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Materials

Characterization
Page
Overview 242 – 243

Good Thermal Analysis Practice 244 – 245
Thermal Analysis Excellence and Premium 246 – 248
Thermal Analysis Options 249
Hot-Stage Microscopy Systems 250

METTLER TOLEDO sets


the standards
in Thermal Analysis,
just like with its
world-class balances
Overview

Materials Characterization
Thermal Analysis and Hot-Stage Microscopy

DSC
Differential
Scanning
Calorimetry
The METTLER TOLEDO thermal analysis DSC determines the enthal-
Excellence and Excellence Premium pies associated with tran-
lines offer tailor-made solutions for sitions and reactions and
academic and industrial applications. the temperatures at which
The unrivalled performance and inno- these processes occur.
vative technology will propel you to the
forefront of your field and guarantee
you the highest level of Swiss quality,
accuracy and efficiency.

Features and benefits:


• Modular concept – tailor-made solu-
tions for current and future needs
• High performance instruments –
accurate analysis of a wide variety
of samples
• High-level competence and support
– training courses and applications
DSC
literature fosters knowledge sharing
and growth
• Service – prompt response and main-
tenance contracts guarantee maximum
system uptime

Hot-stage microscopy yields a wealth of


information that is complementary to the
data obtained from the thermal analysis.
This often greatly facilitates the interpre-
tation of results.

www.mt.com/ta-news
Overview

Flash DSC TGA and TGA/DSC DMA and TMA Hot-Stage


Flash Differential Thermo- Dynamic Mechanical Microscopy
Scanning Gravimetric Analysis and Thermo Thermal Optical
Calorimetry Analysis Mechanical Analysis Analysis

Flash DSC is the ideal TGA/DSC measures sam- DMA and TMA are used to Hot-stage microscopy is
addition for characterizing ple weight as a function measure the mechanical widely used for the visual
modern materials and of temperature. It is used and viscoelastic properties characterization of all kind
optimizing production to perform compositional of materials as a function of of thermal transitions.
processes by thermal analysis or investigate the temperature, time and fre-
analysis. reaction kinetics of your quency.
sample. DMA and TMA
Flash DSC

TGA and TGA/DSC

Hot-Stage Microscopy
Good Thermal Analysis Practice

5 Steps to Excellence 5
Full Life-Cycle Support Routine
Operation
1
Evaluation

METTLER TOLEDO offers comprehensive


support for all of the 5 steps of Good Thermal
Analysis Practice. This not only ensures that
4 GTAP TM

2
Training Selection
you invest in the most suitable equipment and
services, but also that you operate your
3
system correctly, thereby minimizing errors Installation
and improving performance. & Qualification

GTAP™ supports you in fulfilling your requirements from


the beginning. It allows you to make the right decisions
during the entire life-cycle of your system.
• Enables compliance with regulations
• Ensures consistent and accurate results
• Increases productivity at lower costs
• Makes sure users are professionally trained

DQ IQ/OQ EduPac
Design Qualification Installation & Qualification Education Package

The Design Qualification helps The Installation and Operational Under the watchful eye of our
you to define your current and fu- Qualification processes are per- specialist, this training package
ture requirements together with formed carefully and guarantee helps you familiarize yourself
our consultant in order to select that the equipment does what it with the instrument and learn effi-
the most suitable system for your is intended to do. Detailed docu- cient operation through practical
application and protect your in- mentation with a professionally exercises.
vestment for the future. executed qualification procedure • Configuration of the system
ensures conformity and estab- • Setting up experiments
lishes complete traceability from • Measuring your samples
the very start. • Evaluation and interpretation of
the curves
Preventive Maintenance Calibration Evaluate Process Risks

Your system should be tested METTLER TOLEDO offers preven- Perform your own laboratory Thermal Analysis
and calibrated regularly to ensure tive maintenance services that Risk Check with our web-based tool:
that it consistently meets your guarantee high performance.
predefined requirements. Your system will be systematic- www.mt.com/ta-riskcheck
METTLER TOLEDO offers various ally inspected to detect and
calibration services. correct potential failures before
they occur.
Thermal Analysis Excellence and Premium

The STAR e System – the Flexible Solution


Select the Right Thermal Analysis Module

A sound investment. You begin with the instrument configuration that meets
your current needs. Later on, you can upgrade the system with options or
accessories to satisfy your new requirements. It’s a sound investment,
whatever you decide on.

