EP1250950B1 - Nozzle for diluting phosphine - Google Patents

Nozzle for diluting phosphine Download PDF

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Publication number
EP1250950B1
EP1250950B1 EP02006308A EP02006308A EP1250950B1 EP 1250950 B1 EP1250950 B1 EP 1250950B1 EP 02006308 A EP02006308 A EP 02006308A EP 02006308 A EP02006308 A EP 02006308A EP 1250950 B1 EP1250950 B1 EP 1250950B1
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EP
European Patent Office
Prior art keywords
air
nozzle
pipe
air pipe
nozzle according
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.)
Expired - Lifetime
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EP02006308A
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German (de)
French (fr)
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EP1250950A1 (en
Inventor
Franziskus Dr. Horn
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/312—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/312—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof
    • B01F25/3124—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof characterised by the place of introduction of the main flow
    • B01F25/31242—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof characterised by the place of introduction of the main flow the main flow being injected in the central area of the venturi, creating an aspiration in the circumferential part of the conduit
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/10—Mixing gases with gases

Definitions

  • the present invention relates to a nozzle for the dilution of hydrogen phosphide (chemical formula PH 3 ), which consists of a tubular air inlet and an annularly arranged gap (annular gap) and / or at least one laterally arranged tubes as a PH 3 inlet, the strength of the The gap opening and / or the tube opening is a maximum of 1/25 of the diameter of the tubular air inlet and / or the distance of the surface of an air steering element from the inside of the tubular air inlet in the region of the PH 3 inlet.
  • PH 3 has been used for decades for pest control and for prophylaxis in the protection of stored goods, in particular for food and feed.
  • PH 3 forms an easily flammable gas mixture with air, the ignition limit being 1.8% PH 3 concentration. If this value is exceeded, PH 3 tends to self-ignite.
  • German Offenlegungsschrift 198 39 385 which describes an effective process for the direct dilution of PH 3 with air, in which the mixture air / PH 3 is carried out under or in the presence of water.
  • the present invention discloses an easy to use Handheld device in the form of a nozzle that is easily portable and can be used quickly at any location.
  • the nozzle according to the invention was able to mix 90,000 liters of air with PH 3 without problems within one hour, with an air content of 10,000 ppm of PH 3 .
  • reaction zone can spread at supersonic speed.
  • the present invention is based on the surprising finding that the creation of a laminar flow at PH 3 along the inner wall of a tubular air inlet results in an optimal mixing of air and PH 3 without the risk of ignition below the ignition limit.
  • the occurrence of ignition is prevented by the fact that the critical conditions only occur in a very thin layer.
  • the PH 3 layer is immediately swept away by a strong air stream and mixed into the air.
  • the embodiment of Figure 1 consists of a tube open on both sides, which is identified by the reference number 1.
  • This tube has an annular gap 2, which has an annular attachment 3, into which flows in the direction of arrow 4 PH 3 , which then flows at the entry point 5 along the wall of the tube 1.
  • air flows at a very high speed into the opening 6 of the tube 1 in the direction of the arrow 6a, the already laminar flow of the PH 3 forming an even thinner layer.
  • the outlet opening of the air-PH 3 mixture is identified by reference number 7, the direction of flow of which is 7a.
  • the air passed through the pipe has, for example, an overpressure of 350 to 440 mm water column and a speed of 250 to 370 km / h.
  • the exit column 2 for the PH 3 should generally not exceed a diameter of 0.2 mm.
  • the thickness of the air layer 9 above the PH 3 layer preferably does not exceed the value of 5 mm.
  • the nozzle according to the invention can easily be selected from a number of quickly assemble elements to be assembled, which by O-rings are sealed.
  • the nozzle can be just as easy preferably made of stainless steel, disassemble, inspect and clean if necessary.
  • Figure 3 shows a section through the nozzle according to the invention this tube element.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nozzles (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Catching Or Destruction (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Measurement Of Levels Of Liquids Or Fluent Solid Materials (AREA)
  • Jet Pumps And Other Pumps (AREA)

