US2587744A - Preservation of ether - Google Patents

Preservation of ether Download PDF

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US2587744A
US2587744A US76142A US7614249A US2587744A US 2587744 A US2587744 A US 2587744A US 76142 A US76142 A US 76142A US 7614249 A US7614249 A US 7614249A US 2587744 A US2587744 A US 2587744A
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ether
container
coating
tin
oxide
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US76142A
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Jr Edward Mallinckrodt
Archie E Ruehle
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Mallinckrodt Chemical Works
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Mallinckrodt Chemical Works
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Priority to US76142A priority Critical patent/US2587744A/en
Priority claimed from US20939651 external-priority patent/US2639243A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D25/00Details of other kinds or types of rigid or semi-rigid containers
    • B65D25/14Linings or internal coatings

Description

March 1952 E. MALLINCKRODT, JR., ETAL 2,587,744
PRESERVATION OF ETHER Filed Feb. 12. 1949 Patented Mar. 4, 1952 UNITED STATES ATENT OFFICE PRESERVATION F ETHER Application'February 12, 1949,. Serial No; 76,142
'7 Claiins. 1 V
This invention relates to the preservation'of ether and more particularly to improved means for packaging ether.
Among the objects of the present invention are the provision of improved'means for protecting packaged ether against decomposition; the provision of means of the character described-which do not cause corrosion of the container; th'eprovision of an improved container for packaging ether; and, the provision of a process for manufacturing improved ether containers. Other objects will be in part apparent and in part pointed out hereinafter.
The invention accordingly comprises the elements and combinations of elements, steps and sequence of steps, features of construction and manipulation, and arrangements of parts which will be exemplified in the structures and methods hereinafter described, and the scope ofthe application of which will be indicated in the following claims.
In the accompanying drawing, in which one of various possible embodiments of the invention is illustrated,
Fig. 1 is a vertical section through an ether can showing one form of our invention; and,
Fig. 2 is a section taken along the line 22 on Fig. 1 but on an enlarged scale.
Similar reference characters indicate corresponding parts throughout the several views of the drawing.
Because diethyl ether is a highly volatile and inflammable liquid which is hazardous to ship and to store, it is usually packaged in containers made of tin plate in preference to containers made of glass or other fragile materials. From the standpoint of safety, durability, and low cost, tin cans have been entirely satisfactory as containers for ether and their use has been widespread for many years. They are, however, subject to one serious disadvantage. Conventional bright tin-plate greatly increases the tendency for ether to be oxidized by air in the container. Aldehydes and peroxides which may be formed by such oxidation are particularly objectionable in anesthetic ether, as evidenced by their limitation to merest traces by the U. S. Pharmacopoeia.
It has been customary to overcome this disadvantage to a considerable extent by covering the inner surface of the container with either an adherent layer of tin oxide or with a coating of metallic copper. The adherent layer of tin oxide is usually produced by heating the cans at an elevated temperature. The treatment is simple, but it has been found that the protection which it aifordsthe ether is somewhat variable. Copper plating the can, on the other hand, is more complicated and also has the disadvantage that it is difficult to apply a copper coating to the tin surface without increasing the tendency of the container to corrode. Other methods have also been proposed, for example, to package the ether in contact with reducing substances, such as cuprous oxide or iron, but these methods have found little favor.
The improved ether container of the present invention comprises a can made of conventional tin-plate; especially treated to produce an adherent coating of cupric and tin oxides on the inner surface. Containers of this type have been found to possess definite advantages. The coating is easily and inexpensively applied using simple, readily available equipment, and provides reliable protection. It is visible on the surface of the tin as a semi-transparent brown stain which is practically insoluble in ether and is not dislodged by agitation of ether in the container.
Referring now to the drawing, an ether can I having conventional side walls 3', bottom 5 and top! is'shown. An opening 9 in top 7 receives neck H which is of a type to receive a vaportight closure member l3.
The interior of container I is coated as shown at' I5 (see Fig. 2) with an adherent coating of cupric and tin oxides. The relative thickness'of the coating has been exaggerated in the drawing to show its location.
The protective coating is preferably produced by wetting the interior of the container with a solution of a thermally unstable copper compound, then drying the surface of the container bydirecting a stream of warm air against it, and finally heating the container in the presence of air ata temperature and for a time sufficient to convert'substantially all of the copper to a divalent oxide and simultaneously to form a surface layer of tin oxide. Part or all of these oxides may be in'the form of a double oxide of copper and tin, but for the purposes of this invention the exact composition need not be known. What is important is that the oxide layer is adherent and affords reliable protection to the ether.
