Thermal Analysis Excellence

TGA /DSC 2
STARe System
Innovative Technology
Versatile Modularity
Swiss Quality

Thermogravimetry
for Unmatched Performance
 Unrivalled TGA Performance
TGA/DSC Excellence

with Balances from the Market Leader

Thermogravimetry (TGA) is a technique that measures the change in weight

of a sample as it is heated, cooled or held at constant temperature. Its
main use is to characterize materials with regard to their composition.
Application areas include plastics, elastomers and thermosets, mineral
compounds and ceramics as well as a wide range of analyses in the chem-
ical and pharmaceutical industries.

Features and benefits of the TGA/DSC 2:

n High resolution – ultra-microgram resolution over the whole measurement range
n Efficient automation – reliable sample robot for high sample throughput
n Wide measurement range – measure small and large sample masses and volumes
n Broad temperature scale – analyze samples from ambient to 1600 °C
n METTLER TOLEDO ultra-micro balance – rely on the balance technology leader
n DSC heat flow measurement – for simultaneous detection of thermal events
n Gastight cell – ensures a properly defined measurement environment
n Hyphenated techniques – evolved gas analysis using MS and FTIR
n Modular concept – tailor-made solutions for current and future needs

Thanks to its modular design, the TGA/DSC 2 is the ideal instrument

for manual or automated operation in production, quality assurance or
research and development.

TGA with the top-of-the-line METTLER TOLEDO

ultra-micro balance with unique built-in calibra-
tion weights ensures unbeatable accuracy.

2
Unique Sensors
MultiSTAR® TGA/DSC sensors
the Heart of the Instrument If you want to simultaneously measure heat flow
(DSC) in addition to weight change, you can choose
between three different sensors:

the SDTA sensor consists of a platinum support with a

thermocouple that measures the sample temperature.

the DTA sensor measures the sample and the refer-

ence temperatures. The support is made of platinum.
The differential measurement improves the signal-to-
METTLER TOLEDO “Inside” noise performance of the sensor.
The heart of a TGA is the balance cell. Our TGA
instruments use the world’s best METTLER the DSC sensor consists of six thermocouples located
TOLEDO micro and ultra-micro balances. The directly below a protective ceramic support which
internal calibration ring weights ensure unsur- measure the sample and reference temperatures.
passed accuracy. You can also calibrate and
adjust your balance with external weights.

MultiSTAR® sensor amplification technology

The DSC sensor is based on the unique MultiSTAR®
sensor amplification technology. The six thermo-
couples generate a larger measurement signal, which
improves the signal-to-noise ratio.
With all three types of sensors, the heat flow is deter-
mined from the calculated or measured temperature
difference. As with a dedicated DSC, the heat flow is
calibrated and adjusted at different temperatures using
certified reference materials.

Easy sensor cleaning

It is very easy to remove, change and clean the sensor.

High temperature accuracy

The sample temperature sensor
is directly attached to the crucible
holder and detects temperature
deviations of ± 0.25 K. Tempera-
ture calibration and adjustment
is performed using the precise
melting points of certified reference
standards instead of unclearly
defined Curie temperatures.

3
 High Performance
Swiss Quality

Already Built into the Basic Configuration

Horizontal furnace
The horizontal furnace design
helps minimize possible turbulence
caused by thermal buoyancy and
the purge gas.

Precisely defined furnace

atmosphere
The gastight cell can be evacuated
and purged with a defined gas
atmosphere. A controlled closed
system with precisely defined
conditions like this is essential to
obtain unambiguous information
and quality results.

Ergonomic design
If you insert samples manually, you
can rest your hand on an ergonom-
ically shaped support surface.

SmartSens terminal
The color touchscreen display al-
lows visual contact with the instru-
ment, even at a distance. Screen
displays can be switched touch-
free by activating the SmartSens
infrared sensors. Identify your
instrument by placing a label under
the glass cover in the front of the
display.

4
 Complete thermal
analysis system
TGA
A complete thermal analy-
sis system comprises four
different techniques. Each
technique characterizes
the sample in a particular
DSC way.

The combination of all the

results simplifies inter-
pretation. TGA measures
the weight curve, DSC the
TMA heat flow, TMA the length
change, and DMA the
modulus.

All these measurement

quantities change as a
DMA function of temperature or
time.

Important support services

METTLER TOLEDO prides itself in supplying outstanding instruments and the support needed for you to be
successful in your field of work. Our well-trained service and sales engineers are ready and available to help
you in any way possible:
• Service and maintenance
• Calibration and adjustment
• Training and application advice
• Equipment qualification

METTLER TOLEDO also provides comprehensive literature on thermal analysis applications.

