DTA

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Lab Course Lab Course Instruction Instruction

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Laboratory in Physical Materials Diagnostics Laboratory in Physical Materials Diagnostics

Topic of the Experiment

Methods of Thermal Analysis Methods of Thermal Analysis

1 Tasks

1.1.

1.1. Analyse Analyse a a material material sample sample with with assistance assistance of of the the simultaneous simultaneous thermalthermal analysis (STA

analysis (STA DTA/TG).DTA/TG). 1.2.

1.2. Determine Determine the the coefficient coefficient of of linear linear expansion expansion of a of a metal metal sample sample and and comparecompare the expansion with other materials (TMA).

the expansion with other materials (TMA).

2 Basics

2.1 2.1 Differential Thermal

Differential Thermal Analysis

Analysis (DTA) &

(DTA) & Thermogravimetry

Thermogravimetry (TG)

(TG)

Thermal analysis (TA) is the generic name for methods, which allow the Thermal analysis (TA) is the generic name for methods, which allow the determination of physical and chemical properties of a material or a compound and/or determination of physical and chemical properties of a material or a compound and/or the reaction of compounds. In the dynamic thermal analysis the temperature is the reaction of compounds. In the dynamic thermal analysis the temperature is changed slowly (keeping the sample in the thermodynamic equilibrium) and changed slowly (keeping the sample in the thermodynamic equilibrium) and measured together with the physical or chemical property of interest. Typically, the measured together with the physical or chemical property of interest. Typically, the temperature is changed in a linear way versus temperature. In a static thermal temperature is changed in a linear way versus temperature. In a static thermal analysis, the sample

analysis, the sample is moved rather is moved rather fast to a set point tempfast to a set point temperature. erature. Afterwards, theAfterwards, the physical or chemical property of interest is measured versus time.

physical or chemical property of interest is measured versus time. The following overview shows the

The following overview shows the variety of thermal analysis methods:variety of thermal analysis methods:

•• Dynamic Difference Caloric Analysis (DSC)Dynamic Difference Caloric Analysis (DSC)

o

o Difference Thermal Analysis (DTA)Difference Thermal Analysis (DTA) o

o Dynamic Heat Flow Difference Caloric Analysis (DTSC)Dynamic Heat Flow Difference Caloric Analysis (DTSC) o

o Dynamic Power Difference Caloric Analysis (DPSC)Dynamic Power Difference Caloric Analysis (DPSC) •• Thermo Gravimetrical Analysis (TGA)Thermo Gravimetrical Analysis (TGA)

•• Thermo Mechanical Analysis (TMA)Thermo Mechanical Analysis (TMA)

•• Dynamic Mechanical Analysis (DMA)Dynamic Mechanical Analysis (DMA)

•• Thermo Magnetic Analysis (TM)Thermo Magnetic Analysis (TM)

o o OptometryOptometry o o SpectrometrySpectrometry o o Luminescence (TL)Luminescence (TL) o o MicroscopyMicroscopy o o RefractometryRefractometry o o ElectrometryElectrometry o o Sonimetry (TS)Sonimetry (TS)

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•• Dielectric Thermal Analysis (DETA)Dielectric Thermal Analysis (DETA)

•• Thermal Stimulated Current (TSC)Thermal Stimulated Current (TSC)

•• Evolved Gas Analysis (EGA) – Evolved Gas Analysis (EGA) – thermal conductivitythermal conductivity

•• Evolved Gas Detection (EGD) – kind and amount of created gasesEvolved Gas Detection (EGD) – kind and amount of created gases

•• Emanation Thermal Analysis (ETA) - Emanation Thermal Analysis (ETA) - radioactive gasesradioactive gases

This list is not complete. A number of combinations are possible. To give some This list is not complete. A number of combinations are possible. To give some examples thermogravimetry can be combined with gas chromatogaphy (TG-GC) or examples thermogravimetry can be combined with gas chromatogaphy (TG-GC) or infrared spectroscopy (TG-FTIR). Furthermore, different thermal analysis methods infrared spectroscopy (TG-FTIR). Furthermore, different thermal analysis methods are often combined within one experimental setup, e.g. TG-DSC or TG-DTA. Often are often combined within one experimental setup, e.g. TG-DSC or TG-DTA. Often the combination of methods results in an overall sensitivity decrease. However, often the combination of methods results in an overall sensitivity decrease. However, often the simultaneous access to different properties rules out misinterpretations. To give the simultaneous access to different properties rules out misinterpretations. To give an example: A temperature curve measured in DSC indicating an endothermic an example: A temperature curve measured in DSC indicating an endothermic reaction may be the result of a phase transition or a mass loss. The combination with reaction may be the result of a phase transition or a mass loss. The combination with TG allows then a decision on the real process in the sample.

