Inert environment sleeve adapter

Abstract

Many chemicals are sensitive to or can react with compounds in the air. For example, many chemicals can react with water vapor and oxygen, and even trace gases such as carbon dioxide, ammonia, and hydrogen sulfide. Chemicals are typically packed in containers. Devices called adapters have been proposed to provide an inert environment when handling reactive chemicals. Adapters are fitted into containers and allow for the establishment of an inert environment surrounding the container's opening.

Description

Technical Field

[0001] Cross - reference to related applications This application claims the benefit of U.S. Provisional Patent Application No. 63 / 491158, filed Mar. 20, 2023, the entire content of which is incorporated herein by reference.

Background Art

[0002] Many chemical substances are sensitive to, or can react with, compounds in the air. For example, many chemical substances can react with water vapor, oxygen, and even trace gases such as carbon dioxide, ammonia, and hydrogen sulfide. In extreme types of reactions, some chemical substances are pyrophoric (spontaneously flammable) when in contact with the atmosphere, which is very dangerous to people and property. Production costs increase when chemical reagents react undesirably with the atmosphere rather than proceeding towards the desired production product. Therefore, for safety and chemical reasons, it is important to separate such reactive chemicals from the atmosphere when handling chemical substances that react in this way.

[0003] There are several prior - art systems for providing protection against reactive chemicals from the atmosphere. The current state of the art regarding the packaging and handling of air - sensitive chemicals includes: (1) caps for bottles with partitions incorporated into the system, such as those sold under the Sure / Seal (trademark) brand; (2) the use of partitions to cover the openings of containers; (3) the use of combinations of wax and partitions to cover the openings of containers; (4) sealing the area between the cap and the bottle with wax and / or tape.

[0004] These conventional techniques for removing air-sensitive chemicals from their packaging vary depending on the type of protection from the atmosphere provided by the chemical packaging. Many of these systems feature a barrier placed over the opening of the container in which the reactive chemical is stored. This barrier is made of a material that is penetrated to extract the chemical and then resealed after the extraction of the chemical is complete.

[0005] Current systems used to protect chemical substances have various problems. One of the main problems with current systems is that they are easily compromised and therefore exposed to the external environment. When reagents react with the air, the result is at least a decrease in purity, which in turn leads to a decrease in reaction yield, and consequently, an increase in production costs, for example. When chemical reagents are exposed to the air to the maximum extent, it causes several safety problems for both people and property. [Overview of the project] [Problems that the invention aims to solve]

[0006] This disclosure relates to methods and techniques for addressing problems in the current state of the art or other. According to one aspect of this disclosure, an adapter is provided which is configured to supply an inert atmosphere to a space adjacent to a relevant container. [Means for solving the problem]

[0007] In one embodiment, an adapter is provided for supplying an inert atmosphere when transferring a reactive chemical species from its storage container in order to protect the reactive chemical species. The storage container has a sealed opening and is filled with the reactive chemical species. When in use, the adapter is fitted onto the container in a sealed manner from above. After being fitted onto the container, a space is formed between the upper portion of the container defining the container opening and the inner wall of the adapter. The adapter is equipped with a gas inlet fitting that can be connected to an inert gas source via a conduit such as a tube or hose. The space formed between the adapter and the container is filled with an inert gas to supply an inert atmosphere from above, near, adjacent to, etc., the opening of the container. The presence of an inert atmosphere provides a protective environment for removing the reactive chemical species from the container.

[0008] In one embodiment, an adapter is provided for supplying an inert atmosphere to a space adjacent to a relevant container, wherein the longitudinal axis of the container is oriented at an angle between about 0 and about 45 degrees with respect to the vertical. The container has an opening and contains a reactive chemical substance. The adapter comprises a body having a first part and a second part, the first part having an opening positioned at one end of the body and configured to receive a section of the container in a manner that can be sealed through the opening; a cavity disposed within the body and in fluid communication with the opening of the first part, the cavity surrounding the opening of the container when the container is received by the first part; and a gas inlet fitting disposed in fluid communication with the cavity, the gas being introduced into the cavity through the gas inlet fitting to fix an inert atmosphere in the cavity adjacent to the opening of the container.

[0009] In any embodiment, the first and second parts are made from materials that are inert or resistant to reactive chemicals.

[0010] In any embodiment, the first part comprises a material selected from the group consisting of natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

[0011] In any embodiment, the second part includes materials selected from natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

[0012] In any embodiment, the material of the first part and the material of the second part are the same or substantially identical.

[0013] In any embodiment, the material of the first part and the material of the second part are different.

[0014] In any embodiment, the second portion has an opening at its end.

[0015] In any embodiment, the main body of the adapter, the first part of the main body, or the second part of the main body is cylindrical in shape.

[0016] In any embodiment, the first and second parts include concentric cylinders.

[0017] In any embodiment, the first portion has a smaller diameter than the second portion, and the second portion forms at least one section of a cavity for holding an inert gas.

[0018] In any embodiment, the first portion of the main body includes at least one tapered section.

[0019] In any embodiment, the second portion of the main body is cylindrical, and the first portion of the main body includes first and second tapered sections. The first tapered section tapers inward from the second portion to an intermediate section, and the second tapered section tapers outward from the intermediate section to an end that forms an opening in the first portion.

[0020] In any embodiment, the gas inlet fitting is selected from the group of fittings consisting of smooth fittings, barbed fittings, ribbed fittings, threaded fittings, push fittings, pull fittings, straight fittings, tapered fittings, or combinations thereof.