5
 Excellent Performance
Over the Whole Temperature Range
Innovation

Parallel-guided balance
The parallel-guided balance
ensures that the position of the
sample does not influence the
weight measurement. If the position
of the sample changes during melt-
ing, no change in weight occurs.

Outstanding weighing performance

No other TGA can measure up to
50 million resolution points con-
tinuously - weight changes of a
5-gram sample are determined to
0.1 µg. This means you can mea-
sure small and large samples with
the same high resolution without
having to change the weight range.

 

  




 

Thermostating Key 5 Furnace heater

The balance cell is thermostated to 1 Baffles 6 Furnace temperature sensor
minimize environmental influences. 2 Reactive gas capillary 7 Adjustment ring weights
The cryostat is also used to rapidly 3 Gas outlet 8 Protective and purge gas connector
cool the furnace. 4 Temperature sensors 9 Thermostated balance chamber

6
 Full Automation
Allows Around-the-Clock Operation

The sample robot is very robust

and operates reliably 24 hours
a day and throughout the whole
year.

Automatic and efficient

All TGA/DSC 2 models can be
automated. The sample robot can
process up to 34 samples even if
every sample requires a different
method and a different crucible.

Fully automatic weigh-in

Samples can be weighed-in semi
or fully automatically using the
internal TGA balance in combina-
tion with the sample robot. You
only need an additional balance if
you want to measure and weigh- Features and benefits:
in samples at the same time. In n Up to 34 sample positions – dramatically increases efficiency

the first step, all the empty cru- n Simple and rugged design – guarantees reliable results
cibles are automatically weighed. n Unique “wasp” lid piercing accessory – hermetically sealed
Afterward, you insert a sample in crucibles are automatically opened prior to measurement
each crucible, repeat the automatic n Universal gripper – can handle all types of METTLER TOLEDO

weighing process and you are crucibles

ready to start. It’s that easy.
All the samples are then weighed-
in fully automatically.

No weight change before measurement

The sample robot can remove the protective crucible lid from the crucible
or pierces the lid of hermetically sealed aluminum crucibles immediately
before measurement. This unique feature prevents the sample taking up or
losing moisture between weighing-in and measurement. It also protects
oxygen-sensitive samples from oxidation.

7
 Modularity
a Sound Investment for the Future

Furnaces in different sizes and for

different temperature ranges
The measurement of inhomo-
geneous samples requires large
sample amounts and correspond-
ingly large sample volumes. Both
the large furnace (LF) and the high-
temperature furnace (HT) allow you
to use crucibles with volumes of up
to 900 µL.

Sensors SF (1100 °C) LF (1100 °C) HT (1600 °C)

SDTA • • •
DTA • •
DSC • •

Highest temperature accuracy

For the highest temperature ac-
curacy, we recommend the small
furnace with its reduced volume
(SF). This limits sample volumes to
100 µL. Program-controlled
gas switching and gas flow
Gas flows can be automatically
switched, monitored and con-
trolled. This allows you to switch
from an inert gas to a reactive gas
atmosphere during a measurement.

Designed for the future

You can upgrade from one instrument version to another
and add practical accessories any time you like in the future.

Option  required option Balances EGA Sorption Peripheral Switched

(MS, FTIR) control line socket
XP1 XP1U XP5 XP5U
TGA/DSC 2 (SF 1100 °C) • • • • •
TGA/DSC 2 (LF 1100 °C / HT 1600 °C) • • • • • •
Sample Robot no additional options required
GC 10/20 gas controller essential
GC 100/200 gas controller
Cryostat cooling optional
Hyphenated techniques (MS, FTIR and Sorption) essential
• = selectable

8
 Major Accessories
Increase Measurement Power

Hyphenated techniques
All TGA/DSC 2 versions can be con-
nected online to a mass spectrom-
eter or an FTIR spectrometer. Analy-
sis of the decomposition products
yields additional information about
the sample. This enables you to
interpret measurement curves with
greater certainty.

TGA-MS Interface TGA-FTIR Interface

Sorption analysis
The TGA can be converted to a TGA
Sorption analyzer in just a few min-
utes. This allows materials to be
analyzed under precisely defined
conditions of relative humidity and
temperature.

Sorption Interface

Enormous range of crucibles

We have the right crucible for every application.
The crucibles are made of different materials with
volumes ranging from 20 to 900 µL. All of the dif- copper aluminum alumina
ferent types can be used with the sample robot.