Examples of thermally unstable copper compounds of the type which can be used with this invention are copper acetate, copper formate, and copper acetylacetonate. Numerous solvents for the preferred copper compounds are known, but the adherence of the oxide coating formed by the processes of this inventionis to a large degree dependent upon the nature of the solvent employed.
We have found that the use of amines or mixtures of amines as solvents leads to the most strongly adherent coating. For reasons of economy we prefer to dilute the amine solutions of the copper salts with a low cost solvent, for example, isopropyl alcohol. A mixture of equal parts by volume of diethylamine and di-isopropylamine is particularly desirable as this mixture evaporates at substantially the same rate as isopropyl alcohol. The concentration of the copper salts in the solution need be only a few tenths of a per cent for maximum protection. The exact percentage is not critical, but no advantage is derived from using a greater percentage and there is the danger that as the oxide coating becomes thicker it may also become weaker and break away from the surface of the can, thereby producin a residue in the ether. Many solvents may be used as diluents for the amine solution in place of isopropyl alcohol. Among them are ether, the lower aliphatic alcohols, ethyl acetate, petroleum ether, and toluene.
Example A number of tin cans, of the type commonly employed for packaging ether, were treated in the following manner. A stock solution was prepared by dissolving 15 pounds of cupric acetate in a mixture of gallons of di-isopropylamine and 10 gallons of diethylamine. To 1 gallon of this solution, sufiicient isopropyl alcohol was added to make a total volume of 38 gallons. Some of the resulting solution was poured into each of the cans to be treated, the cans were turned and rotated so that the inner surface was entirely wetted with the solution, and the excess solution was then poured out. The cans were dried with a stream of hot air, then baked at a temperature of about 155-160 C. for 36 hours. The containers were filled with anesthetic grade ether, sealed in the customary manner, and then stored at a temperature of 90 F. Periodically, cans were selected at random and the contents were tested for the presence of aldehydes and peroxides.
After thirteen months the ether met all the requirements of the tests of the U. S. Pharmacopoeia. Moreover, when tested by still more sensitive methods no trace of aldehydes or peroxides was found. In control experiments conducted in parallel, ether stored in untreated but otherwise identical containers failed badly in the limiting tests of the U. S. Pharmacopoeia for aldehydes and peroxides within three months, and ether stored in containers which had been given a coating of tin oxide only showed traces of aldehydes within six months and failed to meet the minimum U. S. P. requirements within thirteen months.
Attention is directed to our copending application, Serial No. 209,396, filed February 5, 1951.
In view of the above, it will be seen that the several objects of the invention are achieved and other advantageous results attained.
As many changes could be made in the above constructions and methods without departing from the scope of the invention, it is intended that all matter contained in the above description or shown in the accompanying drawing shall be interpreted as illustrative and not in a limiting sense.
We claim:
1. A container for ether comprising a container member and a coating on the interior of said container member, said coating comprising cupric oxide and a tin oxide.
2. A container for ether comprising a container member and a coating on the interior of said container member, said coating comprising cupric oxide and a tin oxide, said oxides being in intimate admixture.
3. A container for ether comprising a container member and a coating on the interior of said container member, said coating comprising cupric oxide and a tin oxide, said oxides being in intimate admixture and firmly adhering to the interior of the container member.
4. A container for ether comprising a metallic container member, interior surfaces of said container member being tin, said container member having on its internal surfaces a firmly adherent coating of cupric oxide and tin oxide in intimate admixture to form a preservative coating to preserve ether stored in said container member.
5. The method of preventing the deterioration of other which comprises storing ether in a container in the presence of a tin oxide and cupric oxide.
6. The method of preventing the deterioration of ether which comprises storing ether in a container having an interior surface coating including a tin oxide and cupric oxide.
7. The method of preventing the deterioration of ether which comprises storing ether in a container having an interior surface coating of a tin oxide and cupric oxide firmly adhered to a layer of tin.
' EDWARD MALLINCKRODT, JR.
ARCHIE E. RUEHLE.
REFERENCES CITED The following references are of record in the file of this patent:
UNITED STATES PATENTS Number Name Date 1,632,309 Nitardy June 14, 1927 2,105,906 Demers Jan. 18, 1938 2,135,886 Elder Nov. 8, 1938 2,237,259 Marland Apr. 1, 1941 2,245,561 Nelson et a1 June 1'7, 1941 2,272,609 Kennedy et al Feb. 10, 1942 2,315,475 Cobb et al Mar. 30, 1943 2,316,804 Musher Apr. 20, 1943

