EP1309391A1 - Water separation from solvent - Google Patents
Water separation from solventInfo
- Publication number
- EP1309391A1 EP1309391A1 EP01953392A EP01953392A EP1309391A1 EP 1309391 A1 EP1309391 A1 EP 1309391A1 EP 01953392 A EP01953392 A EP 01953392A EP 01953392 A EP01953392 A EP 01953392A EP 1309391 A1 EP1309391 A1 EP 1309391A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- membrane
- layer
- solvent
- reservoir
- fluoropolymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002904 solvent Substances 0.000 title claims abstract description 46
- 238000000926 separation method Methods 0.000 title description 3
- 239000012528 membrane Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 32
- 229920002313 fluoropolymer Polymers 0.000 claims abstract description 29
- 239000004811 fluoropolymer Substances 0.000 claims abstract description 29
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 230000003247 decreasing effect Effects 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 3
- 230000003111 delayed effect Effects 0.000 claims 2
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 description 10
- 235000011152 sodium sulphate Nutrition 0.000 description 10
- 239000000839 emulsion Substances 0.000 description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 description 7
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 230000002238 attenuated effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000001010 compromised effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920001780 ECTFE Polymers 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1213—Laminated layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/18—Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/22—Controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
- G01N2001/4016—Concentrating samples by transferring a selected component through a membrane being a selective membrane, e.g. dialysis or osmosis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
Definitions
- the solvent extracts the compounds from the sample, due to selective chemistry. Before the extract can be analyzed, all residual water should preferably be removed from the extracting solvent. This is due to the adverse effect residual water can have on subsequent sample preparation steps which are required to prepare and analyze the samples.
- Current practice embodies the use of a drying agent called sodium sulfate and has been the standard technique to remove the residual water from solvent extracts.
- Sodium sulfate is a granular material that has a high binding capacity for residual water. The sodium sulfate is first heated to drive off any water that has been adsorbed into the material. This typically requires heating overnight at 400C. The sodium sulfate is then placed into a glass funnel containing filter paper, or a chromatography column.
- Patent 5,268,150 assigned to Corning Incorporated discloses the use of a hydrophobic membrane in an extraction device which allows a solvent to pass therethrough, yet will not allow a significant amount of water from the sample liquid to pass therethrough.
- the patent discloses that hydrophobic membranes incorporating polytetrafluoroethylene (PTFE) have been found to be very effective in achieving the desired results of letting solvent pass, while retaining the sample usually consisting of a relatively large portion of water or an aqueous solution.
- the patent goes on to state that the typical dimensions of the membrane range from 10 to 50 millimeters in diameter with a thickness ranging from 0.1 to 5.0 microns with a pore size ranging from 0.2 to 5.0 microns, depending upon the sample being processed.
- a method/apparatus for separating residual water from a solvent comprising the steps of providing a reservoir containing a solution comprising solvent containing residual water, the reservoir having an opening to allow the solution to drain from the reservoir, and passing the solution in the reservoir through a fluoropolymer membrane supported on a fluoropolymer screen.
- FIG. 1 is a sectional view of a first separator apparatus in accordance with the present invention
- Figure 2 is a sectional view of a second separator apparatus in accordance with the present invention
- Figure 3 is an exploded view of a preferred separator apparatus in accordance with the present invention.
- the concentrator/extractor apparatus 100 comprises a column 102 and fluoropolymer material layers 104 and 105.
- fluoropolymer layer 104 is laminated to fluoropolymer layer 105 to provide a membrane type construction.
- a preferred fluoropolymer for layer 104 is PTFE and a preferred fluoropolymer for layer 105 is ethylene- chlorotrifiuroethylene (ECTFE).
- a screen support layer is shown at 106, in addition to a base assembly 108, and a collection vessel 110.
- the column 102 forms a reservoir to hold a solvent.
- the column 102 which may be pressed down on top of the membrane (fluoropolymer layer 104 laminated to fluoropolymer layer 105) may be used to hold the membrane in place.
- the column 102 may seal the membrane and prevent any solvent from passing around the edge of the membrane.
- the column 102 and the collection vessel 110 are preferably made of glass.
- the screen support member 106 is preferably an ECTFE or ETFE fluoropolymer fabric screen with 0.5- 1.0 mm openings, 0.5 -1.0 mm thick, and a 0.25-0.50 mm thread.
- the membrane comprises layers 104 and 105 are preferably characterized as follows: Pore Size: 0.05 to 0.2 micron; Bubble Point: Individual between 24.0 psi and 34.0 psi (47 mm membrane; isopropanol at 21°C) WEP: 50.0 psi minimum individual Gurley Number: Mean ⁇ 30.0 seconds (100 cc air through 1 in 2 orifice, 4.88" water pressure drop) Thickness: Preferably 1.0 mils to 20 mils.