Description

Die vorliegende Erfindung betrifft eine Düse zur Verdünnung von Phosphorwasserstoff (chem. Formel PH3), die aus einer rohrförmigen Lufteinleitung und einem ringförmig angeordneten Spalt (Ringspalt) und/oder mindestens einem lateral angeordneten Rohren als PH3-Einleitung besteht, wobei die Stärke der Spaltöffnung und/oder der Röhrchenöffnung maximal 1 / 25 des Durchmessers der rohrförmigen Lufteinleitung und/oder des Abstandes der Oberfläche eines Luftlenkungselements von der Innenseite der rohrförmigen Lufteinleitung im Bereich des PH3-Eintritts beträgt.The present invention relates to a nozzle for the dilution of hydrogen phosphide (chemical formula PH 3 ), which consists of a tubular air inlet and an annularly arranged gap (annular gap) and / or at least one laterally arranged tubes as a PH 3 inlet, the strength of the The gap opening and / or the tube opening is a maximum of 1/25 of the diameter of the tubular air inlet and / or the distance of the surface of an air steering element from the inside of the tubular air inlet in the region of the PH 3 inlet.

Bekanntlich wird PH3 seit Jahrezehnten zur Schädlingsbekämpfung und zur Prophylaxe beim Vorratsschutz, insbesondere bei Lebensmitteln und Futtermitteln eingesetzt.As is well known, PH 3 has been used for decades for pest control and for prophylaxis in the protection of stored goods, in particular for food and feed.

PH3 bildet jedoch bekanntlich mit Luft ein leicht entzündbares Gasgemisch, wobei die Zündgrenze bei 1,8 % PH3 -Konzentration liegt. Wird dieser Wert überschritten, so neigt PH3 zur Selbstentzündung.However, as is known, PH 3 forms an easily flammable gas mixture with air, the ignition limit being 1.8% PH 3 concentration. If this value is exceeded, PH 3 tends to self-ignite.

Es wurden daher bereits zahlreiche Verfahren und Vorrichtungen vorgeschlagen, um eine gefahrlose Verdünnung des PH3 mit Luft durchzuführen.Numerous methods and devices have therefore already been proposed for safely diluting the PH 3 with air.

Zum nächstkommenden Stand der Technik ist hierbei auf die Deutsche Offenlegungsschrift 198 39 385 hinzuweisen, die ein wirkungsvolles Verfahren zur direkten Verdünnung von PH3 mit Luft beschreibt, bei dem die Mischung Luft/PH3 unter oder in Gegenwart von Wasser durchgeführt wird.For the closest prior art, reference should be made to German Offenlegungsschrift 198 39 385, which describes an effective process for the direct dilution of PH 3 with air, in which the mixture air / PH 3 is carried out under or in the presence of water.

Zum ferner liegenden Stand der Technik ist weiterhin auf die Deutsche Patentschrift DE 691 29 456 T2, die Internationale Patentanmeldung WO93/25075 A1 hinzuweisen.The further lying state of the art is still on the German Patent specification DE 691 29 456 T2, the international patent application WO93 / 25075 A1 point out.

Demgegenüber offenbart vorliegende Erfindung ein einfach zu bedienendes Handgerät in Gestalt einer Düse, das leicht transportabel und rasch an jedem beliebigen Einsatzort verwendbar ist. In contrast, the present invention discloses an easy to use Handheld device in the form of a nozzle that is easily portable and can be used quickly at any location.

Es handelt sich also um ein universell und rasch einsetzbares Gerät. Die erfindungsgemäße Düse konnte beispielsweise problemlos innerhalb einer Stunde 90.000 Liter Luft mit PH3 vermischen unter Erreichung eines Gehalts der Luft von 10.000 ppm an PH3 .So it is a universal and quick to use device. For example, the nozzle according to the invention was able to mix 90,000 liters of air with PH 3 without problems within one hour, with an air content of 10,000 ppm of PH 3 .

