to 1750°C TGA, TGA-DTA, TGA-DSC inert, red., oxid., vac.
Type W RT to 2400°C TGA, TGA-DTA inert, red., vac.
8
Standard Type S Sensors – High Sensitivity in the High and Highest
Workhorse and Specialty Lower Temperature Range Temperature Range
In the high-temperature range, The type P sensors are standard True DSC measurements up to
type S sensors combine a broad in the lower temperature 1750°C can be monitored by using
temperature range from room range; they are ideally suited the type B sensor. At the highest
temperature to 1650°C with for the steel furnace. temperatures up to 2400°C,
high sensitivity. For measure- All sensors equipped with the type W sensor for TGA and
ments in the presence of corrosive thermocouple E or K are charac- TGA-DTA can be used under inert,
gases, the TGA-DTA sensor terized by the highest level of reducing, and vacuum conditions.
with protected thermocouples sensitivity and resolution. They
provides safe conditions without are particularly well suited
adversely affecting the sensitivity. for detecting small effects.
HIGHEST PRECISION
Maximum Flexibility
9
gas outlet valve
Gas Flow Control
furnace thermocouple
The gas flow is generally
hoisting controlled by frits which are
device installed in the 3 gas flow channels
heating element
(2 purge gases, 1 protective gas).
sample carrier Optionally available is a metal-
housed mass flow control system
protective tube
(MFC) for purge and protective
radiation shield gases, offering optimum control of
the atmosphere around the
evacuating system sample. Well defined gas flow
conditions are crucial for accurate
MFC
purge 1 interpretation of the measured
MFC
purge 2 effects, e.g., to differentiate
MFC
protective between oxidation and pyrolysis
balance reactions.
system
gas supply
unit
10
Automatic Sample Changer Accessories
Robust and
Easy-to-Operate
11
Proteus® software is produced by an ISO-certified company and includes
everything you need to evaluate the resulting data, and even perform
complicated analyses.
12
SIMULATIVE 100
100
Model Based
Model Based
OPTIMIZATION A B C D
100 Model Based
98
98
OF DEBINDING
98 10,0 K/min
96
/% /%
Fit
10,0
5,0 K/min
K/min
Mass
96 Fit
Fit
10,0 K/min
96 5,0 K/min
3,0 Fit
K/min
/%
Mass
94 Fit
5,0Fit
K/min
Mass
3,0Fit
1,0 K/min
K/min
94 Fit
3,0Fit
K/min
94 1,0 K/min
0,3 Fit
K/min
92 Fit
1,0Fit
K/min
0,3Fit
0,1 K/min
K/min
92 Fit
0,3Fit
K/min
92 0,1Fit
K/min
90 0,1 Fit
K/min
50 Fit 100 150 200 250 300 350 400 450 500
90
50 100 150 Temperature
200 250 /°C 300 350 400 450 500
90
Fig. 1: Experimental TGA data (symbols) are in good agreement500
50 100 150 200 250 300
Temperature /°C 350 400 450
with
Temperature
the results of the simulation /°C according to a 3-step kinetic
(solid lines)
model for heating rates at 0.1, 0.3, 1, 5 and 10 K/min.
100 550
Optimization
100 t:; : SignalRate 550
99 Optimization 500
Optimization of the Burn-Out 100
99
98
t:; : SignalRate
Optimization
t:; : SignalRate
550
500
/°C/°C /°C
97
96 400
In sinter metallurgy, a polymeric
Temperature
97
/% /%
350
400
96
binder is added to a metal
Temperature
95
Mass
96 350
Temperature
300
powder to improve adhesion.
