EP0480171B1 - Staubfreie Einbettmasse für passgenaue Gussstücke und Verfahren zur Herstellung dieser Einbettmassen - Google Patents

Staubfreie Einbettmasse für passgenaue Gussstücke und Verfahren zur Herstellung dieser Einbettmassen Download PDF

Info

Publication number: EP0480171B1
Authority: EP; European Patent Office
Prior art keywords: component; silicon dioxide; components; water; embedding compound
Prior art date: 1990-10-11
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

Application number

EP91114886A

Other languages

German (de)

English (en)

French (fr)

Other versions

EP0480171A3 (en

EP0480171A2 (de

Inventor

Gerlinde Dipl.-Ing. Gantert

Bernd Dr. Dipl.-Ing. Kempf

Klaus-Peter Dr. Dipl.-Chem. Gundlach

Ulrich Dr Dipl.-Phys. Kump

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.)

Evonik Operations GmbH

Original Assignee

Degussa GmbH

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.)

1990-10-11

Filing date

1991-09-04

Publication date

1994-07-20

1991-09-04 Application filed by Degussa GmbH filed Critical Degussa GmbH

1992-04-15 Publication of EP0480171A2 publication Critical patent/EP0480171A2/de

1993-01-20 Publication of EP0480171A3 publication Critical patent/EP0480171A3/de

1994-07-20 Application granted granted Critical

1994-07-20 Publication of EP0480171B1 publication Critical patent/EP0480171B1/de

2011-09-04 Anticipated expiration legal-status Critical

Status Expired - Lifetime legal-status Critical Current

Links

238000005495 investment casting Methods 0.000 title claims abstract 3
238000000034 method Methods 0.000 title claims description 7
230000008569 process Effects 0.000 title claims description 7
239000000463 material Substances 0.000 title abstract description 33
VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 60
235000012239 silicon dioxide Nutrition 0.000 claims abstract description 31
239000000377 silicon dioxide Substances 0.000 claims abstract description 26
239000000395 magnesium oxide Substances 0.000 claims abstract description 18
CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 18
AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 18
XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
229910019142 PO4 Inorganic materials 0.000 claims abstract description 12
235000021317 phosphate Nutrition 0.000 claims abstract description 12
239000010452 phosphate Substances 0.000 claims abstract description 8
NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 8
235000012245 magnesium oxide Nutrition 0.000 claims abstract description 6
150000003013 phosphoric acid derivatives Chemical class 0.000 claims abstract description 4
LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
239000007788 liquid Substances 0.000 claims description 21
238000002156 mixing Methods 0.000 claims description 11
PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
238000004519 manufacturing process Methods 0.000 claims description 9
150000002148 esters Chemical class 0.000 claims description 8
150000005846 sugar alcohols Polymers 0.000 claims description 7
125000001931 aliphatic group Chemical group 0.000 claims description 6
239000011230 binding agent Substances 0.000 claims description 6
239000002904 solvent Substances 0.000 claims description 6
125000004432 carbon atom Chemical group C* 0.000 claims description 5
239000003232 water-soluble binding agent Substances 0.000 claims description 5
150000001298 alcohols Chemical class 0.000 claims description 4
239000000203 mixture Substances 0.000 claims description 4
229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
239000001913 cellulose Substances 0.000 claims description 3
229920002678 cellulose Polymers 0.000 claims description 3
239000000843 powder Substances 0.000 claims description 3
LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 2
150000001875 compounds Chemical class 0.000 claims 12
238000000465 moulding Methods 0.000 claims 1
239000003960 organic solvent Substances 0.000 abstract description 3
239000000428 dust Substances 0.000 description 15
238000003860 storage Methods 0.000 description 9
238000005054 agglomeration Methods 0.000 description 8
230000002776 aggregation Effects 0.000 description 8
238000005266 casting Methods 0.000 description 6
239000010453 quartz Substances 0.000 description 6
