High pressure sample injection apparatus and method

• US 3,940,994 A
• Filed: 08/01/1974
• Issued: 03/02/1976
• Est. Priority Date: 08/01/1974
• Status: Expired due to Term

• Current Assignee: Varian Associates
• Original Assignee: Varian Associates
• Inventors: Klee, Richard E., Varozza, Joseph A. III
• Primary Examiner(s): Swisher, S. Clement
• Application Number:
  US05/493,593
• Time in Patent Office: 579 Days
• Field of Search: 73/422, 73/61.1 C
• US Class Current: 73/864.81
• CPC Class Codes: G01N 2030/328 valves, e.g. check valves of pumps
• CPC Class Codes: G01N 30/22 in high pressure liquid systems

Abstract

A high pressure sample injector for liquid chromatographs is disclosed. The apparatus includes structure defining a cylindrical dispensing chamber for receiving the sample to be injected into the flow path of a high pressure stream of carrier fluid in a liquid chromatograph. Control structure is interposed between the dispensing chamber and the flow path of the carrier stream for preventing liquid flow from the carrier stream to the dispensing chamber, and for enabling flow in the opposite direction only when the pressure in the dispensing chamber at least equals the carrier stream pressure. A pressurizing apparatus is connected to the dispensing chamber to raise its pressure, when desired, to a value at least equal to that of the carrier stream, in order that the sample may be injected into the carrier without reducing the carrier stream pressure.

Claims

1. An injector for a liquid chromatograph for injecting a sample liquid into a high-pressure stream of carrier liquid, said injector comprising:

a. structure defining a reservoir for the sample liquid,

b. structure defining a dispensing chamber for receiving a measured volume of the sample liquid from said reservoir,

c. structure defining a flow path for the high-pressure stream of carrier liquid,

d. control structure means interposed between said dispensing chamber and said flow path for substantially preventing liquid flow from said flow path to said dispensing chamber, and for enabling liquid flow from said dispensing chamber to said flow path only when the pressure of said measured volume of sample liquid in said dispensing chamber is at least equal to the pressure of said high pressure stream of carrier liquid, and

e. displacement means for limiting the volume of sample liquid receivable in said dispensing chamber and for imparting to the sample liquid in said dispensing chamber a pressure at least equal to the pressure of said high-pressure stream of carrier liquid.

2. The injector of claim 1 wherein said control structure means comprises:

a check valve.

3. The injector of claim 2 wherein said check valve comprises:

a. structure defining a valve chamber having a ball seat, said ball seat being apertured to enable liquid flow therethrough from said dispensing chamber to said flow path for said high-pressure stream of carrier liquid, and

b. a ball element disposed in said valve chamber, said ball element being configured to seat firmly in said ball seat when the pressure of the carrier liquid in said valve chamber exceeds the pressure of the sample liquid in said dispensing chamber.

4. The injector of claim 3 wherein:

said valve chamber is configured so as to be continuously flushed by said high-pressure stream of carrier liquid.

5. The injector of claim 1 wherein:

a. said dispensing chamber is of cylindrical configuration, and

b. said displacement means comprises a dispensing piston positioned coaxially within said cylindrical dispensing chamber.

6. The injector of claim 5 wherein:

said dispensing piston is connected to an actuating piston whereby said dispensing piston is slidably movable within said dispensing chamber in response to force applied to said actuating piston.

7. The injector of claim 6 further comprising:

resilient means for biasing said actuating piston for moving said dispensing piston within said dispensing chamber so as to reduce the pressure of said sample liquid within said dispensing chamber.

8. The injector of claim 6 wherein:

said actuating piston has a greater cross-sectional area than does said dispensing piston.

9. The injector of claim 1 wherein:

said control structure means is constructed to withstand a carrier stream pressure up to and in excess of 10,000 pounds per square inch gage.

10. A method for injecting a sample liquid into a high-pressure stream of carrier liquid in a liquid chromatograph, said method comprising the steps of:

a. placing a measured volume of said sample liquid in a dispensing chamber,

b. substantially preventing liquid flow from the stream of carrier liquid to the dispensing chamber, and enabling liquid flow from the dispensing chamber to the stream of carrier liquid only when the pressure of said measured volume of sample liquid in the dispensing chamber is at least equal to the pressure of the stream of carrier liquid, and

c. raising the pressure of said measured volume of sample liquid in the dispensing chamber to a value at least equal to the pressure of the stream of carrier liquid.

11. The method of claim 10 wherein said step of placing said measured volume of sample liquid in said dispensing chamber comprises:

a. preliminarily placing a quantity of said sample liquid in a sample reservoir communicable with said dispensing chamber, and

b. transferring said measured volume of the sample liquid from said reservoir into said dispensing chamber by displacement means.

12. The method of claim 10 wherein said step of raising the pressure of said measured volume of sample liquid in said dispensing chamber comprises moving a piston within said dispensing chamber after said measured volume of sample liquid has been transferred thereto.

13. The method of claim 11 wherein said step of transferring said measured volume of said sample liquid from said reservoir to said dispensing chamber comprises:

reducing the pressure in said dispensing chamber to draw said sample liquid from said reservoir.