Zum technologischen Hintergrund ist festzustellen, dass beim Entzünden eines zündbaren Gemisches von Luft und PH3 sich die Reaktionszone mit Überschallgeschwindigkeit verbreiten kann.With regard to the technological background, it should be noted that when an ignitable mixture of air and PH 3 is ignited, the reaction zone can spread at supersonic speed.

Wird ein PH3 -Strom in einen Luftstrom geleitet, so kommt es am Mischpunkt oder der Mischzone sofort zur Selbstzündung, wobei es am Austrittspunkt des PH3 zu kleinen Explosionen kommt, die sofort durch die von der Explosion bewirkten Ausdehnung und nachfolgende Kontraktion einen Resonanzvorgang auslösen.If a PH 3 stream is directed into an air stream, self-ignition occurs immediately at the mixing point or the mixing zone, with small explosions occurring at the exit point of the PH 3 , which immediately trigger a resonance process due to the expansion and subsequent contraction caused by the explosion ,

Dieses Phänomen macht sich durch ein pfeifendes Geräusch bemerkbar. Bei diesen Explosionen entsteht eine gelb-rote flüssige Mischung von Phosphorsäure und Poly-Phosphinen.A whistling sound makes this phenomenon noticeable. These explosions create a yellow-red liquid mixture of phosphoric acid and poly-phosphines.

Die gleichen Phänomene wurden auch beim Zudosieren von PH3 in einen Luftstrom durch kleine Bohrungen hindurch beobachtet, wobei sich die Bohrlöcher stets mit verunreinigender gelber Säure verschmutzten und zusetzten und deren Durchmesser 1-2 mm beträgt.The same phenomena were also observed when PH 3 was metered into an air stream through small bores, the boreholes always becoming soiled and clogged with contaminating yellow acid and the diameter of which was 1-2 mm.

Die vorgenannten nachteiligen Phänomene werden durch das vorgenannte Verfahren gemäß deutscher Offenlegungsschrift 198 39 385 vermieden, da das Wasser eine Resonanz der Explosionen verhindert.The above-mentioned adverse phenomena are caused by the above Procedure in accordance with German Offenlegungsschrift 198 39 385 avoided because the water prevents resonance of the explosions.

Der vorliegenden Erfindung liegt nun die überraschende Erkenntnis zugrunde, dass die Schaffung einer laminaren Strömung an PH3 entlang der Innenwandung einer rohrförmigen Lufteinleitung eine optimale Vermischung von Luft und PH3 ohne Entzündungsgefahr bis unter die Zündgrenze bewirkt.The present invention is based on the surprising finding that the creation of a laminar flow at PH 3 along the inner wall of a tubular air inlet results in an optimal mixing of air and PH 3 without the risk of ignition below the ignition limit.

Bei der erfindungsgemäßen Düse wird das Auftreten einer Zündung dadurch verhindert, dass die kritischen Bedingungen nur in einer sehr dünnen Schicht auftreten. Die PH3 -Schicht wird sofort von einem starken Luftstrom mitgerissen und in die Luft eingemischt. In the nozzle according to the invention, the occurrence of ignition is prevented by the fact that the critical conditions only occur in a very thin layer. The PH 3 layer is immediately swept away by a strong air stream and mixed into the air.

Hierdurch gelingt es, Mischungen herzustellen, die bis zu 10.000 ppm PH3 enthalten, ohne dass es dabei zu einer Zündung in der Mischzone kommt. Dies ist auch dadurch feststellbar, dass sich in der Mischzone keine gelbe Phosphorsäure bildet.This makes it possible to produce mixtures which contain up to 10,000 ppm of PH 3 without ignition in the mixing zone. This can also be determined by the fact that no yellow phosphoric acid forms in the mixing zone.

Wird ein glühender Eisenstab genau vor den Mischpunkt in der Düse gehalten, so kommt es bis zu einer Konzentration von 5000 ppm PH3 nicht zu einer anhaltenden Zündung. Nur solange die Zündung vorhanden ist, ist das pfeifende Geräusch zu hören.If a glowing iron rod is held exactly in front of the mixing point in the nozzle, there is no persistent ignition up to a concentration of 5000 ppm PH 3 . The whistling sound can only be heard as long as the ignition is on.

