Oprogramowanie do analizy termicznej NETZSCH Proteus^®® 

DSC-BeFlat^® (beginning with software version 6.1) and Advanced DSC-BeFlat^® (beginning with the 7^th generation of the NETZSCH Proteus^® software) compensate for all influences on DSC baselines which can be related to thermal asymmetries of the DSC sensor. This results in a minimal amount of curvature in the baseline, in the μW range. TGA-BeFlat^® automatically corrects instrument and buoyancy effects in the TG 209 F1 Libra^® and STA 449 F3 /F5 Jupiter^® (for STA: Proteus^® version 6.1, SiC furnace, appropriate sample carriers) and thus eliminates the need for buoyancy correction measurements.

The “specific heat” software package allows for fast and accurate determination of the Specific Heat Capacity (cp)Heat capacity is a material-specific physical quantity, determined by the amount of heat supplied to specimen, divided by the resulting temperature increase. The specific heat capacity is related to a unit mass of the specimen.specific heat capacity Specific Heat Capacity (cp)Heat capacity is a material-specific physical quantity, determined by the amount of heat supplied to specimen, divided by the resulting temperature increase. The specific heat capacity is related to a unit mass of the specimen.cp (at constant pressure) on solids, powders and liquids in accordance with standardized techniques (e.g., DIN 51007, ASTM E1269, ISO 11357) using DSC or STA instruments. In addition, this software can also be employed to carry out heat-flow calibrations with, for example, sapphire as the standard material.

The software add-on for conducting measurements with rate-controlled temperature management (mass-change-controlled TGA, i.e., RCM; and shrinkage-rate-controlled dilatometry, i.e., Rate-Controlled Sintering (RCS)The properties of sintered products, such as density or particle size distribution, are determined by the sintering conditions (temperature, atmosphere, etc.) and especially by the sintering rates. RCS) is well suited for increasing the resolution of superimposed effects and enhancing sample compaction for SinteringSintering is a production process for forming a mechanically strong body out of a ceramic or metallic powder. sintering processes.

Provided that the sample thermocouple is in close proximity to the sample (as is the case with NETZSCH thermobalances and dilatometers), a DTA signal can be calculated and recorded from the difference between the temperature of the sample and the temperature of the program. This allows for additional information on EgzotermicznyA sample transition or a reaction is exothermic if heat is generated.exothermal or endothermal processes to be gathered during the course of TGA or DIL measurements. Moreover, the c-DTA^® software can also be employed for the temperature calibration of thermobalances or dilatometers.

When applying temperature modulation, which is available for the TG 209 F1 Libra^®, TG 209 F3 Tarsus^®, DSC 214 Polyma, DSC 204 F1 Phoenix^®, DSC 3500 Sirius, DSC 404 F1 Pegasus^®, STA 449 F1 Jupiter^® (TM-DSC), STA 449 F3 Jupiter^® (TM-DSC), DIL 402 Expedis Select, DIL 402 Expedis Supreme and TMA 402 F1 Hyperion^® (for TMA and DIL, beginning with the 7^th generation of the Proteus^® software), the linear heating rate is superimposed by a sinusoidal temperature change. This makes it possible to deconstruct the signals into reversing and non-reversing parts (DSC, DIL, TMA) and thereby separate overlapping effects ‒ for example, glass transitions and RelaxationWhen a constant strain is applied to a rubber compound, the force necessary to maintain that strain is not constant but decreases with time; this behavior is known as stress relaxation. The process responsible for stress relaxation can be physical or chemical, and under normal conditions, both will occur at the same time. relaxation peaks (DSC) or thermal expansions and SinteringSintering is a production process for forming a mechanically strong body out of a ceramic or metallic powder. sintering steps (DIL, TMA) ‒ and to calculate activation energy(ies) from a measurement (TGA).

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  TG 209 F1 Libra^®
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  TG 209 F3 Tarsus^®
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  DSC 214 Polyma
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  DSC 204 F1 Phoenix^®
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  DSC 3500 Sirius
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  DSC 404 F1 Pegasus^®
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  STA 449 F1 Jupiter^®
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  STA 449 F3 Jupiter^®
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  DIL 402 Expedis Select & Supreme
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  TMA 402 F1 /F3 Hyperion^®

For crystalline substances with known molar mass, Purity Determination serves to determine the percentage of eutectic impurities on the basis of the Van ’t Hoff equation. The DSC melting peak is evaluated for each.

Purity Determination is a program for determining the purity of a material through analysis of the DSC melting peak.