TG allows then a decision on the real process in the sample. A

A number number of of methods methods and and their their special special application application fields fields are are standardized standardized by by thethe respective organizations (e.g. ASTM – U.S.A or DIN – Germany). There detailed respective organizations (e.g. ASTM – U.S.A or DIN – Germany). There detailed instructions for experimental setups and guidelines for thermoanalytical experiments instructions for experimental setups and guidelines for thermoanalytical experiments can be found.

can be found.

2.1.1 2.1.1 Differential

Differential Thermal A

Thermal Analysis (DTA)

nalysis (DTA)

In DTA the temperature difference of a sample and a reference material is measured In DTA the temperature difference of a sample and a reference material is measured versus the sample temperature. The temperature is controlled during the versus the sample temperature. The temperature is controlled during the measurement by a suitable control unit or by a computer.

measurement by a suitable control unit or by a computer. A DTA

A DTA setup is shown setup is shown in the in the figure 1 figure 1 below. The diffbelow. The difference of the erence of the temperature of thetemperature of the thermocouples is measured during heating of the furnace. Such difference thermocouples is measured during heating of the furnace. Such difference measurement is realized simply by a series connection of the thermocouples with measurement is realized simply by a series connection of the thermocouples with

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Figure 1: DTA measurement system with special crucibles including thermocouples Figure 1: DTA measurement system with special crucibles including thermocouples

opposite polarity. In the ideal case, the temperature difference between the sample opposite polarity. In the ideal case, the temperature difference between the sample and the reference is zero if the enthalpy of the sample does not change during and the reference is zero if the enthalpy of the sample does not change during heating (the reference material is not changing its enthalpy in the desired heating (the reference material is not changing its enthalpy in the desired temperature range). However, in a real setup the so-called base line, i.e. the temperature range). However, in a real setup the so-called base line, i.e. the measured temperature difference is not always exactly zero. However, changes of measured temperature difference is not always exactly zero. However, changes of the baseline are rather continuous and the curve does not show peaks. Only in case the baseline are rather continuous and the curve does not show peaks. Only in case of endothermic or exothermal processes in the sample, one can observe deviations of endothermic or exothermal processes in the sample, one can observe deviations or peaks to either side of the base line. The area of the peaks is proportional to the or peaks to either side of the base line. The area of the peaks is proportional to the heat quantity. By measuring the temperature of the sample simultaneously, it is heat quantity. By measuring the temperature of the sample simultaneously, it is possible to plot the temperature difference as a function of the temperature of the possible to plot the temperature difference as a function of the temperature of the sample:

sample:

Formula 1: Temperature dependence Formula 1: Temperature dependence

)) ((T T f f T T == ∆ ∆

In order to reduce the influence of systematic measurement errors the temperature is In order to reduce the influence of systematic measurement errors the temperature is commonly changed linearly with time. A number of experimental parameters (sample commonly changed linearly with time. A number of experimental parameters (sample material, preparation, and experimental setup) influence the shape of the base line material, preparation, and experimental setup) influence the shape of the base line and the position, shape and height of the peaks, respectively. Some important and the position, shape and height of the peaks, respectively. Some important parameters are listed below:

parameters are listed below:

•• Heating velocityHeating velocity

•• Sample massSample mass

•• Geometrical dimensions of the materials inside the furnaceGeometrical dimensions of the materials inside the furnace

•• Thermal conductivity of used setup partsThermal conductivity of used setup parts

•• grain size and density of the sample materialgrain size and density of the sample material

•• atmosphere inside the furnace, in case of gas – flow speedatmosphere inside the furnace, in case of gas – flow speed

Often the atmosphere of the sample environment is used as an additional Often the atmosphere of the sample environment is used as an additional experimental parameter, e.g. oxygen influencing oxidation reactions or water vapour experimental parameter, e.g. oxygen influencing oxidation reactions or water vapour influencing dewatering reactions.

influencing dewatering reactions.

