thermal analysis - tec instrumental

Thermal Analysis GuideSeamless Workflow for Routine Analysis

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IntroductoryBooklet

3Thermal Analysis Guide METTLER TOLEDO

Disclaimer

The information contained in this guide is based on the current knowledge and experience of the authors. The guide represents selected, possible application examples. The experiments were conducted and the resulting data evaluated in our lab with the utmost care using the instruments specified in the description of each application. The experiments were conducted and the resulting data evaluated based on our current state of knowledge.However, this guide does not absolve you from personally testing its suitability for your intended methods, instruments and purposes. As the use and transfer of an application example are beyond our control, we cannot accept responsibility therefore.

When chemicals, solvents and gases are used, the general safety rules and the instructions given by the manufacturer or supplier must be observed.

® ™ All names of commercial products can be registered trademarks, even if they are not denoted as such.

Introductory Booklet

Thermal Analysis Guide


Edito

rial Editorial

Dear Reader

Since the first experiments by Henry Louis Le Chatelier in 1887, thermal analysis has developed to a group of measuring techniques that have become essential for material characterization of polymers, metals and inorganics, oils and fats, pharmaceuticals as well as food.

A major breakthrough was the invention of heat flow DSC in 1955 by S. L. Boersma. The heat flow principle still applies to present day instruments. Recent developments and innovations have seen the introduction of the Flash DSC by METTLER TOLEDO. The model Flash DSC 1 allows ultra-high heating rates of up to 2 400 000 K/min in the temperature range of –95°C up to maximum 500 °C.

The availability of powerful computer hardware and software has influenced thermoanalytical methods enormously. It has simplified method setup and instrument operation and has allowed curve evaluation and result calculation to become common and easily understandable tasks. However, thorough thermal analysis knowledge and diligent instrument operational skills remain essential to achieve meaningful and precise results.

This guide presents some solutions to perform thermal analysis tests safely and easily in the daily routine of a laboratory.

Dr. Matthias Wagner and the editorial team of the METTLER TOLEDO Materials Characterization Group:

Nicolas FedelichDr. Elke HempelNi JingDr. Angela HammerDr. Melanie NijmanDr. Rudolf RiesenDr. Jürgen SchaweDr. Markus SchubnellDr. Claus Wrana

6 Thermal Analysis Guide METTLER TOLEDO

Cont

ents Contents

1. Introduction 7

2. Choosing the Thermal Analysis Technique 8

3. How to Design an Experiment 9

4. Taking Samples 10

5. Choice of Crucible 11

6. Starting a Measurement 14

7. Sample Insertion 15

8. Unattended Measurement 16

9. Calibration and Ajustment 17

10. Conclusions 20

11. For More Information 21

12. Index 22


Intro

duct

ion 1. Introduction

When it comes to analysing many samples in a limited time, analytical instruments have to be well "calibrated" and need to perform at their best. These requests are typical for the quality control of received goods, intermediate specimens taken from a production line, produced parts, failure analysis and material research. Furthermore, operation of the instruments should be as simple and safe as possible.

Basic maintenance tasks executed periodically assure good working conditions of the instruments. A seamless workflow ensures that an analysis can be done without any interrupting delays. Automation accessories help to avoid error-prone manual steps.

The METTLER TOLEDO Thermal Analysis Excellence systems offer new possibilities to achieve these goals. Test methods include several work steps and can be set to high automation levels, if desired. Few basic skills and a minimum amount of training are necessary to conduct a complete thermal analysis test. Routine tests can be executed with one click from the instrument's touch screen terminal without the need to have access to the controlling PC.

Efficient and reliable 7 day 24 hour operation is supported by a sample changer robot. Thanks to the design concept, the robot offers flexible crucible handling and reliable single axis movement. It is factory endurance tested, ensuring peace of mind for long term operation.

On the following pages, we will show selected routine maintenance tasks as easy and convenient tools to achieve good thermal analysis results.


