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AU706207B2 - Free-flowing granules based on organic acids, preparation of said granules and their use - Google Patents

Free-flowing granules based on organic acids, preparation of said granules and their use Download PDF

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Publication number
AU706207B2
AU706207B2 AU69286/96A AU6928696A AU706207B2 AU 706207 B2 AU706207 B2 AU 706207B2 AU 69286/96 A AU69286/96 A AU 69286/96A AU 6928696 A AU6928696 A AU 6928696A AU 706207 B2 AU706207 B2 AU 706207B2
Authority
AU
Australia
Prior art keywords
granules
acid
free
covering material
flowing
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.)
Ceased
Application number
AU69286/96A
Other versions
AU6928696A (en
Inventor
Ulrich Brockel
Bruno Kasler
Joachim Meyer
Hans Muschen
Beate Salvador
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Publication of AU6928696A publication Critical patent/AU6928696A/en
Application granted granted Critical
Publication of AU706207B2 publication Critical patent/AU706207B2/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/003—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic followed by coating of the granules
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B2/00—Preservation of foods or foodstuffs, in general
    • A23B2/70—Preservation of foods or foodstuffs, in general by treatment with chemicals
    • A23B2/725—Preservation of foods or foodstuffs, in general by treatment with chemicals in the form of liquids or solids
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
    • A23K30/10—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs of green fodder
    • A23K30/15—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs of green fodder using chemicals or microorganisms for ensilaging
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • 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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/30—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using agents to prevent the granules sticking together; Rendering particulate materials free flowing in general, e.g. making them hydrophobic

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Zoology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Animal Husbandry (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Wood Science & Technology (AREA)
  • Fodder In General (AREA)
  • Fats And Perfumes (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Glanulating (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Detergent Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Medicinal Preparation (AREA)
  • Cereal-Derived Products (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Paints Or Removers (AREA)

