IP Library Granted Patent US 9,108,138
Granted Patent B2
US 9,108,138 · App. 13/357,403 · Granted Aug 18, 2015

Accelerated mixed gas integrity testing of porous materials

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Quick Facts
Patent No.
US 9,108,138
App. No.
13/357,403
Granted
Aug 18, 2015
Kind
B2
Abstract

The invention relates to accelerated mixed gas integrity testing methods, devices, and systems for integrity testing wetted single and multi-layered porous materials, whereby the testing method is non-destructive to the porous materials being tested. The accelerated mixed gas integrity test method includes one or more of the following components: i) a permeate side gas purge component; ii) a permeate side volume reduction component; and iii) a permeate side circulation component. The invention is directed towards reducing the length of time necessary to complete the integrity testing of single and multi layered porous materials, elements and membranes.

Claims (46)

1. A method of assessing the integrity of a porous material loaded into a porous material device using a compressed gas mixture and without the need for any gas component in the gas mixture to achieve a steady state concentration comprising

a) loading a wetted porous material into a device having a housing for receiving the wetted porous material, resulting in a wetted porous material having a feed side and a permeate side;

b) feeding a compressed gas mixture of two or more gas components to the feed side of the wetted porous material, wherein the feed gases have differing permeabilities in the liquid used to wet the porous material, such that one of the gases permeates through the liquid of the wetted porous material faster than the other gas or gases used;

c) flushing out the existing gas in the permeate side volume of the porous material and replacing with a gas mixture that has a composition similar to the expected composition of permeate gas generated from an integral membrane;

d) recirculating the permeate gas and venting excess permeate gas while maintaining a feed side gas sweep flow;

e) assessing the concentration of the gas mixture on the permeate side; and

f) comparing the assessed concentration of the permeate gas with the value expected from an integral device, wherein a deviation from the expected concentration by more than predetermined amount is a signal for a non-integral porous material or porous material device.

2. The method of claim 1 , wherein the liquid in (a) is water.

3. The method of claim 1 , wherein at least one of the gases is CO 2 .

4. The method of claim 1 , wherein at least one of the gases is O 2 .

5. The method of claim 1 , wherein the porous material comprises a hydrophilic material.

6. The method of claim 1 , wherein the porous material comprises a hydrophobic material.

7. The method of claim 1 , wherein the porous material comprises a membrane.

8. The method of claim 7 , wherein the membrane comprises a filtration device.

9. The method of claim 7 , wherein the membrane is an asymmetric membrane.

10. The method of claim 7 , wherein the membrane is a symmetric membrane.

11. The method of claim 7 , wherein the membrane is comprised of a polymer.

12. The method of claim 11 , wherein the polymer is PES.

13. The method of claim 7 , wherein the membrane is a flat sheet in flat plate or spiral wound formats.

14. The method of claim 7 , wherein the membrane is a pleated sheet, in hollow fiber or tubular formats.

15. The method of claim 1 , wherein the porous material is contained in a housing.

16. The method of claim 1 , wherein the porous material is contained in a cartridge.

17. The method of claim 1 , wherein the porous material is a membrane comprising more than 1 layer.

18. The method of claim 1 , wherein the porous material is selected from polyether sulfone, polyamide, nylon, cellulose, polytetrafluoroethylene, polysulfone, polyester, polyvinylidene fluoride, polypropylene, poly(tetrafluoroethylene-co-perfluoro(alkyl vinyl ether)), poly carbonate, polyethylene, glass fiber, polycarbonate, ceramic, and metals.

19. The method of claim 1 , wherein at least one of the gases is hexafluoroethane.

20. A method of assessing the integrity of a porous material loaded into a porous material device using a compressed gas mixture and without the need for any gas component in the gas mixture to achieve a steady state concentration comprising

a) loading a wetted porous material into a device having a housing for receiving the wetted porous material, resulting in a wetted porous material having a feed side and a permeate side;

b) feeding a compressed gas mixture of two or more gas components wherein at least one gas is N 2 and the other gas is O 2 to the feed side of the wetted porous material, wherein the feed gases have differing permeabilities in the liquid used to wet the porous material, such that one of the gases permeates through the liquid of the wetted porous material faster than the other gas or gases used;

c) flushing out the existing gas in the permeate side volume of the porous material and replacing with a gas mixture that has a composition similar to the expected composition of permeate gas generated from an integral membrane;

d) recirculating the permeate gas and venting excess permeate gas while maintaining a feed side gas sweep flow;

e) assessing the concentration of the gas mixture on the permeate side; and

f) comparing the assessed concentration of the permeate gas with the value expected from an integral device, wherein a deviation from the expected concentration by more than predetermined amount is a signal for a non-integral porous material or porous material device.

21. A method of assessing the integrity of a porous material loaded into a porous material device using a compressed gas mixture and without the need for any gas component in the gas mixture to achieve a steady state concentration, comprising:

a) loading a wetted porous material into a device having a housing for receiving the wetted porous material, resulting in a wetted porous material having a feed side and a permeate side;

b) feeding a compressed gas mixture of two or more gas components wherein at least one gas is hexafluoroethane and the other gas is CO 2 to the feed side of the wetted porous material, wherein the feed gases have differing permeabilities in the liquid used to wet the porous material, such that one of the gases permeates through the liquid of the wetted porous material faster than the other gas or gases used;

c) flushing out the existing gas in the permeate side volume of the porous material and replacing with a gas mixture that has a composition similar to the expected composition of permeate gas generated from an integral membrane;

d) recirculating the permeate gas and venting excess permeate gas while maintaining a feed side gas sweep flow;

e) assessing the concentration of the gas mixture on the permeate side; and

f) comparing the assessed concentration of the permeate gas with the value expected from an integral device, wherein a deviation from the expected concentration by more than predetermined amount is a signal for a non-integral porous material or porous material device.

22. A method of assessing the integrity of a porous material loaded into a porous material device using a compressed gas mixture and without the need for any gas component in the gas mixture to achieve a steady state concentration, comprising:

a) loading a wetted porous material into a device having a housing for receiving the wetted porous material, resulting in a wetted porous material having a feed side and a permeate side;

b) feeding a compressed gas mixture of two or more gas components wherein at least one gas is CO 2 and the other gas is O 2 to the feed side of the wetted porous material, wherein the feed gases have differing permeabilities in the liquid used to wet the porous material, such that one of the gases permeates through the liquid of the wetted porous material faster than the other gas or gases used;

c) flushing out the existing gas in the permeate side volume of the porous material and replacing with a gas mixture that has a composition similar to the expected composition of permeate gas generated from an integral membrane;

d) recirculating the permeate gas and venting excess permeate gas while maintaining a feed side gas sweep flow;

e) assessing the concentration of the gas mixture on the permeate side; and

f) comparing the assessed concentration of the permeate gas with the value expected from an integral device, wherein a deviation from the expected concentration by more than predetermined amount is a signal for a non-integral porous material or porous material device.

Assignments (2)
CHANGE OF ADDRESS Recorded Feb 1, 2018
From: EMD MILLIPORE CORPORATION
To: EMD MILLIPORE CORPORATION
Reel/Frame 045225/0156 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 13, 2012
From: HAO, JIBIN; GIGLIA, SALVATORE; JOENS, MICHAEL; TUCELLI, RONALD
To: EMD MILLIPORE CORPORATION
Reel/Frame 028368/0314 →