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The thermal analysis technique that can be used to measure a particular property depends on the effect or property you want to measure. The following table gives an overview of the best ( ) and alternative ( ) techniques:

DSC TGA TMA DMA

Physical properties

Specific heat capacity – –

Expansion coefficient – –

Young’s modulus – –

Physical transitions

Melting and crystallization –

Evaporation, sublimation, drying – –

Glass transition, softening –

Polymorphism (solid-solid transitions) – –

Liquid crystals – – –

Purity analysis – –

Chemical properties

Decomposition, degradation, pyrolysis, oxidation, stability – –

Composition, content (moisture, fillers, ash) – –

Kinetics, reaction enthalpies

Crosslinking, vulcanization (process parameters) –


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ent 3. How to Design an Experiment

The following diagram gives an overview of how to design an experiment. The individual steps in the process are not independent of one another – for example, sample preparation might need to be reassessed after the measurement results have been evaluated [UC 21/1].

The most important point before beginning an analysis is to be absolutely clear about the property you want to measure and the results you hope to get. A more detailed description of the steps involved in the process is given in different chapters and sections of this handbook. The relevant chapter and section numbers are enclosed in brackets after the names of the steps.

Choosing the measuringtechnique:DSC TGATMADMA

Sample preparation

Choosing the crucible

Choosing the temperature program

Choosing the atmosphere

After the measurement

Evaluation

Method validation

Validated method


Taki

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es 4. Taking Samples

A sample has to be representative, clean and original. Thus, good laboratory and good manufacturing practice guidelines (GLP, GMP) point out sampling rules to ensure that final results are meaningful and characteristic.

For thermal analysis, sample size and shape are two additional important aspects that can impact on the final result.

Size In comparison to other analytical techniques, thermal analysis uses small sample sizes. Therefore, the selection of the right part of the sample is crucial for the analysis.

Shape Flat surface to allow for good thermal contact.

Thermal analysis Typical sample size

DSC 5–50 milligrams

Flash DSC 20–100 nanograms

TGA 10–1000 milligrams

TMADepends on mode and sample, e.g. Dilatometry of polymers: 5 x 5 x 3 millimeters (LxWxT)

DMADepends on sample, sample and instruments.For 3 point bending of thermosets: 50 x 2 x 1 millimeters (LxWxT)

For TGA measurements, the sample's minimum weight has to be taken into consideration. The minimum weight depends on the type of the built-in balance and the uncertainty requirements for a certain weight step or the weight of the residue. Also, the upper sample size limit is defined based on available crucible volume, desirable heating rate and analysis time. Both values can be entered into the method in the form of sample limits. This means that an operator having prepared a sample that is either too small, or too large, will not be allowed to start the measurement.


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Figure 2. Weighing samples for DSC tests on a microbalance.

Figure 1. Selection of crucibles for thermal analysis.

5. Choice of Crucible

Good thermal analysis measurements also depend also on the correct choice of crucibles and lids. Typical crucible materials are aluminum, alumina, platinum, steel, gold plated steel, copper, etc. They are selected according to the maximum temperature and to avoid or minimize reactions with the sample.Lids seal the crucible hermetically to avoid evaporation of the sample and to avoid interferences with the surrounding atmosphere. Lids with a small hole e.g. a pre-punched 50 μm hole, allow for a self-generated atmosphere in the crucible due to restricted exchange with the ambient environment. In contrast, open crucibles without a lid (or with a lid with a big hole) allow the ambient atmosphere to come into contact with the sample.

Crucible material Volume µL Recommended use Limits

Aluminum 40 Default for DSC 640 °C

Aluminum 20 For DSC of polymer films, disks and powders 640 °C

Platinum 40 TGA and DSC, better DSC signal than alumina 1700 °C

Gold 40 High chemical resistance 1000 °C

Stainless steel 120 Medium pressure DSC applications 250 °C, 2 MPa

Stainless steel 40 High pressure DSC applications 400 °C, 15 MPa

Alumina 70 Default for TGA 2000 °C

Alumina 900 TGA for larger sample volumes 2000 °C

How different types of samples are filled into crucibles can be viewed in the DSC sample preparation video

www.mt.com/ta-videos

For more details, tips and hints see Thermal Analysis in Practice, Application Handbook, chapters 7.3, 9.3, 10.3 and 11.3.


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e Crucible requirements:• The crucible material must be inert and not show any effects in the measured temperature range.• The melting point of the crucible must be higher than the effects that you want to observe in the sample.• Crucibles must be inert to the sample and its end products in the applied temperature range unless

a catalytic effect is desired, for example:– oxidation measurements with copper crucibles, or– chemical reactions using platinum crucibles.

