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Thermogravimetric Analysis - TGA: Analyzing & Testing
Thermogravimetric Analysis - TGA: Analyzing & Testing
TG 209 F1
TGA Method
Sample
Measuring Principle
Furnace
A thermobalance is used to measure the
mass change of a sample as a function
Thermocouple of temperature or time, under a defined
Sample carrier Compensation and controlled environment with respect
to heating rate, gas atmosphere, flow
rate, crucible type, etc.
Balance
2
Measurement Result
TGA and DTGA curves for the decomposition of calcium oxalate monohydrate
At a Glance
Precise ultra-microbalance
Vacuum-tight design
3
TG 209 F1 Libra® – Trendsetting Technology
High Temperature and Fast Heating The sample carrier type P (Platinel®)
Rates in a Ceramic Furnace provides the highest sensitivity for
the c-DTA® signal, which serves for
The maximum temperature of the recording endothermal and exothermal
corrosion-resistant micro-furnace effects via calculated DTA in a manner
amounts to 1100°C (sample similar to DSC (Differential Scanning
temperature). Its high heating rates Calorimetry).
of up to 200 K/min are suited for Temperature calibration can be carried
identifying the material by a fast QC out by means of the melting point
check. A water-cooled jacket provides determination – easily and without any
the micro-furnace with fast cooling modification of the hardware
and therefore allows for high sample (see page 11).
throughput.
4
Defined Gas Conditions for
Reproducible Measurements
5
TG 209 F1 Libra® – Automatic Sample Changer and Accessories
6
Crucible Types for Various Applications1
Application Material of the Sample Support Sensor Type For Crucible Types
Standard TGA Al2O3 Type P 6.7 mm to 9 mm Ø, 85 µl to 350 µl
Ideal for c-DTA® PdPt/Au/AuPd (Platinel®) Type P (disk) 6.7 mm to 9 mm Ø, 85 µl to 350 µl
For corrosive media Al2O3 Type P, protected 6.7 mm to 9 mm Ø, 85 µl to 350 µl
4
For ASC: max. diameter of the crucible is 8 mm
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Proteus® Software – Flexible, Intelligent, Complete
The TG 209 F1 Libra® runs under General Software Features Main TGA Features
the versatile Proteus® software on
a Windows® operating system. The For Windows® XP and Windows® 7 Mass change in % or mg
Proteus® software includes everything operation systems Automatic evaluation of mass change
you need to carry out a reliable Multi-tasking for simultaneous steps and characteristic temperatures
measurement and evaluate the resulting measurement and evaluation Extrapolated onset and endset
data – or even carry out complicated Multi-moduling for up to 4 different Peak temperatures and values of the
analyses. The Proteus® software is instruments 1st and 2nd derivatives
licensed with the instrument and can Multi-method analysis for curve c-DTA® for multi-point temperature
also be installed on other work station comparison and evaluation of various calibration and evaluation of endo-
or laboratory computers, e.g., for methods and exothermal effects (calculated
evaluations. Snapshot for on-line evaluation of DTA signal)
the running measurement BeFlat® : Automatic correction of
Picture-in-picture presentation buoyancy and drift for rapid TGA
(PIP and FLIP) results
Graphic and data export Multi-curve analysis of simultaneous
Storage and restoration of analyses evaluation of several TGA and DTGA
Context-sensitive help system curves
Macro recorder (option) Super-Res® (Rate-controlled mass
change) for improved resolution and
separation of superimposed mass-
change steps
Advanced Software1
8
User interface of the Proteus® software during evaluation: presentation of the TGA curve (white) together with the DTGA curve (blue, dashed line), the c-DTA® curve
(red) and two gas flow curves (blue, dotted line and green, dashed line) in the main frame.
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TG 209 F1 Libra® – Smart Tools Integrated
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c-DTA® – Calculated DTA for Endothermal and Exothermal Effects
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TG 209 F1 Libra® – Advanced Software
Peak Separation –
Improved Separation of Overlapping
Mass-Change Steps
Good agreement between the experimetal data (symbols) and the cumulative
curve (black) of the calculated peaks (colored lines) as a result of applying
Peak Separation
Normally, a defined constant heating Super-Res® provides a rate-controlled rate (DTGA curve) set by the operator.
rate is applied to the sample in order heating rate according to defined This often results in much better
to study its decomposition behavior. thresholds with respect to the mass-loss separation of overlapping mass-loss steps.
