Abstract: A structural improvement for microwave-assisted high temperature high-pressure chemistry vessel systems is disclosed that among other advantages offers dynamic venting and resealing while a reaction proceeds and eliminates the risk of cross contamination associated with systems that use a common pressurized chamber. The improvement includes a relatively thin-walled disposable liner cylinder that includes one closed end and one open end defining a mouth, and a liner cap positioned in the mouth of the rigid liner cylinder for closing the rigid liner cylinder. The liner cap includes a depending column that engages the inside diameter of the rigid liner cylinder, and a disk at one end of the depending column having a diameter sufficient to rest upon the rigid liner cylinder without falling into the rigid cylinder liner so that the cylindrical liner cap can rest in the rigid liner cylinder at the mouth of the rigid liner cylinder.

Abstract: An extraction method for preparing samples for analytical analysis is disclosed. The method includes the steps of placing a sample matrix containing one or more analytes in a heat conductive sample cup, positioning the heat conductive sample cup in a pressure-resistant reaction chamber, dispensing solvent into the heat conductive sample cup, dispersing the solvent and the sample matrix in the sample cup in the reaction chamber, heating the sample matrix and the extraction solvent in the heat conductive sample cup in the reaction chamber to a temperature at which the dispensed solvent generates an above-atmospheric pressure, and releasing the extraction solvent extract from the sample cup at atmospheric pressure.

Abstract: A structural improvement for microwave-assisted high temperature high-pressure chemistry vessel systems is disclosed that among other advantages offers dynamic venting and resealing while a reaction proceeds and eliminates the risk of cross contamination associated with systems that use a common pressurized chamber. The improvement includes a relatively thin-walled disposable liner cylinder that includes one closed end and one open end defining a mouth, and a liner cap positioned in the mouth of the rigid liner cylinder for closing the rigid liner cylinder. The liner cap includes a depending column that engages the inside diameter of the rigid liner cylinder, and a disk at one end of the depending column having a diameter sufficient to rest upon the rigid liner cylinder without falling into the rigid cylinder liner so that the cylindrical liner cap can rest in the rigid liner cylinder at the mouth of the rigid liner cylinder.

Abstract: An instrument system for acid digestion is disclosed. The instrument includes a heating block, a reaction vessel formed of a polymer that is resistant to acid and other chemical attack at temperatures above 150° C. and that has a structure (thickness, etc.) sufficient to withstand pressures above atmospheric, a metal sleeve surrounding the polymeric reaction vessel, and an opening in the block that has a cross-section corresponding to the cross-section of the metal sleeve.

Abstract: An extraction method for preparing samples for analytical analysis is disclosed. The method includes the steps of placing a sample matrix containing one or more analytes in a heat conductive sample cup, positioning the heat conductive sample cup in a pressure-resistant reaction chamber, dispensing solvent into the heat conductive sample cup, dispersing the solvent and the sample matrix in the sample cup in the reaction chamber, heating the sample matrix and the extraction solvent in the heat conductive sample cup in the reaction chamber to a temperature at which the dispensed solvent generates an above-atmospheric pressure, and releasing the extraction solvent extract from the sample cup at atmospheric pressure.

Abstract: A venting cap is disclosed for pressure vessels for microwave-assisted chemistry. The venting cap includes a flexible circular cover for closing the mouth of a reaction vessel, a flexible annular wall depending from the circular cover, and a flexible annular ring at the bottom of the annular wall and parallel to the circular cover for positioning the cap on a reaction vessel. At least one indentation in the circular cover minimizes distortion when any contents of a reaction vessel exert pressure against the cap, and at least one opening in the annular wall provides a ventilation path through the cap when gas pressure in a reaction vessel flexes the cap sufficiently to partially disengage at least a portion of the cap from the mouth of the reaction vessel.

