Method and device for testing the permeability of membrane filters

• US 4,614,109 A
• Filed: 07/15/1985
• Issued: 09/30/1986
• Est. Priority Date: 12/27/1982
• Status: Expired due to Fees

• Current Assignee: Memtec America Corporation
• Original Assignee: Brunswick Corporation
• Inventors: Hofmann, Frieder
• Primary Examiner(s): Levy, Stewart J.
• Assistant Examiner(s): ROSKOS, JOSEPH
• Application Number:
  US06/754,583
• Time in Patent Office: 442 Days
• Field of Search: 73/38, 73/40
• US Class Current: 73/38
• CPC Class Codes: B01D 65/102 Detection of leaks in membranes
• CPC Class Codes: G01N 15/0826 and measuring fluid flow rate, i.e. permeation rate or pressure change
• CPC Class Codes: G01N 2015/086 of films, membranes or pellicules

Abstract

The invention pertains to a method and device for testing the permeability of membrane filters by submitting a wetted membrane filter on its inlet side to a predetermined testing gas pressure within a first closed system and by measuring pressure variation over time within the closed system. The object of the method of the invention is a sensitive testing method permitting permeability, and thus pore size, of a membrane filter to be determined exclusively by measurements performed on the inlet side of the membrane filter. Such measurement is performed by measuring a pressure differential with respect to a reference pressure, or by measuring the quantity of gas per unit of time flowing with respect to a reference pressure system, or else by measuring the pressure differential twice and draining, during the second measurement, a predetermined quantity of gas from the space being tested.

Claims

1. Method for testing the permeability of membrane filters by submitting, within a first, closed system, the inlet side of a wetted membrane filter to a predetermined testing gas pressure and measuring the pressure gradient over time within said first, closed system, characterized in that a reference pressure system is brought up to the testing gas pressure at the beginning of any measurement and that the pressure gradient is determined by way of the pressure differential between said first, closed system and said reference pressure system.

2. A method for testing the permeability of membrane filters, said method comprising the steps of:

placing a wetted membrane filter into a housing, said housing having an inlet compartment and an outlet compartment separated by said membrane filter, said housing having a gas manifold attached thereto on the inlet side of said membrane filter, said gas manifold having a source of gas pressure connected thereto by means which allow said source of gas pressure to be either open to or isolated from said gas manifold connected to said inlet side of said membrane filter, when said wetted membrane filter is placed into said housing, said source of gas pressure is isolated from said gas manifold connected to said inlet side of said membrane filter, said gas manifold further having a reference pressure system connected thereto, said reference pressure system comprising a reference pressure source and a differential pressure measuring means, said differential pressure measuring means is connected to said gas manifold connected to said membrane inlet side of said membrane filter and connected to said reference pressure source, said differential pressure measuring means is further connected to a recording means, said reference pressure source is connected to said source of gas pressure by means which allow said reference pressure source to be either open to or isolated from said source of gas pressure, when said wetted membrane filter is placed into said housing, said reference pressure source is isolated from said source of gas pressure;

opening said gas pressure source to said gas manifold connected to said inlet side of said membrane filter;

pressurizing said gas manifold connected to said inlet side of said membrane filter and thereby said inlet side of said membrane filter to a predetermined testing gas pressure by flowing gas from said source of gas pressure into said gas manifold connected to said inlet side of said membrane filter;

isolating said gas pressure source from said gas manifold connected to said inlet side of said membrane filter when said predetermined testing gas pressure is reached;

opening said gas pressure source to said reference pressure source;

pressurizing said reference pressure source to said predetermined testing gas pressure by flowing gas from said source of gas pressure into said reference pressure source;

isolating said gas pressure from said reference pressure source when said predetermined testing gas pressure is reached;

measuring the pressure differential, for a predetermined period of time, between the pressure in said reference pressure source and the pressure in said gas manifold connected to said inlet side of said membrane filter using said differential pressure measuring means; and

recording the measurements obtained from said differential pressure measuring means using said recording means.