238000005516 engineering process Methods 0.000 description 5
235000011187 glycerol Nutrition 0.000 description 3
WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
235000019422 polyvinyl alcohol Nutrition 0.000 description 3
230000003679 aging effect Effects 0.000 description 2
239000000956 alloy Substances 0.000 description 2
229910045601 alloy Inorganic materials 0.000 description 2
230000015572 biosynthetic process Effects 0.000 description 2
150000001735 carboxylic acids Chemical class 0.000 description 2
235000014113 dietary fatty acids Nutrition 0.000 description 2
238000001035 drying Methods 0.000 description 2
238000010410 dusting Methods 0.000 description 2
230000000694 effects Effects 0.000 description 2
239000000194 fatty acid Substances 0.000 description 2
229930195729 fatty acid Natural products 0.000 description 2
238000002844 melting Methods 0.000 description 2
230000009467 reduction Effects 0.000 description 2
239000004576 sand Substances 0.000 description 2
239000007787 solid Substances 0.000 description 2
DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
239000004254 Ammonium phosphate Substances 0.000 description 1
229920000084 Gum arabic Polymers 0.000 description 1
241000978776 Senegalia senegal Species 0.000 description 1
201000010001 Silicosis Diseases 0.000 description 1
229920002472 Starch Polymers 0.000 description 1
239000000205 acacia gum Substances 0.000 description 1
235000010489 acacia gum Nutrition 0.000 description 1
239000000654 additive Substances 0.000 description 1
229910000148 ammonium phosphate Inorganic materials 0.000 description 1
235000019289 ammonium phosphates Nutrition 0.000 description 1
125000000129 anionic group Chemical group 0.000 description 1
230000008901 benefit Effects 0.000 description 1
238000003889 chemical engineering Methods 0.000 description 1
230000008602 contraction Effects 0.000 description 1
238000001816 cooling Methods 0.000 description 1
230000001419 dependent effect Effects 0.000 description 1
MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
238000000605 extraction Methods 0.000 description 1
-1 fatty acid esters Chemical class 0.000 description 1
150000004665 fatty acids Chemical class 0.000 description 1
238000011049 filling Methods 0.000 description 1
239000010440 gypsum Substances 0.000 description 1
229910052602 gypsum Inorganic materials 0.000 description 1
239000000383 hazardous chemical Substances 0.000 description 1
231100000206 health hazard Toxicity 0.000 description 1
238000010438 heat treatment Methods 0.000 description 1
229930195733 hydrocarbon Natural products 0.000 description 1
150000002430 hydrocarbons Chemical class 0.000 description 1
230000002209 hydrophobic effect Effects 0.000 description 1
231100001231 less toxic Toxicity 0.000 description 1
210000004072 lung Anatomy 0.000 description 1
238000005259 measurement Methods 0.000 description 1
230000008018 melting Effects 0.000 description 1
229910052751 metal Inorganic materials 0.000 description 1
239000002184 metal Substances 0.000 description 1
YLGXILFCIXHCMC-JHGZEJCSSA-N methyl cellulose Chemical compound COC1C(OC)C(OC)C(COC)O[C@H]1O[C@H]1C(OC)C(OC)C(OC)OC1COC YLGXILFCIXHCMC-JHGZEJCSSA-N 0.000 description 1
238000012986 modification Methods 0.000 description 1
230000004048 modification Effects 0.000 description 1
150000002894 organic compounds Chemical class 0.000 description 1
238000004062 sedimentation Methods 0.000 description 1
238000005204 segregation Methods 0.000 description 1
238000000926 separation method Methods 0.000 description 1
RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
239000002002 slurry Substances 0.000 description 1
235000019698 starch Nutrition 0.000 description 1
239000008107 starch Substances 0.000 description 1
239000004094 surface-active agent Substances 0.000 description 1
238000005303 weighing Methods 0.000 description 1
239000000080 wetting agent Substances 0.000 description 1

Classifications

- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
- B22C1/02—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by additives for special purposes, e.g. indicators, breakdown additives
- B22C1/08—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by additives for special purposes, e.g. indicators, breakdown additives for decreasing shrinkage of the mould, e.g. for investment casting