The combination of DTA with the thermo gravimetrical analysis (TGA) allows the The combination of DTA with the thermo gravimetrical analysis (TGA) allows the simultaneous registration of temperature differences and mass changes. This simultaneous registration of temperature differences and mass changes. This technique improves remarkably the possibility for an accurate data interpretation. technique improves remarkably the possibility for an accurate data interpretation. Therefore, modern commercial equipment allows often the simultaneous acquisition Therefore, modern commercial equipment allows often the simultaneous acquisition of DTA and TGA data. Both data sets – temperature difference as well as mass of DTA and TGA data. Both data sets – temperature difference as well as mass changes – are displayed versus the same time scale. The TGA data are plotted as changes – are displayed versus the same time scale. The TGA data are plotted as derivative of the mass dm/dt, hence directly indicating the changes of the mass.

derivative of the mass dm/dt, hence directly indicating the changes of the mass.

2.1.2 2.1.2 Equipment

Equipment Setup

Setup

A

A typical setup typical setup of Tof TGA GA – – DTA DTA combination is combination is shown in shown in figure figure 2 2 below. The below. The range of range of the experimental parameters could be found in figure 3.

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Figure 2: Device assembly of SETARAM TG-DTA 92-16 Figure 2: Device assembly of SETARAM TG-DTA 92-16

Figure 3: Experimental Parameter of SETARAM TG-DTA 92-16 Figure 3: Experimental Parameter of SETARAM TG-DTA 92-16

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2.1.3 2.1.3 Application

Application Examples

Examples for

for DTA/TG

DTA/TG

The following examples can be reviewed also here: The following examples can be reviewed also here:

http://www.netzsch-thermal-analysis.com/en/products/detail/pid,6,t,4.html

(i) Components of a rubber compound for tires (Fig. 4 below) (i) Components of a rubber compound for tires (Fig. 4 below) The decomposition of the rubber

The decomposition of the rubber takes place in several steps:takes place in several steps:

•• Plasticizer fraction desorbs (about 7% mass Plasticizer fraction desorbs (about 7% mass loss)loss)

•• Rubber decomposition in fraction 1 (38% at 383°C)Rubber decomposition in fraction 1 (38% at 383°C) and fraction 2 (31% at 448°C)

and fraction 2 (31% at 448°C)

The carbon black portion is calculated to be 20% of

The carbon black portion is calculated to be 20% of mass, the ash content is 4%. Themass, the ash content is 4%. The peak positions of the derivative of the TGA-curve (d∆m/dt, i.e. DTGA) allow the exact peak positions of the derivative of the TGA-curve (d∆m/dt, i.e. DTGA) allow the exact determination of the process onset temperatures. For the investigated sample, it has determination of the process onset temperatures. For the investigated sample, it has been concluded that the compound is a

been concluded that the compound is a back-fiulled NR/SBR rubber blend.back-fiulled NR/SBR rubber blend.

Figure 4: Carbon black-filled NR/SBR rubber blend Figure 4: Carbon black-filled NR/SBR rubber blend

Thermal decomposition of dolomite in a CO

Thermal decomposition of dolomite in a CO22-atmosphere-atmosphere

The mass loss steps during the thermal decomposition of the mineral dolomite The mass loss steps during the thermal decomposition of the mineral dolomite [CaMg(CO

[CaMg(CO33))22], shown in figure 5, overlaps when the measurement is performed in a], shown in figure 5, overlaps when the measurement is performed in a

N

N22 atmosphere. By using COatmosphere. By using CO22 as a purge gas, they can be clearly separated. Theas a purge gas, they can be clearly separated. The

calculated DTA signal additionally yields the information that both mass loss calculated DTA signal additionally yields the information that both mass loss processes are endothermic.