Claims (1)

1. A CONTAINER FOR ETHER COMPRISING A CONTAINER MEMBER AND A COATING ON THE INTERIOR OF SAID CONTAINER MEMBER, SAID COATING COMPRISING CUPRIC OXIDE AND A TIN OXIDE.
US76142A 1949-02-12 1949-02-12 Preservation of ether Expired - Lifetime US2587744A (en)

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US20939651 US2639243A (en) 1949-02-12 1951-02-05 Preservation of ether

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2717218A (en) * 1952-07-19 1955-09-06 Gen Am Transport Chemical nickel plating methods and apparatus
US2791074A (en) * 1953-05-29 1957-05-07 Columbia Southern Chem Corp Packaging of anhydrous alkali metal hydroxide

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1632309A (en) * 1927-06-14 Preservation obi ether
US2105906A (en) * 1936-10-26 1938-01-18 Superior Metal Products Compan Method of hot plating containers
US2135886A (en) * 1934-04-16 1938-11-08 American Steel & Wire Co Tire wire and method of making the same
US2237259A (en) * 1939-06-02 1941-04-01 Wood John Mfg Co Inc Process of galvanizing substantially closed containers
US2245561A (en) * 1939-02-08 1941-06-17 Carnation Co Coated container
US2272609A (en) * 1938-11-12 1942-02-10 Revere Copper & Brass Inc Copper coated cooking vessel
US2315475A (en) * 1941-04-23 1943-03-30 Moore Enameling & Mfg Company Enameled cooking utensil
US2316804A (en) * 1939-05-02 1943-04-20 Musher Foundation Inc Tin can container

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1632309A (en) * 1927-06-14 Preservation obi ether
US2135886A (en) * 1934-04-16 1938-11-08 American Steel & Wire Co Tire wire and method of making the same
US2105906A (en) * 1936-10-26 1938-01-18 Superior Metal Products Compan Method of hot plating containers
US2272609A (en) * 1938-11-12 1942-02-10 Revere Copper & Brass Inc Copper coated cooking vessel
US2245561A (en) * 1939-02-08 1941-06-17 Carnation Co Coated container
US2316804A (en) * 1939-05-02 1943-04-20 Musher Foundation Inc Tin can container
US2237259A (en) * 1939-06-02 1941-04-01 Wood John Mfg Co Inc Process of galvanizing substantially closed containers
US2315475A (en) * 1941-04-23 1943-03-30 Moore Enameling & Mfg Company Enameled cooking utensil

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2717218A (en) * 1952-07-19 1955-09-06 Gen Am Transport Chemical nickel plating methods and apparatus
US2791074A (en) * 1953-05-29 1957-05-07 Columbia Southern Chem Corp Packaging of anhydrous alkali metal hydroxide

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