Description

0050/46119 2 maintained. The pulverulent end product should have good storage, flow and processing properties.
We have found that this object is achieved by granules consisting of a core and a coat, wherein the core material contains an organic acid and a porous carrier and the coat has a covering material which is water-soluble or water-swellable at 20 0
C.
The novel granules have the advantage that the highly pungent acid odor is reduced and, in spite of the solid formulation, the acid content is released from the solid powder in readily and rapidly soluble form.
The present invention furthermore relates to a process for the preparation of granules containing organic acids and porous carriers, which comprises impregnating the carrier with the liquid organic acid, then agglomerating it with a covering material which solidifies at room temperature, the covering material being added in an amount such that theresulting granules are coated, and, if required, providing a further odor by adding scents and, if required, ensuring free-flowing properties of the agglomerates by dusting with a finely divided dusting agent.
The liquid organic acid is understood as meaning acids or acid mixtures which are liquid at the processing temperatures or are converted into the liquid state by increasing the temperature or dissolving or dispersing in liquids.
In a preferred embodiment, the novel granules have a dusting agent on the surface of the coat. The core contains preferably 30-90, in particular 50-80, by weight of organic acid. The organic acid preferably consists of one or more C 1
-C
6 -mono- or dicarboxylic acids, in particular formic, acetic and/or propionic acid.
Suitable carriers are porous, organic or inorganic carriers whose particle sizes are from 1 to 1000 pm, preferably from 5 to 100 pm. The core may also contain further solids, for example solids suitable as feed supplements, such as calcium propionate.
Water-soluble polymers, organic acids, salts thereof or inorganic salts having a low melting point may be used as the covering material.
I
0050/46119 3 Cereal brans, silicates, perlite or silicas, in amounts of from to 70, preferably from 20 to 40, by weight, based on the weight of the core, are preferably used as the carrier.
Preferably used covering materials are polyethylene glycols, polyvinylpyrrolidones or C 3
-C
14 preferably C 3
-C
6 organic acids and salts thereof, in particular citric acid, fumaric acid, succinic acid, adipic acid, benzoic acid and salts thereof, or amino acids and salts thereof are preferably used as the covering material.
In a preferred embodiment of the novel process, the carrier is initially taken in a mixer, impregnated with the organic acid and then agglomerated and coated with the covering material.
The loose and impregnated carrier particles are mixed with the covering material (binding liquid), the binding liquid generally consisting of a highly concentrated solution or melt of watersoluble or water-swellable substances which solidify at room temperature (20 0 This binding liquid is preferably applied in the heated state to the impregnated carrier particles and mixed with the latter. The binding liquids solidify on the surface of the impregnated carrier particles. Suitable operating parameters of the mixer result in agglomeration of different particles to give larger granules.
The size of the granules can be established by process parameters in the mixing as well as by subsequent sieving or milling. The granules preferably have a mean diameter of less than 3 mm, in particular 0.3-1.3 mm. If required, residual water may be present in the binding liquid used for coating and agglomeration. After the agglomeration process, this water can be bound by a dry and finely divided dusting agent by means of a dusting process. As a result of this dusting process, it is also possible to prevent subsequent adhesion of the agglomerates and in addition, for example, to apply the salt of the organic acid used (eg. sodium propionate or calcium propionate) to the agglomerate. Furthermore, a scent or flavor material, eg. vanillin, citral or fructin, can, if required, be added during the dusting step, resulting in an additional odor-masking effect and, for example, ensuring that consumption of the animal feed is appealing.
In principle, all nonorganic or inorganic porous carriers are suitable for the preparation of such free-flowing, low-odor agglomerates, provided that they are acid-resistant. Examples are cereal brands, perlite, clay materials, silicates and silicas, 0050/46119 4 the inorganic carriers being preferred since their material properties can be more readily controlled.
Preferably used binding liquids are water-soluble or waterswellable substances which solidify at room temperature. This makes it possible to dispense with the subsequent drying step, in which, apart from the solvent and the additional water, the organic acid too would evaporate off in some cases.
Particularly suitable covering materials (binding liquids) for the agglomeration process and the coating are those which have a softening temperature of more than 30 0 C, preferably more than 0 C, in order to prevent deformation of the agglomerates at a relatively high storage temperature. Covering materials which are preferably to be used are those which furthermore do not counteract the pH-reducing effect of the adsorbed organic acid or, if required, even support or strengthen said effect.
Examples of suitable binding liquids are highly concentrated, heated sugar solutions or alkali metal/alkaline earth metal formate/acetate/propionate solutions. As a result of the final dusting step, the residual water content can be taken up. Polyethylene glycols having a low melting point, eg. PEG 4000, melts of citric acid, of adipic acid, or fumaric acid or of benzoic acid or of salts thereof, highly concentrated solutions of amino acids and mixtures of these acids are preferred as binding liquids. From 5 to 80, preferably from 10 to 25, by weight, based on the weight of the granules, of binding liquid are used.
Suitable dusting agents in addition to the porous carriers themselves are finely divided, milled organic acids or salts thereof, eg. sodium formate, and inorganic salts or Aerosil. 10, preferably from 0.5 to 5, by weight of the dusting agents are added.
In general, the porous carrier is initially taken in the mixer, for example an Eirich mixer, and is impregnated with the organic acid with little energy input. In an alternative procedure, however, the liquid is initially taken in the mixer and the carrier is metered in. In this case, a higher energy input is required.