3. The method of claim 2 wherein:

the steps of opening said gas pressure source to said gas manifold and said reference pressure source occur simultaneously;

the steps of pressurizing said gas manifold and said reference pressure source to said predetermined testing gas pressure occur simultaneously; and

the steps of isolating said gas pressure source from said gas manifold and said reference pressure source occur simultaneously.

4. A method for testing the pemeability of membrane filters, said method comprising the steps of:

placing a wetted membrane filter into a housing, said housing having an inlet compartment and an outlet compartment separated by said membrane filter, said housing having a gas manifold attached thereto on the inlet side of said membrane filter, said gas manifold having a source of gas pressure connected thereto by means which allow said surface of gas pressure to be either open to or isolated from said gas manifold connected to said inlet side of said membrane filter, when said wetted membrane filter is placed into said housing, said source of gas pressure is isolated from said gas manifold connected to said inlet side of said membrane filter, said gas manifold further having a reference pressure system connected thereto, said reference pressure system comprising a reference pressure source and a differential pressure measuring means, said differential pressure measuring means is connected to said gas manifold connected to said inlet side of said membrane filter and connected to said reference pressure source, said differential pressure measuring means is further connected to a recording means, said reference pressure source is connected to said gas manifold by means which allow said reference pressure source to be either open to or isolated from said gas manifold, when said wetted membrane filter is placed into said housing, said reference pressure source is open to said gas manifold connected to said inlet side of said membrane filter;

opening said gas pressure source to said gas manifold connected to said inlet side of said membrane filter;

pressurizing said gas manifold connected to said inlet side of said membrane filter, and thereby said inlet side of said membrane filter and said reference pressure source, to a predetermined testing gas pressure by flowing gas from said source of gas pressure into said gas manifold connected to said inlet side of said membrane filter;

isolating said gas pressure source from said gas manifold connected to said inlet side of said membrane filter when said predetermined testing gas pressure is reached;

isolating said reference pressure source from said gas manifold connected to said inlet side of said membrane filter;

measuring the pressure differential, for a predetermined period of time, between the pressure in said reference pressure source and the pressure in said gas manifold connected to said inlet side of said membrane filter using said differential pressure measuring means; and

recording the measurements obtained from said differential pressure measuring means using said recording means.

5. The method of claim 4 which comprises the further steps of:

prior to said step of isolating said reference pressure source from said said gas manifold connected to said inlet side of said membrane, measuring the drop in pressure in said gas manifold connected to said inlet side of said membrane and in said reference pressure source;

recording the measurements obtained; and

stopping the test if said measurements indicate that said membrane filter is leaking or damaged.

6. A method for calibrating a measurement system for testing the permeability of membrane filters, said method comprising the steps of:

placing a wetted membrane filter into a housing, said housing having an inlet compartment and an outlet compartment separated by said membrane filter, said housing having a gas manifold attached thereto on the inlet side of said membrane filter, said gas manifold having a source of gas pressure connected thereto by means which allow said source of gas pressure to be either open to or isolated from said gas manifold connected to said inlet side of said membrane filter, when said wetted membrane filter is placed into said housing, said source of gas pressure is isolated from said gas manifold connected to said inlet side of said membrane filter, said gas manifold further having a reference pressure system connected thereto, said reference pressure system comprising a reference pressure source and a differential pressure measuring means, said differential pressure measuring means is connected to said gas manifold connected to said inlet side of said membrane filter and connected to said reference pressure source, said differential pressure measuring means is further connected to a recording means, said reference pressure source is connected to said gas manifold by means which allow said reference pressure source to be either open to or isolated from said gas manifold, when said wetted membrane filter is placed into said housing, said reference pressure source is open to said gas manifold connected to said inlet side of said membrane filter;

opening said gas pressure source to said gas manifold connected to said inlet side of said membrane filter;

pressurizing said gas manifold connected to said inlet side of said membrane filter and thereby, said inlet side of said membrane filter and said reference pressure source, to a predetermined testing gas pressure by flowing gas from said source of gas pressure into said gas manifold connected to said inlet side of said membrane filter;

isolating said gas pressure source from said gas manifold connected to said inlet side of said membrane filter when said predetermined testing gas pressure is reached;

isolating said reference pressure source from said gas manifold connected to said inlet side of said membrane filter;