Crucible materials available are:

sapphire gold platinum

9
 Extremely Wide Application Range
Application Power

Thermogravimetry provides quantitative information on the composition and thermal stabil-

ity of many different types of materials. The method is fast and can even be used with very
small samples.

Besides the sample mass, the control in numerous fields such

TGA/DSC simultaneously measures as plastics, building materials,
the heat flow of the sample. This minerals, pharmaceuticals and
enables the instrument to detect foodstuffs.
thermal events that are not accom-
panied by a change in mass, such
as melting, glass transitions, and
solid-solid transitions.

The DSC signal can also be quan-

titatively evaluated, allowing transi-
tion and reaction enthalpies to be
determined.

The TGA/DSC is an exceptionally

versatile tool for the characteriza-
tion of physical and chemical
material properties under precisely
controlled atmospheric conditions.
It yields valuable information for
research, development and quality

Examples of thermal events and processes that can be determined by TGA/DSC

TGA DSC
• Quantitative content analysis (moisture, fillers, polymer content, materials, etc.) • Melting behavior

• Adsorption and desorption of gases • Crystallization

• Kinetics of decomposition processes • Polymorphism

• Sublimation, evaporation and vaporization • Phase diagrams

• Thermal stability • Glass transitions

• Oxidation reactions and oxidation stability • Reaction kinetics

• Identification of decomposition products, solvents and solvates • Heat capacity

• Sorption and desorption of moisture • Reaction and transition enthalpies

• Pseudopolymorphism

• Determination of Curie temperatures

10
Determination of the gypsum
content in cement
Gypsum, CaSO4 · 2H20, is used as a retard-
er in cement and occurs as the dihydrate
and hemihydrate. The two compounds
can be analyzed in cement by measuring
samples in crucibles sealed with lids with
50-µm holes. The TGA curve shows two
weight loss steps corresponding to the
dehydration of the gypsum and the hemi-
hydrate. The weight losses are more easily
determined by integrating the peaks in the
first derivative (DTG) curve. The dihydrate
and hemihydrate contents determined in
this way agree well with the manufacturer’s
specifications.

Rubber analysis of SBR

In rubber analysis, the sample is first
heated to 600 °C under inert conditions.
The volatile components (plasticizers, often
oils) vaporize and pyrolysis of the polymer
begins shortly afterward at about 400 °C.
At 600 °C, the atmosphere is then switched
from inert to oxidative, resulting in the
combustion of the carbon black additive.
Inorganic components remain behind as a
residue. The SBR sample analyzed in the
example contains 6.4% plasticizer, 68.2%
polymer and 21.8% carbon black. The resi-
due (mainly zinc oxide) amounts to 3.6%.

Thermal analysis of gypsum

Gypsum, CaSO4 · 2H20, loses its water of
crystallization below 300 °C. The calcium
carbonate present as an impurity decom-
poses at about 700 °C. Decomposition
of the calcium sulfate occurs in several
steps from about 1200 °C onward. The
simultaneously recorded DSC curve shows
two further effects due to solid-solid transi-
tions at about 390 and 1236 °C: g-CaSO4
(anhydrite III) to b-CaSO4 (anhydrite II),
and b-CaSO4 to a-CaSO4 (anhydrite I). The
latter melts slightly below 1400 °C and is
observed as a sharp endothermic peak.

11
Kaolinite
Kaolin is a white mineral used in the paper
industry, as a filler in plastics and for the
manufacture of porcelain. The main con-
stituent of kaolin is kaolinite, Al2Si2O5(OH)4,
which dehydroxylates between 450 °C and
600 °C. This is the reason for the weight
loss in the TGA curves. The example shows
the measurement of three kaolin samples
with different contents of kaolinite. The DSC
curve for Kaolin A shows a small peak at
about 575 °C. This peak is characteristic
for the solid-solid transition of a-quartz to
b‑quartz. The exothermic peak at about
1000 °C is due to the formation of mullite.

Volatility of oils
The Noack Test according to ASTM D 6375
is used to assess the volatility or evapora-
tion loss of a lubricating oil in comparison
with a reference oil at a particular tempera-
ture. The procedure is summarized in the
figure. The reference oil takes 11.9 min to
lose the specified mass loss of 10.93%.
The oil under test loses 8.8% of its mass
up until this time. Its Noack volatility is
therefore 8.8%. The method allows rapid
and reliable characterization of oil volatility.

Residual solvents
in pharmaceutical substances
Many pharmaceutical substances are
recrystallized from solvents. As a result,
residues of solvents often remain in the
product. Combined techniques such as
TGA-MS are ideal to detect and identify such
undesired residues. In the example, metha-
nol and acetone were used to recrystallize
the active substance. The presence of these
two substances is confirmed by the peaks
in the m/z 43 and m/z 31 fragment ion
curves. The results indicate that the weight
loss step at 200 °C is almost entirely due to
the elimination of acetone.

