Vielitzer Straße 43 Linseis Inc. 95100 Selb 20 Washington Road GERMANY Tel.: 0049 9287 8800 Fax: 0049 9287 70488 Email:info@linseis.de Linseis Inc. 20 Washington Road P.O.Box 666 Princeton-Jct. NJ 08550 Tel.: (609) 799-6282 Fax: (609) 799-7739 Email:info@linseis.com

The Company Since 1957 Linseis Corporation delivers outstanding service, know how and leading innovative products in the field of thermal analysis and thermal physical properties. We are driven by innovation and customer satisfaction. Customer orientation, innovation, flexibility and last but not least highest quality are what Linseis stands for from the very beginning. Thanks to these fundamentals our company enjoys an exceptional reputation among the leading scientific and industrial companies. Claus Linseis Managing Director

The Company Linseis Germany Vielitzerstr. 43 95100 Selb Linseis USA 08550 Princeton Jct. / NJ

What is Thermal Analysis? Materials Additives Plasticizers Impurities Fillers Processing Thermal treatment Mechanical stressing Shaping Storage and use Material Properties

What is Thermal Analysis? O2 Heating heat capacity expansivity modulus Melting melting point crystallinity softening purity Oxidation OIT stabilizers burning profile Decom- position temperature content kinetics Temperature high low

What is Thermal Analysis? Material Properties Melting point / melting range Crystallization behavior Glass transition temperature Coefficient of thermal expansion Thermal stability Decomposition temperatures and kinetics Oxidation induction time / temperature , OIT Crosslinking behavior Purity Visco-elastic properties: modulus, damping and creep Swelling behavior Thermal Conductivity Thermal Diffusivity

What is Thermal Analysis? Chemical Reactions and Properties Reactions between components in the formulation or the atmosphere Effect of catalysts Chemical bonding of plasticizers Crosslinking reactions Chain scission Oxidative reactions Degradation breakdown Molecular structure and bond strengths Chemical weather and ageing effects Effect of additives Polymerizations

What is Thermal Analysis? Physical Properties Specific heat capacity Physical transitions Mass or weight changes Mechanical properties such as dimension, deformation, storage and loss modulus Thermal Conductivity / Thermal Diffusivity Nature of evolved gas

What is Thermal Analysis? Industry Application Research & Development Quality Control Service Labs Academia Polymers Food Cosmetics Forensics Textiles Electronics Automotive Aerospace Packaging Biochemistry Biopolymers Ceramics Metal Composites Adhesives Paints Lacquers Resins Pharmaceutical …

Thermal Analysis Applications Glass transition Crystallization Melting Degradation Oxidation Phase transitions Compatibility Identification Polymers Polyolefins Resins Adhesives Blends Composites Paints Polymers

Thermal Analysis Applications Polymorphism Crystallization Phase transitions Identification of components Compatibility Stability Purity Binary phase diagrams Moisture Drugs Drug delivery systems Excipients Manufacturing additives Packaging materials Pharmaceuticals

Thermal Analysis Applications Formulation Compatibility Stability Polymorphism Glass transition Crystallization Raw material identification Organic content Pigment color analysis Water content Lipsticks Fats Waxes Creams Nail varnish Polymer packaging Cosmetics

Thermal Analysis Applications Polymorphism Identification of components Crystallization Thermal history Stability Glass transition Vaporization Denaturizing Visco-elastic behavior Swelling Edible fats and oils Fatty acids Cocoa butter Starch Sugar Proteins Food

Thermal Analysis Applications Identification of components Crystallization Phase transitions Binary phase diagrams Polymorphism Hazard analysis Oxidation stability Explosives Lubricants Paraffin Waxes Pitches Liquid Crystals Oils Petrochemicals and Organic Chemicals

Thermal Analysis Applications Calibration standards Carbonates Cement Coal Fillers Hydrates Gypsum Metals and alloys Glass Ceramics Minerals Water determinations Phase transitions Inorganics

Product Index DSC Differential Scanning Calorimeter STA Simultaneous Thermal Analysis DSC / DTA High Temperature DTA/DSC DIL Dilatometry TMA Thermomechanical Analysis EGA Gas analysis / Couplings LFA Thermal Diffusivity Thermal Conductivity

Differential Scanning Calorimetry Differential Scanning Calorimetry (DSC) is most popular thermal analysis technique it measures endothermic and exothermic transitions as a function of temperature - Endothermic = heat flows into a sample Exothermic = heat flows out of the sample The instrument is used to characterize polymers, pharmaceuticals, foods/biologicals, organic chemicals and Inorganics. Transitions measured include Tg, melting, crystallization, curing and cure kinetics, onset of oxidation and heat capacity.

