Setaram THEMYS HP High-Pressure Thermogravimetric Analyzer
| Brand | Setaram |
|---|---|
| Origin | France |
| Model | THEMYS HP |
| Temperature Range | Ambient to 1200 °C |
| Pressure Range | Up to 150 bar |
| Sample Capacity | 35 g |
| Balance Sensitivity | 0.0023 µg |
| Baseline Drift | ±200 µg |
| Heating/Cooling Rate | 0.01–100 K/min |
| Crucible Volume | 1300 µL |
| Gas Configuration | 3-channel mass flow controlled (2 MFCs standard with auxiliary gas option) |
| Vacuum Capability | <1 mbar (primary), <5×10⁻² mbar (forced) |
| Safety Compliance | EU PED 2014/68/EU, Group 2 gases |
Overview
The Setaram THEMYS HP High-Pressure Thermogravimetric Analyzer is an engineered platform for simultaneous, real-time monitoring of mass change and thermal behavior under rigorously controlled high-temperature and high-pressure atmospheres. Based on the fundamental principle of thermogravimetry—measuring sample mass as a function of temperature or time under defined gas environments—the THEMYS HP extends conventional TGA capabilities into extreme operational domains. Its monolithic furnace-balance architecture enables stable operation up to 1200 °C and 150 bar, eliminating thermal lag and mechanical hysteresis associated with modular or multi-furnace systems. The system employs a suspended symmetric microbalance operating on electromagnetic force compensation, delivering sub-microgram resolution and exceptional long-term stability. Temperature control is achieved via a platinum-based heating element housed within an alumina protection tube, with a calibrated Type S thermocouple positioned directly beneath the sample crucible for precise in-situ measurement. This configuration ensures traceable, reproducible thermal profiles essential for kinetic modeling and reaction mechanism validation.
Key Features
- Integrated high-pressure furnace and suspension balance unit—single-zone design eliminates inter-chamber thermal gradients and pressure transients
- Dual back-pressure regulation system enabling seamless transition between low-pressure (1–6 bar) and high-pressure (6–150 bar) regimes with <±0.1 bar setpoint accuracy
- Electromagnetic force-compensated balance with 0.0023 µg resolution and ±200 µg baseline drift over full temperature ramp (ambient to 1200 °C)
- Programmable heating/cooling rates from 0.01 to 100 K/min, supporting both slow kinetic studies and rapid thermal screening
- Triple-gas manifold with two independent mass flow controllers (MFCs), configurable for main carrier gas plus auxiliary reactive or inert gas injection
- Two-stage vacuum system: primary roughing (<1 mbar) and forced high-vacuum (<5×10⁻² mbar), compatible with degassing, inert purging, and low-pO₂ oxidation studies
- Comprehensive safety architecture compliant with EU Pressure Equipment Directive 2014/68/EU (Group 2 non-flammable, non-toxic gases), including four strategically located relief valves and interlocked furnace lid actuation below 1.2 bar
Sample Compatibility & Compliance
THEMYS HP accommodates solid samples up to 35 g in standard 1300 µL alumina or graphite crucibles, supporting heterogeneous catalytic solids, metal alloys, coal char, biomass pellets, and ceramic precursors. The system is routinely deployed in laboratories adhering to ASTM E1131, ISO 11358, and USP for thermal decomposition profiling, oxidation kinetics, and pyrolysis/gasification pathway analysis. Its pressure-tight design and audit-ready event logging satisfy GLP and GMP requirements for regulated R&D, particularly in energy materials development and metallurgical process simulation. All firmware and hardware interfaces conform to IEC 61508 functional safety standards for critical instrumentation.
Software & Data Management
Acquisition and analysis are managed through Setaram’s CALISTO software suite, which supports multi-parameter synchronization (mass, temperature, pressure, gas flow, derivative signals) with timestamped metadata embedding. Data export complies with ASTM E1447 and ISO/IEC 17025 traceability requirements—including instrument calibration history, operator ID, environmental logs, and electronic signatures. Audit trail functionality meets FDA 21 CFR Part 11 criteria for secure, immutable recordkeeping. Customizable report templates support automated generation of Arrhenius plots, DTG peak deconvolution, and pressure-dependent activation energy maps using integrated Kissinger-Akahira-Sunose (KAS) and Ozawa-Flynn-Wall (OFW) modules.
Applications
- Kinetic modeling of coal, biomass, or municipal solid waste gasification under syngas-relevant pressures (20–100 bar) and temperatures (700–1100 °C)
- Oxidation resistance evaluation of Ni-based superalloys and refractory metals at elevated pO₂ and T, simulating turbine blade service conditions
- Decomposition thermodynamics of metal-organic frameworks (MOFs) and hydrogen storage materials under controlled H₂ or NH₃ partial pressures
- Catalyst deactivation studies involving coke formation, sintering, or sulfur poisoning under realistic reactor pressure profiles
- Thermal stability assessment of energetic materials and propellants under confinement scenarios
- Carbon capture material regeneration cycles involving CO₂ adsorption/desorption under variable pCO₂ and T
FAQ
What pressure ranges does the THEMYS HP support, and how is pressure stability maintained?
The system operates continuously from ambient pressure up to 150 bar using a dual-range back-pressure regulator. Stability is maintained via closed-loop feedback between pressure transducers and proportional control valves, achieving ±0.1 bar deviation during dynamic temperature ramps.
Can the THEMYS HP perform simultaneous DTA or DSC measurements?
No—the THEMYS HP is a dedicated high-pressure TGA platform. For combined thermal analysis, Setaram offers the LVP DSC or the SETSYS Evolution series with optional high-pressure cells.
Is vacuum capability integrated, and what level is achievable?
Yes—integrated two-stage vacuum pumping achieves <1 mbar (rough vacuum) and <5×10⁻² mbar (high vacuum) with active purge control, enabling degassing, moisture removal, and low-oxygen oxidation studies.
How is sample temperature accuracy ensured at high pressure?
A calibrated Type S thermocouple is mounted directly beneath the crucible base, shielded by the same alumina tube enclosing the heater. This minimizes radiative and convective error, yielding ±1.5 °C accuracy across the full range per NIST-traceable calibration.
Does the system support automated sequence runs for unattended operation?
Yes—CALISTO supports batch-mode execution of up to 99 user-defined methods, including auto-load/unload triggers, pressure ramping synchronized with temperature profiles, and conditional termination based on mass loss thresholds.