[0021] In any embodiment, the gas inlet fitting is attached to a hollow ring, which is sized and configured to be received within a cavity in the main body, and the hollow ring includes one or more gas outlets that communicate with the gas inlet fitting with respect to gas.

[0022] In any embodiment, the second portion of the main body includes an opening at the end of the main body opposite to the opening of the first portion.

[0023] In any embodiment, the opening of the first portion or the opening of the second portion has a diameter of from about 0.5 inches to about 4 inches.

[0024] In any embodiment, the first portion of the body portion includes an outer wall, and the outer wall has a thickness of from about 0.5 mm to about 10 mm.

[0025] In any embodiment, the thickness of the outer wall is from about 1 mm to about 15 mm.

[0026] In any embodiment, the inert gas is heavier than air.

[0027] In any embodiment, the inert gas is selected from the group consisting of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof.

[0028] According to another aspect of the present disclosure, a device for transporting a solid reactive chemical is provided. In one embodiment, the device may comprise a ring, a container attached to the ring, the container having a first opening, and a cover configured to seal the first opening of the container. The device is sized and configured to be insertable within the cavity of any embodiment of the adapter described herein.

[0029] In any embodiment, the ring is selected from a metal ring, a plastic ring, a rubber ring, an elastomeric ring, a ceramic ring, or combinations thereof.

[0030] In any embodiment, the container is selected from a beaker, a cup, a beaker with volume markings, a cup with volume markings, a boat, a closed-end tube, and combinations thereof.

[0031] <00001'05>In any embodiment, the container further comprises a second opening at its bottom, the second opening being selectively closed.

[0032] In any embodiment, the container cover is a stopper, lid, cap, snap-on lid, snap-on cap, and film.

[0033] In any embodiment, the container holds air-reactive chemical species.

[0034] According to another aspect of this disclosure, any of the adapters disclosed herein may be used to fix an inert atmosphere surrounding the opening of the relevant container.

[0035] Another aspect of the present disclosure provides a method for transporting a reactive chemical. In one embodiment, the method includes obtaining a container having a sealed opening, the container containing the reactive chemical; supplying an inert atmosphere surrounding the sealed opening of the container; exposing the reactive chemical to the inert atmosphere; and removing at least a portion of the reactive chemical from the container.

[0036] In any embodiment, the method may also include bonding an adapter to the opening of a container in a sealing manner, wherein the adapter defines an internal cavity.

[0037] In any embodiment, an inert environment surrounding the sealed opening of the container is provided by filling the internal cavity with an inert gas.

[0038] In any embodiment, the inert gas is selected from the group consisting of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof.

[0039] In any embodiment, the air-reactive chemical species is selected from the group consisting of arsine, phosphine, diborane, germane, silane, dicobaltoctacarbonyl, nickelcarbonyl, hydrazine, diphosphane, aluminum, allium, indium, zinc, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, trimethylborane, triethylborane, butyllithium, tert-butyllithium, diethylzinc, triethylaluminum, linseed oil, phosphorus, zirconium, uranium, titanium, tungsten, bismuth, hafnium, thorium, osmium, neodymium, cerium, plutonium, diethylethoxyaluminum, dichloro(methyl)silane, lithium graphite, sodium graphite, potassium graphite, sodium hydride, lithium aluminum hydride, uranium trihydride, diethylaluminum hydride, Grignard compounds, Raney nickel, palladium carbon, iron sulfide, neptunium, and combinations thereof.

[0040] This “Summary of the Invention” introduces a selection of simplified forms of concepts, which will be further described in the following “Modes for Carrying Out the Invention.” This “Summary of the Invention” is not intended to highlight key features of the claimed subject matter, nor is it intended to be used as an aid in defining the scope of the claimed subject matter.

[0041] Many of the aforementioned aspects of the claimed subject matter and their associated advantages will be readily apparent, and even more readily apparent, when taken in conjunction with the attached drawings, by referring to the following detailed description. [Brief explanation of the drawing]

[0042] [Figure 1] This diagram illustrates an example of an adapter designed for the transfer of reactive chemicals. In this example, the adapter is attached to a bottle / container and connected to a gas hose through its inlet. [Figure 2]This is a diagram illustrating the adapter shown in Figure 1. [Figure 3] This figure shows an example of an adapter according to another embodiment of the present disclosure, with two inlets attached. [Figure 4] This figure illustrates a gas distribution device suitable for use with one or more embodiments of the adapters of the present disclosure. [Figure 4B] Figure 4A illustrates an example of an adapter having a gas distribution device. [Figure 5] This figure illustrates an example of a curved adapter that fits into a container of a reactive reagent having an uneven surface, according to another embodiment of the present disclosure. [Figure 6] This figure illustrates an example of a solid material transfer system suitable for use with any of the adapters of this disclosure. [Figure 7] Figure 6 illustrates a solid material transfer system that is attached to a flask for transferring solid materials. [Figure 8] Figure 1 illustrates a container, such as a bottle, for containing divalent samarium, a highly reactive chemical substance in liquid form, with the adapter shown attached. [Figure 9] This diagram illustrates a container holding a samarium diiodide solution. [Figure 10] This figure illustrates one embodiment of an adapter that is attached to the top of a reagent bottle and supplies nitrogen gas, so that the reagent contained in the bottle can be drawn with a syringe without being exposed to the atmosphere. [Figure 11] This figure illustrates how the reagent from Figure 10 is transferred to another flask via a syringe. [Figure 12] This figure illustrates that additional reagents can be easily transferred without requiring additional membrane perforation. [Modes for carrying out the invention]

[0043] Similar numbers refer to similar elements. The detailed descriptions provided below in relation to the accompanying drawings are intended as a description of one of the various embodiments of this disclosure and are not intended to represent embodiments alone. Each embodiment described in this disclosure is provided merely as an example or illustration and should not be construed as being preferable or advantageous to other embodiments. The exemplary examples presented herein are not intended to be exhaustive or to limit this disclosure to the exact form disclosed. Similarly, any step described herein may be interchangeable with other steps or combinations of steps to achieve the same or substantially similar results. Furthermore, some method steps may be performed sequentially, in parallel, or in any order unless otherwise specifically expressed or understood in the context of other method steps.