Samples that do not contain volatile constituents are usually measured in 40-µL standard aluminum crucibles with a pierced lid (this can also be used for TGA/DSC measurements up to 640 °C!). Crucibles with pin cannot be used in the sample robot. Check the weight before and after measurement. If the difference is less than 30 µg, the crucibles have held tight. In TGA measurements, the height-to-width ratio of crucibles influences diffusion, see [UC 9/22]. Information about sample atmospheres can be found in Section 3.1.3.

Background information about crucibles is given in [UC 5/3].

The table below presents an overview over the individual DSC and TGA crucibles (see also www.mt.com/ta-crucibles):

Type of crucible Remarks Picture

Standard aluminum cruciblemax. temp: 640 °C

40 µL (also 25, 100 and 160 µL) (DSC, TGA, TMA, e.g. for curing liquids)

• This is the most frequently used crucible.• Available with or without a pin.• Can be sealed hermetically, available with a 50 µm

hole or larger hole in the lid (see also Section 3.1.3).

Light aluminum cruciblemax. temp: 640 °C

20 µLmax. temp: 640 °C

(DSC, TGA)

• This crucible has the shortest time constant.• It can be used with a lid to compress flexible samples

(films, fibers, powders).• A self-generated atmosphere is produced with a closed lid.

The crucible is not hermetically sealed. • The lid can also be pierced to improve gas contact.

Copper crucible max. temp: 750 °C

40 µL (DSC)

• It can be used to provide a catalytic effect for oxidation studies. No lid is available.

Gold crucible max. temp: 750 °C

Gold-plated cruciblemax. temp: 350 °C

40 µL (DSC)

• This is a very inert crucible.

Cold welding is more difficult after long storage times – heat to 500 °C before use.

Molten metal samples can form alloys and create holes in the crucible.


Type of crucible Remarks Picture

Platinum reusable cruciblemax. temp: 1600 °C

30, 70, 150 µL(TGA, DSC)

• This is used for good quality heat flow measurements at temperatures above 640 °C.

• It can also be used as to promote catalytic effects.

Use sapphire spacer discs for platinum-platinum contact above ~1000 °C (e.g. DTA sensor of TGA/DSC) in order to avoid welding or fusion.

Molten metals can form alloys and create a hole in the cruci-ble. Be aware of platinum poisons such as tin, lead, zinc, aluminum, silver, gold, phosphorus, arsenic, antimony, bismuth, silicon, boron, free carbon and salts or oxides of heavy metals (reduction of salts to metals at high temperatures).

Medium-pressure crucible made of stainless steel

Max. temp: 250 °C

• Needs special dies (male-female) for the crucible sealing press.

• It can be closed without an O-ring for measurements in a self-generated atmosphere.

High-pressure crucible made of gold-plated steel Max. temp: 400 °C

25, 40 µL (DSC)

Various other high-pressure crucibles are available.

• Used for safety measurements and to suppress overlapping effects (e.g. vaporization).

• Special toggle press is needed with die.• The lid is pressed into the crucible with a force of about

1 metric ton so that a membrane, which serves both as seal and burst disk, seals the crucible tightly (weigh the crucible before and after measurement to check that it remains tight).

Aluminum oxide crucibleMax. temp: 2000 °C

30, 70, 150, 300, 600, 900 µL

(TGA, DSC)

• Most frequently used crucible for TGA measurements and is available in different sizes.

• It can be used with a pierced alumina lid.• Aluminum lids are available for unstable samples.• Reusable. • It can be used over the complete temperature range but

be aware of interactions at very high temperatures.

Sapphire/PCA crucibleMax. temp: 2000 °C

70 µL (TGA, DSC)

(TGA, DSC)

• For melting metals (Fe, Ni).• Non-porous.• Reusable.

Oxidation 3-point ceramic support Max. temp: 2000 °C [UC 34/9] (TGA)

• Only for use with solid samples.• Ideal for exposing the maximum surface area to the furnace

atmosphere (e.g. in oxidation studies).

For more information please see: www.mt.com/ta-crucibles.


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Figure 3. One Click™ screen.

6. Starting a Measurement

To guarantee safe and easy starting of thermal analysis measurements, methods are prepared accordingly.

Instruments: Keep the instruments on idle at the starting temperature, monitor gas supply and flow rate and check instrument performance before analysis. Methods: Select optimum measurement parameters such as heating rate, end temperature and sample size limits. Select the most suitable evaluation range and procedure. Store the method so that it is available for One Click™.

