ZA200203488B - Method for recovering fluorinated emulsifiers. - Google Patents
Method for recovering fluorinated emulsifiers. Download PDFInfo
- Publication number
- ZA200203488B ZA200203488B ZA200203488A ZA200203488A ZA200203488B ZA 200203488 B ZA200203488 B ZA 200203488B ZA 200203488 A ZA200203488 A ZA 200203488A ZA 200203488 A ZA200203488 A ZA 200203488A ZA 200203488 B ZA200203488 B ZA 200203488B
- Authority
- ZA
- South Africa
- Prior art keywords
- apfos
- ppm
- emulsifiers
- aqueous
- fluorinated
- Prior art date
Links
- 239000003995 emulsifying agent Substances 0.000 title claims description 27
- 238000000034 method Methods 0.000 title claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 150000001450 anions Chemical class 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 17
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 2
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 2
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 229920001429 chelating resin Polymers 0.000 description 9
- 238000010828 elution Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229920002313 fluoropolymer Polymers 0.000 description 6
- 239000004811 fluoropolymer Substances 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000004816 latex Substances 0.000 description 4
- 229920000126 latex Polymers 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 239000003480 eluent Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 150000003460 sulfonic acids Chemical class 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001348 alkyl chlorides Chemical class 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 150000001983 dialkylethers Chemical class 0.000 description 1
- ZKBBUZRGPULIRN-UHFFFAOYSA-N diethyl 2,2-diethylpropanedioate Chemical compound CCOC(=O)C(CC)(CC)C(=O)OCC ZKBBUZRGPULIRN-UHFFFAOYSA-N 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000004815 dispersion polymer Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229960004592 isopropanol Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 150000004672 propanoic acids Chemical class 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/04—Processes using organic exchangers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19953285A DE19953285A1 (de) | 1999-11-05 | 1999-11-05 | Verfahren zur Rückgewinnung fluorierter Emulgatoren |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| ZA200203488B true ZA200203488B (en) | 2003-08-04 |
Family
ID=7928031
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| ZA200203488A ZA200203488B (en) | 1999-11-05 | 2002-05-02 | Method for recovering fluorinated emulsifiers. |
Country Status (11)
| Country | Link |
|---|---|
| US (1) | US6642415B1 (enExample) |
| EP (1) | EP1240107B1 (enExample) |
| JP (1) | JP2003512931A (enExample) |
| CN (1) | CN1174924C (enExample) |
| AU (1) | AU7924000A (enExample) |
| CA (1) | CA2387781A1 (enExample) |
| DE (2) | DE19953285A1 (enExample) |
| PL (1) | PL354617A1 (enExample) |
| RU (1) | RU2255807C2 (enExample) |
| WO (1) | WO2001032563A1 (enExample) |
| ZA (1) | ZA200203488B (enExample) |
Families Citing this family (41)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002059160A (ja) * | 2000-08-11 | 2002-02-26 | Daikin Ind Ltd | 含フッ素陰イオン系界面活性剤の分離方法 |
| US7279522B2 (en) | 2001-09-05 | 2007-10-09 | 3M Innovative Properties Company | Fluoropolymer dispersions containing no or little low molecular weight fluorinated surfactant |
| JP2003220393A (ja) * | 2001-11-22 | 2003-08-05 | Asahi Glass Co Ltd | 含フッ素乳化剤の吸着・回収方法 |
| EP1364972B1 (en) * | 2002-05-22 | 2006-08-30 | 3M Innovative Properties Company | Process for reducing the amount of fluorinated surfactant in aqueous fluoropolymer dispersions |