[0044] Many problems exist in the current state of technology concerning air-sensitive or toxic chemicals and their separation from the atmosphere. This disclosure presents methods and techniques for supplying an inert atmosphere for the transfer of reactive and air-sensitive chemicals. These methods and techniques can be implemented in inexpensive and user-friendly devices that enhance safety and enable the easy transfer of reactive reagents.

[0045] Figures 1 and 2 illustrate an adapter 20 designed to provide a protective environment for the reactive chemical when it is removed from the associated container 30. The container 30, for example, a bottle, is filled with the reactive chemical 31 and has an opening 32 that is closed with, for example, a cap 33. When the cap 33 is removed, the chemical 31 is exposed to the surrounding environment.

[0046] When in use, the adapter 20 is fitted over the container 30, forming a seal between the adapter 20 and the container 30. The lower part of the adapter 23 fits snugly over the container 30, and the upper part of the adapter 24 extends above the opening 32 of the container. The top of the adapter 34 allows for easy access to the opening 32 of the container.

[0047] After being coupled to the container 30, the adapter 20 surrounds the opening 32 of the container 30, thereby creating a space between the inner wall of the adapter 20 and the upper portion of the container 30. The adapter extends above the opening 32 of the container and is filled with inert gas 21, which forms a blanket over the opening 32 of the container.

[0048] Therefore, by using the adapter 20, the reactive reagents in the container are exposed to the inert gas 21 rather than the atmosphere.

[0049] In one embodiment, the top of the adapter 20 is provided with an opening 34 that allows access to the opening 32 of the container 30 when the adapter 20 is coupled to the container 30. In one embodiment, the adapter opening 34 has a diameter of about 0.5 inches to about 4 inches. In another embodiment, the top of the adapter 20 may be closed to the atmosphere. In some of these embodiments, the adapter 20 may be provided with an exhaust valve for releasing pressurized gas from the space between the inner wall of the adapter 20 and the upper portion of the container 30.

[0050] The adapter 20 is made from a material that is resistant to or inert to the reactive chemical 31. As shown in Figures 1 and 2, the adapter 20 includes a gas inlet fitting 28, a lower portion 23, and an upper portion 24. In one embodiment, the lower portion 23 is narrower than the upper portion 24. The lower portion 23 fits snugly into the container 30. The upper portion 24 extends above the container opening 32.

[0051] Referring again to Figures 1 and 2, the gas inlet fitting 28 is configured to be attached to a tube 40 connected to an inert gas source 21. The gas inlet fitting 28 is configured to introduce the inert gas 21 supplied through the tube 40 into a space formed between the inner walls of adapters 23, 24 that extend over the container opening 32. In such a case, a blanket of inert gas 21 covers the container opening 32, preventing the atmosphere from coming into contact with the reactive chemical 31. In some embodiments, the inert gas is heavier than air.

[0052] After the space is filled with inert gas, the cap 32 of the container 30 can be removed. The inert gas 21 disposed inside the adapter 20 provides a protective blanket over the container 30. With the container 30 open under the inert gas 21, the reactive chemical 31 can be safely removed by a syringe, tube, needle, needle and syringe, or other transport means that continues to protect the reactive chemical 31.

[0053] In the embodiment shown in Figure 2, the adapter 20 is integrally formed with the first and second concentric cylinders 23, 24. In some embodiments, the first or lower cylinder 23 has a smaller diameter than the second or upper cylinder 24. Of course, in other embodiments, the concentric cylinders may have the same or substantially similar diameters. In yet another embodiment, the adapter is formed by a single tube having a constant inner and / or outer diameter. As shown in Figure 2, the gas inlet fitting 28 is attached to the second or upper cylinder 24 of the adapter 20.

[0054] The first or lower cylinder 23, i.e., the lowest portion of the adapter 20, is configured to fit onto the container and form a seal with the container (see Figure 1). In some embodiments, the first or lower cylinder 23 may fit onto the container to a depth of about 0.5 inches to about 4 inches. In another embodiment, the depth is about 0.5 inches to about 6 inches. In one embodiment, the wall thickness of the first or lower cylinder 23 is about 0.5 mm to about 10 mm. In another embodiment, the wall thickness is about 1 mm to about 15 mm.

[0055] The first or lower cylinder 23, or its lower portion, may be made from a material selected from the group consisting of natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

[0056] Similarly, the second or upper cylinder 23 of the adapter 20 may be made from a material selected from the group consisting of natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

[0057] In one embodiment, the first cylinder 23 and the second cylinder 24 are made from the same material. Alternatively, in one embodiment, the first cylinder 23 and the second cylinder 24 of the adapter 20 are made from different materials.

[0058] In one embodiment, the inert gas 21 includes, but is not limited to, nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof.