- Gurley number A measure of the air permeability of the fluoropolymer.
- Gurley number is the time in second required for lOOcc of air to pass through a one square inch area of membrane, when a constant pressure of 4.88 inches of water is applied.
- Bubble point The minimum pressure in KG/CM 2 required to force air through the fluoropolymer that has been prewetted with water, isopropanol, or methanol.
- Water entry pressure The pressure at which water permeates through the membrane. This is a visual test.
- the PTFE layer 104 has usable diameters in the range of 40-100 mm.
- the fluoropolymer layer 104 and fabric support member 105 are positioned in series between the column 102 and the collection vessel 110.
- a 3 mil thick PTFE layer 104 with a 0.1 micron pore size is supported on a 10 mil thick non- woven layer 105, comprised of ECTFE polymer, which ECTFE polymer is preferably obtained from Ausimont and sold under the tradename "HALAR".
- ECTFE polymer which ECTFE polymer is preferably obtained from Ausimont and sold under the tradename "HALAR”.
- a 3.0 mil PTFE layer is laminated to a 10 mil ECTFE layer, and a resulting thickness of 3-7 mils is produced for the laminate as a result of the heat setting laminating process.
- the screen layer 106 is preferably ethylene- trifluroethylene copolymer (ETFE).
- ETFE ethylene- trifluroethylene copolymer
- the screen layer serves to gap or space laminated layers 104 and 105 on the funnel surface such that it is possible to distribute the pressure differential across the entire cross-sectional area of the funnel surface to achieve more efficient performance.
- screen layer 106 is a separate components, it can be appreciated that screen layer 106 may actually be incorporated directly into the surface of the funnel upon which the laminated layers 104 and 106 rest. This would provide the equivalent effect of spacing laminated layers 104 and 106 to evenly distribute the pressure differential created by vacuum.
- the removal of water from a given solvent containing, e.g., some analyte to be evaluated by techniques such as gas-chromatography/mass spectrometry (GC/MS), is such that the removal of water is highly efficient and allows for the generation of a GC/MS analysis that is not compromised by the presence of water.
- GC/MS gas-chromatography/mass spectrometry
- the concentrator/extractor apparatus 200 comprises a column 202, a fluoropolymer layer 204 (PTFE) and a fluoropolymer layer 205 (ECTFE) that, as noted above, are preferably laminated to one another.
- PTFE fluoropolymer layer 204
- ECTFE fluoropolymer layer 205
- a support screen member 206 is shown, a base assembly 208, and a collection vessel 210.
- the apparatus 200 can be coupled to an external low-level vacuum 216.
- a low level vacuum is one that preferably creates a pressure drop of less than 6" Hg.
- the assembly 200 could include a vacuum generator device that uses a compressed gas source to create a pressure differential.
- This assembly 200 could be manufactured as a unit and could sit in a hood, directly underneath a separatory funnel.
- the operator may select one of a plurality of vacuum levels on a vacuum level selector panel 214.
- the vacuum selector panel 214 controls the pressure drop across the membrane. These levels may include: off, low, medium, and high. Alternatively, the vacuum level may be continuously variable. Being able to select from a variety of different vacuum levels has shown to be useful, as samples which create a significant emulsion can be quite easily broken if no vacuum is used. Once the emulsion has broken, then the vacuum setting can be increased to significantly reduce the sample process time.
- a controller 212 coupled to the vacuum 216 can be added that will vary the pressure drop across the membrane as a function of time.
- the controller 212 can be programmed to have an initial predetermined period of time during which no vacuum or a very low first predetermined vacuum level is applied and a second predetermined period of time during which an increased second predetermined vacuum level is applied.
- the controller 212 can also be programmed to turn off the vacuum after a third predetermined period of time to prevent the apparatus from pulling residual water through the membrane.
- FIG. 3 is an exploded view of a preferred separator apparatus in accordance with the present invention.