Modular Design STARe


Software
The STAR e software is designed around the powerful basic
software, which consists of the Evaluation and Module
Control Windows and a simplified Installation Window.
Robo t
Robot Robo t
Robot
The software can easily be expanded to support new
Flash
Flas h
DSC
C TGA
A TMA
TMA DMA
DMA HS
applications or instruments. DSC
DS C

Features and benefits of the STAR e Excellence Software:


• Unlimited evaluation possibilities – enormous flexibility
• Reliable automation – high sample throughput with result assessment dramatically improves efficiency
• Integrated database – guarantees highest level of data security
• 21 CFR Part 11 compliance – supports user level management and electronic signatures
• Modular concept – tailor-made solutions for current and future needs
• Easy and intuitive operation – saves time in training and in daily use

STAR e
Thermal Analysis Software

Multi
Module
Operation
Routine
MaxRes
Window
Relative Method
Loop Window
Conditional
Experiment
Experiment
Termination Window
21 CFR 11
User
Rights Quality
Server Model Control
Mode Free TOPEM
Concurrent LIMS Kinetics
Users

Kinetics
nth Order

The powerful and versatile STAR e


software provides unrivalled
flexibility and unlimited evalua-
tion possibilities.
DSC HP DSC Flash DSC
The DSC utilizes an innovative For material testing, process Flash DSC revolutionizes rapid-
sensor with a patented star- development or quality control scanning DSC. Flash DSC allows
shaped arrangement of 120 there is often no alternative to the user to analyze reorganization
thermocouples that guarantees DSC measurements under pres- processes that were previously
unmatched sensitivity and reso- sure. Measurements performed impossible to measure. Flash
lution. under pressure expand the pos- DSC is the ideal complement to
sibilities of thermal analysis. conventional DSC.

DSC features and benefits: HP DSC features and benefits: Flash DSC features and benefits:
• Amazing sensitivity – for the • Shorter analysis time – higher • Ultra-high heating rates –
measurement of weak effects pressure and temperature reduce measurement times
• Outstanding resolution – accelerate reactions and suppress reorganization
allows measurement of rapid • Measurement under process processes
changes and closelying events conditions – simulation of • Ultra-high cooling rates – allow
• Efficient automation – reliable practical reaction environments materials with defined structural
sample robot for high sample • Better interpretation – effects properties to be prepared
throughput can be separated by suppress- • Fast response sensor – enables
ing vaporization the kinetics of extremely fast
reactions or crystallization pro-
cesses to be studied

www.mt.com/dsc www.mt.com/ta-hpdsc www.mt.com/ta-fdsc


Thermal Analysis Excellence and Premium

TGA and TGA/DSC TMA DMA


The TGA and TGA/DSC instruments The Thermomechanical Analyzer The Dynamic Mechanical Ana-
are equipped with a top-of-the-line incorporates Swiss precision lyzer (DMA) with its revolutionary
METTLER TOLEDO ultramicro bal- mechanics and features nanome- technology offers previously unat-
ance with unique built-in calibra- ter resolution to measure the very tained performance and time-
tion ring weights for unparalleled smallest dimensional changes. saving external sample loading.
accuracy.

TGA and TGA/DSC features: TMA features and benefits: DMA features and benefits:
• Efficient automation – reliable • Nanometer resolution – allows • Wide force range from 1 mN to
sample robot for high sample very small changes to be 40 N – allows very soft and very
throughput measured hard samples to be measured
• METTLER TOLEDO ultramicro • Dynamic load TMA (DLTMA • Frequency range from 1 mHz
balance – rely on the balance mode) – measures weak tran- to 1 kHz – means that mea-
technology leader sitions and elasticity surements can be performed
• DSC heat flow measurement – • SDTA – simultaneous measure- under real conditions or more
for simultaneous detection of ment of thermal effects rapidly at higher frequencies
thermal events • Innovative sample holders –
permit samples to be prepared
and loaded externally
www.mt.com/tga
www.mt.com/tga-dsc www.mt.com/tma www.mt.com/dma
Thermal Analysis Options

Extremely wide application range


Thermal analysis is firmly established as a method for the characterization
of physical and chemical properties of materials in many different fields.

