EP1087919A1 - Gaserzeugende feste pyrotechnische ladungen auf basis von wasserhaltigen zusammensetzungen - Google Patents
Gaserzeugende feste pyrotechnische ladungen auf basis von wasserhaltigen zusammensetzungenInfo
- Publication number
- EP1087919A1 EP1087919A1 EP99920902A EP99920902A EP1087919A1 EP 1087919 A1 EP1087919 A1 EP 1087919A1 EP 99920902 A EP99920902 A EP 99920902A EP 99920902 A EP99920902 A EP 99920902A EP 1087919 A1 EP1087919 A1 EP 1087919A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- composition according
- binder
- composition
- water
- chosen
- 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.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000007787 solid Substances 0.000 title claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- CRJZNQFRBUFHTE-UHFFFAOYSA-N hydroxylammonium nitrate Chemical compound O[NH3+].[O-][N+]([O-])=O CRJZNQFRBUFHTE-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims abstract description 9
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 14
- 239000007791 liquid phase Substances 0.000 claims description 10
- 239000000654 additive Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 5
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 claims description 4
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000028 HMX Substances 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- UZGLIIJVICEWHF-UHFFFAOYSA-N octogen Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 UZGLIIJVICEWHF-UHFFFAOYSA-N 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 229910021538 borax Inorganic materials 0.000 claims description 3
- 238000004898 kneading Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- 230000008719 thickening Effects 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005695 Ammonium acetate Substances 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 235000019257 ammonium acetate Nutrition 0.000 claims description 2
- 229940043376 ammonium acetate Drugs 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 239000012948 isocyanate Substances 0.000 claims description 2
- 150000002513 isocyanates Chemical class 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims 1
- 239000000230 xanthan gum Substances 0.000 claims 1
- 235000010493 xanthan gum Nutrition 0.000 claims 1
- 229940082509 xanthan gum Drugs 0.000 claims 1
- 239000003381 stabilizer Substances 0.000 abstract description 3
- 230000003019 stabilising effect Effects 0.000 abstract 1
- 239000002562 thickening agent Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 4
- 239000000567 combustion gas Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 239000003380 propellant Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- GOPCYLTVKPFMJI-UHFFFAOYSA-N NC=1N=NNC1.[N+](=O)(O)[O-] Chemical compound NC=1N=NNC1.[N+](=O)(O)[O-] GOPCYLTVKPFMJI-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- HAMNKKUPIHEESI-UHFFFAOYSA-N aminoguanidine Chemical compound NNC(N)=N HAMNKKUPIHEESI-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- CNUNWZZSUJPAHX-UHFFFAOYSA-N guanidine nitrate Chemical class NC(N)=N.O[N+]([O-])=O CNUNWZZSUJPAHX-UHFFFAOYSA-N 0.000 description 1
- RBLWMQWAHONKNC-UHFFFAOYSA-N hydroxyazanium Chemical compound O[NH3+] RBLWMQWAHONKNC-UHFFFAOYSA-N 0.000 description 1
- QHDUJTCUPWHNPK-UHFFFAOYSA-N methyl 7-methoxy-2h-indazole-3-carboxylate Chemical compound COC1=CC=CC2=C(C(=O)OC)NN=C21 QHDUJTCUPWHNPK-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- TVIRJXQLFRFUCD-UHFFFAOYSA-N nitric acid;2h-tetrazol-5-amine Chemical compound O[N+]([O-])=O.NC1=NN=NN1 TVIRJXQLFRFUCD-UHFFFAOYSA-N 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- VMPIHZLTNJDKEN-UHFFFAOYSA-O triethanolammonium nitrate Chemical compound [O-][N+]([O-])=O.OCC[NH+](CCO)CCO VMPIHZLTNJDKEN-UHFFFAOYSA-O 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/06—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires containing gas-producing, chemically-reactive components
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B47/00—Compositions in which the components are separately stored until the moment of burning or explosion, e.g. "Sprengel"-type explosives; Suspensions of solid component in a normally non-explosive liquid phase, including a thickened aqueous phase
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
Definitions
- the present invention relates to the field of pyrotechnic compositions generating cold gases, non-toxic and free of solid residues. More precisely, the invention relates to the field of composite pyrotechnic compositions with an amorphous structure comprising one or more oxidants and an organic binder in the gel state.
- the compositions according to 1 'invention are well suited to form loads to inflate protective cushions or to ensure the operation of a pyrotechnic extinguisher.
- cold gases means gases which are produced at a temperature below about 1800 ° C.
- liquid propellants consisting of aqueous solutions of compounds such as hydroxylammonium nitrate, triethanolammonium nitrate, aminotetrazole nitrate, nitrate aminotriazole, urea nitrate, biuret nitrate, etc.
- Such liquid propellants are for example described in US Patents 5,060,973 and US 5,684,269.
- liquid propellants require suitable gas generators, whose structure is complex and which are of a high cost price.
- compositions constituted by a binder such as polyvinyl alcohol and by solid eutectics based on ammonium nitrate and guanidine nitrates or aminoguanidine in the presence of potassium nitrate or perchlorate.