12
Adjustment of
temperature and heat flow
Adjustment of temperature and heat flow
is normally performed with certified pure
metals. Gold and palladium can be used
to calibrate and adjust the temperature and
heat flow up to the maximum temperatures
specified for the TGA/DSC 2 furnace (1100
or 1600 °C). The Curie temperatures of
ferromagnetic metals can also be employed
for temperature adjustment. This is,
however, not recommended because Curie
temperatures are not clearly defined, in
contrast to melting points of pure metals.

MaxRes: high resolution despite

short measurement times
With MaxRes, the heating rate changes au-
tomatically depending on the rate of change
of weight. This enables overlapping weight
loss steps to be optimally separated in the
shortest possible time. The example shows
the dehydration of copper sulfate pentahy-
drate. At 25 K/min, the first two weight loss
steps are not properly separated. Using
MaxRes, the separation is clearly better
than at 5 K/min even though the measure-
ment time is much shorter.

Determination of the
plasticizer content in elastomers
Oils are often used as plasticizers in
elastomers. Usually, the oil vaporizes in the
same temperature range as the elastomer
decomposition begins, making it difficult
to quantify the oil content. In such cases,
the elastomer samples are measured at re-
duced pressure to separate the two effects.
The example shows the weight loss curves
of SBR samples with and without oil at
normal pressure and at 12 mbar. Pressure
hardly influences the measurement curve
of SBR without oil. In contrast, when SBR
with oil is measured at reduced pressure,
the vaporization of the oil and decomposi-
tion of the elastomer are almost completely
separated.

13
TGA/DSC 2 Specifications
Temperature data Small furnace (SF) Large furnace (LF) High temp. furnace (HT)
Temperature range RT to 1100 °C RT to 1100 °C RT to 1600 °C
Temperature accuracy 1) ± 0.25 K ± 0.3 K ± 0.5 K
Temperature precision 1) ± 0.15 K ± 0.2 K ± 0.3 K
Furnace temperature resolution 0.001 K 0.001 K 0.002 K
Heating time 5 min (RT to 1100 °C) 10 min (RT to 1100 °C) 10 min (RT to 1600 °C)
Cooling time 20 min (1100 to 100 °C) 22 min (1100 to 100 °C) 27 min (1600 to 100 °C)
Cooling time with helium ≤ 10 min ≤ 11 min ≤ 13 min
(1100 to 100 °C) (1100 to 100 °C) (1600 to 100 °C)
Heating rate 2) 250 K/min 150 K/min 100 K/min
Cooling rate 2) –20 K/min (≥150 °C) –20 K/min (≥150 °C) –20 K/min (≥200 °C)
Sample volume ≤ 100 µL ≤ 900 µL ≤ 900 µL

Special modes
Automation
Vacuum (10 mbar)
MaxRes optional
TGA-MS
TGA-FTIR
TGA sorption no optional

Balance data XP1 / XP5 XP1U / XP5U

Measurement range ≤1 g / ≤5 g ≤1 g / ≤5 g
Resolution 1.0 µg 0.1 µg
Weighing accuracy 0.005% 0.005%
Weighing precision 0.0025% 0.0025%
Internal ring weights 2
Blank curve reproducibility better than ± 10 μg over the whole temperature range

Calorimetric data
Sensor data Sensor type SDTA DTA DSC
(typical values) Surface material platinum platinum ceramic
Number of thermocouples 1 2 6
Signal time constant at 900 °C 15 s 14 s 14 s
sensitivity 0.5 mW 0.2 mW 0.1 mW
Temperature resolution 0.005 K 0.0001 K 0.00003 K
Enthalpy reproducibility (standard deviation) better than 5%

Sampling
Sampling rate maximum 10 values/second

Approvals
Safety IEC/EN61010-1:2001, IEC/EN61010-2-010:2003
CAN/CSA C22.2 No. 61010-1-04 & -2-010
UL Std. No. 61010-1 (2nd Edition)
EMC EN61326-1:2006 (Industrial environments)
EN61326-1:2006 (class B)
AS/NZS CISPR 11, AS/NZS 61000.4.3
1)
based on metal standards
2)
depends on instrument configuration

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For more information

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CH-8603 Schwerzenbach, Switzerland
Tel. +41 44 806 77 11 Environmental management system
Fax +41 44 806 72 60 according to ISO 14001.

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