Differential Scanning Calorimeter – DSC DSC PT 10 The DSC PT10 comprises the advantages of latest technology, highest resolution and a robust easy to use instrument design. The measurement principle of heat flux allows ultimate measurement precision. The used sensor has a very high resolution and can be calibrated very accurately. The optional software controlled gas box enables Oxidation Induction Time (OIT) measurements. The Kinetic software and many other features provide the perfect solution for any calorimetric experiment.

Specifications Temperature range: -150 up to 700°C Heating and cooling rates: 0.01 up to 100°C/min Resolution: 0.125 uW Cooling: Air, LN2, intracooler Gas control box: up to 4 gases Atmosphere: inert, oxid., red.

Application - Food

Application - PET

Simultaneous Thermal Analysis (STA) TG – DTA/DSC Simultaneous TGA-DTA/DSC measures both heat flow and weight changes in a material as a function of temperature or time in a controlled atmosphere. Simultaneous measurement of these two material properties not only improves productivity but also simplifies interpretation of the results. The complimentary information obtained allows differentiation between endothermic and exothermic events which have no associated weight loss (e.g., melting and crystallization) and those which involve a weight loss (e.g., degradation).

STA - System open protection tube for EGA Sensor Furnace Gas inlet Vacuum Purge gas Sensor Gas inlet Gas outlet

STA - Sensors DSC (enthalpy): E / K / S / B DSC Cp: E / K / S / B DTA: E / K / S /B / W TG: different designs

STA PT1000 The Linseis STA PT1000 is a top loading Thermobalance, which offers a highly user friendly design. Even at a sample weight of up to 10g the Tara is done electronically. The specially designed furnaces allow fast heating and cooling rates as well as a highly precise temperature control. Exchanging the different TGA, DTA or DSC measuring systems is only a question of minutes.

STA PT1600 The STA PT1600 is the high end Simultaneous Thermobalance from Linseis. The system offers unparalleled TG and DSC resolution in combination with highest vacuum capabilities and TG drift stability. The system is modular due to five exchangeable furnaces, many different measuring systems and crucibles. The coupling ability and many other optional accessories guarantee the perfect setup for whatever application.

STA Specifications STA PT 1000 STA PT 16000 Temperature range: RT up to 1100°C -150 up to 500°C, RT up to 1400/1500°C RT up to 1600/1750°C RT up to 2000/2400°C Sample mass: 5 / 10g 5 / 10 / 25g Resolution: 0.1 / 0.5ug 0.1 / 0.5ug Atmosphere: inert, oxid., red., vac. Inert, oxid., red., vac. Vacuum: 10E-2 mbar 10E-5 mbar Pressure: optional 2/5 bar Sample Carriers: TG – DTA/DSC TG – DTA/DSC DSC meas. systems: E/K/S E/K/S/B

Application – Decomposition of CaC2O4

Application - Cement

High Temperature DSC / DTA Differential Scanning Calorimetry (DSC) is most popular thermal analysis technique it measures endothermic and exothermic transitions as a function of temperature - Endothermic = heat flows into a sample - Exothermic = heat flows out of the sample Linseis offers a unique line of high temperature DTA and DSC systems.

High Temperature DSC / DTA The Linseis high temperature DTA/DSC are designed to deliver highest calorimetric sensitivity, short time constants and a condensation free sample chamber. These features guarantee superior resolution, baseline stability over the entire instrument lifetime. Thus providing a indispensable tool for material development, R&D and quality control. The modular concept of the DSC and DTA systems allows the use of different furnaces with a temperature range from -150 up to 2400°C, different measuring systems for DSC and DTA as well as many different crucibles. The vacuum tight design enables quantitative enthalpy and Cp (Specific Heat) determination under cleanest atmospheres as well as under vacuum 10E-5mbar. Additionally the systems can be coupled to a MS or FTIR.

