Syrris Application Note: Analysing Endotherms using Atlas

Key features of the ATLAS Potassium:

• Quick change vessel: The oil drain unit, jacketed vessel clamp and quick oil connectors allow vessels to be changed in under a minute.
• Easy to use: No tools required, twist and click control knob, large display and intuitive.
• Full data capture: Data such as temperatures and stirrer speed is logged in a .csv file and can be downloaded to a USB stick.
• Easy to upgrade: A wide range of accessories are available including vessels, stirrers, probes, etc.

1. Summary

This application note shows how atlas and reaction monitoring can be used to look at endothermic processes.

2. Experimental

Atlas was set-up with a 500ml jacketed reactor, scorpion stirrer system with propellor blade, an oil-drain unit (together with temperature nodes and RTDs), three temperature nodes (with triple node socket) and a Julabo recirculating heater/chiller (controlled by the atlas base). The Atlas system was set-up and connected to the circulator. 300ml of water was added to the reactor and was set to heat to 25ºC. Once the temperature was stable (ca. 20 minutes) 10g of solid urea was added (as a single dose) into the reactor. The temperature responses were recorded in a .csv on the Atlas base unit and downloaded (using a standard USB key) to PC for later analysis.

3. Results

4. Conclusions

Atlas reaction monitoring is an easy way to detect whether processes are exothermic, endothermic or enthalpy neutral. The ease of set-up, short equilibration time and stand alone operation make this system ideal for use in any process chemistry laboratory.

Syrris Application Note: Tracking Exotherms using Atlas Reaction Monitoring

Key features of the ATLAS Potassium:

• Quick change vessel: The oil drain unit, jacketed vessel clamp and quick oil connectors allow vessels to be changed in under a minute.
• Easy to use: No tools required, twist and click control knob, large display and intuitive.
• Full data capture: Data such as temperatures and stirrer speed is logged in a .csv file and can be downloaded to a USB stick.
• Easy to upgrade: A wide range of accessories are available including vessels, stirrers, probes, etc.

1. Summary

This application note shows how atlas and reaction monitoring can be used to look at exothermic processes.

2. Experimental

Atlas was set-up with a 500ml jacketed reactor, scorpion overhead stirrer with propeller stirrer, an oil-drain unit, three temperature nodes (with node tree) and a Julabo recirculating heater/chiller (controlled by the Atlas base). 300ml of water was added to the reactor, which was heated to 25ºC. Once the temperature was stable (ca. 15 minutes) 10g of sodium hydroxide pellets were added into the reactor. It was subsequently found that two of the pellets were stuck to the addition funnel and these were added after 5 minutes as indicated on the graph. The temperature responses were recorded in a .csv file on the Atlas base unit and downloaded (using a standard USB key) to PC for later analysis.

3. Results

Upon analysis it is clear that the dissolution of solid sodium hydroxide in water is a strongly exothermic process. The addition of only two additional pellets of the sodium hydroxide caused an increase in Tr-Tj after 6 minutes on the above chart. This event was not visible on the temperature trace.

4. Conclusions

The Atlas system is able to monitor rapid exothermic events using Tr-Tj type reaction monitoring. The magnitude of the exothermic signal was over 12 degrees (compared with a reaction temperature shift of 5ºC). A smaller subsequent addition was only visible by considering the Tr-Tj graph. The complete experiment (including initial stabilisation) was conducted in less than thirty minutes showing how rapidly Atlas can be used to monitor exothermic reactions.