The Flash DSC 1A Novel Rapid Scanning Calorimeter

Hay BerdenMettler-Toledo B.V.

Tiel.

Version 1.0. July, 2010Author: J. SchaweReview: A. Hammer

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Contents

§ Who is Mettler-Toledo

§ The DSC Technique- Conventional DSC Curve of PET

§ Reorganization During the Measurement

§ The Flash DSC 1- The Chip Sensor

§ DSC of Metastable Materials

§ Flash DSC Basics- Typical Experiment- Variation of Heating Rates- Variation of Cooling Rates- Isothermal Experiment

§ Application Areas of the Flash DSC 1

§ Applications

§ Summary

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Our Group

METTLER TOLEDO is a global manufacturer and marketer of precision instruments for use in the laboratories, manufacturing, and food retailing.

<Worldwide presence<10’000 employees<Sales approx.

mSD 1.800

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Group Sales

in mUSD

1595

1482

936 10

96 1148 12

14 1304 14

04

1998

1999

2000

2001

2002

2003

2004

2005

2006

2007

2008

2009

1065

1794 19

7317

29

44

1595

1482

936 10

96 1148 12

14 1304 14

04

1997

1998

1999

2000

2001

2002

2003

2004

2005

2006

2007

2008

1065

878

1794 19

73

Sales per Region

in mUSD

Americas 35%

Europe41%

Asia / RoW24%

555

Strongest Brand

666

Global Manufacturing, Sales & ServiceInnovation Centers MT Partners

MT Sales & Service Organizations

Global manufacturing strategy with focused innovation centersApprox. 5’400 employees in sales & service in 35 countries

777

Customer Processes

Solutions to support customer processes

<Accelerate processes

<Improve product quality<Increase efficiency

<Comply with regulations

Customer Benefits

Laboratory SolutionsIndustrial SolutionsRetail Solutions

R&D DrugDiscovery

QualityControl

RetailLogistics

PackagingManufacturing

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Analytical Chemistry

Thermal Analysis

Automated Chemistry Solutions

Laboratory Weighing Solutions

§ Improving processes in R&D, drug discovery and quality control§ Application-specific software§ Interface with your information systems§ Enhanced accuracy, productivity and compliance

Laboratory Balances

Pipettes

Advancing Research and Quality Control

LaboratorySolutions

999

LogisticsReceiving

Improving Productivity

IndustrialSolutions

§ Optimizing your operations from receiving to shipping§ Improved product quality§ Accelerated and automated processes & ERP integration § Increased efficiency§ Regulatory compliance

Process Analytics

IndustrialWeighing

End-of-Line Product Inspection

101010

Optimizing Fresh Foods Management

RetailSolutions

Counter Self-Service CheckoutCentral Pack Receiving Prepack

§ Effectively manage your fresh foods inventory and merchandising § Maximize your efficiency and profitability§ Enhance the satisfaction of your customers§ Integrated in existing IT infrastructures

111111

830 R&D professionals work daily on maintaining our technology lead

Innovation Competencies

Man / MachineInterface

Automation& Robotics

Technology Integration

CustomerApplications

In Process Technology

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Maintenance and Support

Calibration

RegulatoryCompliance

Vali-dation

Maintenance and Support

Calibration

Qualification

Vali-dation

Support

Service Solutions

Improved service tools enhance customer processes

Service XXL Customer Benefits

Validation methods and protocols ensure process reproducibility, user monitoring and safe data management.

Documented equipment qualification ensures compliance with quality assurance systems such as GLP, GMP and ISO.

Calibration processes ensure accurate, reliable and traceable results.

Proactive maintenance maximizes uptime and productivity. User training ensures equipment knowledge which leads to safer working processes.

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The Success Story of Thermal Analysis

Dr Erhard Mettler

In 1945, a Swiss engineer named Dr Erhard Mettler started a

precision mechanics company near Zurich, Switzerland.

The «Mettler balance» became a synonym for the lab balance.

Dr Hans-Georg Wiedemann

In the early 1960s, Dr Wiedemann convinced Dr Mettler to combine the

advanced weighing technology with a furnace. This lead to the

introduction of the TA1.

The analytical balance from 1945

The TA1 from 1964The first TGA/DTA

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The Success Story of Thermal Analysis

Modular concept (1960s)

Multi-pile TGA-DSC

sensor (1970s)

Microprocessor-controlled system

(1980s) Automation (1990s)

DMA with high frequencies

(2002)

MultiSTAR®

DSC sensors (2004)TOPEM®

TMDSC (2005)

Innovation since 1945

Thermal Analysis Excellence (2007)

Substitution balance (1940s)

Flash DSC 1 (2010)

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Thermal Analysis Excellence

Innovative Technology

Versatile Modularity

Swiss Quality

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Overview on Thermal Analysis: Video

The Futureof Thermal Analysis

§ Innovative Technology§ Versatile Modularity§ Swiss Quality

Click to watch the video

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The DSC Technique

Conventional DSC Measuring Principle

ReferenceSample

Heat flow

Typical experimental conditions:

Sample weight: 1 … 20 mgHeating rate: 0.1 … 100 K/minMeasured property: Heat flow

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Innovative Technology

Flash DSC 1:A Quantum Leap in InnovationOpens up New Frontiers

} Heart of the Flash DSC 1 is the chip sensor based on MEMS technologyMEMS: Micro-Electro-Mechanical Systems

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The DSC Technique: DSC Curve of PET

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Reorganization During the Measurement

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The Flash DSC 1

§ Heating rates up to 2 400 000 K/min§ Cooling rates up to 240 000 K/min§ Overlap with conventional DSC§ Simple sample preparation§ Measures from -95 °C … 450 °C

The DSC 1 and the Flash DSC 1 together cover a scanning rate range of more than 7 decades.

