Apparatus, and process, for automatically sampling solids and semi-solids materials for analysis

An apparatus useful for the pick up from a septum sealed vial of a specimen contained in a slurried liquid phase above which is provided a gas phase, for transport of the specimen to a specimen collector for delivery to an analytical instrument, comprising in combination:

• a vial sealed with a septum,
• a specimen collector within which a specimen is contained, and concentrated,
• a probe assembly, having a pair of concentrically mounted needles, wherein a first one of said concentrically mounted needles is
• an inner tubular needle having a bore therethrough formed by an enclosing wall, a gas outlet at a lower closed terminal end of the needle formed by a plurality of wall apertures providing a filter opening within the bore, and an upper gas inlet communicated with the bore of said inner tubular needle, and
• the second of said concentrically mounted needles is an outer tubular needle having a bore therethrough formed by an enclosing wall of diameter sufficiently large to encompass said inner tubular needle and provide an annular passageway between the outside wall face of said inner tubular needle and the inside wall face of said encompassing outer tubular needle, a gas inlet at the lower terminal end of the outer tubular needle terminating above the gas outlet at the lower terminal end of said inner tubular needle, said inlet consisting of a plurality of wall apertures providing a filter opening to the annular passageway, and gas outlet at the upper terminal end of the outer tubular needle in communication with the annular passageway,
• a line from a gas supply source connected to the gas inlet of said inner tubular needle through which a gas is passed into the bore thereof to exit via the gas outlet at the lower terminal end of the inner tubular needle into the vial for pressurizing the contents of said vial, and mix with a slurried liquid within the vial, which carries a specimen,
• a line connected to the outlet of the upper end of said outer tubular needle through which the specimen-containing gas is transported to the specimen collector for delivery to an analytical instrument after the lower terminal end of the inner tubular needle has been passed through the septum of the vial and vapor phase into the liquid phase of the vial.

In a process for the extraction and separation for analysis of an organic fluid or solids specimen from a semi-solids or solids sample carried within a septum sealed vial having a single compartment

• the combination of steps which comprise
• projecting a probe assembly through said septum into the compartment of the vial,
• said probe assembly including
• a pair of concentrically mounted needles, wherein a first one of said concentrically mounted needles is an inner tubular needle having a bore therethrough formed by an enclosing wall, a gas outlet at a lower closed terminal end of the needle formed by a plurality of wall apertures providing a filter opening into the bore, and an upper gas inlet communicated with the bore of said inner tubular needle, and the second of said concentrically mounted needles is an outer tubular needle having a bore therethrough formed by an enclosing wall of diameter sufficiently large to encompass said inner tubular needle and provide an annular passageway between the outside wall face of said inner tubular needle and the inside wall face of said outer tubular needle, a gas inlet at the lower terminal end of the outer tubular needle terminating above the gas outlet at the lower terminal end of said inner tubular needle, said inlet consisting of a plurality of wall apertures providing a filter opening to the annular passageway, and gas outlet at the upper terminal end of the outer tubular needle in communication with the annular passageway,
• a first line from a gas supply source connected to the gas inlet of said inner tubular needle through which a gas is passed into the bore thereof to exit via the gas outlet at the lower terminal end of the inner tubular needle to pressurize the contents of the vial,
• a second line connected to the gas outlet at the upper end of said outer tubular needle through which a specimen-containing gas is transported,
• injecting a liquid solvent via said first line into the bore of said inner tubular needle, the liquid solvent exiting at the opening at the lower terminal end of the inner tubular needle to fill the vial compartment to a predetermined liquid level, heating, crushing, and grinding the semi-solids or solids sample within the liquid solvent to form a slurry,
• injecting a gas via said first line into the bore of said inner tubular needle, the gas exiting from the lower terminal end of said inner tubular needle, pressurizing the contents of the vial and mixing with the liquid slurry, and passing gas into the annular passageway of the outer tubular needle, the gas exiting from the second line to a specimen collector for concentration therein, and transfer therefrom for analysis in an analytical instrument.