Description
To the point
Special field of application: Nuclear materials
Since the 1950s nuclear energy is the worldwide most important energy source around the world. With their advantage of clean and cheap power supply, core reactors were undergoing a continuous global improvement during the last 50 years. Meanwhile the reactors of the 4th generation such as very high temperature reactors (VHTR) or sodium cooled fast reactors (SFR) as well as the unique molten salt reactor (MSR) are currently under development and will be the future for nuclear energy.
Due to the research that is done in that field, there is a need of analytical equipment and especially instruments for thermal analysis. Of course these special applications and safety requirements need a lot of modifications of the standard devices, that makes Linseis become the worldwide leader in thermal analysis of nuclear materials as we are the most flexible and most experienced player on that market.
Thermal analysis of nuclear materials
In case of any of the mentioned dangers, it gets tricky to operate the system and also to do service and maintenance.
To avoid such problems, the following points must be solved:
- The system must be able to be controlled from a safe place (other room, glovebox, hood)
- All critical parts that have to be accessed for maintenance must be accessible
- Samples must be placed in the system and removed from the system somehow
- All components that get in touch with corrosive substances must be able to withstand them
Calorimetry and thermogravimetric analysis of radioactive samples
The STA – Principle of Thermogravimetric Measurement
The standard DSC is available in versions up to 1000°C as well as up to 1750°C. Both versions can be also used as a combined unit with a balance build in as STA or as a stand-alone balance.
For radioactive samples there is also a version that has a separated control unit and can be put into a glovebox or fume hood. For the easy handling, all unnecessary cover parts are removed and all service and settings can be done waring gloves.
Principle of Tg measurement
Principle of DSC mesurement
Contacting area between thermocouple and crucible
- Differential Scanning Calorimetry (DSC) is most popular thermal analysis technique
- DSC measures endothermic and exothermic transitions as a function of temperature
Endothermic heat flows into a sample
Exothermic heat flows out of the sample
Setup for “HOT CELL” STA
„HOT“ environment
The measurement unit can be placed in „hot“ environment. All plastic components and critical components are removed or replaced by special materials.
Normal environment
All electronic boards, controllers, chiller and gas controls are separated and can be placed outside the „hot“ area and are easily accessible for service and maintenance.
Unique features
High-resolution DTA
(3 thermocouples)
Large temperature range
Shielded DTA
for corrosive
applications
Vacuum and controlled atmosphere
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Specifications
MODEL | STA PT 1600 |
|---|---|
| Temperature range: | -150°C up to 500 / 700 / 1000°C RT up to 1000 / 1400 / 1600 / 1750 / 2000 / 2400°C |
| Vacuum: | 10-2 mbar (depending on the vacuum pump) |
| Pressure: | Up to 5 bar (optional) |
| Heating speed: | 0.01 up to 100K/min |
| Temperature precision: | 0.001°C |
| Sample robot: | Optional 42 |
TG | 1 | 2 | 3 |
|---|---|---|---|
| Resolution: | 0.025 μg | 0.1 μg | 0.1 μg |
| Sample weight: | The scale can recognize the weight automatically | The scales can recognize the weight automatically | The scales can recognize the weight automatically |
| Measuring range: | 25 / 2500 mg | 25 / 2500 mg | 35000 mg |
DSC | 1 | 2 | 3 |
|---|---|---|---|
| DSC sensors: | E /K / S / B / C (C = DTA only) | E /K / S / B / C (C = DTA only) | E /K / S / B / C (C = DTA only) |
| DSC resolution: | 0.3 / 0.4 / 1 / 1.2 μW | 0.3 / 0.4 / 1 / 1.2 μW | 0.3 / 0.4 / 1 / 1.2 μW |
| Calorimetry sensitivity: | ca. 4 / 6 / 17.6 / 22.5 μW | ca. 4 / 6 / 17.6 / 22.5 μW | ca. 4 / 6 / 17.6 / 22.5 μW |
DTA | 1 | 2 | 3 |
|---|---|---|---|
| DTA resolution: | 0.03 nV | 0.03 nV | 0.03 nV |
| Sensitivity: | 1.5 μV / mW | 1.5 μV / mW | 1.5 μV / mW |
| DTA measuring ranges: | 250 / 2500 μV | 250 / 2500 μV | 250 / 2500 μV |
Furnace program
TEMPERATURE | TYPE | ELEMENT | ATMOSPHERE | TC-TYPE |
|---|---|---|---|---|
| -70°C – 400°C | L81/24/RCF | Hanging only, Intracooler / Kanthal | inert, oxide, red, vac. | K |
| -150°C – 500°C | L81/24/500 | Kanthal | inert, oxide, red, vac. | K |
| -150°C – 700°C | L81/24/700 | Kanthal | inert, oxide, red, vac. | K |
| -150°C – 1000°C | L81/24/1000 | Kanthal | inert, oxide, red, vac. | K |
| RT – 1000°C | L81/20AC | SiC | inert, oxide, red, vac. | K |
| RT – 1600°C | L81/20AC | SiC | inert, oxide, red, vac. | S |
| RT – 1750°C | L81/250 | MoSi2 | inert, oxide, vac. | B |
| RT – 2000°C | L81/20/G/2000 | graphite | inert, red | C |
| RT – 2400°C | L81/20/G/2400 | graphite | inert, red | Pyrometer |
| RT – 2800°C | L81/20/G/2800 | graphite | inert, red | Pyrometer |
| RT – 2400°C | L81/20/T | Tungsten | inert, red | C |
| RT – 1000°C | L81/200 | Glow igniter | inert, oxide, red, vac. | S/K |
Software
Making values visible and comparable
All LINSEIS thermoanalytical devices are software-controlled.
