High-Pressure Differential Scanning Calorimetry

Transcription

1 Analyzing & Testing High-Pressure Differential Scanning Calorimetry Up to 15 MPa DSC 204 HP

2 DSC 204 HP Phoenix Highlights The versatile high-pressure DSC 204 HP Phoenix is part of our successful 200 series. This also includes the heat flux Differential scanning calorimeter DSC 204 F1 Phoenix and DSC 200 F3 Maia, the Thermomicrobalances TG 209 F1 Libra and TG 209 F3 Tarsus, the Thermomechanical analyzer TMA 402 F1/F3 Hyperion, the Dynamic mechanical analyzer DMA 242 E Artemis and the Dielectric analyzer series DEA 288 Epsilon. The DSC 204 HP Phoenix can also be operated simultaneously with hightemperature instruments of the 400 series in a multimoduling mode. Accessories Electronic pressure Electronic gas Adapters for Vacuum pump CC 200 controller flow controller various gases L for controlled cooling with liquid nitrogen Calibration kit for temperature and sensitivity 2

3 Technical Data Wide pressure range: vacuum MPa (2140 psi) Exact pressure adjustment Pressure accuracy ± 0,075 MPa Temperature range: -150 C to 600 C (Temperature range is pressure and gas type dependent: -150 C to 600 C (at 1 bar) -90 C to 600 C (at 50 bar) -50 C to 450 C (at 150 bar)) inert (N 2, He, Ar) Heating rates: 0.01 K/min to 100 K/min Measurements in different atmospheres reducing (H 2 ) oxidizing (O 2, air) other gas types on request Exact gas flow regulation (up to 500 ml/min) Exchangeable sensor plate Allows measurements in according with ASTM D5483, D6186, E1782, E1858, E2009 Evaluation of oxidative-induction time (OIT) included thermostat hose connection (outlet) knurled nut thermostated lid sensor thermostat hose connection (inlet) LN 2 cooling DSC 204 HP Phoenix measuring part for the connection of the LN 2 colling device 3

4 DSC 204 HP Phoenix Maximum Flexibility regarding Gas Types, Flow Rates and Pressures Numerous physical processes and chemical reactions are influenced by atmospheric pressure. In practice it is therefore often necessary to conduct DSC measurements under pressure. With the high-pressure DSC 204 HP Phoenix thermal effects of a sample can be analyzed in the pressure range of vacuum to 15 MPa (approx psi) from -150 C to 600 C. The reliable CC 200 L control cooling system is available for this temperature range. Measurements in different gas atmospheres such as O 2, N 2, Ar, He, H 2, CO 2 and CH 4 are no problem in the robust measuring cell. The sample atmosphere is either static or dynamic. The electronic pressure control device as well as exact regulation of the purge gas flow are the main features for outstanding accuracy and reproducibility of the measurements. Of course, the DSC 204 HP Phoenix meets all safety requirements which are required for measurements under pressure. An array of crucibles in various sizes, shapes and materials for different applications is also available. Possible Operation Modes* Mode I Mode II Mode III Mode IV Mode V Measurement under static gas atmosphere with defined gas pressure (up to 15 MPa) Measurement under dynamic gas atmosphere with defined pressure and defined gas flow Use of an inert gas (e.g. Ar) to establish a defined pressure and measurement under dynamic reaction gas atmosphere (e.g. O 2 at 100 ml/min) Measurement in static or dynamic gas mixture Measurement under adjustable reduced pressure * Depending on pressure device 4

5 Wide-Ranging Applications Determination of vapor pressure and evaporation heat (ASTM E1782) Separation of reactions with overlapped evaporation Measurement of adsorption and desorption, e.g. on metallic compounds Oxidation stability of oils, fats and lubricants (ASTM E1858, ASTM D6186, ASTM E2009, ASTM D5483) Curing of thermosets, e.g. phenolic resin Vulcanization of elastomers Hydration of unsaturated fatty acids DSC measurements under ambient pressure can, of course, also be conducted with the DSC 204 HP Phoenix and even under reduced pressure 5

6 Wide-ranging Applications Versatile High-Pressure DSC Synetic Oil Oxidation behavior of a stabilized synthetic oil (sample mass mg) at 2 C/min in oxygen (100 ml/min) at defined pressures. With increasing oxygen pressure, oxidation starts earlier, i.e. at a lower temperature. Precise Pressure Control Precision of the Pressure Control: the pressure variations detected during the measurement ( MPa/ bar) are 100 times smaller than is prescribed by ASTM D6186, influences of the pressure on the DSC signal (e.g. noise) can therefore be minimized. DSC / mw/mg tolerated pressure deviation according to ASTM /- 0.2 MPa +/- 2 bar measured pressure deviation +/ MPa +/ bar Fläche: J/g Peak*: C Onset: C Temperature / C pressure / bar

7 Curing Behavior of Phenolic Resins lot A lot B Partial area evaluation of the curing peak of two phenolic resin lots (A, B) at a practical pressure of 9 MPa in an inert gas atmosphere at 10 C/min (sample mass 10.5 mg, heating rate 10 C/min). Hydration of a Metal Catalyst Exothermal hydration of a metal catalyst at 7 MPa in a pure hydrogen atmosphere (sample mass 6.09 mg, heating rate 10 C/min). 7

8 The NETZSCH Group is a mid-sized, family-owned German company engaging in the manufacture of machinery and instrumentation with worldwide production, sales, and service branches. The three Business Units Analyzing & Testing, Grinding & Dispersing and Pumps & Systems provide tailored solutions for highest-level needs. Over 3,000 employees at 210 sales and production centers in 35 countries across the globe guarantee that expert service is never far from our customers. When it comes to Thermal Analysis, Calorimetry (adiabatic & reaction) and the determination of Thermophysical Properties, NETZSCH has it covered. Our 50 years of applications experience, broad state-of-the-art product line and comprehensive service offerings ensure that our solutions will not only meet your every requirement but also exceed your every expectation. NETZSCH-Gerätebau GmbH Wittelsbacherstraße Selb Germany Tel.: Fax: at@netzsch.com NGB DSC 204 HP Phoenix EN 0815 NWS Technical specifications are subject to change.