[0059] In one embodiment, the reactive chemical substance 31 contained in the container 30 is not limited to arsine, phosphine, diborane, germane, silane, dicobalt octacarbonyl, nickel carbonyl, hydrazine, diphosphane, aluminum, gallium, indium, zinc, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, trimethylborane, triethylborane, butyllithium, tert-butyllithium, diethylzinc, tri This includes ethylaluminum, linseed oil, phosphorus, zirconium, uranium, titanium, tungsten, bismuth, hafnium, thorium, osmium, neodymium, cerium, plutonium, diethylethoxyaluminum, dichloro(methyl)silane, lithium graphite, sodium graphite, potassium graphite, sodium hydride, lithium aluminum hydride, uranium trihydride, diethylaluminum hydride, Grignard compounds, Raney nickel, palladium carbon, iron sulfide, neptunium, and combinations thereof.

[0060] Figure 3 illustrates another embodiment of the adapter 20 according to this application. The adapter 20 is substantially similar in structure and operation to the adapter of Figure 2, with the differences which will be described below. In that respect, the adapter 20 shown in Figure 3 includes first and second gas inlet fittings 27, 28 which are mounted on the second or upper cylinder 24 and configured to introduce an inert gas into the adapter 20. The gas inlet fittings 27, 28 may be used to introduce the same or different inert gases into the adapter 20. In the illustrated embodiment, the gas inlet fittings 27, 28 are arranged opposite each other, but other arrangements may be employed.

[0061] Figure 4 illustrates a gas distribution device 25 that may be implemented with one or more embodiments of the adapter 20 described herein. As shown in Figure 4A, the gas distribution device 25 comprises a gas inlet fitting 28 that supplies inert gas to a plurality of inert gas outlets 26. In the illustrated embodiment, the gas distribution device 25 comprises a ring 25 having equally spaced gas outlets 26. As shown in Figure 4B, the gas outlets 26 introduce the inert gas supplied to the gas inlet fitting 28 into the interior of the second or upper cylinder 24 of the adapter 20.

[0062] Figure 5 illustrates another embodiment of the adapter according to this application. The adapter of Figure 5 is substantially similar in structure and operation to the adapter of Figure 2, except for the differences which will be described below. In that respect, the adapter of Figure 5 includes a lower section 50 that is somewhat hourglass-shaped instead of the lower cylindrical section 23. In other words, the lower section 50 includes an upper section 51 and a lower section 53, each tapering inward to a narrow intermediate section 52. Of course, sections 51, 52, and 53 can have any dimensions suitable for the particular container into which the adapter is fitted. Although not shown for the sake of illustration, the adapter of Figure 5 may include any of the gas inlet fitting arrangements shown in Figures 2, 3, and 4B.

[0063] Figure 6 illustrates a typical system for transferring solid reactive chemicals according to one embodiment of the present disclosure. As shown in Figure 6, the solid reactive chemical transfer system can be used in conjunction with any of the adapters shown in Figures 2 to 5. In the illustrated embodiment, the solid reactive chemical transfer system includes a ring 60 that is sized and configured to fit inside the upper cylinder 24 of the adapter 20. In some embodiments, the ring 60 may include, but is not limited to, a metal ring, a plastic ring, a rubber ring, an elastomer ring, a ceramic ring, and the like.

[0064] As shown in Figure 6, the solid reactive chemical transfer system also includes a container 62 attached to the ring 60. The container 62 is configured to hold the solid reactive chemical. The container 62 is made of one or more materials that are nonreactive to the solid reactive chemical being transferred thereto. The container 62 has an opening at its upper end. A cap or stopper 61 is provided to seal the opening of the container 62. The bottom of the container 62 optionally includes a bottom 63 that can move, for example, by a hinge. In some embodiments, the container 62 may include, but is not limited to, a beaker, a cup, a beaker with volume markings, a cup with volume markings, a boat, a closed-end tube, and the like.

[0065] During use, tube 40 supplies an inert gas to the gas inlet fitting 28 and thus into the adapter 20. The inert gas 21, as such, fills the cavity / headspace resulting from the adapter 20 being fitted onto the container 30. In one embodiment, this cavity can then accommodate a solid reactive chemical transfer system by inserting a ring 60 into a bottomless cylinder 24 and sliding the ring 60 downward over the neck of the container 30. Alternatively, the solid reactive chemical transfer system may be inserted into a second or upper cylinder 24 before fitting the adapter 20 onto the container 30 from above.

[0066] In any embodiment, the cap or stopper 61 can then be removed from the container 62. The container 30 is also opened in the presence of an inert atmosphere provided by an inert gas 21 that protects the solid reactive material 36 contained within the container 30. The solid material 31 can then be transferred from the container 30 to the container 62. The container 62 is then capped with the cap / stopper 61, and the solid reactive chemical transfer system can be removed from the adapter 20.

[0067] Figure 7 illustrates an example of transferring a solid reactive chemical contained in a container 62 of the solid reactive chemical transfer system shown in Figure 6. The container 62 with a cap / stopper 61 is attached to a conventional flask 70 into which the solid reactive substance 36 is introduced. The optional hinged bottom 63 of the container 62 is then opened, and the reactive solid can fall from the container 62 into the flask 70 by gravity.

[0068] (Examples) (Example 1) As shown in Figure 8, one embodiment of adapter 20 was tested using a bottle of 1.6 M n-butyllithium. n-butyllithium is a highly reactive chemical species that is spontaneously combustible. The adapter was fitted over the bottle, and the inert gas inlet was connected to a nitrogen gas source. The headspace formed by the cavity of the adapter on top of the bottle was filled with nitrogen, and the cap of the container was removed. A 1 mL syringe flushed with nitrogen was filled with n-butyllithium solution (nBuLi) by inserting a pre-dried 1-inch 18G needle into the opening of the bottle containing the n-butyllithium. The plunger on top of the syringe was slowly raised to fill the syringe with 1 mL of nBuLi. The n-butyllithium concentration was monitored using titration. Titration was performed using standard chemical methods by first drying 15 mL vials equipped with a 1 cm stirring rod and a red rubber septum ("subaseal") using standard Schlenk technique, and then placing them under a dry nitrogen (N2) atmosphere. Approximately 1 mmol of diphenylacetic acid (DPA) was added to each vial, followed by 8 mL of dried THF. These methods are described below.

