US3563866A - Electrodeposition of nickel - Google Patents
Electrodeposition of nickel Download PDFInfo
- Publication number
- US3563866A US3563866A US787271A US3563866DA US3563866A US 3563866 A US3563866 A US 3563866A US 787271 A US787271 A US 787271A US 3563866D A US3563866D A US 3563866DA US 3563866 A US3563866 A US 3563866A
- Authority
- US
- United States
- Prior art keywords
- nickel
- satin
- deposits
- bath
- baths
- 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
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title abstract description 61
- 229910052759 nickel Inorganic materials 0.000 title abstract description 31
- 238000004070 electrodeposition Methods 0.000 title description 3
- 238000007747 plating Methods 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 8
- 229940124530 sulfonamide Drugs 0.000 abstract description 7
- 150000003456 sulfonamides Chemical class 0.000 abstract description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract description 4
- UCAGLBKTLXCODC-UHFFFAOYSA-N p-Aminosulfonyl-benzoic Acid Natural products NS(=O)(=O)C1=CC=C(C(O)=O)C=C1 UCAGLBKTLXCODC-UHFFFAOYSA-N 0.000 description 15
- 229920001223 polyethylene glycol Polymers 0.000 description 15
- 239000000243 solution Substances 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 13
- 229920001515 polyalkylene glycol Polymers 0.000 description 12
- 239000002202 Polyethylene glycol Substances 0.000 description 10
- 239000002659 electrodeposit Substances 0.000 description 9
- -1 fluoborate Chemical compound 0.000 description 9
- 238000000151 deposition Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000002310 reflectometry Methods 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 6
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 6
- MMNTZXRQPVRSSO-UHFFFAOYSA-N sulfamoylformic acid Chemical compound NS(=O)(=O)C(O)=O MMNTZXRQPVRSSO-UHFFFAOYSA-N 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920001451 polypropylene glycol Polymers 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- KHBQMWCZKVMBLN-UHFFFAOYSA-N Benzenesulfonamide Chemical compound NS(=O)(=O)C1=CC=CC=C1 KHBQMWCZKVMBLN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- DYNFCHNNOHNJFG-UHFFFAOYSA-N 2-formylbenzoic acid Chemical compound OC(=O)C1=CC=CC=C1C=O DYNFCHNNOHNJFG-UHFFFAOYSA-N 0.000 description 1
- KDNIOKSLVIGAAN-UHFFFAOYSA-N 2-sulfamoylbenzoic acid Chemical compound NS(=O)(=O)C1=CC=CC=C1C(O)=O KDNIOKSLVIGAAN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 101000913968 Ipomoea purpurea Chalcone synthase C Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 101000907988 Petunia hybrida Chalcone-flavanone isomerase C Proteins 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 150000008331 benzenesulfonamides Chemical class 0.000 description 1
- CSKFLHAERVCLRT-UHFFFAOYSA-N benzenesulfonyl(carboxy)carbamic acid Chemical compound OC(=O)N(C(O)=O)S(=O)(=O)C1=CC=CC=C1 CSKFLHAERVCLRT-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
Definitions
- the invention relates to the electrodeposition of nickel on a substrate to provide a finished product whose surface has a satin-like appearance, as well as having enhanced corrosion resistance properties.
- satin-like appearance is meant that the deposits, rather than being fully bright and highly reflective, exhibit a soft, lustrous sheen with reduced reflectivity and gloss approaching a matte finish.
- Plating baths providing such deposits are particularly useful for the plating of motor vehicle components to reduce reflective glare on the driver of the vehicle, as well as on the operators of other vehicles.
- federal legislation has recently been enacted whereby certain components of military vehicles such as windshield moldings and Wiper arms and blades, rear view mirrors, mounting and trim hardware, etc., must not have a specular gloss rating beyond a stated maximum.
- a plating bath capable of depositing uniform electrodeposits having a satin appearance with reduced reflectivity.
- a second technique to obtain satin finishes previously used has been to add fine, bath insoluble powders to the nickel plating bath.
- the particles are occluded in the otherwise smooth nickel deposits thereby providing an irregular surface having a lustrous, satin-like finish.
- US. Patents 3,l52,97123 While such baths have provided outstanding results, there are certain disadvantages in using such baths. For example, it is not possible to filter these solutions without removal therefrom of the fine powders, and provisions must be made to continually agitate the baths to keep the particles dispersed.
- An object of this invention is to provide a process for electro-depositing nickel having a satin-like appearance without the necessity of mechanical abrasion of the metal surface and without the use of fine insoluble particles in the plating bath. Another object is to provide nickel plating baths containing organic agents which make possible deposition therefrom of nickel electrodeposits having a uniform, satin finish of reduced reflectivity.