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The Flash DSC 1

Easy sample preparation and sensor change thanks to the ergonomic design.

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The Flash DSC 1: The Chip Sensor

The MultiSTAR UFS 1 chip sensor is a DSC sensor based onMEMS technology (Micro-Electro-Mechanical Systems).

The sensor consists of two identical silicon-nitride/oxide membranes,1.6 mm × 1.6 mm, 2 μm thick, mounted in a silicon frame, 300 μm thick.

Ceramic plate

Silicon frame

Bonding wire

Thermocouple Resistance heater

Aluminum plate

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The Flash DSC 1: The Chip Sensor

The sample area is 0.5 mm in diameter and coated with aluminum to achieve a homogeneous temperature distribution.

Eight thermocouples measure the temperature on each side.

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Metastable Materials

§ Polymers § Polymorphic substances§ Many blends and alloys § Many composites

The structure of such materials depends on the cooling conditions used when they were prepared or produced.

On heating, reorganization can occur. This is the reason why the conventional DSC curve does not always correspond to the structure of the original sample.

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Flash DSC Basics: A Typical Experiment

Melting of the sample optimizes thermal contact.

Different cooling rates allow defined sample structures to be formed.

High heating rates suppress the reorganization of the sample. It can therefore be measured “as received”.

Sample preparation

Formation of sample structure Analysis

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Flash DSC Basics: Variation of Heating Rate

Examples of reorganization processes:§ Separation or elimination of phases § Melting of unstable crystallites with formation of more stable crystals § Transitions of polymorphic phases

Reorganization is often determined by kinetic processes and is therefore time dependent.

The possible influence of reorganization on the heating curve can be detected by varying the heating rate of the Flash DSC 1 over a wide range.

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Flash DSC Basics: Variation of Cooling Rate

§ The formation of structure can be investigated by performing measurements at different cooling rates.

§ In particular, technical processes carried out at high cooling rates can be simulated in the Flash DSC 1.

§ Information is obtained about the effect of additives such as nucleating agents under near-process conditions.

Spritzgussform für LEGO® SteineQuelle: http://de.wikipedia.org/wiki/Lego

Source: LEGO Systems, Inc.www.lego.com

Injection molding equipment

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Flash DSC Basics: Isothermal Experiment

The high cooling rates and accurate temperature control often allow materials to be cooled from the melt to the crystallization temperature without undesired formation of structure.

Isothermal measurements provide detailed and direct information on the kinetics of fast transitions and reactions that take place in a few seconds.

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Application areas of the Flash DSC 1

Determination of technical data for simulation calculations

Analysis of very small amounts of sample

Comprehensive thermal analysis of materials in a very short time

Investigation of the mechanism of action of additives under near-production conditions

Determination of the reaction kinetics of fast reactions

Direct measurement of fast crystallization processes

Detailed analysis of structure formation processes in materials.

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Flash DSC Applications 1 Calibration substances

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Flash DSC Applications 2 Melting of PET

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Flash DSC Applications 2 Melting of PET

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Flash DSC Applications 3 Reorganization of iPP

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Flash DSC Applications 4 Isothermal crystallization

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Flash DSC Applications 4 Isothermal crystallization

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Flash DSC Applications 5 Nanofiller in PA 11

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Flash DSC Applications 6 Melting and decomposition

Kurve mit 10 K/min löschen

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Flash DSC Applications 7 Polymorphism

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Summary

The Flash DSC 1 is the ideal complement to conventional DSC for the characterization of modern materials and optimization of production processes.

§ Fast and variable measurements save time in the analysis and development of materials.

§ The quality of products can be improved through knowledge of structure formation under actual process cooling conditions.

§ This data can be used to optimize processing conditions, molds, and tools.

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Features and Benefits of the Flash DSC 1§ Ultra-high cooling rates – allow materials with defined structural

properties to be prepared

§ Ultra-high heating rates – reduce measurement times and suppress reorganization processes

§ Fast-response sensor – enables the kinetics of extremely fast reactions or crystallization processes to be studied

§ High sensitivity – low heating rates can also be used; scan rates overlap with those of conventional DSC

§ Wide temperature range – measurements can be performed in the range -95 to 450 °C

§ User-friendly ergonomics and functionality – sample preparation is quick and easy

Summary

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For More Information

§ News www.mt.com/ta-news§ Handbooks www.mt.com/ta-handbooks§ Webinars www.mt.com/ta-webinars§ Thermal analysis in general www.mt.com/ta

Thank You