[0069] A dry vial was assembled with a red septum, stirring rod, DPA solution, and nitrogen tubing. A 1 mL syringe assembly containing nBuLi was then removed from the bottle opening and quickly inserted through the red rubber septum into the headspace above the DPA solution contained in one of the 15 mL vials. nBuLi was added dropwise to the DPA solution, while stirring (approximately 500 rpm) until a pale yellow color persisted. The amount required to produce a persistent yellow color was recorded, and this procedure was repeated two more times (total of three times).

[0070] The results of these tests are shown in Table 1.

[0071] [Table 1]

[0072] n-butyllithium was initially titrated to a concentration of 1.409 M. As shown in Table 1, the concentration of n-butyllithium remained virtually unchanged after 24 hours using the adapter of this disclosure. After using the adapter for one week, the n-butyllithium concentration was tested again. As shown in Table 1, the n-butyllithium concentration measured after one week of using the adapter was 1.430 M. Again, this change was negligibly small from when the container was first opened. The data in Table 1 demonstrate that the adapter by the method and technique of this disclosure provides protection against flammable n-butyllithium, and that the concentration of n-butyllithium does not change with the use of such an adapter.

[0073] (Example 2) Samarium diiodide was tested using adapter 20 according to the methods and techniques of this disclosure. Samarium diiodide is an extremely air-sensitive reagent. When handled properly, samarium diiodide forms a bright blue solution. When exposed to oxygen, it reacts with atmospheric oxygen to form Sm 2+ Sm 3+Because it is oxidized, a solution of samarium diiodide rapidly turns yellow. Exposure of samarium diiodide to any amount of air significantly reduces the yield of the desired product.

[0074] Samarium diiodide is often sold in glass bottles. Since the bottles are generally not sealed, a partition is sold with the bottle, as shown in Figure 9. This configuration allows oxygen to enter the bottle once opened, oxidizing the divalent samarium to trivalent samarium, leading to low reaction yields and a short reagent shelf life.

[0075] Figure 10 illustrates a test setup for using samarium diiodide with an adapter. Adapter 20 is fitted over the bottle containing the samarium diiodide. The adapter's cavity is filled with nitrogen gas, and the bottle of samarium diiodide is opened. A syringe fitted with a needle is then used to fill the syringe with the samarium diiodide solution. A blue color, due to divalent samarium ions, was observed inside the syringe. Thus, adapter 20 maintained a protective atmosphere for removing samarium diiodide. When adapter 20 is used, divalent samarium can be easily transferred to a flask, as shown in Figure 11. Thus, a working volume of the reagent can be easily, quickly, and safely transferred, as shown in Figure 12. Exemplary Embodiments

[0076] A collection of exemplary embodiments, including at least some explicitly listed as “EC” (exemplary combinations), is presented below to provide an additional description of various types of embodiments in accordance with the concepts described herein. These examples are not intended to be mutually exclusive, exhaustive, or restrictive, and the claimed subject matter is not limited to these exemplary embodiments, but rather encompasses all possible modifications and variations within the scope of the published claims and their equivalents.

[0077] EC A. Adapter for supplying an inert atmosphere to a space adjacent to a relevant container. The longitudinal axis of the container is oriented at an angle between, for example, about 0 to about 45 degrees with respect to the vertical. The container has an opening and contains a reactive chemical substance. The adapter comprises a main body having a first part and a second part, the first part having an opening positioned at one end of the main body and configured to receive a section of the container in a manner that can be sealed through the opening; a cavity disposed within the main body and in fluid communication with the opening of the first part, the cavity surrounding the opening of the container when the container is received by the first part; and a gas inlet fitting disposed in fluid communication with the cavity, the gas being introduced into the cavity through the gas inlet fitting to establish an inert atmosphere in the cavity adjacent to the opening of the container.

[0078] EC B. The first and second parts of the adapter described in any one of the preceding or succeeding exemplary combinations, made from materials that are inert or resistant to reactive chemicals.

[0079] EC C. The first part of the adapter is one of the preceding or succeeding exemplary combinations described in any one of the preceding or succeeding clauses, comprising a material selected from the group consisting of natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

[0080] EC D. The second part is an adapter described in any one of the preceding or succeeding exemplary combinations, comprising materials selected from natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

[0081] EC E. The material of the first part and the material of the second part are the same or substantially identical to the preceding or succeeding exemplary combinations of the adapter described in any one of the clauses.

[0082] EC F. The material of the first part and the material of the second part are different preceding or succeeding exemplary combinations of the adapter as described in one of the clauses.

[0083] EC G. The second part is an adapter according to any one of the preceding or succeeding exemplary combinations, having an opening at its end.

[0084] EC H. The adapter according to any one of the preceding or succeeding exemplary combinations, wherein at least one of the main body, the first part, or the second part is cylindrical in shape.

[0085] EC I. The first and second parts are concentric cylinders, and the adapter is one of the preceding or succeeding exemplary combinations described in either of the clauses.

