WO2004003482A2 - Procede et dispositif pour mesurer la permeabilite gazeuse de membranes - Google Patents
Procede et dispositif pour mesurer la permeabilite gazeuse de membranes Download PDFInfo
- Publication number
- WO2004003482A2 WO2004003482A2 PCT/US2003/020592 US0320592W WO2004003482A2 WO 2004003482 A2 WO2004003482 A2 WO 2004003482A2 US 0320592 W US0320592 W US 0320592W WO 2004003482 A2 WO2004003482 A2 WO 2004003482A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- membrane
- cell
- electrode
- permeability
- tube
- Prior art date
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 75
- 230000035699 permeability Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005259 measurement Methods 0.000 title claims description 12
- 230000000694 effects Effects 0.000 claims abstract description 10
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 25
- 239000001257 hydrogen Substances 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000012466 permeate Substances 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 4
- 239000012465 retentate Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 description 20
- 241001354243 Corona Species 0.000 description 16
- 210000004027 cell Anatomy 0.000 description 14
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 6
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 6
- 210000002381 plasma Anatomy 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/40—Semi-permeable membranes or partitions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules
Definitions
- High voltage pulses with duration of about tens of nanoseconds, create an intense electric field in the reaction zone leading to the formation of non-thermal plasma.
- the temperature of the electrons formed from the ionization of the gaseous medium, as characterized by electron velocity/energy, is much higher than the temperature of the much larger bulk gas molecules and other ionic/ charged/excited species leading to a highly efficient process.
- the present invention is described for the characterization of hydrogen-permeable membranes.
- the device and method of the present invention will, in particular, find application where the permeability of hydrogen must be measured for membranes to be used in reactors that employ electrical/electrochemical/photo-electrochemical fields that lead to generation of hydrogen.
- FIG. 1 is a schematic view illustrating the device and method for the measurement of gas permeability through membranes, constructed in accordance with the present invention, membrane characterization and evaluation cell; and
- FIG. 2 is a schematic view illustrating the device and method for the measurement of gas permeability through membranes, constructed in accordance with the present invention, with field and ion flow of the rod-plane corona.
- the present invention is a device for the measuring membrane permeability in electrical/ electrochemical/photo-electrochemical fields.
- the device comprises a permeation cell and a tube mounted within the cell.
- An electrode is mounted at one end of the tube.
- a membrane is mounted within the cell wherein a corona is discharged from the electrode in a general direction toward the membrane thereby generating heated hydrogen atoms adjacent the membrane.
- the present invention further includes a method for measuring the effects of temperature and pressure on membrane permeability and selectivity.
- the method comprises providing a permeation cell, mounting a tube within the cell, mounting an electrode at one end of the tube, mounting a membrane within the cell, introducing gas into the permeation cell, discharging a corona in a general direction toward the membrane thereby generating heated hydrogen atoms adjacent the membrane, measuring the permeate gas and the retentate gas, and determining the hydrogen flux across the membrane.
- the present invention is a device, indicated generally at 10, for the measurement of membrane permeability in electrical/electrochemical/ photo-electrochemical fields.
- the device 10 includes a high field, spherical electrode 12, mounted at the end of a long glass or ceramic tube 14 and inserted into a dome- shaped permeation cell 16 from the top.
- the test membrane 18 is mounted at the bottom of the permeation cell 16.
- the configuration as illustrated herein facilitates a corona discharge, which is a self-sustained electrical discharge in a Laplacian electric field, for the generation of hot hydrogen atoms in the immediate vicinity of the membrane 18.
- a corona discharge consists of high field electrodes or surfaces surrounded by ionization regions producing free charges; low field drift regions in which the free charges drift and react; and low field passive electrodes acting as charge collectors.
- the three regions are illustrated in FIG. 2 for a typical rod-plane corona test configuration.
- the breakdown of the gas leads to the formation and transient propagation of streamers characterized by a luminous track of conduction visible to naked eye; the field and ion flow are also shown as dotted lines in FIG. 2.
- a pulsed voltage will be applied to the electrodes 12 to facilitate the formation of branched streamers.
- the gap break down voltage is dependent on the gap distance and pressure under Paschen's Law.
- the spark gaps tend to have short lifetime of operation and do not provide any control over the initiation of breakdown.
- a thyratron switch 30 can be employed.
- the thyratron switch 30 has a control element known as the grid, which initiates the conduction or breakdown.