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Figure 5: Thermal decomposition of dolomite in a CO2-atmosphere Figure 5: Thermal decomposition of dolomite in a CO2-atmosphere

Plasticizer content in a rubber compound Plasticizer content in a rubber compound

In a standard measurement, the evaporation of a low-molecular plasticizer is In a standard measurement, the evaporation of a low-molecular plasticizer is overlapped by the decomposition of the elastomeric components (red curves in fig. overlapped by the decomposition of the elastomeric components (red curves in fig. 6). If the measurement is performed in vacuum, the evaporation of the plasticizer is 6). If the measurement is performed in vacuum, the evaporation of the plasticizer is shifter to lower temperatures (black curves in fig. 6). This behaviour is a direct shifter to lower temperatures (black curves in fig. 6). This behaviour is a direct consequence from the reduced pressure and the resulting reduction of the boiling consequence from the reduced pressure and the resulting reduction of the boiling temperature of the plasticizer. In this way, the plasticizer content can be determined temperature of the plasticizer. In this way, the plasticizer content can be determined much more precisely.

much more precisely.

Figure 6: Plasticizer content in a rubber compound measured in air(red) or vacuum (black) Figure 6: Plasticizer content in a rubber compound measured in air(red) or vacuum (black)

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2.2 TMA

TMA is the abbreviation for thermo-mechanical analysis. In this type of thermal TMA is the abbreviation for thermo-mechanical analysis. In this type of thermal analysis changes of sample geometry are monitored versus temperature changes. analysis changes of sample geometry are monitored versus temperature changes. The most popular TMA is the dilatometry, i.e. the measurement of geometry changes The most popular TMA is the dilatometry, i.e. the measurement of geometry changes in one dimension. In general, dilatometers are used to measure linear length variation in one dimension. In general, dilatometers are used to measure linear length variation of a sample as a function of the

of a sample as a function of the temperature. The application fields cover the analysistemperature. The application fields cover the analysis of shrinking, length changes due to recrystallization or simply the det

of shrinking, length changes due to recrystallization or simply the det ermination of theermination of the linear thermal expansion coefficient α(T).Figure 7 shows the principle design of a linear thermal expansion coefficient α(T).Figure 7 shows the principle design of a dilatometer.

dilatometer.

Figure 7: Dilatometer with a rod shaped sample in horizontal configuration (WA - expansion Figure 7: Dilatometer with a rod shaped sample in horizontal configuration (WA - expansion

measurement unit, A - supporting unit, S - push rod, O - furnace, P - sample) measurement unit, A - supporting unit, S - push rod, O - furnace, P - sample)

In a furnace, the sample is placed on a sample holder. The sample holder should In a furnace, the sample is placed on a sample holder. The sample holder should allow the movement of the sample with minimum friction losses. Attached to the allow the movement of the sample with minimum friction losses. Attached to the sample the push rod is found. The push rod transfers the sample movement to the sample the push rod is found. The push rod transfers the sample movement to the expansion measurement unit. Inside of this unit, the movement is detected based on expansion measurement unit. Inside of this unit, the movement is detected based on electrical induction.

electrical induction.

The determination of the correct thermal expansion of the sample requires the The determination of the correct thermal expansion of the sample requires the measurement of the length change (rod + sample) but also the knowledge of the measurement of the length change (rod + sample) but also the knowledge of the thermal expansion coefficient of the transfer rod.

thermal expansion coefficient of the transfer rod.

Further requirements for a dilatometric measurement are: Further requirements for a dilatometric measurement are:

•• No forces or torques introduced by the setup or sample geometryNo forces or torques introduced by the setup or sample geometry

•• Sample holder must have same temperature as Sample holder must have same temperature as the sample throughout thethe sample throughout the experiment

experiment

2.2.1 2.2.1 TMA

TMA Equipment

Equipment

A schematic drawing of the available ex

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Figure 8: Overview NETZSCH TMA 402 Figure 8: Overview NETZSCH TMA 402

2.2.2 2.2.2 Application

Application Examples

Examples for

for TMA

TMA

The following examples you can look

The following examples you can look up at this hyperlink:up at this hyperlink:

http://www.netzsch-thermal-analysis.com/en/products/detail/pid,15,t,4.html

Polycrystalline Alumina (Al Polycrystalline Alumina (Al22OO33))

Figure 9 presents comparison of three test runs (lines) of a polycrystalline alumina Figure 9 presents comparison of three test runs (lines) of a polycrystalline alumina with the corresponding literature data (crosses) between room temperature and with the corresponding literature data (crosses) between room temperature and 1575°C. No visible deviations exist between the individual curves. Evaluation of the 1575°C. No visible deviations exist between the individual curves. Evaluation of the thermal expansion values at 500°C, 1000°C and 1500°C clearly shows that the thermal expansion values at 500°C, 1000°C and 1500°C clearly shows that the measurement results are within 1% of the corresponding literature data. The test measurement results are within 1% of the corresponding literature data. The test demonstrates the outstanding reproducibility and accuracy of the