[0086] EC J. The adapter according to any one of the preceding or succeeding exemplary combinations, wherein the first part has a smaller diameter than the second part, and the second part forms at least one section of a cavity for holding an inert gas.

[0087] EC K. The first part is the adapter described in any one of the preceding or succeeding exemplary combinations, which includes at least one section.

[0088] EC L. The adapter according to any one of the preceding or succeeding exemplary combinations, wherein the second portion is cylindrical, and the first portion comprises first and second tapered sections, the first tapered section tapering inward from the second portion to an intermediate section, and the second tapered section tapering outward from the intermediate section to an end forming an opening in the first portion.

[0089] EC M. The gas inlet fitting is an adapter described in any one of the preceding or succeeding exemplary combinations selected from the group of fittings consisting of smooth fittings, barbed fittings, ribbed fittings, threaded fittings, push fittings, pull fittings, straight fittings, tapered fittings, or combinations thereof.

[0090] EC N. The adapter is configured such that a gas inlet fitting is attached to a hollow ring, the hollow ring is sized to be received within a cavity in the main body, and the hollow ring includes one or more gas outlets communicating with the gas inlet fitting with respect to gas, in any one of the preceding or succeeding exemplary combinations described in any of the preceding or succeeding clauses.

[0091] EC O. The adapter described in any one of the preceding or succeeding exemplary combinations, the second part including an opening at the end of the main body opposite to the opening of the first part.

[0092] EC P. The opening of the first part or the opening of the second part of the adapter having a diameter of about 0.5 inches to about 4 inches, in any of the preceding or succeeding exemplary combinations described in one of the paragraphs.

[0093] EC Q. The first part of the main body includes an outer wall, the outer wall having a thickness of approximately 0.5 mm to approximately 10 mm, the adapter as described in any one of the preceding or succeeding exemplary combinations.

[0094] EC R. The thickness of the exterior wall is approximately 1 mm to approximately 15 mm, as described in one of the preceding or succeeding exemplary combinations of the adapter.

[0095] EC S. The adapter is one of the preceding or succeeding exemplary combinations of an inert gas that is heavier than air, as described in one of the clauses.

[0096] EC T. The inert gas is selected from the group consisting of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof, as described in any one of the preceding or succeeding exemplary combinations of the adapter described in item 1.

[0097] EC U. A device for transferring solid reactive chemicals, comprising a ring, a container attached to the ring having a first opening, and a cover configured to seal the first opening of the container, wherein the device is sized and configured to be insertable into a cavity of any of the adapters described herein.

[0098] EC V. The ring is a metal ring, plastic ring, rubber ring, elastomer ring, ceramic ring, or any of the preceding or succeeding exemplary combinations described in any one of the clauses.

[0099] EC W. The container is a device described in any one of the preceding or succeeding exemplary combinations selected from beakers, cups, beakers with volume markings, cups with volume markings, boats, closed-end tubes, and combinations thereof.

[0100] EC X. The device according to any one of the preceding or succeeding exemplary combinations, wherein the vessel further comprises a second opening at its bottom, the second opening being selectively closed.

[0101] EC Y. The container cover is a stopper, lid, cap, snap-on lid, snap-on cap, and film, in any one of the preceding or succeeding exemplary combinations of the device as described in one of the clauses.

[0102] EC Z. The container is an adapter described in any one of the preceding or succeeding exemplary combinations for housing air-reactive chemical species.

[0103] EC AA. Air-reactive chemical species include arsine, phosphine, diborane, germane, silane, dicobalt octacarbonyl, nickel carbonyl, hydrazine, diphosphane, aluminum, allium, indium, zinc, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, trimethylborane, triethylborane, butyllithium, tert-butyllithium, diethylzinc, triethylaluminum, linseed oil, phosphorus, zirconium, uranium, titanium, and tungsten. The adapter described in any one of the preceding or succeeding exemplary combinations selected from the group consisting of bismuth, hafnium, thorium, osmium, neodymium, cerium, plutonium, diethylethoxyaluminum, dichloro(methyl)silane, lithium graphite, sodium graphite, potassium graphite, sodium hydride, lithium aluminum hydride, uranium trihydride, diethylaluminum hydride, Grignard compounds, Raney nickel, palladium carbon, iron sulfide, neptunium, and combinations thereof.

[0104] EC BB. A method using an adapter described in any one of the preceding or succeeding exemplary combinations to fix an inert atmosphere surrounding the opening of a relevant container. A method for transferring a reactive chemical is to acquire a container having a sealed opening, wherein the container contains the reactive chemical; to supply an inert atmosphere surrounding the sealed opening of the container; to expose the reactive chemical to the inert atmosphere; and to remove at least a portion of the reactive chemical from the container.

[0105] EC CC. The method according to any one of the preceding or succeeding exemplary combinations, comprising sealing an adapter over the opening of a container, wherein the adapter further comprises defining an internal cavity.

[0106] EC DD. The method according to any one of the preceding or succeeding exemplary combinations, comprising filling an internal cavity with an inert gas, to provide an inert atmosphere surrounding a sealed opening of a vessel.

[0107] EC EE. The inert gas is selected from the group consisting of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof, according to any one of the preceding or succeeding exemplary combinations described in the preceding or succeeding clause.

