摘要:
An instrument and associated method are disclosed for preparing samples for column chromatography. The method includes the steps of applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products, thereafter mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography, thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy, and thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating the components of the remaining sample for identification and purification purposes.
摘要:
A pressure-measuring vessel system for microwave assisted chemical processes is disclosed. The vessel system includes a pressure resistant vessel that is otherwise transparent to microwave radiation, a pressure-resistant closure for the mouth of the vessel, with portions of the closure including a pressure resistant synthetic membrane, a pressure transducer external to the vessel, and a tube extending from the transducer, through the membrane and into the vessel for permitting the pressure inside the vessel to be applied against the transducer while the closure and membrane otherwise maintain the pressure resistant characteristics of the vessel.
摘要:
A controlled-flow microwave instrument is disclosed for chemical synthesis using heterogeneous or highly viscous starting materials. The instrument includes a microwave source for generating electromagnetic radiation in the microwave frequencies, a microwave cavity in wave communication with the source for exposing compositions placed therein to microwave radiation, a microwave-transparent pressure resistant reaction vessel in the cavity, a source reservoir for starting materials and related compositions, a pump in communication with the source reservoir for pumping heterogeneous or highly viscous materials from the source reservoir to the reaction vessel, and a pressure-resistant valve between the pump and the reaction vessel for isolating the reaction vessel from the pump and the source reservoir during application of microwave energy to compositions in the vessel and from any resulting high pressure generated therein.
摘要:
A method and associated instrument are disclosed for increasing the sequential rate at which a series of microwave assisted chemical reactions that potentially generate high pressure can be carried out. The method includes the steps of opening a pressure-resistant valve on a microwave-transparent pressure-resistant vessel to define a unpressurized pathway through the valve into the vessel, inserting a tube through the pathway in the valve and into the vessel, transferring at least one composition into the vessel through the tube, removing the tube from the vessel and from the pathway in the valve, closing the valve to seal the vessel against pressure release, and exposing the vessel and its contents to microwave radiation. The instrument includes a source of microwave radiation, a cavity in microwave communication with the source, an attenuator that forms at least a portion of the cavity, a pressure-resistant microwave-transparent reaction vessel having portions in the cavity and portions in the attenuator, a pressure-resistant valve on the mouth of the vessel, a reciprocating tube for passing through the valve and into the vessel when the valve is open, and means for mechanically inserting and retracting the tube through the valve and into the vessel when the vessel is in the cavity and the attenuator.
摘要:
An instrument and associated method are disclosed for preparing samples for column chromatography. The method includes the steps of applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products, thereafter mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography, thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy, and thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating the components of the remaining sample for identification and purification purposes.
摘要:
A method and associated instrument are disclosed for increasing the sequential rate at which a series of microwave assisted chemical reactions that potentially generate high pressure can be carried out. The method includes the steps of opening a pressure-resistant valve on a microwave-transparent pressure-resistant vessel to define a unpressurized pathway through the valve into the vessel, inserting a tube through the pathway in the valve and into the vessel, transferring at least one composition into the vessel through the tube, removing the tube from the vessel and from the pathway in the valve, closing the valve to seal the vessel against pressure release, and exposing the vessel and its contents to microwave radiation. The instrument includes a source of microwave radiation, a cavity in microwave communication with the source, an attenuator that forms at least a portion of the cavity, a pressure-resistant microwave-transparent reaction vessel having portions in the cavity and portions in the attenuator, a pressure-resistant valve on the mouth of the vessel, a reciprocating tube for passing through the valve and into the vessel when the valve is open, and means for mechanically inserting and retracting the tube through the valve and into the vessel when the vessel is in the cavity and the attenuator.
摘要:
A method and associated instrument are disclosed for increasing the sequential rate at which a series of microwave assisted chemical reactions that potentially generate high pressure can be carried out. The method includes the steps of opening a pressure-resistant valve on a microwave-transparent pressure-resistant vessel to define a unpressurized pathway through the valve into the vessel, inserting a tube through the pathway in the valve and into the vessel, transferring at least one composition into the vessel through the tube, removing the tube from the vessel and from the pathway in the valve, closing the valve to seal the vessel against pressure release, and exposing the vessel and its contents to microwave radiation. The instrument includes a source of microwave radiation, a cavity in microwave communication with the source, an attenuator that forms at least a portion of the cavity, a pressure-resistant microwave-transparent reaction vessel having portions in the cavity and portions in the attenuator, a pressure-resistant valve on the mouth of the vessel, a reciprocating tube for passing through the valve and into the vessel when the valve is open, and means for mechanically inserting and retracting the tube through the valve and into the vessel when the vessel is in the cavity and the attenuator.
摘要:
An instrument and associated method are disclosed for performing microwave assisted organic chemical synthesis at low temperatures. The instrument includes a reaction vessel formed of a microwave transparent material that defines an interior reaction chamber for carrying out microwave assisted reactions in the chamber, a cooling jacket immediately surrounding the reaction vessel for cooling the vessel and the vessel contents during the application of microwave energy to contents in the vessel when a microwave transparent media used as a fluid coolant is present in the jacket. The instrument includes means for supplying a microwave transparent fluid coolant to the cooling jacket and means for venting the fluid coolant from the cooling jacket, a fluid coolant reservoir in communication with the cooling jacket, and a pump in communication with the reservoir and the cooling jacket for circulating fluid coolant from the fluid coolant reservoir through the cooling jacket and around the reaction vessel.
摘要:
A controlled-flow microwave instrument for chemical synthesis that includes heterogeneous or highly viscous materials includes a fluid reservoir for supplying or receiving fluids, a fluid pump in fluid communication with the reservoir for pumping fluids to or from the reservoir, a microwave transparent reaction vessel in fluid communication with the pump for supplying or receiving fluids to or from the pump and the reservoir, a pressure sensor in fluid communication with the reservoir and the vessel for measuring the pressure of fluids in the instrument at the sensor, and a processor in signal communication with the pressure sensor and the pump for controlling the pump and the flow of fluids in the instrument based at least in part on the pressure measured at the sensor.
摘要:
A controlled-flow microwave instrument for chemical synthesis using heterogeneous or highly viscous starting materials includes a microwave source for generating electromagnetic radiation in the microwave frequencies, a microwave cavity in wave communication with the source for exposing compositions placed therein to microwave radiation, a microwave-transparent pressure resistant reaction vessel in the cavity, a source reservoir for starting materials and related compositions, a pump in communication with the source reservoir for pumping heterogeneous or highly viscous materials from the source reservoir to the reaction vessel, and a pressure-resistant valve between the pump and the reaction vessel for isolating the reaction vessel from the pump and the source reservoir during application of microwave energy to compositions in the vessel and from any resulting high pressures generated therein.