It is necessary to ensure uniform impregnation and to avoid local overmoistening, which leads to formation of lumps. After impregnation is complete, a free-flowing, slightly cohesive heap of particles is present. The viscosity of the binding liquid should be established by an appropriate choice of temperature so that it is less than 1000, preferably less than 100 mPa.s, in order to achieve a fine drop size distribution when spraying the
I
0050/46119 binding liquid. Owing to the temperature difference between the heated binding liquid and the cooler impregnated carrier, the drops of binding liquid initially solidify rapidly in this preferred embodiment. In the further course of the agglomeration process, the temperature of the bed increases by 10-30 0 C, depending on the type of binding liquid, due to the mechanical and the thermal energy input. Further drops of binding liquid accumulate on the agglomerates already formed and some of these drops coalesce with one another. The energy input increases by about 20% during the agglomeration.
Finally, a finely divided odor-imparting material may also be added with the dusting agent, as described above. In principle, a large number of scents and flavor materials are suitable for this purpose and can be chosen in accordance with the subsequent use of the agglomerates. The amount of these scents may be 1, preferably from 0.05 to 0.5, by weight, based on the granules. The agglomerates thus produced have a low dust content and little odor and their organic acid content is readily water-soluble.
The novel granules are suitable for the treatment of foods and animal feeds and for use in silages. Foods and animal feeds are to be understood in particular as meaning harvest products, such as hay, silage, moist cereals, pulses or grains, as well as milk substitutes, liquid, mixed and mineral feeds, fish silages or fish meal.
Novel granules may contain other additives, for example minerals, vitamins, antibiotics or protein supplements.
Examples (Content of formic acid used 99%/propionic acid used 99%) A. Comparative examples Comparative example 1 100 g of wheat bran are initially taken in a household mixer and impregnated with 100 g of formic acid. The acid is readily taken up; the product exhibits cohesive behavior but can be easily divided up. It has a strong odor of formic acid.
0050/46119 6 Comparative example 2 100 g of Sipernat® (finely divided silica, from Degussa) are initially taken in a household mixer and impregnated with 100 g of an acid mixture consisting of equal amounts of formic acid and propionic acid. The acid mixture is readily taken up; a loose, free-flowing product forms. The product has a pungent unpleasant odor of formic acid/propionic acid.
Comparative example 3 100 g of perlite are initially taken and are impregnated with the formic acid, similarly to Example 1. The acid is readily taken up but the product shows a strong tendency to cake and has a strong pungent odor of formic acid.
B. Impregnation, agglomeration and coating tests Example 1 460 g of Sipernat® (finely divided silica, from Degussa) are initially taken in an Eirich mixer (R02) and are impregnated with 905 g of formic acid; the formic acid content is then 67%. 200 g of sodium formate melt at 80°C are then sprayed, as the binding liquid, from a heated storage container via a binary nozzle into the mixing space containing 1000 g of this mixture. The resulting agglomerates are dusted with 44 g of Sipernat The content of free acid is 54%. The resulting product is free-flowing and has little odor.
Example 2 400 g of Sipernat® are initially taken in an Eirich mixer and are impregnated with 1000 g of formic acid (formic acid content: For agglomeration and coating, 180 g of a concentrated dextral solution at 80 0 C are sprayed, as binding liquid, from a heated storage container via a binary nozzle into the mixing space. The resulting agglomerates are dusted with 45 g of Sipernat and 12 g of citral. The acid content is then 61%. The resulting agglomerates are free-flowing. The power consumption after the impregnation is 400 W, and that after coating is 500 W. The speed is increased from 340 rpm to 460 rpm during the agglomeration step.
Example 3 400g of Sipernat® are initially taken in an Eirich mixer and are impregnated with 11OOg of formic acid, similarly to Example 2; the formic acid content is then 71%. 260g of citric acid melt at 1700C are sprayed, as binding liquid, from a heated storage container via a binary nozzle into the mixing space. The resulting agglomerates are dusted with 44g of Sipernat® and 8g of vanillin. The total acid content is 74%. The resulting agglomerates have a substantially reduced odour of formic acid.
Example 4 8.7kg of Sipernat® are initially taken in a ploughshare mixer (Lo 130) and are impregnated with 24kg of formic acid (formic acid content: For 0 6: agglomeration and coating, 5.5kg of citric acid melt at 170 0 C are sprayed from a :0 heated storage container via a binary nozzle into the mixing space. The resulting agglomerates are dusted with 650g of Sipernat® and 24g of vanillin.
The total acid content is 74%. The resulting agglomerates have a substantially reduced odour and are free-flowing.
S• "Comprises/comprising" when used in this specification is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps, components or groups thereof.
i ":9 9.
o9 9.
THE CLAIMS DEFINING THE INVENTION ARE AS FOLLOWS: 1. Free-flowing granules including of a core and of a coat, wherein the core material contains an organic acid and a porous carrier and the coat has a covering material which is water-soluble or water-swellable at 20 0
C.
2. Granules as claimed in claim 1, wherein the coat additionally has a dusting agent on the surface.
3. Granules as claimed in claim 1, wherein the core contains 30-90% by weight of organic acids.
4. Granules as claimed in claim 1, wherein the organic acid is a C 1
-C
6 mono- or dicarboxylic acid or a mixture of such carboxylic acids.
5. Granules as claimed in claim 1, wherein the carrier used is a porous, organic or inorganic carrier whose particle sizes are from 1 to 1000 gm, preferably from 5 to 100 m.
6. Granules as claimed in claim 1, wherein the covering material used is a water-soluble polymer, an organic acid, a salt thereof or an inorganic salt having a low melting point.
7. Granules as claimed in claim 5, wherein the carrier used is a cereal bran, a silicate, perlite or a silica, in an amount of from 10 to 70, preferably from 20 to by weight.
8. Granules as claimed in claim 6, wherein the covering material used is polyethylene glycol, a polyvinylpyrrolidone or a C 3
-C
14 preferably C 3
-C
6 organic acid or a salt thereof, in particular citric acid, fumaric acid, succinic acid, adipic acid, benzoic acid, sorbic acid or a salt thereof or an amino acid or a salt S thereof.