| DE60301322T2 (de) * | 2003-02-28 | 2006-06-08 | 3M Innovative Properties Co., St. Paul | Fluoropolymerdispersion enthaltend kein oder wenig fluorhaltiges Netzmittel mit niedrigem Molekulargewicht |
| WO2005065800A1 (en) * | 2003-12-30 | 2005-07-21 | Daikin Industries, Ltd. | Process for separating fluorine-containing surfactant |
| US20060014887A1 (en) * | 2004-07-19 | 2006-01-19 | 3M Innovative Properties Company | Method of hydrolyzing a dispersion of ionic fluoropolymer |
| US7304101B2 (en) * | 2004-07-19 | 2007-12-04 | 3M Innovative Properties Company | Method of purifying a dispersion of ionic fluoropolymer |
| US7666927B2 (en) * | 2004-12-22 | 2010-02-23 | E.I. Du Pont De Nemours And Company | Removing fluorosurfactant from aqueous fluoropolymer dispersions using anion exchange polymer with functional groups resistant to degradation to trialkylamines |
| EP1700869A1 (en) * | 2005-03-11 | 2006-09-13 | 3M Innovative Properties Company | Recovery of fluorinated surfactants from a basic anion exchange resin having quaternary ammonium groups |
| US7671112B2 (en) | 2005-07-15 | 2010-03-02 | 3M Innovative Properties Company | Method of making fluoropolymer dispersion |
| US20080015304A1 (en) | 2006-07-13 | 2008-01-17 | Klaus Hintzer | Aqueous emulsion polymerization process for producing fluoropolymers |
| GB0525978D0 (en) | 2005-12-21 | 2006-02-01 | 3M Innovative Properties Co | Fluorinated Surfactants For Making Fluoropolymers |
| GB0514398D0 (en) | 2005-07-15 | 2005-08-17 | 3M Innovative Properties Co | Aqueous emulsion polymerization of fluorinated monomers using a fluorinated surfactant |
| GB0523853D0 (en) | 2005-11-24 | 2006-01-04 | 3M Innovative Properties Co | Fluorinated surfactants for use in making a fluoropolymer |
| CN101282788B (zh) | 2005-10-14 | 2011-04-06 | 旭硝子株式会社 | 碱性阴离子交换树脂的再生方法 |
| US7728087B2 (en) | 2005-12-23 | 2010-06-01 | 3M Innovative Properties Company | Fluoropolymer dispersion and method for making the same |
| US7754795B2 (en) | 2006-05-25 | 2010-07-13 | 3M Innovative Properties Company | Coating composition |
| US7666928B2 (en) * | 2006-05-31 | 2010-02-23 | E.I. Du Pont De Nemours And Company | Staged addition of non-fluorinated anionic surfactant to reduced fluorosurfactant fluoropolymer dispersion |
| US8119750B2 (en) | 2006-07-13 | 2012-02-21 | 3M Innovative Properties Company | Explosion taming surfactants for the production of perfluoropolymers |
| KR101500018B1 (ko) * | 2007-02-16 | 2015-03-06 | 쓰리엠 이노베이티브 프로퍼티즈 캄파니 | 물로부터 불소화합물계 물질을 제거하는 시스템 및 방법 |
| US20080264864A1 (en) * | 2007-04-27 | 2008-10-30 | 3M Innovative Properties Company | PROCESS FOR REMOVING FLUORINATED EMULSIFIER FROM FLUOROPOLMER DISPERSIONS USING AN ANION-EXCHANGE RESIN AND A pH-DEPENDENT SURFACTANT AND FLUOROPOLYMER DISPERSIONS CONTAINING A pH-DEPENDENT SURFACTANT |
| JP5492084B2 (ja) * | 2008-08-12 | 2014-05-14 | 和光純薬工業株式会社 | 前処理カラムの充填剤用ポリマー |
| JP5256002B2 (ja) * | 2008-11-25 | 2013-08-07 | オルガノ株式会社 | フォトレジスト現像排水の排水処理システム |
| CN102740974A (zh) | 2010-02-03 | 2012-10-17 | 旭硝子株式会社 | 阴离子性含氟乳化剂的回收方法 |
| JP2013519517A (ja) * | 2010-02-18 | 2013-05-30 | ランクセス・ドイチュランド・ゲーエムベーハー | フッ素化酸またはそれらの塩を含む廃水の処理 |
| EP2431334A1 (de) | 2010-09-16 | 2012-03-21 | LANXESS Deutschland GmbH | Behandlung von Abwässern aus der Galvanikindustrie |
| WO2015053235A1 (ja) * | 2013-10-10 | 2015-04-16 | 旭硝子株式会社 | 含フッ素乳化剤の回収方法 |
| DE102014100694A1 (de) | 2014-01-22 | 2015-07-23 | Friedrich-Alexander-Universität Erlangen-Nürnberg | Verfahren und Vorrichtung zur Abtrennung von fluorierten Kohlenwasserstoffen aus einer wässrigen Phase |
| CN106232231B (zh) * | 2014-04-18 | 2020-11-20 | 3M创新有限公司 | 支链氟化乳化剂的回收 |
| JP6123864B2 (ja) * | 2015-10-19 | 2017-05-10 | ダイキン工業株式会社 | 炭素数２〜７の含フッ素有機酸および不純物を含む組成物の処理方法 |
| WO2017151935A1 (en) | 2016-03-04 | 2017-09-08 | 3M Innovative Properties Company | Method for removing perfluorinated alkanoic acids |