- the present invention comprises the conjoint use of a polyalkylene glycol and a carboxy sulfonamide in a nickel plating bath of the usual composition to make possible deposition therefrom of electrodeposits having the satin appearance described above.
- These baths are more easily controllable, provide uniform deposits, and obviate the problems associated with other techniques previously known for obtaining satin deposits.
- the baths of the invention comprise a solution of certain organic addition agents to be more fully described below, in otherwise conventional nickel plating baths.
- the compositions of conventional nickel plating baths are well known and include nickel salts, such as nickel chloride, sulfate, fluoborate, or sulfamate and usually contain a bufler such as boric acid.
- a particularly useful bath is the well-known Watts Bath with a composition of from about 50 to 200 g./l. of nickel chloride, 50 to 300 g./l. of nickel sulfate, and 30 to 50 g./l. of boric acid.
- the bath may also contain the usual wetting agents and/or anti-pitting agents.
- the baths are generally operated at a pH range of 2 to 6 and a temperature of from. 60 to F.
- the first class of these compounds is of the following formula:
- CHOHzO R and R are the same or different and are H, CH or C H and n is an integer from 6 to 15 inclusive when X is CH CH O, and is from 5 to 11 when X is CH3 -(IJHCH2O'
- the compounds described above are polyethylene glycols, polypropylene glycols, methoxy and ethoxy polyethylene glycols and methoxy and ethoxy polypropylene glycols having a molecular weight of from about 300 to about 700.
- a preferred group of compounds for use in the baths of this invention are compounds described above having a molecular weight of from about 350 to 500.
- glycol compounds of this invention are used in a concentration of from about 0.25 to 15 milligrams per liter, preferably 0.5 to 4 milligrams per liter of plating bath.
- the polyethylene and methoxy polyethylene glycols are available from the Union Carbide Corporation under the trademark Carbowax.
- the second class of compounds to be used in the plating baths of this invention is of the following formula:
- par oxy enzene su onann e 12 " ⁇ Mtthoxy ptullyethylenenglycoht Lw. 750- 0. 30% Unacceptable dark recess parboxy enzeue su onami e 13 g, g g fiif d 1 Unacceptable, bright recess par oxy enzene s onami e l 14 th glycol, 350 0 0005 Acceptable, uniform; Satin like deposits 15 p-Carboxy benzene snlfonannde 1. 0 Do Polyethylene glycol, M W 409...- 0. 003 16 p-Carboxy benzene sulfonamide" 1. 5 D o.
- sulfonamides are substituted benzene sulfonamides having as an essential requisite a carboxy group in the para position.
- the preferred compound of this group is p-carboxy benzene sulfonamide, i.e., where n is zero in the above formula.
- the sulfonamides are used in a concentration of from about 0.5 to about 5 grams per liter, preferably 1 to 3 grams per liter of plating bath.
- An outstanding benefit of the baths of the invention is that satin deposits can be obtained that are uniform in appearance over the complete area of the part being plated. Because commercial parts have contours and therefore varying current densities are obtained during plating, it is very difficult to obtain uniform deposits. Thus, while the use of either of the addition agents of the invention alone, or in combination with a variety of other materials may produce deposits with reduced gloss, such deposits are not uniform and therefore unacceptable for commercial purposes. On the other hand, while it may be possible to obtain uniform deposits with such combinations, the deposits do not have the proper gloss, i.e., they are either too dull or they approach being fully bright, and therefore not acceptable for the purpose of this invention. It is only when the specific additives of the in vention are used in combination are deposits with the requisite properties obtained.
- the baths of this invention may be used for the deposition of nickel with a satin-like appearance on a variety of basis materials.
- the plating can be carried out directly on the basis metals such as steel, zinc die castings, or other metals, or the basis metal may be first plated with copper or a semi-bright nickel, or both.
- plastic materials such as ABS or polypropylene, approximately made conductive by conventional techniques may be plated using the baths of this invention.
- methyl polyethylene glycol sold as Carbowax 350 by Union Carbide Corp.
- Five smaller steel panels were then plated under the same conditions as the prior panel. The deposits on all five panels were observed to be uniform, with a soft, satin-like appearance.
- the panels were then chromium plated using a conventional chromium plating bath and then subjected to a specular gloss test in accordance with the widely accepted A'STM method for specular glass determination identified as ASTM Designation: D 523-62T, revised 1962. using a Gardner Glossmeter.
- Deposition of the satin-nickel deposits of this invention is generally followed by chromium plating thereon, using any of the chromium plating baths well known to the art.
- Such baths may comprise mixtures of chromic acid or chromic acid anhydride, or dichromates or polychromates with appropriate amounts of certain anions such as sulfate, fluoride, fluosilicate, etc.
