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Reactions performed under atmospheric conditions, at the boiling point of the reaction mixture, are the mainstay of traditional synthetic methods. Traditional reflux is easily adapted to a wide range of reaction volumes, glass components are easy to configure, and reaction homogeneity is accomplished with the constantly boiling solution or through the use of a stirring mechanism.
Reflux in a microwave field offers the chemist the opportunity to investigate the unique effects of microwaves on reaction rates and mechanisms. Microwave enhancement of reflux reactions depends entirely on relative absorption of microwaves as well as differential and localized heating of the various components of the reaction mixture.
Milestone supports reflux reactions in either a traditional single vessel or in a unique multi-vessel format.
Milestone's NP (normal pressure) reflux system offers the following features and benefits in support of reflux reactions:
- The Ethos MicroSYNTH can use ordinary laboratory glassware with ground glass joints. No special glassware is needed. Any reflux reactions you are performing now with a hot plate, heating mantle, or steam bath as the heat source can be immediately transferred to work in the microwave field.
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Access through the top of the MicroSYNTH into the multimode microwave cavity allows connection of standard laboratory glassware inside the cavity, via pass-through adapters, to distillation side arms and condensers outside the cavity. - All reactions take place inside the cavity, so the chemistry is processed safely and securely inside its steel walls.
- Stirring ensures homogeneous reaction mixtures, even bi-phasic mixtures of liquids and slurries. Ordinary magnetic stir bars can be used in the vessel in conjunction with the variable speed stirring available in every Ethos MicroSYNTH labstation.
- Milestone's unique Weflon buttons and stir bars, when introduced in a vessel, facilitate microwave heating, even of non-microwave-absorbing reaction mixtures.
- Reaction temperatures are monitored using a fiber-optic temperature probe inserted into the reaction vessel. Alternatively, a contactless infrared sensor can be used to monitor the surface temperature of the vessel. Accurate temperature monitoring and precise feedback control is achieved using the easyWAVE software, resulting in reproducible reaction temperature conditions, ± 1 °C precision.
- Controlled reaction temperatures to 200 °C are possible.
- The facility to create a controlled-intensity mercury vapor spectrum, to induce photochemical reactions in each vessel, can be achieved through the use of electrodeless plasma lamp inserts.
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