The individual software modules run exclusively under Microsoft® Windows® operating systems.
The complete software consists of 3 modules: temperature control, data acquisition and data evaluation.
The Windows® software contains all the essential functions for preparing, carrying out and evaluating a thermoanalytical measurement.
Thanks to our specialists and application experts, LINSEIS was able to develop a comprehensive, easy-to-understand and user-friendly software.
Features software
- Program suitable for text editing
- Data backup in the event of a power failure
- Thermocouple breakage protection
- Repeat measurements with minimal
parameter input - Evaluation of the current measurement
- Curve comparison up to 50 curves
- Saving and exporting evaluations
- Export and import of ASCII data
- Data export to MS Excel
- Multi-method analysis (DSC TG, TMA, DIL, etc.)
- Zoom function
- 1 and 2 Derivation
- Curve arithmetic
- Statistical evaluation package
- Automatic calibration
- Optional kinetics and service life prediction
- Software packages
TG features:
- Mass change in % and mg
- Rate-controlled mass loss (RCML)
- Evaluation of the mass loss
- Residual mass evaluation
- “Notes on dynamic TGA measurement” (optional, chargeable service)
HDSC features:
- Glass transition temperature
- Complex peak evaluation
- Multi-point calibration for sample temperature
- Multi-point calibration for the enthalpy change
- Cp calibration for the heat flow
- Signal-controlled measuring methods
Measuring system
The LINSEIS Thermal Library software package is an option for the well-known, user-friendly LINSEIS Platinum evaluation software, which is integrated in almost all our devices.
The Thermal Library allows you to compare the complete curves with a database containing thousands of references and standard materials in just 1-2 seconds.
Multi-instrument
All LINSEIS instruments DSC, DIL, STA, HFM, LFA, etc. can be controlled via a software template.
Multilingual
Our software is available in many different user-interchangeable languages, such as: English, Spanish, French, German, Chinese, Korean, Japanese, etc.
Report generator
Convenient template selection for creating individual measurement reports.
Multi-user
The administrator can set up different user levels with different rights to operate the device.
An optional log file is also available.
Kinetic software
Kinetic analysis of DSC, DTA, TGA data to investigate the thermal behavior of raw materials and products.
Database
The state-of-the-art database enables simple data management with up to 1000 data records.
Applications
Figure 1 shows the results of the measurement. The blue curve represents the mass loss, and the red curve represents the DSC signal.
The first peak in the DSC signal corresponds to the melting of the sample. The onset of the melting peak is at 46°C.
After complete melting of the sample, a second endothermic peak emerges with an onset at 141°C. The TG signal exhibits a weight loss of 32% in this temperature range, indicating the dehydration of calcium nitrate tetrahydrate to form solid anhydrous salt.
During the isothermal hold at 180°C, the sample undergoes no further changes, indicating that this temperature is ideal for drying the salt and obtaining the anhydrous salt.
Upon reheating to 541°C, an endothermic peak is observed, corresponding to the melting of the anhydrous salt. However, the TG signal shows a weight loss, suggesting decomposition of the salt upon melting. Therefore, the enthalpy of fusion and heat capacity of the molten anhydrous salt cannot be directly measured.
However, this can be achieved through further TG-DSC measurements of salt mixtures. Calcium nitrate needs to be mixed with lithium, sodium, or potassium nitrate at different mole percentages. From the DSC melting peaks of the mixtures, the enthalpies of fusion can be determined. The enthalpy of fusion of pure calcium nitrate can then be calculated by extrapolating to a mole percentage of 100% relative to calcium nitrate.
The same procedure is employed to measure the heat capacity of the molten anhydrous calcium nitrate.
Well informed