In der Praxis werden für Begasungszwecke keine Mischungen mit einem höheren PH3 -Anteil als 2000 ppm angewendet.In practice, no mixtures with a PH 3 content higher than 2000 ppm are used for fumigation purposes.

Das Wesen vorliegender Erfindung wird nun anhand der beiliegenden Figuren 1 - 3, die beispielhaft eine bevorzugte Ausführungsform zeigen, weiterhin erläutert. Die Figuren zeigen einen Schnitt durch die erfindungsgemäße Vorrichtung.The essence of the present invention will now become apparent from the accompanying Figures 1-3, which exemplify a preferred embodiment show, further explained. The figures show a section through the device according to the invention.

Die Ausführungsform der Figur 1 besteht aus einer beidseitig offenen Röhre, die mit der Bezugsziffer 1 gekennzeichnet ist. Diese Röhre weist einen Ringspalt 2 auf, der einen ringförmigen Vorsatz 3 aufweist, in den in Richtung des Pfeils 4 PH3 strömt, das sodann an der Eintrittsstelle 5 entlang der Wandung des Rohrs 1 strömt. Gleichzeitig strömt Luft mit sehr hoher Geschwindigkeit in die Öffnung 6 des Rohrs 1 in Richtung des Pfeils 6a, wobei die an sich schon laminare Strömung des PH3 noch eine wesentlich dünnere Schicht bildet. Die Austrittsöffnung des Luft-PH3 -Gemischs ist mit der Bezugsziffer 7, dessen Strömungsrichtung mit 7a gekennzeichnet.The embodiment of Figure 1 consists of a tube open on both sides, which is identified by the reference number 1. This tube has an annular gap 2, which has an annular attachment 3, into which flows in the direction of arrow 4 PH 3 , which then flows at the entry point 5 along the wall of the tube 1. At the same time, air flows at a very high speed into the opening 6 of the tube 1 in the direction of the arrow 6a, the already laminar flow of the PH 3 forming an even thinner layer. The outlet opening of the air-PH 3 mixture is identified by reference number 7, the direction of flow of which is 7a.

Um nun den Druck der sehr schnell strömenden Luft auf das laminar strömende PH3 noch zu verstärken, ist gemäss einer bevorzugten Ausführungsform im Rohr 1 ein geschossähnlicher Körper 8 angeordnet, dessen Spitze in Richtung der Lufteintrittsöffnung 6 zeigt, wobei die dickste Stelle des geschossähnlichen Körpers 8 im Bereich des Ringspalts 2 angeordnet ist. 8 = Luftlenkungselement. Die durch das Rohr geleitete Luft hat beispielsweise einen Überdruck von 350 bis 440 mm Wassersäule und eine Geschwindigkeit von 250 bis 370 km/h. In order to increase the pressure of the very rapidly flowing air on the laminar flowing PH 3 , a projectile-like body 8 is arranged in the tube 1, the tip of which points in the direction of the air inlet opening 6, the thickest point of the projectile-like body 8 is arranged in the area of the annular gap 2. 8 = air steering element. The air passed through the pipe has, for example, an overpressure of 350 to 440 mm water column and a speed of 250 to 370 km / h.

Die Austrittspalte 2 für das PH3 soll einen Durchmesser von 0.2 mm in der Regel nicht überschreiten. Es wurden Düsen mit Ringspaltdurchmessern von 0,6 mm; 0,3 mm und 0,1 mm getestet, wobei sich der letztere Wert als optimal herausstellte.The exit column 2 for the PH 3 should generally not exceed a diameter of 0.2 mm. There were nozzles with an annular gap diameter of 0.6 mm; 0.3 mm and 0.1 mm tested, the latter value being found to be optimal.