Materials characterization by DSC Flash TGA TMA DMA


DSC

Physical properties
Melting/crystallization • • • •
Enthalpy of crystallization • •
Solid fat index •
Purity determination •
Vaporization / drying • •
Sorption and desorption •
Glass transition • • • •
Specific heat capacity • •
Expansion coefficient, shrinkage behavior •
Polymorphism, crystalline transitions • • •
Liquid-crystalline transitions • •
Viscoelastic behavior, elastic modulus • • www.mt.com/ta-usercoms
Chemical changes
Decomposition, pyrolysis • • •
Oxidation, stability • • •
Curing, vulcanization, gelation • • •
Dehydration • • •
Denaturation • •
Swelling and foaming • •
Reaction process, reaction enthalpy and kinetics • • •

www.mt.com/ta-webinars
www.mt.com/ta-etraining

Crucibles and sensors for thermal analysis


Crucibles serve as containers for Part no. Crucible type Quantity Volume Max. Max. for for
samples during thermoanalytical in uL pressure tempera- DSC TGA
in MPa ture in °C
measurements. The type of crucible 51119810 Aluminum crucible light 100 20 0.2 640 • •
used for a measurement can have 00026763 Aluminum crucible standard 100 40 0.2 640 •
a large effect on the quality of the 51140407 Copper crucible 100 40 750 • •
51140842 Platinum crucible small 4 30 1600 • •
results obtained, and in addition,
51119654 Platinum crucible medium 4 70 1600 • •
also influences important charac- 00027220 Gold crucible 6 40 0.25 750 • •
teristics of the DSC measuring cell. 00029990 Medium pressure crucible 25 120 2 250 •
In Flash DSC, the sample is placed 51140405 Reusable, gold plated high
3 30 15 350 •
pressure crucible
directly onto the MultiSTAR chip
00026731 High pressure crucible 25 40 15 750 •
sensor. The patented dynamic 51140845 Sapphire crucible medium 4 70 2000 •
power compensation control circuit 51140843 Alumina crucible small 20 30 2000 •
allows measurements to be per- 00024123 Alumina crucible medium 20 70 2000 •
00024124 Alumina crucible large 20 150 2000 *
formed with minimum noise level
51119960 Alumina crucible large 4 900 2000 *
at high heating and cooling rates.
* only with large furnace

For more crucibles please see


www.mt.com/ta-crucibles
or ask for the crucible brochure.
Hot-Stage Microscopy Systems

Hot-Stage Microscopy Systems


Seeing is Believing

The hot-stage microscopy is a powerful tool that is widely used for the visual characteri-
zation of all kind of thermal transitions. The possibility of directly observing morphological
changes in a sample as it is heated or cooled is of enormous value. Changes in the shape,
structure and color of crystals are seen as well as their size and number. The technique
allows phase transitions to be characterized and provides infor-mation on expansion and
shrinkage behavior.

Features and benefits: Choice of thermal events and operations


• Imaging possibilities – allow polymorphic which can be defined using the HS82/HS84
transitions to be studied visually
Industry Thermal events HS82 HS84
• Closed furnace design – guarantees excellent Pharmaceutical, pet- Melting characteristics
temperature control rol, food, cosmetics, • •
academia
• High sensitivity – optical sensitivity is not
Pharmaceuticals, Polymorphism
influenced by the heating or cooling rates food, cosmetics • •

Chemicals, cosmetics Liquid crystal transitions • •


Polymers, pharma- Crystallization and
• •
ceuticals nucleation
Chemicals, petrol Cloud point •
Chemicals, academia, Purity

test laboratories
Pharmaceuticals, Decomposition tem-
• •
chemicals, polymers perature
Polymers Curing •
Pharmaceuticals, Reaction and transfor-
polymers, chemicals, mation enthalpy

academia, test labo-
ratories
Forensic science Oil immersion / tem-
perature variation •
method

The HS82 hot-stage microscopy system is an easy-to-use and precise thermal measuring cell for visual sample
observation. The HS84 hot-stage microscopy system allows DSC heat flow measurements in addition. Two dif-
ferent software packages allow evaluation of heat flow or video image capture.

Image at 100 °C Image at 90 °C

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