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

• US 5,578,495 A
• Filed: 04/03/1995
• Issued: 11/26/1996
• Est. Priority Date: 10/31/1994
• Status: Expired due to Term

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Dynatech Precision Sampling Corp (Siemens AG)
• Inventors: Wilks, Terry S.
• Primary Examiner(s): Housel, James C.
• Assistant Examiner(s): FREED, RACHEL
• Application Number:
  US08/415,317
• Time in Patent Office: 603 Days
• Field of Search: 436/174, 436/177-178, 436/807, 422/99-102, 422/68.1, 422/81, 73/863.81, 73/864.01, 73/864.21, 73/864.11, 73/864.81, 73/864.91
• US Class Current: 436/178
• CPC Class Codes: G01N 2001/2826 Collecting by adsorption or absorption
• CPC Class Codes: G01N 2001/4066 using difference of solubility between liquid and gas, e.g. bubbling, scrubbing or sparging
• CPC Class Codes: G01N 35/1079 with means for piercing stoppers or septums
• CPC Class Codes: Y10S 436/807 Apparatus included in process claim, e.g. physical support structures
• CPC Class Codes: Y10T 436/255 including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

Apparatus, and process, for extracting organic fluids and solids specimens from weighed amounts of semi-solids and solids samples for collection, concentration and transfer to an analytic unit. The organic specimen is picked up by a probe assembly from a single compartment septum-sealed vial by heating and slurrying the sample, contacting with a gas; and then transferring the organic specimen with the gas to a collection device, e.g., a syringe or adsorbent trap. The specimen is then transported to an analytical instrument for analysis.

Claims

1. 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 vial

the combination of steps which comprise locating a septum sealed vial having a single compartment within which is contained said semi-solids or solids sample adjacent a probe assembly,

projecting said probe assembly through said septum into the compartment of the vial, said probe assembly including

a pair of concentrically mounted needles, an inner needle having a bore

therethrough formed by an enclosing wall, an outlet at the lower terminal end of the needle opening into the bore through which a gas or liquid can be passed, and an upper inlet communicated with the bore of said inner needle for use in introducing a gas or liquid into the bore, and

an outer needle having a bore therethrough formed by an enclosing wall of diameter sufficiently large to provide an annular passageway between the outside wall face of said inner needle and inside wall face of said outer needle, a gas inlet at the lower terminal end of the outer needle terminating above the outlet at the lower terminal end of said inner needle, and gas outlet at the upper terminal end of the outer needle communicated with the annular passageway,

a first line from a supply source of both gas and liquid connected to the inlet of said inner needle through which gas can be passed to exit via the outlet at the lower terminal end of the inner needle to pressurize the contents of the vial, or liquid introduced as a solvent to disperse the semi-solids or solids sample,

a second line connected to the gas outlet at the upper end of said outer needle through which a specimen-containing gas can be transported,

whereby, when the probe assembly is inserted into the septum sealed vial, the gas inlet at the lower terminal end of the outer needle remains above said semi-solids or solids sample,

injecting a liquid solvent via said first line of said probe assembly into the bore of said inner needle, the liquid solvent exiting at the opening at the lower terminal end of the inner needle to fill the vial compartment to a predetermined liquid level, and disperse 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 needle, the gas exiting from the lower terminal end of said inner needle, thereby pressurizing the contents of the vial and mixing with the liquid slurry, and passing gas into the annular passageway of the outer needle, the gas exiting from the second line to a specimen collector for concentration therein, and transfer therefrom for analysis in an analytical instrument.

2. The process of claim 1 wherein the terminal lower end of the inner needle of the probe assembly terminates as a point to facilitate passage through the septum of the vial.

3. The process of claim 1 wherein the semi-solids or solids sample contained, with liquid solvent, within the vial compartment is heated, crushed and ground to disperse the semi-solids or solids sample within the liquid solvent to form the slurry.

4. The process of claim 1 wherein the single compartmented septum sealed vial within which the semi-solids or solids sample is provided contains means for crushing and grinding same to facilitate separation of the organic fluid or solids specimen therefrom.

5. The process of claim 4 wherein the means for crushing and grinding the semi-solids or solids sample is a stir bar driven by a magnetic motor.

6. The process of claim 1 wherein a pair of lines, alternately operable, are connected with the inlet to the inner needle, one line providing during part of the operating cycle a means for delivery of liquid from a liquid supply source to the vial to clean the needle, and at another part of the operating cycle a liquid solvent for slurrying the solids or semi-solids organic specimen-containing material.

7. 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 vial

the combination of steps which comprise

locating a septum sealed vial having a single compartment within which is contained said semi-solids or solids sample adjacent a probe assembly,

projecting a pair of hollow needles of said probe assembly through said septum into the compartment of the vial,

said pair of hollow needles including,

a first needle having a bore therethrough formed by an enclosing wall, an outlet at the lower terminal end of the first needle opening into the bore through which a gas or liquid can be passed, and an upper inlet communicated with the bore of said first needle for use in introducing a gas or liquid into the bore, and

a second needle having a bore therethrough formed by an enclosing wail, a gas inlet at the lower terminal end of the second needle and gas outlet at the upper terminal end of the second needle communicated with the passageway provided by the bore through said second needle,

a first line from a supply source of both gas and liquid connected to the inlet of said first needle through which gas can be passed to exit via the outlet at the lower terminal end of the first needle to thereby pressurize the contents of the vial, or liquid introduced as a solvent to disperse the semi-solids or solids sample,

a second line connected to the gas outer at the upper end of said second needle through which a specimen-containing gas can be transported,

whereby, when the pair of hollow needles of said probe assembly is inserted into the septum-sealed vial, the gas inlet to the second needle at the lower terminal end thereof remains above said semi-solids or solids sample,

injecting a liquid solvent via said first line into the bore of said first needle, the liquid solvent exiting at the opening at the lower terminal end of the needle to fill the vial compartment to a predetermined liquid level, dispersing 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 first needle, the gas exiting from the lower terminal end of said needle, pressurizing the contents of the vial and mixing with the liquid slurry, and passing gas from the vial into the bore of the second needle to transport the specimen for analysis, the gas exiting from the second line to a specimen collector for concentration therein, and transfer therefrom for analysis in an analytical instrument.