[0108] EC FF. Reactive chemicals include arsine, phosphine, diborane, germane, silane, dicobalt octacarbonyl, nickel carbonyl, hydrazine, diphosphane, aluminum, allium, indium, zinc, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, trimethylborane, triethylborane, butyllithium, tert-butyllithium, diethylzinc, triethylaluminum, linseed oil, phosphorus, zirconium, uranium, titanium, tungsten. The method according to any one of the preceding or succeeding exemplary combinations selected from the group consisting of bismuth, hafnium, thorium, osmium, neodymium, cerium, plutonium, diethylethoxyaluminum, dichloro(methyl)silane, lithium graphite, sodium graphite, potassium graphite, sodium hydride, lithium aluminum hydride, uranium trihydride, diethylaluminum hydride, Grignard compounds, Raney nickel, palladium carbon, iron sulfide, neptunium, and combinations thereof.

[0109] The foregoing description provides specific details to enable a full understanding of representative embodiments of the disclosure. However, it will be apparent to those skilled in the art that embodiments disclosed herein can be implemented without embodying all specific details. In some cases, well-known process steps are not described in detail so as not to unnecessarily complicate the various aspects of the disclosure. Furthermore, it will be understood that embodiments of the disclosure may employ any combination of the features described herein.

[0110] In the detailed description herein, references to “one embodiment,” “embodiment,” “exemplary embodiment,” etc., indicate that the embodiments described may have certain features, structures, or characteristics, but not all embodiments may necessarily include those features, structures, or characteristics. Furthermore, such phrases do not necessarily refer to the same embodiment. In addition, when a particular feature, structure, or characteristic is described in relation to one embodiment, it is considered within the knowledge of those skilled in the art that such features, structures, or characteristics will be affected in relation to other embodiments, whether explicitly described or not. After reading the description, it will be clear to those skilled in the art how to implement the disclosure in alternative embodiments. Thus, it will be understood that embodiments of the disclosure may adopt any combination of the features described herein. All such combinations or partial combinations of features fall within the scope of the disclosure.

[0111] This application may refer to quantities and numbers. Unless otherwise specified, such quantities and numbers should not be considered restrictive, but are illustrative of possible quantities or numbers relevant to this application. In this regard, this application may use the word “plural” to refer to quantities or numbers. In this regard, the word “plural” means any number greater than one, for example, 2, 3, 4, 5, etc. Words such as “about” and “approximately” mean plus or minus 5% of the stated value.

[0112] With regard to the purposes of this disclosure, terms such as “upper,” “lower,” “vertical,” “horizontal,” “front,” “rear,” “inside,” “outside,” “front part,” and “rear part” should be interpreted descriptively and not limit the scope of the claimed subject matter. Furthermore, “including,” “comprising,” or “having,” and their variations herein, mean to encompass the items described thereafter and their equivalents, as well as additional items. Unless otherwise limited, the terms “connected,” “combined,” and “attached,” and their variations herein, are used broadly and include direct and indirect connection, combination, and attachment.

[0113] Throughout this specification, technical terms may be used. Unless otherwise specifically defined herein or the context of their use suggests otherwise, these terms have their ordinary meanings in the art from which they originate.

[0114] The drawings in the figures are not to scale. Similar elements are generally indicated by similar references in the figures. For the purposes of this specification, identical or similar elements may be given the same reference number. Furthermore, the presence of reference numbers or letters in the drawings is not considered limiting, even if such numbers or letters are indicated in the claims.

[0115] The principles, representative embodiments, and modes of operation of this disclosure have already been described in the preceding description. However, the embodiments of this disclosure intended to be protected should not be construed as being limited to the specific embodiments disclosed. Furthermore, the embodiments described herein should be considered illustrative, not restrictive. It will be understood that variations and modifications may be made by others and equivalents may be adopted without departing from the spirit of this disclosure. Accordingly, all such variations, modifications, and equivalents are expressly intended to fall within the spirit and scope of this disclosure as described in the claims.

[0116] Embodiments of the present invention that claim to be exclusive or privileged are defined below. [Explanation of symbols]

[0117] 20 adapters 21 Inert gas 23 Lower part 24 Upper part 25 Gas distribution devices 26 Inert gas outlet, gas outlet 27 Gas inlet fitting 28 Gas inlet fitting 30 containers 31 Reactive Chemicals 32 openings 33 caps 34 adapters 36. Solid Reactive Substances 40 tubes 50 lower part 51 Upper section 52. Intermediate Section 53 Lower section 60 Rings 61 Caps / Stoppers 62 Container 63 Bottom 70 Flasks

Claims

1. An adapter for supplying an inert atmosphere to a space adjacent to a related container, wherein the longitudinal axis of the container is oriented at an angle between about 0 and about 45 degrees with respect to the vertical, the container has an opening and contains a reactive chemical substance, and the adapter is A main body having a first part and a second part, wherein the first part has an opening positioned at one end of the main body, and the first part is configured to receive a section of the container through the opening in a manner that can seal it, A cavity disposed within the main body and fluidly communicating with the opening of the first portion, the cavity surrounding the opening of the container when the container is received by the first portion, A gas inlet fitting is arranged to communicate fluidly with the aforementioned cavity, Equipped with, An adapter that allows an inert gas to be introduced into the cavity through the gas inlet fitting to establish an inert atmosphere in the cavity adjacent to the opening of the container.

2. The adapter according to claim 1, wherein the first and second parts are made of a material that is inert or resistant to the reactive chemical substance.

3. The adapter according to claim 1, wherein the first portion comprises a material selected from the group consisting of natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

4. The adapter according to claim 1, wherein the second portion comprises a material selected from natural rubber, butyl rubber, polyvinyl chloride, polybrominated vinyl, polyethylene, polypropylene, polyvinyl acetate, polyvinyl butyral, silicone, nitrile rubber, fluorosilicone, Teflon, polyvinyl ether, fluorinated polyvinyl ether, neoprene, styrene-butadiene rubber, EPDM (ethylene propylene diene monomer) rubber, polyacrylate, Hypalon, Viton, polyurethane, Calrex, Aflas, glass fiber, glass, steel, copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, iron, ruthenium, osmium, chromium, molybdenum, tungsten, manganese, rhenium, and combinations thereof.