- the grid is driven through a driver circuit 32 controlled by a computer. This can provide precise control of the magnitude of the applied pulse voltage.
- a control led-resistance heating jacket 34 is provided around the permeation cell 16 closer to the membrane 18 to facilitate the investigation of the effect of temperature on membrane permeability.
- Various measurement sensors are provided to characterize the permeability of the membrane 18 in terms of input power, and luminosity.
- voltage and current sensors are introduced. These sensors, connected to the oscilloscope, facilitate the measurement of the actual electric power injected into the corona discharge region. In addition, the sensors also provide a time-based description of the voltage and current pulses.
- the luminosity sensor is provided to perform a spectral analysis, if required, of the corona discharge region. A view port is provided to view the streamer corona by the naked eye. Gas flow into the reactor will depend on the type of measurement required. Metered gas, which is hydrogen in a carrier gas for a membrane permeability test, hydrogen with other gases in a carrier gas for a membrane selectivity test, will be introduced into the test cell as shown in FIG. 2.
- the permeate and the retentate will be analyzed to determine the hydrogen flux, corrected for pressure, across the membrane 18.
- the device 10 can then be used to evaluate the effects of: • Pressure; • Temperature; and • Luminosity and input power (related to the production of hot hydrogen atoms) on membrane performance, in terms of permeability and selectivity, for a broad range of operating conditions of interest.
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Fluid Mechanics (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2003263761A AU2003263761A1 (en) | 2002-06-28 | 2003-06-27 | Device and method for the measurement of gas permeability through membranes |
US11/022,245 US7088106B2 (en) | 2003-06-27 | 2004-12-23 | Device and method for the measurement of gas permeability through membranes |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US39220402P | 2002-06-28 | 2002-06-28 | |
US60/392,204 | 2002-06-28 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2004003482A2 true WO2004003482A2 (fr) | 2004-01-08 |
WO2004003482A3 WO2004003482A3 (fr) | 2004-05-06 |
Family
ID=30000827
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2003/020592 WO2004003482A2 (fr) | 2002-06-28 | 2003-06-27 | Procede et dispositif pour mesurer la permeabilite gazeuse de membranes |
Country Status (2)
Country | Link |
---|---|
AU (1) | AU2003263761A1 (fr) |
WO (1) | WO2004003482A2 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2959314A1 (fr) * | 2010-04-26 | 2011-10-28 | Commissariat Energie Atomique | Diagnostic in-situ des proprietes barrieres d'un module photovoltaique |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4046843A (en) * | 1974-09-05 | 1977-09-06 | Sumitomo Chemical Company, Limited | Process for preparing membranes for separation of substances |
US4410338A (en) * | 1979-06-25 | 1983-10-18 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Gas separating members and a method of making the same |
US5062936A (en) * | 1989-07-12 | 1991-11-05 | Thermo Electron Technologies Corporation | Method and apparatus for manufacturing ultrafine particles |
US6245309B1 (en) * | 1996-12-24 | 2001-06-12 | H2-Tech S.A.R.L | Method and devices for producing hydrogen by plasma reformer |
-
2003
- 2003-06-27 WO PCT/US2003/020592 patent/WO2004003482A2/fr not_active Application Discontinuation
- 2003-06-27 AU AU2003263761A patent/AU2003263761A1/en not_active Abandoned
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4046843A (en) * | 1974-09-05 | 1977-09-06 | Sumitomo Chemical Company, Limited | Process for preparing membranes for separation of substances |
US4410338A (en) * | 1979-06-25 | 1983-10-18 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Gas separating members and a method of making the same |
US5062936A (en) * | 1989-07-12 | 1991-11-05 | Thermo Electron Technologies Corporation | Method and apparatus for manufacturing ultrafine particles |
US6245309B1 (en) * | 1996-12-24 | 2001-06-12 | H2-Tech S.A.R.L | Method and devices for producing hydrogen by plasma reformer |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2959314A1 (fr) * | 2010-04-26 | 2011-10-28 | Commissariat Energie Atomique | Diagnostic in-situ des proprietes barrieres d'un module photovoltaique |
Also Published As
Publication number | Publication date |
---|---|
WO2004003482A3 (fr) | 2004-05-06 |
AU2003263761A1 (en) | 2004-01-19 |
AU2003263761A8 (en) | 2004-01-19 |
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