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Figure 9: Polycrystalline Alumina Figure 9: Polycrystalline Alumina

Glass Glass

Coefficients of thermal expansion (CTE), glass transition temperatures and softening Coefficients of thermal expansion (CTE), glass transition temperatures and softening points are crucial parameters for the characterization of glass materials. Presented in points are crucial parameters for the characterization of glass materials. Presented in figure 10 there are three tests on same types of glass but from different batches. One figure 10 there are three tests on same types of glass but from different batches. One can see that the coefficients of thermal expansion are in good agreement within the can see that the coefficients of thermal expansion are in good agreement within the instrument’s uncertainty boundaries. The glass transition temperature and the instrument’s uncertainty boundaries. The glass transition temperature and the softening point of sample 3 (blue curve) show slightly lower values, indicating a softening point of sample 3 (blue curve) show slightly lower values, indicating a slightly different composition.

slightly different composition.

Figure 10: Glass Figure 10: Glass

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Sintering of Zircon Sintering of Zircon

During the production of high-tech ceramics, a ceramic powder is mixed with a binder During the production of high-tech ceramics, a ceramic powder is mixed with a binder and pressed to a so-called green body. By thermal treatment, the binder is removed and pressed to a so-called green body. By thermal treatment, the binder is removed (burned out) and the ceramic is sintered to the final part. In order to determine the (burned out) and the ceramic is sintered to the final part. In order to determine the quality of the final part, the binder burnout and sintering temperatures as well as the quality of the final part, the binder burnout and sintering temperatures as well as the shrinkage during sintering have to be known. These properties can be measured shrinkage during sintering have to be known. These properties can be measured quickly and easily using push rod dilatometry. Presented in the figure 11 are tests on quickly and easily using push rod dilatometry. Presented in the figure 11 are tests on an yttrium-stabilized zircon green body and on the sintered ceramic.

an yttrium-stabilized zircon green body and on the sintered ceramic.

Figure 11: Sintering of Zircon Figure 11: Sintering of Zircon

Production of Cordierite Ceramic Production of Cordierite Ceramic

Cordierite is a popular magnesia-alumina-silica ceramic used in various kinds of Cordierite is a popular magnesia-alumina-silica ceramic used in various kinds of industrial applications. It is used, for example, as a carrier for catalysts in the industrial applications. It is used, for example, as a carrier for catalysts in the automotive industry. During the production of this ceramic, various raw materials are automotive industry. During the production of this ceramic, various raw materials are ground and mixed to form a green body. During firing under oxidizing atmospheres, ground and mixed to form a green body. During firing under oxidizing atmospheres, the organic additives are burned out and the cordierite phase is formed at high the organic additives are burned out and the cordierite phase is formed at high temperatures.

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Figure 12: Heating in the production process of cordierite ceramic Figure 12: Heating in the production process of cordierite ceramic

3 3 Preparation

Preparation of

of the

the Experiment

Experiment

You should inform yourself about:

•• Definition of thermal analysisDefinition of thermal analysis

•• This definition included analysis proceduresThis definition included analysis procedures

•• Understanding of the working principle of DTA, TG and TMAUnderstanding of the working principle of DTA, TG and TMA

•• Examples of use for this methodsExamples of use for this methods

•• Possibilities of temperature measurement with different temperature regionsPossibilities of temperature measurement with different temperature regions Please also inform yourself about typical values of the thermal expansion coefficients Please also inform yourself about typical values of the thermal expansion coefficients of metals, glasses and synthetics.

of metals, glasses and synthetics.

Solve the problems listed below in advance of the experiment. Solve the problems listed below in advance of the experiment.