/%
95 350
Mass
94
95
During the sintering process, 300
Mass
94 250
300
the binder is carefully removed 93
94 250
to prevent micro cracks caused 93
92
200
250
93
by the release of gases. Slow 92 Signal 0,05 %/min 200
91 150
200
heating results in time loss during 92 Temperature
Signal 0,05 %/min
150
production, while fast heating 91
90 Temperature
Signal 0,05 %/min 100
150
91 0 20 40 60 80 100
Temperature 120 140 160 180 200
results in quality loss due to 90 Time /min 100
intensive gas development 90 0 20 40 60 80 100 120 140 160 180 200
100
0 20 40 60 80 Time100/min
120 140 160 180 200
during polymer decomposition. Time /min
Fig. 2: Optimized temperature program for the burn-out of the
polymer binder under laboratory conditions
With these conditions in mind, 100 450
the objective here is to find the 100
Prediction
450
99 t:; : MultipleStep 400
optimum temperature program 100 Prediction 450
99 t:; : MultipleStep
Prediction
for a tunnel kiln. The production 98
99 t:; : MultipleStep
400
350
400
process is simulated by six TGA 98
97 350
300
measurements (Fig. 1) conducted 98
/°C/°C /°C
350
97
96
at different heating rates and a 300
Temperature
97
/% /%
250
96 300
kinetic model based on them. 95
Mass
Temperature
96 250
In this example, a mass loss rate 200
Temperature
/%
95 250
Mass
94
of 0.05%/min yields optimal 95 200
Mass
94 150
200
material quality. Under laboratory 93
94 150
conditions, the temperature 93
92
100
150
93
program in Fig. 2 achieves this. 92 Mass
100
50
91 100
Fig. 3 shows the optimum temper- 92 Temperature
Mass
91 50
ature curve for the different 90
91 0
Temperature
Mass 0
50
20 40 60 80 100 120 140 160 180 200
zones in the tunnel kiln. 90 Temperature
Time /min 0
90 0 20 40 60 80 100 120 140 160 180 200 0
0 20 40 60 80Time100
/min 120 140 160 180 200
We also offer “Kinetics as a Service“. Time /min
For more information, please refer Fig. 3: Optimized zone temperatures for the burn-out of the
to www.kinetics.netzsch.com polymer binder in the tunnel kiln during the production process
13
APPLICATION EXAMPLES
Meaningful Material
Characterization
LOW-TEMPERATURE
Burn-Out of Linoleum
The building material linoleum was
invented in 1863 and is most often
used as floor covering. It is very
robust and has an insulating effect
even at small thicknesses. This STA
measurement in air reflects the
natural contents of linoleum: after
the evaporation of humidity below
150°C, the stepwise, strongly
exothermic burn-out of linseed
oil, natural resins, cork flour, wood
flour and the substrate jute
followed between approx. 200°C
and 500°C. The entire heat released
during the oxidation was 14.5 kJ/g.
Between 600°C and 750°C, the
endothermic decomposition of the
The measurement was carried out in the SiC furnace on a linoleum sample (5.52 mg)
filler CaCO3 (chalk) is observed.
at a heating rate of 10 K/min in air atmosphere.
Above 750°C, the residual mass
remains constant.
14
Characterization of Explosives
The highly explosive material
hexogen (also called RDX, T4, etc.)
starts to lose mass already at about
150°C, as can be seen from the
TGA curve. The endothermic DSC
peak at an onset temperature of
206°C with an enthalpy of 123 J/g
is due to melting of the sample,
followed by a strongly exothermic
decomposition, releasing 1.38 kJ/g
of energy. This experiment was
carried out in a synthetic air
atmosphere at a heating rate of
5 K/min using an initial sample
mass of only 2.32 mg.
The hexogen measurement was made in the SiC furnace at a heating rate of
5 K/min in air atmosphere.
15
Meaningful Material
Characterization
HIGH-TEMPERATURE
Characterization of Porcelain
Raw Material
16
Building Material –
Glass Wool
17
Technical Specifications
STA 449 F3 Jupiter®
Design Top-loading
Temperature range -150°C to 2400°C
Variety of furnaces incl. high-speed, water-vapor, low to
Furnace
highest temperature, e.g., silver, platinum, tungsten, etc.
Double hoist for two furnaces or one furnace +
Motorized furnace hoist
automatic sample changer
··TGA: up to 5 ml
Sample volume (max.) ··DTA: 0.9 mlml
DSC: 0.19
··
DSC enthalpy accuracy ± 2% (for most materials)
Evolved gas analysis QMS, GC-MS and/or FT-IR couplings, PulseTA® (options)
Optional instrument ··Glove box version
specialties ··Corrosion-resistant version
18
STA 449 F3 Jupiter®
Features
··Super-Res for rate-controlled mass change
··Specific heat capacity
··DSC-BeFlat
··Tau-R®
Optional software ··c-DTA
Packages
··Purity
··Peak Separation
··Kinetics Neo
··Identify
Software Features
19
The NETZSCH Group is a mid-sized, family-owned German company
engaging in the manufacture of machinery and instrumentation with
worldwide production, sales, and service branches.
The three Business Units – Analyzing & Testing, Grinding & Dispersing and
Pumps & Systems – provide tailored solutions for highest-level needs. Over
3,500 employees at 210 sales and production centers in 35 countries across
the globe guarantee that expert service is never far from our customers.
NGB · STA 449 F3 Jupiter® · EN · 0919 · NWS · Technical specifications are subject to change.
NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
95100 Selb
Germany
Tel.: +49 9287 881-0
Fax: +49 9287 881 505
at@netzsch.com