- a binder such as polyvinyl alcohol
- solid eutectics based on ammonium nitrate and guanidine nitrates or aminoguanidine in the presence of potassium nitrate or perchlorate.
- the invention therefore relates to solid pyrotechnic compositions producing by combustion gases free of solid residues and constituted by at least one organic binder with gelling effect and by at least one main oxidizing system in liquid phase absorbed by said binder, said compositions being characterized in that:
- the said organic binder with gelling effect is chosen from the group consisting of polyvinyl alcohol, hydroxyethylcellulose, and xantham gum.
- the said main oxidizing system in the liquid phase consists of a mixture of water and hydroxylammonium nitrate (HAN).
- Polyvinyl alcohol is the preferred binder because it improves the chemical stability of the compositions according to the invention.
- the solid compositions according to the invention thus have an amorphous structure in which the binder is in the form of a solid gel impregnated with the aqueous hydroxylammonium phase.
- these compositions release the water included in the gel in the form of water vapor which contributes to very significantly lowering the temperature of the combustion gases.
- the water content by weight of the compositions according to the invention will be between 5 and 20%.
- the invention thus makes it possible to have available compositions which contain water contents much higher than the moisture contents of the previously known compositions.
- the weight of the hydroxylammonium nitrate represents at least 50% of the total weight of the composition, the content of the latter in hydroxylammonium nitrate being preferably between 60% and 70%.
- One of the advantages of the present invention resides in the fact that at the indicated contents the water / hydroxylammonium nitrate mixtures remain liquid as long as the temperature of the latter does not drop below zero degrees Celsius.
- the compositions according to the invention also contain secondary oxidants which are advantageously chosen from the group consisting of ammonium nitrate, hexogen (RDX) and octogen (HMX).
- secondary oxidants which are advantageously chosen from the group consisting of ammonium nitrate, hexogen (RDX) and octogen (HMX).
- compositions when the compositions are intended to constitute pyrotechnic charges for gas generators having to inflate protective cushions for the occupants of a motor vehicle, the use of ammonium nitrate will be avoided or in any case the weight content of the ammonium nitrate composition will be limited to a few percent.
- the compositions will most often contain stabilizing additives which will be chosen from bipyridine, ammonium hydrogen phosphate and ammonium acetate. The weight content of these stabilizers in the composition will be close to 2%. Bipyridine and ammonium hydrogen phosphate are preferred stabilizers.
- compositions will contain thickening additives which will be chosen from the group consisting of water-soluble isocyanates, melamine-formaldehyde resins and borax which is a sodium tetraborate of formula: Na 2 B 4 O 7 , 10H 2 O.
- the invention also relates to a process for the continuous production of solid pyrotechnic charges with an amorphous structure, the composition of which corresponds to the compositions described above and which is characterized in that:
- a mixing and extrusion apparatus is fed continuously on the one hand with a liquid phase containing at least water and hydroxylammonium nitrate and on the other hand with solid granules comprising at least one binder gelling effect,
- a profiled rod is extruded which is hardened in an oven and cut to the desired length, for example in the form of tubes or crowns.
- the kneading and extrusion apparatus is a twin-screw extruder.
- the binder with gelling effect is polyvinyl alcohol and the twin-screw extruder is heated to a temperature between 50 ° C. and 60 ° C., the temperature inside the oven being close to 80 ° C.
- all the constituents other than the binder and which are soluble in water will be mixed with the liquid phase containing the water and the hydroxylammonium nitrate before introduction of the latter into the twin-screw extruder.
- the pyrotechnic charges thus obtained can in particular be used either in pyrotechnic extinguishers to constitute the source of engine gas in these extinguishers, or in pyrotechnic gas generators intended to inflate protective cushions for the occupants of a motor vehicle.
- FIG. 1 represents the diagram of an installation for continuously manufacturing loads according to the invention.
- the installation shown in FIG. 1 basically comprises a twin-screw extruder 1 extended by an extrusion head 2, a conveyor belt 3 passing inside an oven 4 and a cutting system 5. At the start of 1 'extruder are provided two feed devices.
- the first device consists of a pipe 6 connected via a tap 7 to a tank 8 provided with an agitator 9. Downstream in the operating direction of the extruder 1 is a second feed device constituted by a hopper 10 and a conveyor belt 11.
- the tank 8 contains a liquid mixture A consisting of water, hydroxylammonium nitrate and, where appropriate, the constituents other than the binder and soluble in water such as ammonium nitrate.
- the reactive constituents with respect to water are not incorporated into this aqueous liquid phase.
- the conveyor belt 11 feeds the hopper 10 with a mixture of granules B comprising granules of binder and, where appropriate, granules of additives which are not soluble in water and in particular granules of oxidizers which are not soluble in water such hexogen or octogen.
- the extruder 1 is temperature controlled to have an internal temperature between 50 ° C and 60 ° C when the binder is polyvinyl alcohol.
- the liquid phase A and the granules B are mixed in the extruder 1 to form, by gelation of the binder, a composite paste with an amorphous structure which is extruded through the extrusion head 2 in the form of a profiled rod 12.