Abstract: A precision volumetric liquid dispensing instrument is disclosed that includes two pressure sensors and a fluid passageway with a defined volume portion in communication with the two sensors for receiving and distributing liquid in relatively small volumes. One of the pressure sensors is positioned to measure pressure at one portion of the defined volume portion of the fluid passageway and the other of the gas pressure sensors is positioned to measure gas pressure at a different portion of the defined volume portion of the passageway. At least one valve is in communication with the passageway for moving fluids into or out of the defined volume portion of the fluid passageway, and a processor carries out a step selected from the group consisting of (i) calculating the volume of the liquid based upon the measured pressure and (ii) metering a liquid into the defined volume portion of the fluid passageway until the measured pressure indicates that a desired volume of fluid is in the fluid passageway.

Abstract: An energized dispersive extraction method for sample preparation for analysis is disclosed. The method includes the steps of placing an extraction solvent, sorbent particles, and a sample matrix containing an analyte in a heat conductive sample cup; positioning the sample cup in a pressure-resistant reaction chamber; dispersing the solvent and the sample matrix in the sample cup in the reaction chamber; heating the sample matrix and the solvent in the sample cup in the reaction chamber to a temperature that generates an above-atmospheric pressure; draining the solvent extract from the sample cup at atmospheric pressure; and collecting the solvent extract for analysis.

Abstract: An extraction method for preparing samples for analytical analysis is disclosed. The method includes the steps of placing a sample matrix containing one or more analytes in a heat conductive sample cup, positioning the heat conductive sample cup in a pressure-resistant reaction chamber, dispensing solvent into the heat conductive sample cup, dispersing the solvent and the sample matrix in the sample cup in the reaction chamber, heating the sample matrix and the extraction solvent in the heat conductive sample cup in the reaction chamber to a temperature at which the dispensed solvent generates an above-atmospheric pressure, and releasing the extraction solvent extract from the sample cup at atmospheric pressure.

Abstract: An energized dispersive extraction method for sample preparation for analysis is disclosed. The method includes the steps of placing an extraction solvent, sorbent particles, and a sample matrix containing an analyte in a heat conductive sample cup; positioning the sample cup in a pressure-resistant reaction chamber; dispersing the solvent and the sample matrix in the sample cup in the reaction chamber; heating the sample matrix and the solvent in the sample cup in the reaction chamber to a temperature that generates an above-atmospheric pressure; draining the solvent extract from the sample cup at atmospheric pressure; and collecting the solvent extract for analysis.

Abstract: An instrument for extraction based molecular sample preparation and related processes is disclosed. The instrument includes a thermally conductive pressure resistant heating chamber and a thermally conductive sample cup positioned in the thermally conductive pressure resistant healing chamber for heating liquids and solids together in the thermally conductive sample cup. A liquid delivery inlet fixture in the thermally conductive pressure resistant heating chamber delivers liquids (solvent) from a supply to the thermally conductive sample cup in the thermally conductive pressure resistant heating chamber, and a chiller in liquid communication with the thermally conductive sample cup in the thermally conductive pressure resistant heating chamber receives heated liquids from the thermally conductive pressure resistant heating chamber when the chamber is opened to atmospheric pressure.

Abstract: An extraction method for preparing samples for analytical analysis is disclosed. The method includes the steps of placing a sample matrix containing one or more analytes in a heat conductive sample cup, positioning the heat conductive sample cup in a pressure-resistant reaction chamber, dispensing solvent into the heat conductive sample cup, dispersing the solvent and the sample matrix in the sample cup in the reaction chamber, heating the sample matrix and the extraction solvent in the heat conductive sample cup in the reaction chamber to a temperature at which the dispensed solvent generates an above-atmospheric pressure, and releasing the extraction solvent extract from the sample cup at atmospheric pressure.

Abstract: An energized dispersive extraction method for sample preparation for analysis is disclosed. The method includes the steps of placing an extraction solvent, sorbent particles, and a sample matrix containing an analyte in a heat conductive sample cup; positioning the sample cup in a pressure-resistant reaction chamber; dispersing the solvent and the sample matrix in the sample cup in the reaction chamber; heating the sample matrix and the solvent in the sample cup in the reaction chamber to a temperature that generates an above-atmospheric pressure; draining the solvent extract from the sample cup at atmospheric pressure; and collecting the solvent extract for analysis.