Beim Vorhandensein des geschossähnlichen Körpers 8 wird erreicht, dass die Stärke der Luftschicht 9 über der PH3 -Schicht bevorzugtermassen den Wert von 5 mm nicht überschreitet.If the projectile-like body 8 is present, it is achieved that the thickness of the air layer 9 above the PH 3 layer preferably does not exceed the value of 5 mm.

Bei der Ausführungsform gemäss Figur 2 ist gegenüber Figur 1 der geschossähnliche Körper nicht vorhanden.In the embodiment according to FIG. 2, compared to FIG bullet-like body does not exist.

Die erfindungsgemäße Düse lässt sich leicht aus einer Reihe von rasch zusammen zu bauenden Elementen herstellen, welche durch O-Ringe abgedichtet sind. Genauso leicht lässt sich die Düse, die bevorzugtermassen aus Edelstahl besteht, wieder zerlegen, besichtigen und gegebenenfalls reinigen.The nozzle according to the invention can easily be selected from a number of quickly assemble elements to be assembled, which by O-rings are sealed. The nozzle can be just as easy preferably made of stainless steel, disassemble, inspect and clean if necessary.

Nach einer weiteren Ausführungsform, die in Figur 3 dargestellt ist, wird die Funktion der PH3 -Einleitung von Einzelröhrchen, welche die Bezugsziffer 9 tragen, übernommen, d.h. der Ringspalt kann teilweise oder ganz von den Röhrchen ersetzt werden, deren Austrittsöffnungen parallel zur Innenwand des Rohrs 1 liegen.According to a further embodiment, which is shown in Figure 3, the function of the PH 3 introduction of individual tubes, which bear the reference number 9, is taken over, that is, the annular gap can be partially or completely replaced by the tubes, the outlet openings parallel to the inner wall of the Rohrs 1 lie.

Figur 3 zeigt einen Schnitt durch die erfindungsgemäße Düse mit diesem Röhrchenelement.Figure 3 shows a section through the nozzle according to the invention this tube element.

Mit der Bezugsziffer 1 ist das beidseitig offene Rohr, mit 9 die Röhrchen, mit 8 das geschossähnliche Luftlenkungselement und mit 10 ein ringförmiges Vorsatzelement bezeichnet.With the reference number 1 is the tube open on both sides, with 9 the tubes, with 8 the projectile-like air steering element and with 10 denotes an annular attachment element.

Claims (4)

  1. Nozzle for the dilution of phosphine (chemical formula PH3) with gases, in particular with air,
    characterised in that it consists of a tubular air pipe (6) with an annular aperture (2) and/or with at least one small lateral pipe (9), which is used to add the phosphine. The width of the annular aperture and/or of the small pipe must not exceed 1/25 of the diameter of the tubular air pipe and/or of the distance between the surface of an air direction element and the inside of the tubular air pipe at the point where PH3 is fed into the system.
  2. Nozzle according to claim 1,
    characterised in that
    in the tubular air pipe (6) there is a projectile shaped body (8), which serves as an air direction element. The tip of this body points towards the aperture used for air access. The diameter of this body (8) is at its largest at the point where PH3 is fed into the tubular air pipe (6).
  3. Nozzle according to claim 1-2,
    characterised in that
    it consists of stainless steal.
  4. Nozzle according to claim 1-3,
    characterised in that
    it consists of parts that can be interconnected.
EP02006308A 2001-04-17 2002-03-21 Nozzle for diluting phosphine Expired - Lifetime EP1250950B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE20106613U DE20106613U1 (en) 2001-04-17 2001-04-17 Nozzle for using hydrogen phosphide
DE20106613U 2001-04-17

Publications (2)

Publication Number Publication Date
EP1250950A1 EP1250950A1 (en) 2002-10-23
EP1250950B1 true EP1250950B1 (en) 2004-02-11

Family

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EP02006308A Expired - Lifetime EP1250950B1 (en) 2001-04-17 2002-03-21 Nozzle for diluting phosphine

Country Status (13)