Definitions

the invention relates to a water-soluble phosphate, magnesium oxide and silicon dioxide containing, mixed with liquids, non-dusting investment material for the production of precisely fitting castings in dental technology and in the jewelry industry and a method for producing such investment materials.
tooth replacement parts or jewelry parts are usually produced by casting processes.
the tooth replacement part or jewelry part is modeled in wax, embedded, the wax is removed by melting and the molten alloy is poured into the resulting mold.
the investment materials used for the production of the molds are subject to high demands with regard to the accuracy of fit of the parts produced therein. Due to the expansion of the setting and the thermal expansion of the investment, the contraction of the cast metal part by cooling after casting must be exactly compensated.
Phosphate-bonded investment materials containing magnesium oxide and silicon dioxide, since they are resistant to high temperatures and can also serve as a casting mold for high-melting alloys.
Phosphate-bonded investment materials are mixed with water or a water / silica sol mixture. The addition of the water leads to the setting reaction of the two binder components ammonium phosphate and magnesium oxide.
DE-PS 37 07 853 describes a powdered investment material which only shows a low level of dust formation. This is achieved by adding 0.5 - 5% of a wetting agent consisting of liquid hydrophobic hydrocarbons, fatty acid esters or fatty acids to the powder mixture of soluble phosphate, magnesium oxide and quartz. Since these liquids have a low vapor pressure, these are always relatively long-chain, organic compounds which lead to an oily grip in the investment materials and reduce the kneadability, so that anionic, surface-active agents must also be added. However, this can have a negative impact on the technical properties of the investment material (low strength, excessive setting expansion, unpleasant smell).
a wetting agent consisting of liquid hydrophobic hydrocarbons, fatty acid esters or fatty acids
a liquid to the investment can also be done for other reasons.
an investment is described in Derwent Abstract 84-003437 / 01, to which an aliphatic alcohol is added in amounts of 0.01 to 0.3% by weight in order to prevent the reaction of the binder material due to the atmospheric humidity, and thus to increase the storage stability increase.
the amounts added are so small that no dust-free is obtained.
a process for the production of these investment materials should also be developed.
This object is achieved in that the investment is divided into two components a and b, of which component a contains the entire magnesium oxide and component b contains the entire phosphate, while the silicon dioxide content either only added to component b or to the two components a and b is distributed, component b containing at least 0.5% by weight of water and component a in the presence of silicon dioxide containing 0.4 to 6% by weight of a hydrophilic aliphatic solvent with a vapor pressure of less than 600 Pa.
Component a preferably contains the magnesium oxide, part of the silicon dioxide and 0.4 to 6% by weight of a monohydric alcohol having 4 to 7 carbon atoms or a liquid polyhydric alcohol or the corresponding esters.
component a can also contain hydrophilic carboxylic acids having 3 to 7 carbon atoms or their esters.
the organic solvent can be dispensed with, since magnesium oxide is less dusty and far less toxic than silicon dioxide.
the two components a and b can be packed and stored separately in the moist state. Only when they are processed are they mixed together in the correct mixing ratio and mixed with the mixing liquid.
a polyhydric alcohol such as e.g. Ethylene glycol or glycerin.
Ethylene glycol or glycerin may be advantageous to add the entire mixing water necessary for the production of the investment to component b. This means that only components a and b are required to prepare the investment material and no additional mixing water.
Components a and / or b advantageously additionally each contain a water-soluble binder, in particular polyvinyl alcohols in amounts of 0.1 to 2% and / or cellulose derivatives in amounts of 0.1 to 5%. This enables the powder mixtures to be agglomerated, with agglomerate diameters of 0.5 to 5 mm having proven best.
a water-soluble binder in particular polyvinyl alcohols in amounts of 0.1 to 2% and / or cellulose derivatives in amounts of 0.1 to 5%.
This agglomeration has the essential advantage that the two components can then be mixed again after drying, without a reaction taking place or a dust load exceeding the legal limit value being able to occur.
the dust-free investment material is produced by dividing the investment material consisting of water-soluble phosphates, magnesium oxide and silicon dioxide into two components a and b, component a, which contains all of the magnesium oxide and possibly part of the silicon dioxide, in the presence of silicon dioxide with 0.4 to 6% by weight of a hydrophilic aliphatic solvent with a vapor pressure of less than 600 Pa, and component b, which contains the water-soluble phosphate and the remaining part of the silicon dioxide, with at least 0.5% by weight of water is transferred.
the hydrophilic aliphatic solvent used is preferably monohydric alcohols having 4 to 7 carbon atoms, liquid polyhydric alcohols or the corresponding esters.
components a and / or b optionally with the addition of a water-soluble binder in the form of 0.1 to 2% of a polyvinyl alcohol or from 0.1 to 5% of a cellulose derivative, are agglomerated to form agglomerates of preferably 0.5 to 5 mm in diameter and then dried. This makes it possible to mix the two components again without a setting reaction taking place.
the refractory components silicon dioxide can be divided arbitrarily between the two components a and b. However, it has proven useful to keep the proportions approximately the same size in order to ensure that the mixing is as homogeneous as possible during the mixing.
the amount of liquid required to keep dust-free essentially depends on the grain size of the investment material. The finer the material, the more liquid is required. Since ethylene glycol leads to a reduction in the setting reaction at higher concentrations, it makes sense not to increase the glycol requirement by too much sand or by too large a grain size. A glycol content of 5% should never be exceeded.
ethylene glycol butanediol or glycerin can also be used as the binding liquid for component a.
the use of water does not have a negative effect on the dental properties of the investment material. Since this is also not quantity-dependent, the water requirement can always be set as required in addition to the a-component due to the fineness of grain and the amount of sand.
the handling of the investment material according to the invention can be further improved if the two components are agglomerated separately and mixed together again after drying.
water-soluble binders can still be dissolved in the liquid used in both components.
liquid used in both components For example, proven: polyvinyl alcohols, tylose, sugar, gum arabic and soluble starch.
binders that are usually used in agglomeration processes are also conceivable. Such binders are e.g. in "Chemical Engineering, December 4, 1967".
the agglomeration of both components takes place in commercially available mixers, with a fine agglomeration of the respective agglomeration liquid leading to a build-up agglomeration.
a size of approx. 0.5 -5 mm is permitted for the agglomerates.
the liquid requirement for the desired agglomerate formation is 4 to 60 ml / kg solids for component a and 5 to 200 ml / kg for component b.
component b is dried by heating to 50-110 ° C., while component a can be left in the moist state. The two components can then be mixed together without impairing the storage stability and the dental properties.
component a contains only magnesium oxide and no silicon dioxide, it can be agglomerated or tableted without the addition of organic solvents in the form of alcohols, carboxylic acids or esters.
Such agglomerated investment materials are distinguished from conventional investment materials by significantly reduced dust pollution during processing.
To measure the dust load a sample of the investment was mixed in a vessel in a tumble mixer for one minute.
the vessel was then opened and the dust load was measured immediately using a dust measuring device. It was found that the total amount of dusts released is considerably less than the legally permissible limit values, so that a hazard from inhalable, quartz-containing dusts can be excluded.
Components a and b were first homogenized in a mixer in the dry state for 3 minutes, then the liquid was added with continuous mixing and mixed again for 5 minutes.
the setting expansion was determined in accordance with DIN draft 13919, part 2. To determine the accuracy of fit, schematic crown rings were cast and then measured optically. To check the storage stability, repeat measurements were carried out after different storage times.