Claims (3)

  1. 9. A process for the preparation of granules containing organic acids and porous carriers, which includes impregnating the carrier with a liquid organic acid, then agglomerating it with a liquefied covering material which solidifies at room temperature, the covering material being added in an amount such that the resulting granules are coated, and, if required, providing a further odour by adding scents and, if required,ensuring free-flowing properties of the agglomerates by dusting with a finely divided dusting agent. A process as claimed in claim 9, wherein the carrier is initially taken in a mixer, impregnated with the organic acid and then agglomerated and coated with the covering material. a. •11. Use of granules as claimed in claim 1 for acid treatment and preservation of foods and animal feeds, and in silages.
  2. 12. Granules substantially as herein described with reference to the S" examples.
  3. 13. A process substantially as herein described with reference to the Sexamples. :examples. 0050/46119 Free-flowing granules based on organic acids, preparation of said granules and their use Abstract In free-flowing granules consisting of a core and a coat, the core material contains an organic acid and a porous carrier and the coat has a covering material which is water-soluble or water- swellable at
AU69286/96A 1995-08-30 1996-08-26 Free-flowing granules based on organic acids, preparation of said granules and their use Ceased AU706207B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19531782A DE19531782A1 (en) 1995-08-30 1995-08-30 Free-flowing granules based on organic acids, process for their preparation and their use
DE19531782 1995-08-30
PCT/EP1996/003757 WO1997007687A1 (en) 1995-08-30 1996-08-26 Pourable organic acid-based granulates, process for their preparation and their use

Publications (2)

Publication Number Publication Date
AU6928696A AU6928696A (en) 1997-03-19
AU706207B2 true AU706207B2 (en) 1999-06-10

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AU69286/96A Ceased AU706207B2 (en) 1995-08-30 1996-08-26 Free-flowing granules based on organic acids, preparation of said granules and their use

Country Status (19)

Country Link
EP (1) EP0847243A1 (en)
JP (1) JPH11511969A (en)
KR (1) KR19990044266A (en)
CN (1) CN1193892A (en)
AU (1) AU706207B2 (en)
BR (1) BR9609990A (en)
CA (1) CA2227282A1 (en)
CZ (1) CZ49998A3 (en)
DE (1) DE19531782A1 (en)
EA (1) EA000874B1 (en)
GE (1) GEP20002062B (en)
HU (1) HUP9802322A3 (en)
IL (1) IL122355A (en)
NO (1) NO980861D0 (en)
NZ (1) NZ316933A (en)
PL (1) PL325169A1 (en)
SK (1) SK22898A3 (en)
TR (1) TR199800344T1 (en)
WO (1) WO1997007687A1 (en)