- An electroplating bath for the deposition of nickel comprising an aqueous acidic nickel salt solution containing therein a polyalkylene glycol of the formula:
- R and R are the same or different and are H, CH or C H and n is an integer from 6 to 15 inclusive when X is --CII CH O, and is from 5 to 11 when X is CH 3H-oH20- and a carboxy sulfonamide of the formula:
- said polyalkylene glycol has a molecular weight of from about 300 to about 700 and is present in a concentration of from about 0.25 to about 15 milligrams per liter of solution, and said carboxy sulfonamide is present in an amount of from about 0.5 to about 5 grams per liter of solution.
- a method of electrodepositing nickel on a conductive substrate which comprises the step of electrodepositing nickel from an aqueous acid nickel plating bath containing dissolved therein a polyalkylene glycol of the formula:
- X is -CH2CI'I20 0! CH3 -oHcH o R and R are the same or different and are H, CH
- n is an integer from 6 to 15 inclusive when X is CH CH O, and is from 5 to 11 when X is l S OzNHz wherein R is CH C H OH; and n is an integer from 0 to 3 inclusive, said glycol and said sulfonamide each being present in an amount such that the combination is effective to produce a satin-like finish nickel electrodeposit.
- said polyalkylene glycol has a molecular weight of from about 300 to about 700 and is present in a concentration of from about 0.25 to about 15 milligrams per liter of solution.
- said polyalkylene glycol has a molecular weight of from about 300 to about 700 and is present in a concentration of from about 0.25 to about 15 milligrams per liter of solution and said carboxy sulfonamide is p-carboxy benzene sulfonamide and is present in an amount of from about 0.5 to about 5 grams per liter of solution.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US78727168A | 1968-12-26 | 1968-12-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3563866A true US3563866A (en) | 1971-02-16 |
Family
ID=25140935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US787271A Expired - Lifetime US3563866A (en) | 1968-12-26 | 1968-12-26 | Electrodeposition of nickel |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US3563866A (xx) |
| JP (1) | JPS4837896B1 (xx) |
| BE (1) | BE742662A (xx) |
| DE (1) | DE1963424A1 (xx) |
| FR (1) | FR2027115A1 (xx) |
| GB (1) | GB1247258A (xx) |
| NL (1) | NL144337B (xx) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6045682A (en) * | 1998-03-24 | 2000-04-04 | Enthone-Omi, Inc. | Ductility agents for nickel-tungsten alloys |
-
1968
- 1968-12-26 US US787271A patent/US3563866A/en not_active Expired - Lifetime
-
1969
- 1969-12-04 BE BE742662D patent/BE742662A/xx unknown
- 1969-12-04 FR FR6941921A patent/FR2027115A1/fr not_active Withdrawn
- 1969-12-18 DE DE19691963424 patent/DE1963424A1/de active Pending
- 1969-12-19 NL NL696919055A patent/NL144337B/xx unknown
- 1969-12-22 GB GB62414/69A patent/GB1247258A/en not_active Expired
- 1969-12-25 JP JP44103891A patent/JPS4837896B1/ja active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6045682A (en) * | 1998-03-24 | 2000-04-04 | Enthone-Omi, Inc. | Ductility agents for nickel-tungsten alloys |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS4837896B1 (xx) | 1973-11-14 |
| NL144337B (nl) | 1974-12-16 |
| GB1247258A (en) | 1971-09-22 |
| DE1963424A1 (de) | 1970-08-27 |
| NL6919055A (xx) | 1970-06-30 |
| BE742662A (xx) | 1970-05-14 |
| FR2027115A1 (xx) | 1970-09-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AS | Assignment |
Owner name: OXY METAL INDUSTRIES CORPORATION Free format text: CHANGE OF NAME;ASSIGNOR:OXY METAL FINISHING CORPORATION;REEL/FRAME:003967/0084 Effective date: 19741220 |
|
| AS | Assignment |
Owner name: HOOKER CHEMICALS & PLASTICS CORP. Free format text: MERGER;ASSIGNOR:OXY METAL INDUSTRIES CORPORATION;REEL/FRAME:004075/0885 Effective date: 19801222 |
|
| AS | Assignment |
Owner name: OCCIDENTAL CHEMICAL CORPORATION Free format text: CHANGE OF NAME;ASSIGNOR:HOOKER CHEMICAS & PLASTICS CORP.;REEL/FRAME:004126/0054 Effective date: 19820330 |
|
| AS | Assignment |
Owner name: OMI INTERNATIONAL CORPORATION, 21441 HOOVER ROAD, Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:OCCIDENTAL CHEMICAL CORPORATION;REEL/FRAME:004190/0827 Effective date: 19830915 |
|
| AS | Assignment |
Owner name: MANUFACTURERS HANOVER TRUST COMPANY, A CORP OF NY Free format text: SECURITY INTEREST;ASSIGNOR:INTERNATIONAL CORPORATION, A CORP OF DE;REEL/FRAME:004201/0733 Effective date: 19830930 |