Temperature Programmed Desorption, Reduction, Oxidation and Pulse Chemisorption

By Thermal Conductivity Detector

TPDRO 1100

The TPDRO 1100 is a new concept instrument designed to the characterization of heterogeneous supported catalysts and reactive solids. Full automation by computer control and high accuracy detection, make it ideal for quality control and basic research applications. The TPDRO 1100 can perform unattended and reproducible catalysts activation (pre-treatment), TPD, TPR, TPO and pulse chemisorption analyses.

The "heart" of the system is a special reactor that can be sealed from the external environment. Catalysts, after the sample activation, can be stored without time limits under a suitable inert gas atmosphere. The complete closed reactor with the activated sample can be therefore transferred. The TPDRO 1100 features two independent reactor connections: one is used for catalyst pre-treatment and the other for the analysis. Thanks to the possibility of moving the reactor, the operator can save a lot of valuable time performing simultaneously and independently the selected activation procedure on one catalyst and the analytical cycle on a second catalyst. The TPDRO 1100 permits to increase the number of measurements per day because the pre-treatment procedures very often require more time than the analysis itself. Finally, dedicated software controls in real time the activation steps, the analytical cycle and contains routines for data processing (baseline subtraction, integration, reporting, etc.).

Analytical Performance

Features/Benefits

  • Simultaneous sample preparation and analysis on two different samples

  • Special shut-off reactor

  • High sensitivity TCD detector

  • Single carrier line passing through TCD reference/analysis filaments

  • Two separate independent anti-magnetic ovens

  • Ovens fast cooling by compressed air

  • High precision mass flow controller

  • Corrosion resistant plumbing and valves

  • Special design loop valve for pulse chemisorption

  • "Zero Shutter Volume" loop micro-valves

  • Type K thermocouple, 0.5 mm located inside the catalyst bed

  • Reactor thermocouple protected by a quartz shield

  • Easy connection to other detectors (i.e. mass spectrometer)

  • Increases productivity in terms of complete analyses per day

  • Activated catalysts can be moved in inert gas storage and/or pre-treated in other equipment
  • Permits to analyze small amount of sample avoiding the risk of re-adsorption phenomena

  • Increases baseline stability and avoids baseline drift

  • Reduce dramatically baseline oscillation and drift during temperature increase with polar carrier gases

  • Shortens dead times between two sequentialruns

  • Shortens the TCD stabilization time before the analysis start (average of 10 minutes)

  • For applications requiring corrosive gases

  • Permits to inject small doses of reactive gas (from 20 µL)

  • Eliminates the baseline jump before the peaks detection for precise and easy integration

  • Detects the real sample temperature during the analysis. Permits the immediate detection of temperature deviations in case of endo or eso-thermal reactions

  • Avoids chemical reactions between the carrier and the thermocouple

  • Increases the analytical performances

Instrument control and data processing for the TPDRO 1100

The TPDRO 1100 is connected to the computer through a serial communication cable for what concerns the instrument control. A 16 bit A/D converter installed in the PC performs the data acquisition. The acquisition card collects the signals of the TCD detector and of the thermocouple which is fixed in the reactor (catalyst bed temperature).

The TPDRO is completely computer control. Manual operations are also possible by an electronic keyboard and display installed in the instrument front panel. Software has been developed under Windows 95/NT/98 ® operative system.