measuring the pressure differential, for a predetermined period of time, between the pressure in said reference pressure source and the pressure in said gas manifold connected to said inlet side of said membrane filter using said differential pressure measuring means;

recording the measurements obtained from said differential pressure measuring means using said recording means;

opening said reference pressure source to said gas manifold connected to said inlet side of said membrane filter;

opening said gas pressure source to said gas manifold connected to said inlet side of said membrane filter;

repressurizing said gas manifold connected to said inlet side of said membrane filter, and thereby said inlet side of said membrane filter and said reference pressure source to a second predetermined testing gas pressure, which may be the same as said first predetermined testing gas pressure, by flowing gas from said source of gas pressure into said gas manifold connected to said inlet side of said membrane filter;

isolating said gas pressure source from said gas manifold connected to said inlet side of said membrane filter when said second predetermined testing gas pressure is reached;

isolating said reference pressure source from said gas manifold connected to said inlet side of said membrane filter;

measuring the pressure differential, for a predetermined period of time, between the pressure in said reference pressure source and the pressure in said gas manifold connected to said inlet side of said membrane filter using said differential pressure measuring means;

recording the measurements obtained from said differential pressure measuring means using said recording means;

releasing a predetermined volume of gas from said gas manifold connected to the inlet side of said membrane filter;

measuring the pressure differential, resulting from said release of said predetermined volume of gas between the pressure in said reference pressure source and the pressure in said gas manifold connected to said inlet side of said membrane filter using said differential pressure measuring means;

recording the measurements obtained from said differential pressure measuring means using said recording means;

stopping said release of gas from said gas manifold once said predetermined volume of gas has been released; and

calculating the flow rate through said membrane filter.

7. A device for testing the premeability of membrane filters, said device comprising:

a housing, said housing having an inlet compartment and an outlet compartment separated by a wetted membrane filter;

a gas manifold attached to said housing on the inlet side of said membrane filter;

a source of gas pressure connected to said gas manifold by means which allow said source of gas pressure to be either open to or isolated from said gas manifold connected to said inlet side of said membrane filter;

a reference pressure system comprising a reference pressure source and a differential pressure measuring means;

said differential pressure measuring means connected to said reference pressure source and connected to said gas manifold connected to said inlet side of said membrane filter;

said reference pressure source connected to said source of gas pressure by means which allow said reference pressure source to be either open to or isolated from said source of gas pressure; and

recording means connected to said differential pressure measuring means.

8. The device of claim 7 wherein said means which allow said reference pressure source to be either open to or isolated from said source of gas pressure is a pneumatically controlled shut-off valve.

9. The device of claim 8 wherein an electromagnetically controlled valve is provided to control said pneumatically controlled shut-off valve.

10. The device of claim 7 wherein a second pressure measuring device is connected to said inlet side of said membrane filter.

11. A device for testing the premeability of membrane filters, said device comprising:

a housing, said housing having an inlet compartment and an outlet compartment separated by a wetted membrane filter;

a gas manifold attached to said housing on the inlet side of said membrane filter;

a source of gas pressure connected to said gas manifold by means which allow said source of gas pressure to be either open to or isolated from said gas manifold connected to said inlet side of said membrane filter;

a reference pressure system comprising a reference pressure source and a differential pressure measuring means;

said differential pressure measuring means connected to said reference pressure source and connected to said gas manifold connected to said inlet side of said membrane filter;

said reference pressure source connected to said gas manifold by means which allow said reference pressure source to be either open to or isolated from said gas manifold; and

recording means connected to said differential pressure measuring means.

12. The device of claim 11 wherein said means which allow said reference pressure source to be either open to or isolated from said gas manifold is a pneumatically controlled shut-off valve.

13. The device of claim 12 wherein an electromagnetically controlled valve is provided to control said pneumatically controlled shut-off valve.

14. The device of claim 11 wherein a second pressure measuring device is connected to said inlet side of said membrane filter.

15. The device of claim 11 wherein a gas release control valve is connected to said gas manifold connected to said inlet side of said membrane filter.

16. The device of claim 15 wherein said gas release control valve is connected to a measuring device which measures gas volume.