3.1 Problems

3.1.1 3.1.1 Which of the

Which of the following physical changes

following physical changes could NOT

could NOT be detected

be detected by

by

the thermogravimetry?

a)

a) Loss Loss of of moisturemoisture b) Sublimation b) Sublimation c) Melting c) Melting d)

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3.1.2 3.1.2 Which of the

Which of the following physical changes

following physical changes could NOT

could NOT be detected

be detected by

by

the thermogravimetry?

a) CaCO

a) CaCO33 + SO+ SO22  CaSOCaSO44 + CO+ CO22

b) CaCO

b) CaCO33 + SiO+ SiO22  CaSiOCaSiO33 + CO+ CO22

c) CaCO

c) CaCO33 + Na+ Na22SOSO44  CaSOCaSO44 + Na+ Na22COCO33

3.1.3 3.1.3 Which thermal

Which thermal effects can

effects can be visualised by

be visualised by DTA?

DTA?

a)

a) Loss Loss of of moisturemoisture b) Sublimation b) Sublimation c)

c) Desorption Desorption of of vapour vapour d)

d) 4FeO 4FeO + + OO22  2Fe2Fe22OO33

3.1.4 3.1.4 A sample of

A sample of polymer was analysed

polymer was analysed by simultaneous TG-DTA.

by simultaneous TG-DTA.

Which of the following thermal changes, that might occur, would

be detected by DTA and which by TG?

a)

a) Glass Glass transitiontransition b)

b) Plasticizer Plasticizer lossloss c)

c) Residual Residual curingcuring d) Crystallisation d) Crystallisation e) Melting

e) Melting f)

f) Oxidation Oxidation and and degradationdegradation

3.1.5 3.1.5 The decomposition

The decomposition of zinc

of zinc oxalate dehydrate

oxalate dehydrate (ZnC

(ZnC

22

O

44

*2H

22

O) was

shown by TG and DTA to occur in two stages with a loss of mass

of about 19% at 200°C and a total loss of 57% at 400°C. If we

suggest the reactions as described below, how could we identify

both gaseous and solid products?

a) ZnC

a) ZnC22OO44*2H*2H22OO ZnCZnC22OO44 + 2H+ 2H22OO

b) ZnC

b) ZnC22OO44 ZnO +CO +COZnO +CO +CO22

3.1.6 3.1.6 How much water

How much water and carbon dioxide

and carbon dioxide would result from

would result from the

the

decomposition of 25mg ZnC

22

O

44

*2H

22

O?

4 4 Useful

Useful hints

hints

General: Have a data storage device with you (e.g. USB - stick) to pick t

General: Have a data storage device with you (e.g. USB - stick) to pick t he electroniche electronic

data after the experiment. data after the experiment.

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4.1 DTA/TG

•• Weight the sample (powder) inside the crucible (depending on the density inWeight the sample (powder) inside the crucible (depending on the density in the range of 20 - 50mg)

the range of 20 - 50mg)

•• Prepare the reference material (AlPrepare the reference material (Al22OO33-powder) inside the reference crucible-powder) inside the reference crucible

•• Definition of the Definition of the measurement conditions (temperature region, heating rate,measurement conditions (temperature region, heating rate, temperature profile)

temperature profile)

•• Check, if a tare measurement (without sample) for the Check, if a tare measurement (without sample) for the temperature profiletemperature profile already exists

already exists

•• Check the device parameters:Check the device parameters:

o

o Cooling water onCooling water on o

o Inert gas supply Argon on (inside of the furnace)Inert gas supply Argon on (inside of the furnace) o

o Gas carrier (air, argon, nitrogen) for Gas carrier (air, argon, nitrogen) for the sample onthe sample on

•• PC input of the measurement parameters and start of the measurementPC input of the measurement parameters and start of the measurement

4.2 TMA

•• Estimate the chosen sample regarding to Estimate the chosen sample regarding to size, shape and homogeneitysize, shape and homogeneity

•• Definition of the Definition of the measurement conditions (temperature region, heating rate,measurement conditions (temperature region, heating rate, temperature profile)

temperature profile)

•• Check cooling water onCheck cooling water on

•• PC input of the measurement parameters and start of measurementPC input of the measurement parameters and start of measurement

5 5 Hints

Hints for

for a

a Correct

Correct Analysis

Analysis

During the discussion of the equipment setup, make notes on important constructive During the discussion of the equipment setup, make notes on important constructive details, which may guide you to the best measuring results. Which conditions have to details, which may guide you to the best measuring results. Which conditions have to be fulfilled?

be fulfilled?