DTA/DSC - System open protection tube for EGA Sensor Furnace Gas inlet Vacuum Sensor Gas inlet Gas outlet

High Temperature DSC DSC PT1600 Temperature range: -150 up to 500°C RT up to 1400/1500/1600 RT up to 1650/1750°C Sensors: E / K / S / B DSC- Cp, DSC, DTA Vacuum: 10E-5 mbar Atmospheres: inert, oxid., red., vac.

High Temperature DTA DTA PT1600 Temperature range: -150 up to 500°C RT up to 1400/1500/1600 RT up to 1650/1750°C RT up to 2000/2400°C Sensors: E / K / S / B / W DTA Vacuum: 10E-5 mbar Atmospheres: inert, oxid., red., vac.

Application – Magnetic Ferrites

Dilatation Dilatometry (DIL) is a technique in which a dimension of a substance under negligible load is measured as a function of temperature while the substance is subjected to a controlled temperature program in a specified atmosphere.

Dilatometer L76 & L75 DIL L76 Horizontal DIL L75 Vertical

DIL System Measuring System Pushrod Sample Display Furnace L75 PLATINUM SERIES DILATOMETER

DIL Measuring Systems Quartz Measuring System for large Samples 20mmØ Quartz Measuring System standard Al2O3 Measuring System standard Adapter for powders & pastes Al2O3 Measuring System contact free

Specifications Model L76 PT Horizontal L75 PT Horizontal L75 PT Vertical Temperature range : -150 up to 500°C -150 up to 500°C RT up to 1000/1400/ RT up to 1000/1400 RT up to 1000/1400 1600°C 1600/2000°C RT up to 1600/1750 2000/2400/2800°C Resolution: 1.25 nm/digit 0.125 nm/digit 0.125 nm/digit Sample length: 25/50 mm 25/50 mm 25/50 mm Sample diameter: 7/14/20 mm 7/14/20 mm 7/14 mm Sample number: Single or differential Single or differential Single, differential or Quattro Atmosphere: inert, red. inert, oxid., red., vac. inert, oxid., red., vac. Sample holders: Fused Silica, Al2O3 Fused Silica, Al2O3, Fused Silica, Al2O3, Sapphire, Graphite Sapphire, Graphite

Application – Softening Point Glass Sample

Application – Ceramic RCS (Rate Controlled Sintering)

Special Dilatometers Laser Dilatometer The next step in expansion measurements. The L75 Laser Dilatometer outperforms any conventional pushrod dilatometer by offering a 33 times higher resolution. The measurement principle is based on a Michelson interferometer thus eliminating all mechanical errors. This outstanding patented measurement principle can cope with latest high tech ultra low expansion (ULE) materials. Linseis Specifications Method : Laser Dilatometer ”Michelson Principe“ Temperature range: -180 up to 500°C RT up to 1000°C Sample length: up to 20 mm Sample diameter: up to 7 mm Resolution: 0.3 nm Atmosphere: inert, oxid., red., vac. Vacuum: 10E-5 mbar Sample preparation: same as conventional dilatometer

Special Dilatometers Quenching Dilatometer The Quenching Dilatometer L78 RITA is especially suitable for the determination of TTT, CHT and CCT diagrams. The special induction furnace enables heating and cooling speeds in excess of 400°C/s. The system complies with ASTM A1033. All critical parameters such as heat up and cool down speed, gas control and safety features are software controlled. Certainly export functions in ASCII-format as well as graphic output is possible. Quenching Dilatometer Specifications Temperature range: RT up to 1000°C RT up to 1600°C Heating / cooling rates: up to 400°C/s for solid samples Hollow samples even faster Sample holders: Fused Silica, Al2O3 Sample length: 10 mm Sample diameter: 6-7 mm Atmosphere: inert, oxid., red, vac. Vacuum: 10E-5 mbar (with turbomolecular pump)

TMA – Thermomechanical Analysis Thermomechanical analysis (TMA) measures linear or volumetric changes in the dimensions of a sample as a function of time, temperature and force in a controlled atmosphere.

TMA - System TMA PT1000 TMA PT1600

TMA – Measuring Systems Stress/Strain Volumetric Expansion 3 Point Bending Expansion Penetration E-Modulus

TMA PT1000 TMA PT1000 The Thermomechanical Analyzers TMA PT1000 and TMA PT1000 EM uniquely combine the flexibility of several measurement procedures under changing requirements. The instrument can measure expansion and deformation at highest precision.