Methods started with One Click™ provide increased safety and efficiency: • No confusion about methods to apply. • No operating errors. • No time consuming method entry. • Minimized error-prone manual data entry.

The unique One Click™ functionality introduced by METTLER TOLEDO to a variety of instruments allows easy and safe starting of predefined measuring methods.After one click on the instruments’ touchscreen color display, the method is started automatically or the next screen asks for further data displaying entry fields for sample name, sample weight and position if a sample robot is used.

To avoid transcription errors and simplify the task even further, it is recommended that a barcode reader is used for sample identification entry.


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Sample insertion modes for TMA:

Penetration or expansion measurement

Tension measurement Swellling measurement

Figure 6a. Sample placed on sample support and topped by sensor probe.

Figure 6b. Sample fixed by clamps and hanging in sample support.

Figure 6c. Sample in crucible topped by sensor probe.

7. Sample Insertion

Sample insertion to DSC and TGA instruments can be done in two ways:

1. Manual insertion The DSC and TGA instruments stand out through

their intelligent ergonomic design concept. In particular, a tray of prepared crucibles can be placed very near to the sensor area, where the measurement takes place. Hand rests, with ergonomically shaped and soft touch coated surfaces support the operator. Thus, operators can easily and safely insert the samples into the measurement cell.

2. Automatic insertion using the sample robot The main advantages of a sample robot are unattended operation for increased efficiency, extended

working periods to overcome regular shifts and improved repeatability by reducing operator influence.

The METTLER TOLEDO sample robot can process up to 34 samples, even if every sample requires a different method and a different crucible. The robot can remove the protective crucible lid from the crucible or pierce the lid of hermetically sealed aluminium crucibles immediately before measurement. This unique feature prevents the sample taking up or losing moisture between weighing and the measurement. It also protects oxygen-sensitive samples from oxidizing.

The design of the sample robotics means that the piercing pin does not come into contact with the sample, preventing cross contamination during operation.

Please see the sample changer robot in action at www.mt.com/ta-automation

Figure 5. Sample robot handling several types of crucibles.

For DMA measurements, the sample needs to be fixed by clamps and then inserted. Several insertion modes are applied in DMA measurement.

Figure 4. DSC oven ready for manual sample entry


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8. Unattended Measurement

Unattended measurements are a perfect set for error free, safe and reliable experiments. All experimental parameters entered beforehand to the method are stored for repetitive use. Thus, any recall of the method assures correct execution of the test. Once the measurement has started, the method works automatically.

Many features of METTLER TOLEDO's Thermal Analysis Excellence instruments contribute to safe and unattended measurements. Selection of these features that benefit the thermal analysis user include:

• FlexCal®, a function of the STARe software, ensures that the correct calibration data is applied to the calculated results. FlexCal®, automatically considers method variants such as gases, crucibles and the heating rate to name a few, from one measurement to the next. This method flexibility results in accurate and precise measurements.

• The gas flow is programmed within the method and no manual adjustments are necessary. FlexCal® takes this flow rate into account for the calculated results.

• Setting the TGA instrument for automatic buoyancy compensation. This is an easy and effective approach to achieve accurate TGA results. Buoyancy compensation reduces the experimental time needed to produce accurate results by more than 50%:

• It eliminates the need to run and subtract blank curves.

• It makes the waiting period for cooling, between blank and sample measurements, obsolete.

• After the measurement has been completed, the resulting curve is recorded and a pre-programmed macro evaluates the areas of interest performing conformity checks against user defined limits. A result text can be displayed, e.g. "The sample has passed".

The evaluated curve, including results, can be printed and/or transferred to a LIMS system automatically.

• When a measurement has finished, the method can be set to inform the user by email. This is especially helpful when operating an instrument manually, as you are alerted to insert the next sample saving laboratory time.

Another aspect of unattended measurement is the application of a sample changer robot. It extends the period of unattended operation considerably and allows for operation out of regular laboratory working hours. METTLER TOLEDO's sample robot, for the DSC and TGA, stores up to 34 samples. Its universal gripper handles various crucible types and utilizes the lid piercing option when specified in the method.

Figure 8. Preconfigured gas supply which does not need any user interaction.

Figure 7. Excellent agreement between the time saving buoyancy compensated and a conventional TGA measurement.