Landscapes

Engineering & Computer Science (AREA)
Chemical & Material Sciences (AREA)
Materials Engineering (AREA)
Mechanical Engineering (AREA)
Mold Materials And Core Materials (AREA)
Dental Preparations (AREA)
Dental Prosthetics (AREA)
Molds, Cores, And Manufacturing Methods Thereof (AREA)
Noodles (AREA)
Analysing Materials By The Use Of Radiation (AREA)
Silicon Compounds (AREA)
Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)

EP91114886A 1990-10-11 1991-09-04 Staubfreie Einbettmasse für passgenaue Gussstücke und Verfahren zur Herstellung dieser Einbettmassen Expired - Lifetime EP0480171B1 (de)

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
DE4032254		1990-10-11
DE4032254A DE4032254C2 (de)	1990-10-11	1990-10-11	Staubfreie Einbettmasse für passgenaue Gußstücke und Verfahren zur Herstellung dieser Einbettmassen

Publications (3)

Publication Number	Publication Date
EP0480171A2 EP0480171A2 (de)	1992-04-15
EP0480171A3 EP0480171A3 (en)	1993-01-20
EP0480171B1 true EP0480171B1 (de)	1994-07-20

Family

ID=6416069

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP91114886A Expired - Lifetime EP0480171B1 (de)	1990-10-11	1991-09-04	Staubfreie Einbettmasse für passgenaue Gussstücke und Verfahren zur Herstellung dieser Einbettmassen

Country Status (13)

