Method and apparatus for detecting rapid barrier coating integrity characteristics

• US 9,903,782 B2
• Filed: 11/15/2013
• Issued: 02/27/2018
• Est. Priority Date: 11/16/2012
• Status: Active Grant

• Current Assignee: SiO2 Medical products Inc.
• Original Assignee: SiO2 Medical products Inc.
• Inventors: Fisk, Thomas E., Sagona, Peter J., Jones, Joseph A.
• Primary Examiner(s): Rogers, David A
• Application Number:
  US14/442,372
• Publication Number:
  US 20150316440A1
• Time in Patent Office: 1,565 Days
• CPC Class Codes: G01M 3/202 using mass spectrometer detection systems
• CPC Class Codes: G01M 3/205 Accessories or associated equipment; Pump constructions
• CPC Class Codes: G01M 3/229 removably mounted in a test cell

Abstract

An apparatus and methods for testing the integrity of a barrier coating on a vessel. An off gas test fixture includes a face seal positioned about an opening of the vessel. A side seal is positioned about a portion of the vessel'"'"'s wall and separated from the face seal by a space. Additionally, a cover may be secured to the fixture that encompasses an interface portion of the fixture and the vessel. Before and/or during testing, gas in the space between the side and face seals may be evacuated, as well as gas present in an interior area of the vessel. The vessel may be exposed to test gas(es) that is soluble by the plastic material of the vessel before and/or after being secured to the fixture. During testing, test gas(es) desorbed by the vessel may be evacuated, with the molecular flow being measured using a mass extraction unit.

Claims

1. An off gas test fixture for testing the barrier coating integrity of a vessel having at least one opening, the off gas test fixture comprising:

an interface portion having a surface and a wall, the surface configured to abut against a portion of the vessel adjacent to the opening, the surface further including a face seal configured to provide a first seal about the opening when the vessel is secured to the off gas test fixture, the wall including a recess configured to house a side seal, the side seal configured to provide a second seal between a portion of the wall of the vessel and the interface portion;

a vacuum line in communication with a space separating the first seal and the second seal, the vacuum line configured to be operably connected to a vacuum to evacuate gas from the space when the vessel is secured to the off gas test fixture;

a source of a test gas that is soluble, absorbed, adsorbed or permeable in or on a surface of the molded material of the wall of the vessel; and

a compression nut configured to threadingly engage at least a portion of the wall of the interface portion, the compression nut further configured to provide a compressive force against the side seal to deform the side seal in a manner that prevents gas from passing through the second seal.

2. An off gas test fixture for testing the barrier coating integrity of a vessel having at least one opening, the off gas test fixture comprising:

an interface portion having a surface and a wall, the surface configured to abut against a portion of the vessel adjacent to the opening, the surface further including a face seal configured to provide a first seal about the opening when the vessel is secured to the off gas test fixture, the wall including a recess configured to house a side seal, the side seal configured to provide a second seal between a portion of the wall of the vessel and the interface portion;

a vacuum line in communication with a space separating the first seal and the second seal, the vacuum line configured to be operably connected to a vacuum to evacuate gas from the space when the vessel is secured to the off gas test fixture;

a source of a test gas that is soluble, absorbed, adsorbed or permeable in or on a surface of the molded material of the wall of the vessel; and

a cover that defines an inner area, the inner area configured to encompass the vessel and interface portion when the cover is secured to a base, and wherein the interface portion extends from the base.

3. The off gas test fixture of claim 2, further including a connector that is operably connected to the cover, the connector having a first end and a second end, the first end being configured for connection to a hose, the second end being in communication with the inner area.

4. The off gas test fixture of claim 2, further including a seal positioned between the cover and the base, the seal configured to prevent gas from passing into or out of the inner area when the cover is secured to the base.

5. A method for testing the barrier coating integrity of a vessel having a wall, at least one opening, and a barrier coating, the method comprising:

providing an off gas test fixture comprising a base and a cover, the base including an interface portion having a surface and the cover generally defining an interior area;

securely engaging a portion of the vessel against the surface of the interface portion of the off gas test fixture;

sealing the engagement between the portion of the vessel and the surface of the interface portion to provide a first gas seal;

sealing an area between a portion of the wall of the vessel and the interface portion to provide a second gas seal, the second gas seal positioned to provide a space between the first gas seal and the second gas seal;

securing the cover to the base with the vessel and the interface portion within the interior area; and

exposing the vessel to a test gas, wherein the gas is delivered into an inner area of the cover, the test gas being soluble by the material of the vessel;

evacuating gas out of the space between the first and second gas seal;

applying a vacuum to the vessel to remove any test gas that had been absorbed by, or permeated into, the vessel; and

measuring the test gas removed by the vacuum to determine the integrity of the barrier coating.