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US (1) US7163161B2 (en)
EP (1) EP1250950B1 (en)
JP (1) JP4030315B2 (en)
CN (1) CN1234463C (en)
AR (1) AR032272A1 (en)
AT (1) ATE259256T1 (en)
AU (1) AU784088B2 (en)
BR (2) BRPI0200276B1 (en)
CA (1) CA2377121C (en)
DE (2) DE20106613U1 (en)
ES (1) ES2215151T3 (en)
MX (1) MXPA02001287A (en)
ZA (1) ZA200200563B (en)

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DE10319582B4 (en) * 2003-04-24 2007-03-22 Lechler Gmbh Binary spray nozzle
US20050089408A1 (en) * 2003-05-09 2005-04-28 Solomon Jason D. Fluid ejector pumps
CL2004001316A1 (en) * 2004-05-28 2005-03-18 Fosfoquim S A PROCEDURE FOR CONTROLLING FRUIT PESTS WITHOUT WRITING THE QUALITY OF THE FRUIT INCLUDING THE EXPOSURE OF THE FRUIT AT A HIGH PHOSPHINE CONCENTRATION BETWEEN 700 TO 3500 PPM AT A TEMPERATURE BETWEEN (-1.5 to 15) CELSIUS DEGREES DURING A TIE PERIOD
JP5240886B2 (en) * 2005-06-27 2013-07-17 国立大学法人 熊本大学 Fine droplet generator, fine droplet generator, and fine droplet generation method
US20110230679A1 (en) * 2010-03-16 2011-09-22 Dow Global Technologies, Inc. Reactive Static Mixer
WO2016135299A1 (en) * 2015-02-27 2016-09-01 Technip France Waste heat boiler system, mixing chamber, and method for cooling a process gas
WO2017033747A1 (en) * 2015-08-24 2017-03-02 株式会社村田製作所 Gas mixer and gas mixing device
US20220168695A1 (en) * 2020-11-27 2022-06-02 Huei Tarng Liou Venturi Tube

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US272863A (en) * 1883-02-27 Hydrocarbon-burner
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US3371618A (en) * 1966-02-18 1968-03-05 Chambers John Pump
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US4334783A (en) * 1978-12-21 1982-06-15 Showa Denko Kabushiki Kaisha Mixing device
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DE3724344A1 (en) * 1987-07-23 1989-02-02 Huels Chemische Werke Ag Mixing nozzle for mixing two gas streams
US4915300A (en) * 1987-08-20 1990-04-10 John Ryan High pressure mixing and spray nozzle apparatus and method
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US5403475A (en) * 1993-01-22 1995-04-04 Allen; Judith L. Liquid decontamination method
ES2120189T3 (en) * 1994-03-25 1998-10-16 Siemens Ag COMBINED FEEDING AND MIXING DEVICE.
DE19534107A1 (en) * 1995-09-14 1997-03-20 Wacker Siltronic Halbleitermat Nozzle for mixing fluids
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DE19839385A1 (en) * 1998-08-28 2000-03-23 Horn Pedro Miguel Method and device for diluting hydrogen phosphide with air without risk of ignition

Also Published As

Publication number Publication date
CN1234463C (en) 2006-01-04
AU1355002A (en) 2002-10-24
US20020148913A1 (en) 2002-10-17
ATE259256T1 (en) 2004-02-15
CA2377121A1 (en) 2002-10-17
DE20106613U1 (en) 2001-07-12
BRPI0200276B1 (en) 2019-06-18
EP1250950A1 (en) 2002-10-23
ES2215151T3 (en) 2004-10-01
AU784088B2 (en) 2006-02-02
CA2377121C (en) 2012-10-02
AR032272A1 (en) 2003-10-29
CN1381315A (en) 2002-11-27
BR0200276A (en) 2003-01-07
ZA200200563B (en) 2002-07-26
JP4030315B2 (en) 2008-01-09
DE50200239D1 (en) 2004-03-18
JP2002320882A (en) 2002-11-05
MXPA02001287A (en) 2005-11-04
US7163161B2 (en) 2007-01-16

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