5.1 DTA/TG

Plot the data of the DTA- and TGA-curve (transfer the data per mail or storage Plot the data of the DTA- and TGA-curve (transfer the data per mail or storage media)! Describe the observed effects between the single temperature regions and media)! Describe the observed effects between the single temperature regions and interpret them qualitatively! If it is possible, then analyse the TGA curve quantitatively interpret them qualitatively! If it is possible, then analyse the TGA curve quantitatively and compare it with the results of a t

and compare it with the results of a theoretical model or other references!heoretical model or other references!

5.2 TMA

Plot the length variation ∆l/l

Plot the length variation ∆l/l00 versus temperature (transfer the data per mail or versus temperature (transfer the data per mail or

storage media)! Evaluate the shape of the curve qualitatively! Consider particularly storage media)! Evaluate the shape of the curve qualitatively! Consider particularly any sudden changes of the slope. Indicate the linear thermal expansion coefficient in any sudden changes of the slope. Indicate the linear thermal expansion coefficient in selected temperature regions!

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6 Literature

Device producer: Device producer:

•• http://www.setaram.com/ (SETARAM Instrumentation)http://www.setaram.com/ (SETARAM Instrumentation)

•• http://www.netzsch-thermal-analysis.com/en/http://www.netzsch-thermal-analysis.com/en/home/ home/ (Netzsch Instruments)(Netzsch Instruments)

•• http://glo.mt.com/home (Mettler Toledo TA)http://glo.mt.com/home (Mettler Toledo TA)

•• http://www.perkinelmer.com/ (PerkinElmer Instruments)http://www.perkinelmer.com/ (PerkinElmer Instruments)

•• http://www.linseis.de/html_en/thermal/thermal_start.php (Linseis)http://www.linseis.de/html_en/thermal/thermal_start.php (Linseis)

•• http://www.tainstruments.com/ (TA Instruments)http://www.tainstruments.com/ (TA Instruments)

•• http://www.shimadzu.com/products/labhttp://www.shimadzu.com/products/lab/thermal/index.html /thermal/index.html (SHIMADZU)(SHIMADZU)

•• http://www.baehr-thermo.de/uk/index_ukhttp://www.baehr-thermo.de/uk/index_uk.html (Bähr .html (Bähr Thermoanalyse GmbH)Thermoanalyse GmbH) Available at the FH library:

Available at the FH library:

•• Methoden der thermischen Analyse / Wolfgang F. Hemminger. - Berlin [u.a.] :Methoden der thermischen Analyse / Wolfgang F. Hemminger. - Berlin [u.a.] : Springer, 1989

Springer, 1989

•• Grundlagen der Kalorimetrie : mit 6 Tab. / WGrundlagen der Kalorimetrie : mit 6 Tab. / Wolfgang Hemminger. - Berlin :olfgang Hemminger. - Berlin : Akad.-Verl, 1980

Akad.-Verl, 1980

•• Theory of calorimetry / Wojciech Zielenkiewicz. - Dordrecht [u.a.] : Kluwer,Theory of calorimetry / Wojciech Zielenkiewicz. - Dordrecht [u.a.] : Kluwer, 2002

2002

•• Differential scanning calorimetry : an introduction for practitioners ; with 13Differential scanning calorimetry : an introduction for practitioners ; with 13 tables / Günther Walther Heinrich Höhne. - Berlin [u.a.]

tables / Günther Walther Heinrich Höhne. - Berlin [u.a.] : Springer, 1996: Springer, 1996

•• Modulation calorimetry : theory and applications ; with 27 tables / YaakovModulation calorimetry : theory and applications ; with 27 tables / Yaakov Kraftmakher. - Berlin [u.a.] : Springer, 2004

Kraftmakher. - Berlin [u.a.] : Springer, 2004

•• Thermal analysis : a revision 5.0 tutorial / Thermal analysis : a revision 5.0 tutorial / Swanson Analysis SysSwanson Analysis Systems. -tems. -Houston, PA :

Houston, PA : Swanson Analysis Systems, c1992Swanson Analysis Systems, c1992

•• Low thermal expansion glass ceramics : with 18 tables / Hans Bach. - BerlinLow thermal expansion glass ceramics : with 18 tables / Hans Bach. - Berlin [u.a.] : Springer, 1995