Abstract: An instrument for extraction based molecular sample preparation and related processes is disclosed. The instrument includes a thermally conductive pressure resistant heating chamber and a thermally conductive sample cup positioned in the thermally conductive pressure resistant heating chamber for heating liquids and solids together in the thermally conductive sample cup. A liquid delivery inlet fixture in the thermally conductive pressure resistant heating chamber delivers liquids (solvent) from a supply to the thermally conductive sample cup in the thermally conductive pressure resistant heating chamber, and a chiller in liquid communication with the thermally conductive sample cup in the thermally conductive pressure resistant heating chamber receives heated liquids from the thermally conductive pressure resistant heating chamber when the chamber is opened to atmospheric pressure.

Abstract: An extraction method for preparing samples for analytical analysis is disclosed. The method includes the steps of placing a sample matrix containing one or more analytes in a heat conductive sample cup, positioning the heat conductive sample cup in a pressure-resistant reaction chamber, dispensing solvent into the heat conductive sample cup, dispersing the solvent and the sample matrix in the sample cup in the reaction chamber, heating the sample matrix and the extraction solvent in the heat conductive sample cup in the reaction chamber to a temperature at which the dispensed solvent generates an above-atmospheric pressure, and releasing the extraction solvent extract from the sample cup at atmospheric pressure.

Abstract: An instrument for extraction based molecular sample preparation and related processes is disclosed. The instrument includes a thermally conductive pressure resistant heating chamber and a thermally conductive sample cup positioned in the thermally conductive pressure resistant heating chamber for heating liquids and solids together in the thermally conductive sample cup. A liquid delivery inlet fixture in the thermally conductive pressure resistant heating chamber delivers liquids (solvent) from a supply to the thermally conductive sample cup in the thermally conductive pressure resistant heating chamber, and a chiller in liquid communication with the thermally conductive sample cup in the thermally conductive pressure resistant heating chamber receives heated liquids from the thermally conductive pressure resistant heating chamber when the chamber is opened to atmospheric pressure.

Abstract: An instrument and method for high pressure microwave assisted chemistry are disclosed. The method includes the steps of applying microwave radiation to a sample in a sealed vessel while measuring the temperature of the sample and measuring the pressure generated inside the vessel and until the measured pressure reaches a designated set point, opening the vessel to release gases until the pressure inside the vessel reaches a lower designated set point, closing the vessel, and repeating the steps of opening the vessel at designated pressure set points and closing the vessel at designated pressure set points to the sample until the sample reaction reaches a designated high temperature. The designated set points can controllably differ from one another as the reaction proceeds. Microwave energy can be applied continuously or intermittently during the opening and closing steps.

Abstract: A venting cap is disclosed for pressure vessels for microwave-assisted chemistry. The venting cap includes a flexible circular cover for closing the mouth of a reaction vessel, a flexible annular wall depending from the circular cover, and a flexible annular ring at the bottom of the annular wall and parallel to the circular cover for positioning the cap on a reaction vessel. At least one indentation in the circular cover minimizes distortion when any contents of a reaction vessel exert pressure against the cap, and at least one opening in the annular wall provides a ventilation path through the cap when gas pressure in a reaction vessel flexes the cap sufficiently to partially disengage at least a portion of the cap from the mouth of the reaction vessel.

Abstract: An instrument and method for high pressure microwave assisted chemistry are disclosed. The method includes the steps of applying microwave radiation to a sample in a sealed vessel while measuring the temperature of the sample and measuring the pressure generated inside the vessel and until the measured pressure reaches a designated set point, opening the vessel to release gases until the pressure inside the vessel reaches a lower designated set point, closing the vessel, and repeating the steps of opening the vessel at designated pressure set points and closing the vessel at designated pressure set points to the sample until the sample reaction reaches a designated high temperature. The designated set points can controllably differ from one another as the reaction proceeds. Microwave energy can be applied continuously or intermittently during the opening and closing steps.

Abstract: An instrument system for acid digestion is disclosed. The instrument includes a heating block, a reaction vessel formed of a polymer that is resistant to acid and other chemical attack at temperatures above 150° C. and that has a structure (thickness, etc.) sufficient to withstand pressures above atmospheric, a metal sleeve surrounding the polymeric reaction vessel, and an opening in the block that has a cross-section corresponding to the cross-section of the metal sleeve.