6. The method of claim 5, wherein said measuring includes measuring the molecular flow of the test gas desorbed by, and/or permeated through, the vessel.

7. The method of claim 6, wherein said measuring includes measuring the flow of test gas using of a mass extraction unit.

8. The method of claim 7, wherein said measuring includes quantifying the concentration of the test gas using a mass spectrometer.

9. The method of claim 5, wherein said exposing the vessel to a test gas includes exposing the vessel to the test gas before securely engaging the portion of the vessel against an interface portion.

10. The method of claim 5, further including said delivering a test gas through a passageway in the interface portion and to the interior area of the vessel.

11. The method of claim 10, wherein said evacuating a test gas out of the interior area involves evacuating test gas that has been desorbed by the material of the vessel.

12. The method of claim 5, wherein said securely engaging the portion of the vessel against the surface includes tightening a compression member that abuts against a portion of the vessel, the compression member providing a force to secure the vessel between the compression member and the surface.

13. The method of claim 5, wherein said sealing the engagement between the portion of the vessel and the surface of the interface portion includes deforming an 0-ring positioned in a groove in the upper surface to form the first gas seal.

14. The method of claim 5, wherein said sealing the area between a portion of the wall of the vessel and the interface portion includes engaging a compression nut against a side seal to deform the side seal to form the second gas seal, the side seal being an O-ring.

15. The method of claim 5, wherein the vessel is a vial, syringe, or blood.

16. The method of claim 5, wherein said exposing a vessel to a test gas includes exposing the vessel to a test gas pressure of approximately 25 psig to 2000 psig.

17. The method of claim 5, wherein said exposing a vessel to a test gas includes exposing both the interior area and exterior surfaces of the vessel to the test gas.

18. The method of claim 5, wherein the test gas comprises one or more members selected from the group consisting of:

carbon dioxide, helium, nitrogen, oxygen, water vapor, neon, hydrogen, carbon monoxide, argon, methane, krypton, ethane, ethylene, and xenon.

19. The method of claim 5, wherein the test gas consists essentially of a member selected from the group consisting of:

carbon dioxide, helium, nitrogen, oxygen, water vapor, neon, hydrogen, carbon monoxide, argon, methane, krypton, ethane, ethylene, and xenon.

20. An off gas test fixture for testing the barrier coating integrity of a vessel having at least one opening, the off gas test fixture comprising:

a base;

an interface portion extending from the base and having a surface and a wall, the surface configured to abut against a portion of the vessel adjacent to the opening, the surface further including a face seal configured to provide a first seal about the opening when the vessel is secured to the off gas test fixture, the wall including a recess configured to house a side seal, the side seal configured to provide a second seal between a portion of the wall of the vessel and the interface portion;

a vacuum line in communication with a space separating the first seal and the second seal, the vacuum line configured to be operably connected to a vacuum to evacuate gas from the space when the vessel is secured to the off gas test fixture; and

a cover configured to be secured to the base to define an inner area between them, the inner area configured to encompass the vessel and interface portion when the cover is secured to the base.

21. An off gas test fixture for testing the barrier coating integrity of a vessel having at least one opening, the off gas test fixture comprising:

an interface portion having a surface and a wall, the surface configured to abut against a portion of the vessel adjacent to the opening, the surface further including a face seal configured to provide a first seal about the opening when the vessel is secured to the off gas test fixture, the wall including a recess configured to house a side seal, the side seal configured to provide a second seal between a portion of the wall of the vessel and the interface portion;

a vacuum line in communication with a space separating the first seal and the second seal, the vacuum line configured to be operably connected to a vacuum to evacuate gas from the space when the vessel is secured to the off gas test fixture; and

a compression nut, the compression nut configured to threadingly engage at least a portion of the wall of the interface portion, the compression nut further configured to provide a compressive force against the side seal to deform the side seal in a manner that prevents gas from passing through the second seal.