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DE19710127A1 (en) * 1997-03-12 1998-09-17 Herbert Dr Widulle Purification of drinking water to reduce the germ content
DE19933906A1 (en) * 1999-07-22 2001-01-25 Eckhard Eltz Blower assembly to conserve the edible characteristics of stored animal feed suitable for use on small farms
DE10055390A1 (en) * 2000-11-09 2002-05-29 Nutrinova Gmbh Use of an acid preparation as a feed additive in livestock rearing
AU2003209182A1 (en) * 2002-01-08 2003-07-24 Can Technologies, Inc. Encapsulation by coating with a mixture of lipids and hydrophobic, high melting point compounds
KR100451545B1 (en) * 2002-03-18 2004-10-06 김유용 The product method of mixing compound containing hydrochloric acid and scoria, mixing compound and feed
DE10231891A1 (en) * 2002-07-12 2004-01-22 Basf Ag Coated formulation containing sodium, potassium, cesium and/or ammonium diformate is used in premix for animal feed or additive, as performance and/or growth promoter; acidifier; preservative or silage or in fertilizer
SE528410C2 (en) * 2004-06-30 2006-11-07 Kemira Grow How Ab Antimicrobial acidifying feed product and process for its preparation
TW200635959A (en) * 2005-02-04 2006-10-16 Basf Ag Water swellable material
DE102006021392B4 (en) * 2006-05-08 2013-06-27 Ligrana Gmbh composition
DE102007031039A1 (en) * 2007-07-04 2009-01-08 Süd-Chemie AG Process for the careful refining of vegetable oils with natural bleaching earth
LU500270B1 (en) 2021-06-10 2022-12-12 Lucas Brendler Carboxylic Acid Loaded Salt Carrier and the Method for Producing thereof
DE102021115047A1 (en) 2021-06-10 2022-12-15 André Brendler Carboxylic acid loaded salt carrier and the process for the preparation thereof

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NL149989B (en) * 1967-03-08 1976-07-15 Philips Nv GRANULAR PREPARATION.
CH484625A (en) * 1969-04-03 1970-01-31 Libavia Ag Process for the production of granulated animal feed
AR206283A1 (en) * 1971-01-27 1976-07-15 Chinoin Gyogyszer Es Vegyeszet A COMPOSITION FOR THE PRESERVATION OF PRODUCTS OF ANIMAL OR PLANT ORIGIN
CH613607A5 (en) * 1975-06-11 1979-10-15 Lonza Ag Ensiling agent and process for preparation thereof
US4199606A (en) * 1977-09-22 1980-04-22 Bland Bobby Propionic acid on a carrier material as a preservative
DE3103623A1 (en) * 1979-08-03 1982-09-16 Siegfried Dr. 8069 Sünzhausen Moser Mineral-rich supplementary feed and use thereof
IT1185550B (en) * 1985-04-12 1987-11-12 Dox Al Italia Spa NON-DUSTY MIXTURES OF FLOURS OR FLOURS WITH ACTIVE INGREDIENTS FOR MANGIMISTICS
IT1229930B (en) * 1988-10-14 1991-09-16 Dox Al Italia Spa PROCEDURE FOR THE PREPARATION OF MIXTURES FOR FOOD AND FOOD USE INCLUDING ACTIVE SUBSTANCES UNIFORMLY DISTRIBUTED
US5082675A (en) * 1989-07-29 1992-01-21 Bp Chemicals Limited Ensiling composition
DE4117399A1 (en) * 1990-06-14 1992-01-09 Micro Plus Konzentrate Gmbh Agent for conditioning granular fodder material - is mixt. of molasses and e.g. dextrin additive, forming film which inhibits dust formation
DE4217971C1 (en) * 1992-05-30 1993-10-21 Boehringer Ingelheim Vetmed Process and fluid bed apparatus for granulating and / or wrapping
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Publication number Publication date
PL325169A1 (en) 1998-07-06
CZ49998A3 (en) 1998-08-12
CA2227282A1 (en) 1997-03-06
SK22898A3 (en) 1998-12-02
EP0847243A1 (en) 1998-06-17
KR19990044266A (en) 1999-06-25
CN1193892A (en) 1998-09-23
HUP9802322A2 (en) 1999-01-28
NO980861L (en) 1998-02-27
IL122355A0 (en) 1998-04-05
DE19531782A1 (en) 1997-03-06
WO1997007687A1 (en) 1997-03-06
HUP9802322A3 (en) 2001-08-28
BR9609990A (en) 1999-07-06
NZ316933A (en) 1999-01-28
GEP20002062B (en) 2000-05-10
AU6928696A (en) 1997-03-19
NO980861D0 (en) 1998-02-27
EA000874B1 (en) 2000-06-26
JPH11511969A (en) 1999-10-19
TR199800344T1 (en) 1998-05-21
IL122355A (en) 2000-08-31
EA199800229A1 (en) 1998-12-24
MX9801399A (en) 1998-05-31

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