Method and apparatus for on-line measurement of the permeation characteristics of a permeant through dense nonporous membrane

• US 6,335,202 B1
• Filed: 06/10/1999
• Issued: 01/01/2002
• Est. Priority Date: 06/11/1998
• Status: Expired due to Fees

• Current Assignee: Korea Research Institute of Chemical Technology
• Original Assignee: Korea Research Institute of Chemical Technology
• Inventors: Kim, Beom Sik, Yeom, Choong Kyun, Kim, Kwang Joo, Kim, Chul Ung, Lee, Jung Min
• Primary Examiner(s): LUDLOW, JAN M
• Application Number:
  US09/329,492
• Time in Patent Office: 936 Days
• Field of Search: 422/68.1, 422/89, 436/161, 436/5, 73/38, 73/644.7
• US Class Current: 436/161
• CPC Class Codes: G01N 15/0826 and measuring fluid flow rate, i.e. permeation rate or pressure change
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 30/82 Automatic means therefor

Abstract

This invention relates to a method and apparatus for on-line measurement of permeation characteristics (transmitting chemicals) through dense nonporous membrane. This invention is intended to facilitate various research activities, such as simultaneous analyses of diffusion coefficient, solubility coefficient, permeation rate and permeant composition, and presentation of new analysis about the permeation behavior, kinetics and so on. The object of this invention is to provide the method and apparatus for measurement of permeation characteristics of permeants in liquid, vapor or gas phase through dense nonporous membrane and more practicuraly, to provide permeation apparatus for measurement of permeation characteristics by analyzing permeation rate and permeation concentration of permeants through an on-line type dense porous membrane with time, not only for a steady state but also for an unsteady state in an accurate and reliable manner.

Claims

1. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane, comprising:

(a) storing a liquid feed in a feed tank at a prescribed temperature;

(b) permeating said liquid feed from said feed tank through a membrane from which moisture residues and volatile components have been eliminated and the temperature of which is kept constant by a heating oven;

(c) passing the permeant from said membrane through a mass flow meter to generate a potential difference, which is simultaneously displayed and recorded with time in a recorder that is connected to a digital display, to measure the permeation rate thereof;

(d) measuring the composition of the permeant on-line by passing the permeant from said mass flow meter through a gas chromatograph equipped with a thermal conductivity detector; and

(e) condensing the permeant after passing said gas chromatograph with a condenser equipped with a refrigerator.

2. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 1, wherein nitrogen gas or dry air from a gas inlet that is connected to a gas supplier purges the top surface of said membrane in order to keep said membrane dry by removing the moisture residues and volatile components, and wherein the bottom surface of said membrane is vacuous prior to said permeating.

3. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 1, further comprising controlling the temperature in order to prevent condensing the permeant between said membrane and said mass flow meter.

4. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 1, wherein the potential difference detected by the mass flow meter is recorded with time, and, at the same time, this potential difference is converted into the permeation rate by the relation equation of the magnitude of the potential difference and the permeation rate, and recorded.

5. An apparatus for measuring permeation characteristics of a permeant through a dense nonporous membrane, comprising:

(a) a feed tank, capable of storing a liquid feed, attached to a cooler and an electric heater, and connected to a temperature controller for controlling the temperature of said liquid feed;

(b) a feed pump, connected to said feed tank by a first line, in order to discharge said liquid feed;

(c) a membrane installed inside a cell in a heating oven, connected to said feed pump by a second line, through which said liquid feed is discharged and circulated by the propulsion of said feed pump;

(d) a mass flow meter, connected to the lower part of said cell including said membrane by a third line which is enclosed by a heating band, capable of measuring the permeation rate of said permeant;

(e) a digital display, in communication with said mass flow meter, which displays the permeation rate detected by the mass flow meter in the form of a volume flow rate;

(f) a recorder, in communication with said digital display, which converts the change of the potential difference of said mass flow meter to the change of the permeation rate and records the permeation rate with time;

(g) a gas chromatograph, connected to an outlet of said mass flow meter by a fourth line, for measuring the permeant composition by an on-line method;

(h) a secondary condenser and a condenser, connected by a fifth line to said gas chromatograph, for condensing the permeant located after said gas chromatography and

(i) a vacuum, in communication with said membrane.

6. An apparatus for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 5, wherein said mass flow meter and said recorder are connected directly to each other in order to detect potential differences generated by said permeant in the mass flow meter.

7. An apparatus for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 5, further comprising a gas inlet on said second line between said feed pump and said membrane, and further comprising a back pressure controller to control the pressure of the feed at said purge gas inlet.

8. An apparatus for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 5, further comprising a solenoid valve on said third line between said membrane and said mass flow meter in order to automatically shut off the flow of the permeant.

9. An apparatus for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 5, further comprising a temperature controller on said fifth line between said gas chromatograph and said secondary condenser in order to control the temperature of said third line enclosed by the heating band for the prevention of condensation of said permeant on the lower part of said membrane.

10. An apparatus for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 5, further comprising a temperature controller on said fifth line between said gas chromatograph and said secondary condenser in order to control the temperature of said third line for the prevention of condensation of said permeant on the lower part of said membrane.

11. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane, comprising:

(a) injecting a vapor phase feed into a gas inlet;

(b) permeating said vapor phase feed from said gas inlet through a membrane from top surface to a bottom surface while evacuating the bottom surface from which moisture residues and volatile components have been eliminated and the temperature of which is kept constant by a heating oven;

(c) passing the permeant from said membrane through a mass flow meter to generate a potential difference, which is simultaneously displayed and recorded with time in a recorder that is connected to a digital display, to measure the permeation rate thereof;

(d) measuring the composition of the permeant on-line by passing the permeant from said mass flow meter through a gas chromatograph equipped with a thermal conductivity detector; and

(e) condensing the permeant after passing said gas chromatograph with al condenser equipped with a refrigerator.

12. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 11, wherein nitrogen gas or dry air from a gas inlet that is connected to a gas supplier purges a top surface of said membrane in order to keep said membrane dry by removing the moisture residues and volatile components, and wherein the bottom surface of said membrane is vacuous prior to said permeating.

13. A method for measuring permeation characteristics of a permelant through a dense nonporous membrane according to claim 11, further comprising controlling the temperature in order to prevent condensing the permeant between said membrane and said mass flow meter.

14. A method for measuring permeation characteristics of a permeant through a dense nonporous membrane according to claim 11, wherein the potential difference detected by the mass flow meter is recorded with time and, at the same time, this potential difference is converted into the permeation rate by the relation equation of the magnitude of the potential difference and the permeation rate, and recorded.