Country	Link
US (1)	US5250110A (da)
EP (1)	EP0480171B1 (da)
JP (1)	JP3242680B2 (da)
AT (1)	ATE108642T1 (da)
AU (1)	AU651137B2 (da)
BR (1)	BR9104393A (da)
CA (1)	CA2053138A1 (da)
DE (2)	DE4032254C2 (da)
DK (1)	DK0480171T3 (da)
ES (1)	ES2059004T3 (da)
IL (1)	IL99711A (da)
MX (1)	MX9101480A (da)
ZA (1)	ZA918090B (da)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
JP3529523B2 (ja) *	1995-11-17	2004-05-24	株式会社ジーシー	歯科用リン酸塩系埋没材組成物
DE102006012630B4 (de) *	2006-03-20	2010-04-08	Amann Girrbach Ag	Dosiervorrichtung zum Mischen von mindestens einer pulverförmigern Substanz mit mindestens einer flüssigen Substanz
JP2010529091A (ja) *	2007-06-06	2010-08-26	インノテーレ・ゲゼルシャフト・ミト・ベシュレンクテル・ハフツング	水硬性セメントをベースとするインプラント材料ならびにその使用
ATE453471T1 (de) *	2007-11-02	2010-01-15	Shera Werkstofftechnologie Gmb	Keramische einbettmasse zur herstellung einer giessform sowie damit verbundene herstellungsverfahren
CA2885237A1 (en) *	2012-10-18	2014-04-24	Cermatco Ltd	Investment binder and use of the investment binder
GB2569193B (en)	2017-12-11	2021-09-29	Dudley Shaw Richard	Investment casting compositions
KR102285589B1 (ko) *	2019-10-22	2021-08-04	시노베스트 주식회사	경화 팽창 증대형 치과주조용 매몰재

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
US2479504A (en) *	1943-07-12	1949-08-16	Ransom & Randolph Company	Investment material
US2466138A (en) *	1944-09-20	1949-04-05	Nat Lead Co	Refractory mold composition
US2875073A (en) *	1955-05-23	1959-02-24	Corn Prod Refining Co	Core binder and process of making cores
US3074803A (en) *	1960-09-27	1963-01-22	Nat Starch Chem Corp	Molding starch composition
US3081177A (en) *	1962-01-25	1963-03-12	J Bird Moyer Co Inc	Dental impression compositions
JPS62212254A (ja) *	1986-03-12	1987-09-18	而至歯科工業株式会社	低粉塵性粉末状歯科用埋没材組成物
JPS63141906A (ja) *	1986-12-03	1988-06-14	G C Dental Ind Corp	歯科鋳造用埋没材

1990
- 1990-10-11 DE DE4032254A patent/DE4032254C2/de not_active Expired - Fee Related
1991
- 1991-09-04 ES ES91114886T patent/ES2059004T3/es not_active Expired - Lifetime
- 1991-09-04 AT AT91114886T patent/ATE108642T1/de not_active IP Right Cessation
- 1991-09-04 DK DK91114886.4T patent/DK0480171T3/da active
- 1991-09-04 DE DE59102243T patent/DE59102243D1/de not_active Expired - Lifetime
- 1991-09-04 EP EP91114886A patent/EP0480171B1/de not_active Expired - Lifetime
- 1991-10-07 US US07/771,558 patent/US5250110A/en not_active Expired - Fee Related
- 1991-10-08 MX MX919101480A patent/MX9101480A/es unknown
- 1991-10-09 JP JP26161391A patent/JP3242680B2/ja not_active Expired - Fee Related
- 1991-10-09 ZA ZA918090A patent/ZA918090B/xx unknown
- 1991-10-10 CA CA002053138A patent/CA2053138A1/en not_active Abandoned
- 1991-10-10 BR BR919104393A patent/BR9104393A/pt not_active Application Discontinuation
- 1991-10-10 AU AU85744/91A patent/AU651137B2/en not_active Ceased
- 1991-10-10 IL IL9971191A patent/IL99711A/en not_active IP Right Cessation

Also Published As

Publication number	Publication date
IL99711A (en)	1995-11-27
IL99711A0 (en)	1992-08-18
ES2059004T3 (es)	1994-11-01
JPH0558834A (ja)	1993-03-09
ATE108642T1 (de)	1994-08-15
EP0480171A3 (en)	1993-01-20
EP0480171A2 (de)	1992-04-15
ZA918090B (en)	1992-07-29
DE4032254C2 (de)	1994-04-21
MX9101480A (es)	1992-04-01
JP3242680B2 (ja)	2001-12-25
CA2053138A1 (en)	1992-04-12
BR9104393A (pt)	1992-06-09
DK0480171T3 (da)	1994-10-17
DE4032254A1 (de)	1992-04-16
DE59102243D1 (de)	1994-08-25
US5250110A (en)	1993-10-05
AU8574491A (en)	1992-05-07
AU651137B2 (en)	1994-07-14

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