The following features set this program apart from the known solutions as well as from ASTM E 928:

 

• determination of purity using the VAN'T HOFF equation without a mathematical approximation. Thus, the range of application can be extended beyond the threshold of impurity of 5 mol%. The estimated upper boundary could be 10 mol%
• adjustment of the thermal resistance in such a way that the nominal value is calculated for a substance with a known degree of purity. This yields not only a high degree of precision in the high purity range, but substances of a lower purity can be used to determine the thermal resistance

The names and the molar masses of the substances used are stored in a table and are available after every start. ASCII-Files serve as the general interface for the transfer of data. The data can be corrected using three different baselines:

• linear,
• horizontal area-proportional and
• tangential area-proportional.

The non-linear regression automatically links with the baseline determination. The required initial parameters are prepared in a starting calculation.

To increase reliability, the results of several measurements can be averaged and the mean printed out with the standard deviation.

These errors are avoided in NETZSCH Purity Determination by using a non-linear regression routine.

The following are listed in the results:

The results can be printed out with the graph.

This extra package allows for the calculation of the density change in a material (with the initial density as a reference value) during a DIL or TMA investigation. Even measurements that finish in a molten state (in a container of sapphire, graphite or quartz) can be evaluated this way. Below the Melting Temperatures and EnthalpiesThe enthalpy of fusion of a substance, also known as latent heat, is a measure of the energy input, typically heat, which is necessary to convert a substance from solid to liquid state. The melting point of a substance is the temperature at which it changes state from solid (crystalline) to liquid (isotropic melt).melting temperature, the density can be calculated based on an isotropic material; above the Melting Temperatures and EnthalpiesThe enthalpy of fusion of a substance, also known as latent heat, is a measure of the energy input, typically heat, which is necessary to convert a substance from solid to liquid state. The melting point of a substance is the temperature at which it changes state from solid (crystalline) to liquid (isotropic melt).melting temperature, all influences of the container and sample preparation are taken into consideration.

The program Density Determination serves in the determination of the temperature-dependent density of solid samples beyond the Melting Temperatures and EnthalpiesThe enthalpy of fusion of a substance, also known as latent heat, is a measure of the energy input, typically heat, which is necessary to convert a substance from solid to liquid state. The melting point of a substance is the temperature at which it changes state from solid (crystalline) to liquid (isotropic melt).melting temperature. The calculations are based on dilatometer measurements carried out in a container stable against temperature (sapphire, graphite, quartz glass, etc.). During melting, the sample completely fills the container. Therefore, with correct sample preparation, there is a monotonic transition of the dL/L0 curve into the liquidus range.

This software is of interest for all researchers who require a more accurate determination of Phase TransitionsThe term phase transition (or phase change) is most commonly used to describe transitions between the solid, liquid and gaseous states.phase transitions. The data should also be of interest to designers who work in the area of casting technology. It is absolutely critical for analyses in which the density is required beyond the Melting Temperatures and EnthalpiesThe enthalpy of fusion of a substance, also known as latent heat, is a measure of the energy input, typically heat, which is necessary to convert a substance from solid to liquid state. The melting point of a substance is the temperature at which it changes state from solid (crystalline) to liquid (isotropic melt).melting point (e.g. determination of the Thermal DiffusivityThermal diffusivity (a with the unit mm2/s) is a material-specific property for characterizing unsteady heat conduction. This value describes how quickly a material reacts to a change in temperature.thermal diffusivity by means of laser flash analysis).

However, if the sample diameter is smaller than the inside diameter of the container, the slope of the dL/L0 curve decreases with the start of melting. If the sample diameter is considerably smaller, a drop in the curve can even be seen. For technical reasons, it is often impossible or too costly to prepare perfect samples. In order to obtain correct results for such samples as well, the almost linear segment of the liquidus curve (red), indicated by the two markers ( < ) is approximated by a polynomial and this area is extended to the vertical cursor, which characterizes the start of the melting process.

The approximated curve, together with the red part of the liquidus curve that follows, is shifted such that it begins at the point of intersection of the vertical cursor with the solidus curve (pink). Thus, errors which result from the limited precision of the sample preparation are corrected to a great extent.

In the DSC 204 F1 Phoenix^®, DSC 214 Polyma and DSC 3500 Sirius, the AutoCooling function allows for automatic recognition of the connected cooling system and, as a resource-saving measure, activates it only when required.

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  DSC 214 Polyma
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  DSC 204 F1 Phoenix^®
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  DSC 3500 Sirius

AutoCalibration allows for the automatic generation of calibration curves for the DSC 204 F1 Phoenix^®, DSC 214 Polyma, DSC 3500 Sirius, TG 209 F1 Libra^® and TG 209 F3 Tarsus^®. Current calibrations are automatically loaded with consideration to the selected measurement conditions and checked for their period of validity.

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  TG 209 F1 Libra^®
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  TG 209 F3 Tarsus^®
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  DSC 214 Polyma
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  DSC 204 F1 Phoenix^®
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  DSC 3500 Sirius