Instrument for Analytical Sample Preparation

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.

1 . A combination for solvent extraction comprising:
 a heated, pressure-sealed reaction chamber;   a heat conductive sample cup in said reaction chamber, said reaction vessel including one open filtered end and a mouth opposite said open filtered end;   an extraction sample in said sample cup; and   a liquid extraction solvent inside said sample cup and outside said sample cup between the exterior of said sample cup and the interior of said reaction chamber.   
     
     
         2 . A combination according to  claim 1  wherein said reaction chamber is formed of a thermally conductive material. 
     
     
         3 . A combination according to  claim 1  wherein said opened filtered end is a foraminous floor and a filter media on foraminous floor. 
     
     
         4 . A combination according to  claim 3  wherein said filter media is selected from the group consisting of filter paper, glass fibers, quartz fibers, nonwoven polymers and combinations thereof. 
     
     
         5 . A combination according to  claim 1  wherein said extraction sample is selected from the group consisting of soil, plastics, prepared foods, food packaging, agricultural products, and mixtures thereof. 
     
     
         6 . A combination according to  claim 1  wherein said liquid extraction solvent is selected from the group consisting of water, weak acids, weak bases, ethyl acetate, methyl tertiary-butyl ether (“MTBE”), methylene chloride, hexane, acetone, hexane 2-propanol, cyclohexane, acetonitrile, methanol and mixtures thereof. 
     
     
         7 . An instrument for extraction based molecular sample preparation and related processes, comprising:
 a thermally conductive pressure resistant heating chamber;   a thermally conductive sample cup positioned in said thermally conductive pressure resistant heating chamber and for heating liquids and solids together in said thermally conductive sample cup,   a liquid delivery inlet fixture in said thermally conductive pressure resistant heating chamber for delivering liquids from a supply to said thermally conductive sample cup in said thermally conductive pressure resistant heating chamber; and   a chiller in liquid communication with said thermally conductive sample cup in said thermally conductive pressure resistant heating chamber for receiving heated liquids from said thermally conductive pressure resistant heating chamber when said chamber is opened to atmospheric pressure.   
     
     
         8 . A molecular sample preparation instrument according to  claim 7  wherein said pressure resistant heating chamber further comprises a gas delivery inlet fixture in said thermally conductive pressure resistant heating chamber positioned at or near the top of said thermally conductive sample cup for delivering an inert gas from a supply to said thermally conductive sample cup and said reaction chamber to increase the pressure in said heating chamber and in said sample cup. 
     
     
         9 . A molecular sample preparation instrument according to  claim 7  wherein an the ultrasonic generator is in communication with said thermally conductive pressure resistant heating chamber for carrying out secondary agitation of materials in said sample cup. 
     
     
         10 . A molecular sample preparation instrument according to  claim 7  wherein said ultrasonic generator is a piezoelectric transducer. 
     
     
         11 . A molecular sample preparation instrument according to  claim 7  wherein said chiller comprises a cooling coil in liquid communication with said drain, said cooling coil having a length sufficient to reduce the temperature of common liquid extraction solvents from between about 50° C. and 180° C. to between about 25° C. and 40° C. as the liquid solvent travels the length of said cooling coil. 
     
     
         12 . A molecular sample preparation instrument according to  claim 7  wherein said pressure resistant heating chamber further comprises a pressure resistant chamber closure. 
     
     
         13 . A molecular sample preparation instrument according to  claim 7  further comprising a gas delivery inlet fixture in said thermally conductive pressure resistant heating chamber positioned at or near the bottom of said thermally conductive sample cup for delivering an inert gas from a supply to said thermally conductive sample cup to agitate the contents of said thermally conductive sample cup. 
     
     
         14 . An instrument for extraction based molecular sample preparation and related processes, comprising:
 a plurality of sample cups and a plurality of collection vials carried in a common rack;   a robot arm for moving one of said sample cups between said rack and an opened pressure chamber;   a pressure resistant chamber closure that reciprocates vertically to open and close said pressure chamber;   a liquid inlet fixture for delivering liquids to said pressure chamber when said pressure chamber is closed;   a heater for raising the temperature of liquids in said pressure chamber when said pressure chamber is closed;   a gas inlet fixture for delivering an agitating gas flow to said pressure chamber when said pressure chamber is closed; and;   a drain for releasing liquids from said pressure chamber under pressure generated by delivered heated liquids in said chamber.   
     
     
         15 . An extraction based molecular sample preparation instrument according to  claim 14  and further comprising a cooling coil in liquid communication with said drain, said cooling coil having a length sufficient to reduce the temperature of common liquid extraction solvents from between about 50° C. and 180° C. to between about 25° C. and 40° C. as the solvent travels the length of said cooling coil. 
     
     
         16 . An extraction based molecular sample preparation instrument according to  claim 14  and further comprising:
 a liquid delivery faucet on said a robot arm; and 
 a tube between said cooling coil and said faucet for delivering cooled liquids from said faucet to one of said collection vials. 
 
     
     
         17 . An extraction based molecular sample preparation instrument according to  claim 15  further comprising a first valve between said heated pressure chamber and said cooling coil for draining liquid solvent from said heated pressure chamber into said cooling coil. 
     
     
         18 . An extraction based molecular sample preparation instrument according to  claim 17  further comprising a second valve at the terminal end of said cooling coil so that the vapor pressure of heated liquid solvent in said thermally conductive chamber pushes liquid solvent into said cooling coil. 
     
     
         19 . An extraction based molecular sample preparation instrument according to  claim 14  and further comprising a gas fixture for delivering an agitating gas flow to a position at or near the bottom of said sample cup in said pressure chamber when said pressure chamber is closed and heated. 
     
     
         20 . An extraction based molecular sample preparation instrument according to  claim 14  further comprising:
 a piezoelectric transducer ultrasonic generator positioned adjacent said chamber and; 
 a rod connecting said transducer to a wall of said pressure chamber to agitate contents of said sample cup.