5. The adapter according to claim 2, wherein the material of the first portion and the material of the second portion are the same or substantially identical.

6. The adapter according to claim 1, wherein the material of the first part and the material of the second part are different.

7. The adapter according to claim 1, wherein the second portion has an opening at its end.

8. The adapter according to claim 1, wherein at least one of the main body, the first portion, or the second portion is cylindrical in shape.

9. The adapter according to claim 8, wherein the first and second parts are concentric cylinders.

10. The adapter according to claim 9, wherein the first portion has a smaller diameter than the second portion, and the second portion forms at least one section of the cavity for holding the inert gas.

11. The adapter according to claim 1, wherein the first part includes at least one tapered section.

12. The adapter according to claim 11, wherein the second portion is cylindrical, and the first portion includes first and second tapered sections, the first tapered section tapering inward from the second portion to an intermediate section, and the second tapered section tapering outward from the intermediate section to the end forming the opening of the first portion.

13. The adapter according to claim 1, wherein the gas inlet fitting is selected from the group consisting of smooth fittings, barbed fittings, ribbed fittings, threaded fittings, push fittings, pull fittings, straight fittings, tapered fittings, or combinations thereof.

14. The adapter according to claim 1, wherein the gas inlet fitting is attached to a hollow ring, the hollow ring is sized and configured to be received within the cavity of the main body, and the hollow ring includes one or more gas outlets that communicate with the gas inlet fitting with respect to gas.

15. The adapter according to claim 1, wherein the second portion has an opening at the end of the main body portion opposite to the opening of the first portion.

16. The adapter according to claim 1, wherein the inert gas is heavier than air.

17. The adapter according to claim 1, wherein the inert gas is selected from the group consisting of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof.

18. A device for transferring solid reactive chemicals, A ring, A container attached to the ring, wherein the container has a first opening, A cover configured to seal the first opening of the container Equipped with, The device is configured to be sized so as to be insertable into the cavity of the adapter described in claim 1.

19. The device according to claim 18, wherein the ring is selected from a metal ring, a plastic ring, a rubber ring, an elastomer ring, a ceramic ring, or a combination thereof.

20. The device according to claim 18, wherein the container is selected from beakers, cups, beakers with volume markings, cups with volume markings, boats, closed-end tubes, and combinations thereof.

21. The device according to claim 18, wherein the container further comprises a second opening at its bottom, the second opening being selectively closed.

22. The device according to claim 18, wherein the cover of the container is a stopper, a lid, a cap, a snap-on lid, a snap-on cap, and a film.

23. The container is an adapter that provides an inert atmosphere according to claim 1, containing air-reactive chemical species.

24. The adapter according to claim 23, wherein the air-reactive chemical species is selected from the group consisting of arsine, phosphine, diborane, germane, silane, dicobalt octacarbonyl, nickel carbonyl, hydrazine, diphosphane, aluminum, gallium, indium, zinc, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, trimethylborane, triethylborane, butyllithium, tert-butyllithium, diethylzinc, triethylaluminum, linseed oil, phosphorus, zirconium, uranium, titanium, tungsten, bismuth, hafnium, thorium, osmium, neodymium, cerium, plutonium, diethylethoxyaluminum, dichloro(methyl)silane, lithium graphite, sodium graphite, potassium graphite, sodium hydride, lithium aluminum hydride, uranium trihydride, diethylaluminum hydride, Grignard compounds, Raney nickel, palladium carbon, iron sulfide, neptunium, and combinations thereof.

25. A method for transporting reactive chemical substances, A step of obtaining a container having a sealed opening, wherein the container contains a reactive chemical substance, The steps include providing an inert atmosphere surrounding the sealed opening of the container, The steps include: exposing the reactive chemical substance to the inert atmosphere, The steps of removing at least a portion of the reactive chemical substance from the container and Methods that include...

26. The method according to claim 25, further comprising the step of sealing an adapter over the opening of the container, wherein the adapter defines an internal cavity.

27. The step of providing an inert atmosphere surrounding the sealed opening of the container is: The method according to claim 26, further comprising the step of filling the internal cavity with an inert gas.

28. The method according to claim 27, wherein the inert gas is selected from the group consisting of nitrogen, helium, neon, argon, krypton, xenon, carbon dioxide, carbon disulfide, sulfur hexafluoride, methane, ethane, propane, butane, isobutane, neopentane, and combinations thereof.

29. The method according to any one of claims 25, wherein the reactive chemical substance is selected from the group consisting of arsine, phosphine, diborane, germane, silane, dicobaltoctacarbonyl, nickelcarbonyl, hydrazine, diphosphane, aluminum, allium, indium, zinc, lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium, strontium, barium, trimethylborane, triethylborane, butyllithium, tert-butyllithium, diethylzinc, triethylaluminum, linseed oil, phosphorus, zirconium, uranium, titanium, tungsten, bismuth, hafnium, thorium, osmium, neodymium, cerium, plutonium, diethylethoxyaluminum, dichloro(methyl)silane, lithium graphite, sodium graphite, potassium graphite, sodium hydride, lithium aluminum hydride, uranium trihydride, diethylaluminum hydride, Grignard compounds, Raney nickel, palladium carbon, iron sulfide, neptunium, and combinations thereof.

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