Water intrusion test for filters

• US 5,786,528 A
• Filed: 09/10/1996
• Issued: 07/28/1998
• Est. Priority Date: 09/10/1996
• Status: Expired due to Term

• Current Assignee: EMD Millipore Corporation (Merck & Co., Inc.)
• Original Assignee: Millipore Corporation (Merck & Co., Inc.)
• Inventors: Dileo, Anthony J., Gray, Richard W.
• Primary Examiner(s): BROCK, MICHAEL J
• Application Number:
  US08/711,755
• Time in Patent Office: 686 Days
• Field of Search: 73/38, 73/40, 210/85, 210/87, 210/90
• 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 15/088 Investigating volume, surface area, size or distribution of pores; Porosimetry

Abstract

An improved water flow test for determining the integrity and/or pore size distribution of a porous filter is disclosed. The improvement involves the ability to determine and take into account the changes in filter structure due to filter compaction or creep resulting from compressive forces when pressure is applied to the surfaces of the filter. By proper characterization of the filter under test, the initial system volume and the volume change associated with pressurizing the filter can be accurately determined at all points in time during a test cycle. As a result, composite flowrate changes (i.e. the flow due to filter compaction/creep plus the flow due to liquid intrusion) can be evaluated to distinguish between various flow components to accurately determine the pore size of the filter being tested or a filter defect.

Claims

1. A method for determining the integrity and/or pore size distribution of a porous filter by water intrusion flow testing which comprises:

positioning said filter in a test cell,

introducing into said test cell a liquid a liquid which does not instantaneously filter into said test cell, the volume of said liquid being sufficient to surround said filter;

providing an enclosed gas space in fluid communication with said liquid, the combination of the volume of said gas space, the volume of said liquid surrounding said filter device and the volume of liquid within said filter device defining a system volume;

applying a pressure through said gas space to produce a composite liquid flowrate in said test cell consisting of a first flow component representative of a change in volume of said filter due to structural changes of said filter resulting form the compressive effects of applied pressure and a second flow component representative of liquid intrusion into and leaking from the pores of said filter;

calculating the cumulative volume of said gas space while pressure is applied to said filter to derive a value of said system volume at any time while pressure is applied;

determining an adjusted composite liquid flowrate measurement from said derived value of said system volume which is essentially solely indicative of said second flow component; and

correlating said adjusted composite liquid flowrate with a pre-determined flowrate value indicative of known integral and/or rated pore size filters whereby the integrity and/or pore size distribution of said filter under test may be accurately determined.

2. The method of claim 1 wherein the cumulative gas volume is calculated by combining a predetermined characteristic response of the change in volume of said filter as a function of pressure, temperature and time with a determination of the initial volume of said gas space prior to applying pressure thereto.

3. The method of claim 2 wherein said characteristic response is determined a priori by applying a constant pressure source at constant temperature to said test cell and monitoring over time the change in volume of said filter.

4. The method of claim 2 wherein said initial volume of said gas space is determined by measuring the pressure changes resulting from adding a known gas volume at elevated pressure to said gas space and computing the corresponding volume change resulting from said added known gas volume and subtracting a second smaller cumulative gas volume at the time of said computing step, said second volume being determined in accordance with said characteristic response, to arrive at said initial volume.

5. The method of claim 2 wherein said initial volume of said gas space is determined by measuring the pressure changes resulting from the addition of a known mass of gas to said gas space and computing the corresponding volume change resulting from said added known mass of gas and subtracting a second smaller cumulative gas volume at the time of said computing step, said second volume being determined in accordance with said characteristic response, to arrive at said initial volume.

6. The method of claim 2 wherein said adjusted flowrate is determined by the product of a measured pressure change from applying pressure at the time an integrity and/or pore size distribution test isconducted and the cumulative gas volume calculated at that point in time.

7. The method of claim 1 wherein the cumulative gas volume is calculated by combining a linear characteristic response of the change in volume of said filter which includes a linear response constant and a function of time with a measure of the initial volume of said gas space prior to applying pressure thereto.

8. The method of claim 7 wherein said initial volume of said gas space is determined by measuring pressure changes resulting from the adding known gas volumes at elevated pressure to said gas space while simultaneously determining said linear response characteristic.

9. The method of claim 8 wherein said initial volume of said gas space is determined by measuring the pressure change in said test cell after a predetermined period of time after adding a known gas volume at an elevated first pressure followed by the step of measuring the pressure change after a predetermined period of time after adding a second known gas volume at an elevated second pressure greater than said first pressure and combining each of said measured pressure changes to determine said cumulative gas volume and said linear response characteristic.

10. The method of claim 7 wherein said initial volume of said gas space is determined by measuring the pressure changes resulting from adding a known mass of gas to said gas space while simultaneously determining said linear response characteristic.

11. The method of claim 7 wherein said adjusted flowrate is determined by the product of a measured pressure change from applying pressure at the time an integrity and/or pore size distribution test is conducted and the cumulative gas volume calculated at that point in time.