| CN113667247A (zh) | 2017-03-31 | 2021-11-19 | 大金工业株式会社 | 包含含氟聚合物的组合物及其成型体 |
| US12378138B2 (en) | 2019-06-19 | 2025-08-05 | The Johns Hopkins University | Contaminant-sequestering coatings and methods of using the same |
| US11452987B2 (en) | 2019-06-19 | 2022-09-27 | The Johns Hopkins University | Contaminate sequestering coatings and methods of using the same |
| US12240767B2 (en) | 2019-06-28 | 2025-03-04 | Katholieke Universiteit Leuven | Adsorptive removal of perfluorinated or partially fluorinated surfactants |
| EP3945075A1 (en) | 2020-07-30 | 2022-02-02 | 3M Innovative Properties Company | Process for removal of fluoroorganic compounds from emulsions |
| EP3945099A1 (en) | 2020-07-30 | 2022-02-02 | 3M Innovative Properties Company | Process for removal of fluoroorganic compounds from aqueous media |
| EP3945074A1 (en) | 2020-07-30 | 2022-02-02 | 3M Innovative Properties Company | Process to reduce the concentration of fluoroorganic acidic compound in aqueous dispersions |
| US12410071B1 (en) | 2020-10-19 | 2025-09-09 | Wm Intellectual Property Holdings, L.L.C. | System and method for removal of PFAS and other emerging contaminant micro-constituents from landfill leachate and other impacted liquids |
| EP4219412A1 (en) | 2022-01-27 | 2023-08-02 | 3M Innovative Properties Company | Closed-loop technologies for purifying fluorine containing water streams |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3882153A (en) | 1969-09-12 | 1975-05-06 | Kureha Chemical Ind Co Ltd | Method for recovering fluorinated carboxylic acid |
| DE2903981A1 (de) | 1979-02-02 | 1980-08-07 | Hoechst Ag | Rueckgewinnung fluorierter emulgatorsaeuren aus basischen anionenaustauschern |
| JPS632656A (ja) * | 1986-06-23 | 1988-01-07 | Furukawa Electric Co Ltd:The | ウエハ研磨方法及びそれに用いるウエハ研磨基板 |
| DE4318258A1 (de) * | 1993-06-02 | 1994-12-08 | Hoechst Ag | Verfahren zur Rückgewinnung von fluorierten Carbonsäuren |
| DE19824615A1 (de) | 1998-06-02 | 1999-12-09 | Dyneon Gmbh | Verfahren zur Rückgewinnung von fluorierten Alkansäuren aus Abwässern |
| DE19824614A1 (de) | 1998-06-02 | 1999-12-09 | Dyneon Gmbh | Verfahren zur Rückgewinnung von fluorierten Alkansäuren aus Abwässern |
| DE19932771A1 (de) | 1999-07-14 | 2001-01-18 | Dyneon Gmbh | Verfahren zur Eluierung fluorierter Emulgatoren |
-
1999
- 1999-11-05 DE DE19953285A patent/DE19953285A1/de not_active Withdrawn
-
2000
- 2000-10-28 JP JP2001534724A patent/JP2003512931A/ja not_active Ceased
- 2000-10-28 CN CNB008154090A patent/CN1174924C/zh not_active Expired - Fee Related
- 2000-10-28 WO PCT/EP2000/010638 patent/WO2001032563A1/de not_active Ceased
- 2000-10-28 DE DE50002876T patent/DE50002876D1/de not_active Expired - Fee Related
- 2000-10-28 AU AU79240/00A patent/AU7924000A/en not_active Abandoned
- 2000-10-28 RU RU2002111410/15A patent/RU2255807C2/ru not_active IP Right Cessation
- 2000-10-28 US US10/110,643 patent/US6642415B1/en not_active Expired - Fee Related
- 2000-10-28 CA CA002387781A patent/CA2387781A1/en not_active Abandoned
- 2000-10-28 PL PL00354617A patent/PL354617A1/xx unknown
- 2000-10-28 EP EP00969564A patent/EP1240107B1/de not_active Expired - Lifetime
-
2002
- 2002-05-02 ZA ZA200203488A patent/ZA200203488B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| JP2003512931A (ja) | 2003-04-08 |
| PL354617A1 (en) | 2004-02-09 |
| CN1174924C (zh) | 2004-11-10 |
| AU7924000A (en) | 2001-05-14 |
| DE19953285A1 (de) | 2001-05-10 |
| DE50002876D1 (de) | 2003-08-14 |
| EP1240107A1 (de) | 2002-09-18 |
| CN1387498A (zh) | 2002-12-25 |
| WO2001032563A1 (de) | 2001-05-10 |
| RU2255807C2 (ru) | 2005-07-10 |
| EP1240107B1 (de) | 2003-07-09 |
| US6642415B1 (en) | 2003-11-04 |
| CA2387781A1 (en) | 2001-05-10 |
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