- This rod may be a simple cylindrical strand, possibly provided with internal channels, to give, after cutting, loose grains or be a rod of larger dimensions, with, if necessary, a worked external profile, to give after cutting. solid or annular blocks.
- This rod 12 is led via the conveyor belt 3 through a heated oven to cause hardening of the gelled binder.
- the binder is polyvinyl alcohol the temperature of the oven will be close to 80 ° C and the residence time of the rod in the oven will be a few minutes.
- the rod 12 is cut using the cutting system 5 into elementary loads 13 which are stored in a container 14.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Air Bags (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatment Of Sludge (AREA)
- Glanulating (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9807090 | 1998-06-05 | ||
| FR9807090A FR2779426B1 (fr) | 1998-06-05 | 1998-06-05 | Chargements pyrotechniques solides generateurs de gaz a base de compositions contenant de l'eau |
| PCT/FR1999/001206 WO1999064375A1 (fr) | 1998-06-05 | 1999-05-21 | Chargements pyrotechniques solides generateurs de gaz a base de composition contenant de l'eau |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1087919A1 true EP1087919A1 (de) | 2001-04-04 |
| EP1087919B1 EP1087919B1 (de) | 2002-12-04 |
Family
ID=9527056
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP99920902A Expired - Lifetime EP1087919B1 (de) | 1998-06-05 | 1999-05-21 | Gaserzeugende feste pyrotechnische ladungen auf basis von wasserhaltigen zusammensetzungen |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1087919B1 (de) |
| JP (1) | JP2002517376A (de) |
| AT (1) | ATE228984T1 (de) |
| DE (1) | DE69904326T2 (de) |
| FR (1) | FR2779426B1 (de) |
| WO (1) | WO1999064375A1 (de) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100357235C (zh) * | 2006-04-14 | 2007-12-26 | 安徽盾安化工集团有限公司 | 无梯粉状改性铵油炸药及其制备方法 |
| CN100357234C (zh) * | 2006-04-14 | 2007-12-26 | 安徽盾安化工集团有限公司 | 一种粉状铵油炸药及其制备方法 |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5110256B2 (ja) * | 2006-12-12 | 2012-12-26 | 独立行政法人 宇宙航空研究開発機構 | ガス発生剤組成物 |
| JP2009190911A (ja) * | 2008-02-13 | 2009-08-27 | Daicel Chem Ind Ltd | ガス発生剤組成物 |
| DE102012104087A1 (de) * | 2012-05-09 | 2013-11-14 | Bayern-Chemie Gesellschaft Für Flugchemische Antriebe Mbh | Gasgenerator-Treibstoff |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ZA835342B (en) * | 1982-08-02 | 1985-01-30 | Jet Research Center | A stable single phase liquid explosive |
| GB2293820B (en) * | 1988-12-20 | 1996-07-03 | Aerojet General Co | Liquid oxidizer compositions and their use in energetic formulations |
| US5060973A (en) * | 1990-07-23 | 1991-10-29 | General Electric Company | Liquid propellant inflator for vehicle occupant restraint apparatus |
| US5386777A (en) * | 1992-02-10 | 1995-02-07 | Aero-Jet General Corporation | Rocket motor construction from porous binder core |
| US5684269A (en) * | 1996-03-15 | 1997-11-04 | Morton International, Inc. | Hydroxylammonium nitrate/water/self-deflagrating fuels as gas generating pyrotechnics for use in automotive passive restraint systems |
| US5703323A (en) * | 1996-09-17 | 1997-12-30 | Olin Corporation | Pyridine and pyridone stabilizers for hydroxylammonium nitrate and hydroxylamine-containing compositions |
-
1998
- 1998-06-05 FR FR9807090A patent/FR2779426B1/fr not_active Expired - Fee Related
-
1999
- 1999-05-21 EP EP99920902A patent/EP1087919B1/de not_active Expired - Lifetime
- 1999-05-21 JP JP2000553386A patent/JP2002517376A/ja active Pending
- 1999-05-21 AT AT99920902T patent/ATE228984T1/de not_active IP Right Cessation
- 1999-05-21 DE DE69904326T patent/DE69904326T2/de not_active Expired - Lifetime
- 1999-05-21 WO PCT/FR1999/001206 patent/WO1999064375A1/fr active IP Right Grant
Non-Patent Citations (1)
| Title |
|---|
| See references of WO9964375A1 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100357235C (zh) * | 2006-04-14 | 2007-12-26 | 安徽盾安化工集团有限公司 | 无梯粉状改性铵油炸药及其制备方法 |
| CN100357234C (zh) * | 2006-04-14 | 2007-12-26 | 安徽盾安化工集团有限公司 | 一种粉状铵油炸药及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| DE69904326D1 (de) | 2003-01-16 |
| WO1999064375A1 (fr) | 1999-12-16 |
| FR2779426B1 (fr) | 2000-07-13 |
| JP2002517376A (ja) | 2002-06-18 |
| DE69904326T2 (de) | 2003-08-28 |
| EP1087919B1 (de) | 2002-12-04 |
| ATE228984T1 (de) | 2002-12-15 |
| FR2779426A1 (fr) | 1999-12-10 |
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