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US21505500P | 2000-06-29 | 2000-06-29 | |
US215055P | 2000-06-29 | ||
PCT/US2001/020555 WO2002002211A1 (en) | 2000-06-29 | 2001-06-27 | Water separation from solvent |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1309391A1 true EP1309391A1 (en) | 2003-05-14 |
EP1309391A4 EP1309391A4 (en) | 2005-04-27 |
Family
ID=22801455
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP01953392A Withdrawn EP1309391A4 (en) | 2000-06-29 | 2001-06-27 | Water separation from solvent |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP1309391A4 (en) |
JP (1) | JP4150586B2 (en) |
AU (1) | AU2001275846A1 (en) |
CA (1) | CA2413799C (en) |
WO (1) | WO2002002211A1 (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7935536B2 (en) | 2005-07-27 | 2011-05-03 | HorizonTechnology, Inc. | System for water removal and solvent evaporation |
ITFI20130016A1 (en) * | 2013-01-21 | 2014-07-22 | Aautomag S R L | "CONTAINER FOR FILTER ELEMENTS, DEVICE USING THIS CONTAINER AND MICROFILTRATION METHOD" |
KR102314988B1 (en) * | 2014-12-26 | 2021-10-21 | 솔브레인 주식회사 | Graphene Membrane Film and Method for Solvent Purification and Solvent Purification System using the Same |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5066403A (en) * | 1990-07-12 | 1991-11-19 | The United States Of America As Represented By The Secretary Of Commerce | Process for separating azeotropic or close-boiling mixtures by use of a composite membrane, the membrane, and its process of manufacture |
US5552023A (en) * | 1993-12-15 | 1996-09-03 | Alliedsignal Inc. | Recovery of spent deicing fluid |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5579011A (en) * | 1978-12-13 | 1980-06-14 | Asahi Chem Ind Co Ltd | Separation of oil emulsion |
JPS5922603A (en) * | 1982-07-27 | 1984-02-04 | Kanegafuchi Chem Ind Co Ltd | Method and device for separating two phase mixed liquid |
DE68915554T2 (en) * | 1988-01-26 | 1995-01-12 | Asahi Glass Co Ltd | For vapor permselective membrane. |
JPH0822372B2 (en) * | 1989-06-24 | 1996-03-06 | 日東電工株式会社 | Composite porous membrane |
JPH03249926A (en) * | 1990-02-28 | 1991-11-07 | Ishikawa Seisakusho:Kk | Filter device |
US5454951A (en) * | 1993-03-05 | 1995-10-03 | Minnesota Mining And Manufacturing Company | Separation-science medium support plate |
JP3094135B2 (en) * | 1993-09-20 | 2000-10-03 | 東洋濾紙株式会社 | Structure of filter sheet made of all fluororesin |
US5603900A (en) * | 1995-05-19 | 1997-02-18 | Millipore Investment Holdings Limited | Vacuum filter device |
US5976380A (en) * | 1997-05-01 | 1999-11-02 | Millipore Corporation | Article of manufacture including a surface modified membrane and process |
JPH11244667A (en) * | 1998-02-27 | 1999-09-14 | Mitsubishi Rayon Co Ltd | Crude oil treating device and treatment of crude oil using the device |
-
2001
- 2001-06-27 CA CA2413799A patent/CA2413799C/en not_active Expired - Lifetime
- 2001-06-27 AU AU2001275846A patent/AU2001275846A1/en not_active Abandoned
- 2001-06-27 JP JP2002506831A patent/JP4150586B2/en not_active Expired - Lifetime
- 2001-06-27 WO PCT/US2001/020555 patent/WO2002002211A1/en active Application Filing
- 2001-06-27 EP EP01953392A patent/EP1309391A4/en not_active Withdrawn
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5066403A (en) * | 1990-07-12 | 1991-11-19 | The United States Of America As Represented By The Secretary Of Commerce | Process for separating azeotropic or close-boiling mixtures by use of a composite membrane, the membrane, and its process of manufacture |
US5552023A (en) * | 1993-12-15 | 1996-09-03 | Alliedsignal Inc. | Recovery of spent deicing fluid |
Non-Patent Citations (2)
Title |
---|
No further relevant documents disclosed * |
See also references of WO0202211A1 * |
Also Published As
Publication number | Publication date |
---|---|
EP1309391A4 (en) | 2005-04-27 |
CA2413799A1 (en) | 2002-01-10 |
JP4150586B2 (en) | 2008-09-17 |
WO2002002211A1 (en) | 2002-01-10 |
AU2001275846A1 (en) | 2002-01-14 |
CA2413799C (en) | 2010-08-24 |
JP2004501756A (en) | 2004-01-22 |
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AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO SI |
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A4 | Supplementary search report drawn up and despatched |
Effective date: 20050310 |
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RIC1 | Information provided on ipc code assigned before grant |
Ipc: 7G 01N 1/40 B Ipc: 7G 01N 1/34 B Ipc: 7B 01D 71/36 B Ipc: 7B 01D 71/32 B Ipc: 7B 01D 69/12 B Ipc: 7B 01D 69/10 B Ipc: 7B 01D 61/22 B Ipc: 7B 01D 61/18 B Ipc: 7B 01D 61/14 B Ipc: 7B 01D 17/00 B Ipc: 7B 01D 61/00 A |
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17Q | First examination report despatched |
Effective date: 20071123 |
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Free format text: STATUS: THE APPLICATION HAS BEEN WITHDRAWN |
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18W | Application withdrawn |
Effective date: 20111108 |