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General Calibration is the determination of the deviation of the measurement result from a reference/literature value (it is equivalent to a check). Adjustment is the adaptation of instrumental parameters after calibration. Be aware of the certification of your reference materials: depending on the vendor’s certification status and testing procedure, substances might be certified for purity, melting point, enthalpy of fusion, modulus, and so on.

The following procedure can be followed to check and improve the performance capability of DSC, TGA, TMA and DMA instruments:

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Define measuring combination

Define limits of permissible errors

Define calibration interval

Adapt calibration methods

AdjustCalibrate

Calibration values OK

Measure

Yes

Yes

Yes

No

No

End ofcalibration

interval


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• Define the calibration interval: With a new and unknown instrument, a check should be performed once a week. When it becomes clear that the instrument does not drift over time, the check can be lengthened to once every 2 or even 3 weeks. Only adjust the instrument if the check is wrong! (In addition, make sure you reproduce the faulty check with a newly prepared indium/zinc sample). The long term drift of the instrument can be followed by collecting the accumulated check data in a spreadsheet or the statistics functionality of the STARe software. An indium check only takes only 6 minutes; the indium pill can be used up to 25 times for normal checks.

• Define limits of permissible error: The limits that are defined here depend on the application. The standard limits for indium are for example set to ±0.3 °C. Make sure you use realistic limits: if the reproducibility of the melting point of your substance is only ±2 °C (e.g. with polymers), an indium check requirement of ±0.3 °C will just waste the additional time needed to adjust the instrument to better than ±2 °C.

• Define measuring combination• Define the temperature range: The adjusted temperature range should begin and end 50 K below and measurement range.• Define the heating rates: Same heating rate as used in the methods (10, 20 K/min…). When the tau lag time has been adjusted, any heating rate can be used for a measurement, irrespective of whether that particular heating rate has been adjusted or not. See example below.• Define the atmosphere: Perform the adjustment using the same atmosphere as used in the analysis/method (N2, air…).The gas used influences the tau lag time and the enthalpy.• Define the type of crucible: Perform the adjustment for the same crucible as used in your analysis/method (e.g. Al 40 µL, Al2O3 70 µL…).The crucible defined influences temperature, tau lag and enthalpy.

If the tau lag time is correctly adjusted, the same melting point will be obtained at all heating rates:


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Some general adjustment tips:• Switch on the instrument and all its cooling options and allow it to stabilize for at least two hours before

performing checks.• Do not use the data from the pre-melting of a fresh indium pill (1st heating run), use the data from

subsequent heating runs (up to 25).• The adjustment will be more accurate if the reference samples are positioned manually and not using the

robot.

It is up to the user to specify the tolerance limits!

Further information about calibration and adjustment can be found in the “Calibration and Adjustment in Thermal Analysis” webinar and in [UC 6/1]. Detailed information about the underlying algorithms used in the software can be found in Chapter 8 of the STARe Software “User Handbook”.

Figure 9. Indium measured at diffrent heating rates.


Conc

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Instrument maintenance, test method setup and sample preparation are important pillars of good measurements. They have to be carried out carefully and contribute equally to accurate and reliable results.They are also a prerequisite to laboratory efficiency, to enable seamless workflows.

Thermal Analysis Excellence instruments support users in many ways. From crucible selection to instrument check and measurement accuracy, they help to safely achieve the ultimate target of reliable and trustworthy test results.

Sampling and sample preparation

Start experiment with One Click™

Measurement of sampleCorrect experimental data including- Automatic load of most current calibration data- Automatic gas delivery and control- Automatic buoyancy compensation (for the TGA)

Printout of the result and/or

Transfer to a LIMS system

Automatic evaluation of the resulting curve Automatic results calculation

For example Pass/fail decisions, material conformity check and curing rate.

Sample identification with barcode

Table 4. A seamless thermal analysis workflow.