12
Thermokinetics for the Optimization of any Process
70
The TGA plot (upper illustration)
presents a biomass sample measured
at 4 different heating rates – from
50 5 K/min to 40 K/min – in an inert gas
atmosphere. The higher the heating
rate, the more the curves are shifted
to higher temperature values. This is
30
typical behavior for effects caused by
150 250 350 450 550
Temperature/°C kinetic processes. There is an excellent
congruence between the TGA raw data
Comparison of the TGA raw data (symbols) and the curves (solid lines) (symbols) and the calculated curves
calculated on the basis of a 4-step reaction model
(solid lines). The formal model used
consists of four consecutive reactions.
For the first one, a 3-dimensional
Mass/% Temperature/°C
diffusion type was selected; the other
100 300
three are n-th order reactions.
90 250
Based on this model, a prediction was
computed: Starting at 30°C, heating
80 200
to 300°C at a heating rate of
150 K/min, and then holding the
70
150 temperature constant at 300°C for
1 hour yields the blue mass-change
60
100 curve shown here (lower illustration).
The calculation forecasts a residual mass
50
50 of about 45% after 62 minutes.
0 10 20 30 40 50 60
Time/min
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TG 209 F1 Libra® for a Wide Variety of Applications
Polyamide
SEBS+PP
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Magnesium Stearate
Coal
Mica
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TG 209 F1 Libra® with Evolved Gas Analysis (EGA)
Additional Information
Evaluation of GC-MS-TIC chromatograms
www.netzsch.com/gcms
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-10.60 %
100 NR/SBR 5.283 mg, 20 K/min, N2
continuous heating
-35.72 %
80
60
NR/SBR 6.89 mg, 20 K/min, N2, -25.97 %
event-controlled with 3 thresholds
40 1.3 %/min, 7 %/min, 6 %/min
20
0
100 200 300 400 500 600
transfer line
adapter
sample loop
micro furnace
valve sample
on off
sample carrier
JAS UNIS 500
GC carrier
injector system
gas inlet
(He 5 bar)
TGA cell
17
TG 209 F1 Libra® with Evolved Gas Analysis (EGA)
High-level material research and “More than just the sum of its parts” means of the Perseus TG 209 F1
characterization can be achieved by is the motto for our comprehensive Libra®, a TG-FT-IR system was
coupling the TG 209 F1 Libra® to our coupling system incorporating an created that is an excellent alliance
QMS 403 Aëolos® quadrupole mass FT-IR (Fourier Transform Infrared) with a compact Bruker Optics
spectrometer. Any gases evolved are spectrometer manufactured by our FT-IR spectrometer. The integrated
introduced directly into the electron cooperation partner, Bruker Optics. design for both systems sets new
impact ion source of the MS through a The purge gas flow from the TGA standards for state-of-the-art coupling
quartz glass capillary heated to 300°C. carries the volatiles through a short techniques. The built-in heatable gas
heated transfer line to the vacuum- cell is directly connected with the
tight gas cell of the FT-IR. All evolved gas outlet of the TGA furnace. The
gases with a changing dipole moment small volume of the short transfer
are identified by their typical absorption path guarantees fast transport and
spectrum, and complex gas mixtures is advantageous for condensable
can be spectroscopically separated.By gases.
Additional Information
www.netzsch.com/ftir
Perseus TG 209 F1
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Simultaneous TGA-MS-FT-IR
Coupling and PulseTA®
Coupling of Tensor 27, external gas cell, TG 209 F1 Libra® with ASC and QMS 403 D Aëolos®
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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
3,000 employees at 163 sales and production centers in 28 countries across
the globe guarantee that expert service is never far from our customers.
When it comes to Thermal Analysis, Calorimetry (adiabatic & reaction) and the
determination of Thermophysical Properties, NETZSCH has it covered. Our 50 years
of applications experience, broad state-of-the-art product line and comprehensive
service offerings ensure that our solutions will not only meet your every requirement
but also exceed your every expectation.
NGB · TG 209 F1 Libra® · EN · 1000 · 0514 · LH · 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 www.netzsch.com