TMA PT1600 TMA PT1600 The TMA PT1600 offers a broad temperature range (RT up to 1600°C) for all kinds of Thermomechanical investigations.

TMA Specifications Model TMA PT1000 EM TMA PT1000 TMA PT1600 Temperature range: -150 -1000°C -150 -1000°C -150 – 500°C RT up to 1600°C Cryo option: available available available Force: 1/5.7N 1/5.7/20N 1N Frequency: 1/5Hz — 1Hz Resolution: 0.125nm 0.125nm 0.125nm Atmosphere: inert, oxid inert, oxid inert, oxid red., vac. red., vac. red., vac. Vacuum: 10E-5mbar 10E-5mbar 10E-5mbar

Application – Creep Behaviour

Application - PVC

EGA – Evolved Gas Analysis TGA measures weight changes (quantitative) Difficult to separate, identify, and quantify individual degradation products (off-gases) Direct coupling to identification techniques (Mass Spec, FTIR) reduces this problem

TGA / STA – Mass Spectroscopy MS – Mass Spectroscopy Advantages: Higher sensitivity and wider dynamic range than FTIR (1ppm vs. 10ppm). Measures non-IR absorbing gases. More rapid response. Disadvantage: Cannot distinguish between isomers. (e.g. N2 and CO)

TGA / STA - FTIR FTIR (Fourier transformation infrared spectroscopy): Advantages: On-line measurement Hydrocarbons are easy to identify Disadvantages: No detection of inert gases (no dipole moment) Detection of inorganic gases limited

Application – Calcium Oxalate Decomposition of Calcium Oxalate monohydrate CaC2O4 under Argon Atmosphere The evolved gases from the decomposition of Calcium Oxalate have been fed into the Mass Spectrometer with a heated capillary. The ion currents for mass numbers 18 (water), 28 (carbon monoxide) and 44 (carbon dioxide) have been imported into the graph.

LFA – Thermal Conductivity / Thermal Diffusivity The sample is positioned horizontally on a sample robot, located in a furnace. The furnace is then held at a predetermined temperature. At this temperature the sample bottom is then irradiated with a programmed energy pulse (laser or xenon flash). This energy pulse results in a homogeneous temperature rise at the sample top. The resulting temperature rise of the sample top is measured by a high speed IR detector and thermal diffusivity values are computed from the temperature rise versus time data. The resulting measuring signal computes the thermal diffusivity, and in most cases the specific heat (Cp) data. If the density (r) is identified, the thermal conductivity can be calculated: λ(T)=α(T)*Cp(T)*ρ(T)

LFA - Systems XFA 500 & LFA 1000 Information of the thermo physical properties of materials and heat transfer optimization of final products is becoming more and more vital for industrial applications. Over the past few decades, the flash method has developed into the most commonly used technique for the measurement of the thermal diffusivity and thermal conductivity of various kinds of solids, powders and liquids.

XFA/LFA Design

Measuring Range

XFA/LFA Specifications Model XFA 500 LFA 1000 Temperature range: RT up to 500 -125 up to 500°C RT up to 1250/1600°C Vacuum: 10E-5mbar 10E-5mbar Atmosphere: inert, oxidizing or reducing inert, oxidizing or reducing Sample dimensions: Ø 10 / 12.7 / 25.4 mm Ø 10 / 12.7 / 25.5 mm □ 10x10 mm □ 10x10 mm 0.1 up to 6 mm thick 0.1 up to 6 mm thick Max. Sample number: 6 samples 10 / 12,7mm 6 samples 10 / 12,7mm 3 samples Ø 25,4mm 3 samples Ø 25,4mm Measuring range: Thermal Diffusivity 0.01 mm2/s - 1000 mm2/s 0.01 mm2/s - 1000 mm2/s Thermal Conductivity 0.1 W/(m·K) - 2000 W/(m·K) 0.1 W/(m·K) - 2000 W/(m·K) Pulse source: Xenon Flash Nd: YAG Laser Pulse energy: 10J/pulse 25J/pulse

Application – Graphite

Application – Aluminum / Copper