For M

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ion 11. For More Information

Outstanding ServicesMETTLER TOLEDO offers you valuable support and services to keep you informed about new developments and help you expand your knowledge and expertise, including:

News on Thermal AnalysisInforms you about new products, applications and events. www.mt.com/ta-news www.mt.com/ta-app

HandbooksWritten for thermal analysis users with background information, theory and practice, useful tables of material properties and many interesting applications. www.mt.com/ta-handbooks

TutorialThe Tutorial Kit handbook with twenty-two well-chosen application examples and the corresponding test substances provides an excellent introduction to thermal analysis techniques and is ideal for self-study.

www.mt.com/ta-handbooks VideosOur technical videos explain complex issues concerning thermal analysis instrumentation and the STARe software – whether it’s sample preparation, installation, creating experiments or evaluating measurement results. www.mt.com/ta-videos

UserComOur popular, biannual technical customer magazine, where users and specialists publish applications from different fields. www.mt.com/ta-usercoms

ApplicationsIf you have a specific application question, you may find the answer in the application database. www.mt.com/ta-applications

WebinarsWe offer web-based seminars (webinars) on different topics. After the presentation, you will have the opportunity to discuss any points of interest with specialists or with other participants. www.mt.com/ta-webinars (Live Webinars) www.mt.com/ta-ondemand (On Demand Webinars)

TrainingClassroom training is still one of the most effective ways to learn. Our User Training Courses will help you get the most out of your equipment. We offer a variety of one-day theory and hands-on courses aimed at familiarizing you with our thermal analysis systems and their applications. www.mt.com/ta-training (Classroom) www.mt.com/ta-etraining (Web-based)

Title Order Number

Tutorial Kit (handbook only) 30281946

Tutorial Kit (handbook and samples) 30249170


Inde

x 12. Index

Aajustment ........................................................... 17

Ccalibration .......................................................... 17composition ..........................................................8content .................................................................8crucible ................................................... 11, 12, 13crystallization ........................................................8

Ddecomposition ......................................................8DMA ........................................................... 8, 9, 10drying ...................................................................8DSC.................................8, 9, 10, 11, 12, 13, 15, 16

Eevaporation ...........................................................8expansion coefficient .............................................8experiment ............................................................9

FFlash DSC ........................................................... 10FlexCal® .............................................................. 16

Gglass transition ......................................................8

KKinetics ................................................................8

LLIMS ................................................................... 16liquid crystals ........................................................8

Mmelting .................................................................8

Ooxidation ..............................................................8

PPolymorphism 8purity analysis .......................................................8

Ssoftening...............................................................8specific heat capacity .............................................8sublimation ...........................................................8

TTGA .................................8, 9, 10, 11, 12, 13, 15, 16Thermal Analysis Technique ....................................8TMA.......................................................8, 9, 10, 15

Vvulcanization .........................................................8

YYoung’s modulus ...................................................8

For more informationwww.mt.com/ta

Mettler-Toledo GmbH, AnalyticalSonnenbergstrasse 74CH-8603 Schwerzenbach, SwitzerlandPhone +41-44 806 77 11Fax +41-44 806 72 60Internet www.mt.com

Subject to technical changes© 03/2016 Mettler-Toledo GmbH, 30324796Marketing MatChar / MarCom Analytical

Overview of METTLER TOLEDO Thermal Analysis Application Handbooks

The following application handbooks are available and can be purchased: www.mt.com/ta-handbooks

Introductory handbooks Language Order number DetailsThermal Analysis in PracticeVolume 1Fundamental Aspects (327 pages)

English 51725244

Thermal Analysis in PracticeVolume 2Tips and Hints (48 pages)

English 30306885

Thermal Analysis in PracticeVolume 3Tutorial Examples (86 pages)

English 30281946 Handbook and Tutorial samples 30249170

Validation in Thermal AnalysisA Guide (232 pages)

English 51725141

Applications handbooks Language Order number DetailsThermal Analysis of ElastomersVolumes 1 and 2Collected Applications (275 pages)

English 517250615172505751725058

Volumes 1 and 2Volume 1Volume 2

Thermal Analysis of ThermoplasticsCollected Applications (150 pages)

English 51725002

Thermal Analysis of ThermosetsVolumes 1 and 2Collected Applications (315 pages)

English 517250695172506751725068

Volumes 1 and 2Volume 1Volume 2

Thermal Analysis of PharmaceuticalsCollected Applications (100 pages)

English 51725006

Thermal Analysis of FoodCollected Applications (65 pages)

English 51725004

Evolved Gas AnalysisSelected Applications (65 pages)

English 51725056

Thermal Analysis of PolymersSelected Applications (40 pages)

EnglishGermanFrenchRussian JapaneseKorean

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thermal analysis - tec instrumental

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