Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/24—Vacuum evaporation
  • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/14—Metallic material, boron or silicon
  • C23C14/20—Metallic material, boron or silicon on organic substrates
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
  • A61J1/00—Containers specially adapted for medical or pharmaceutical purposes
  • A61J1/05—Containers specially adapted for medical or pharmaceutical purposes for collecting, storing or administering blood, plasma or medical fluids ; Infusion or perfusion containers
  • A61J1/06—Ampoules or carpules
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
  • A61J1/00—Containers specially adapted for medical or pharmaceutical purposes
  • A61J1/05—Containers specially adapted for medical or pharmaceutical purposes for collecting, storing or administering blood, plasma or medical fluids ; Infusion or perfusion containers
  • A61J1/06—Ampoules or carpules
  • A61J1/067—Flexible ampoules, the contents of which are expelled by squeezing
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/14—Metallic material, boron or silicon
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/14—Metallic material, boron or silicon
  • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/24—Vacuum evaporation
  • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
  • C23C14/325—Electric arc evaporation

Definitions

• the present invention relates to the sealing of containers, to the coating of containers made of plastics material which can be used for cosmetic and / or pharmaceutical formulations, and in particular to coating ampoules to achieve a sealing effect.
• the invention relates also to the sealed or coated containers, in particular sealed or coated ampoules.
• compositions are presented in a variety of different packaging, including packaging made of glass, metal, plastic and natural materials.
• packaging made of glass, metal, plastic and natural materials.
• liquid formulations e.g. solutions or suspensions
• the packaging must be and remain sealed to prevent leakage.
• a number of technical and practical difficulties exist with all such containers.
• Some formulations may contain highly volatile substances or other relatively small molecules that can diffuse out through the material of the container. This is a particular problem with, say, perfumes. Shelf-life is thus limited as products may lose potency, aroma or flavour. As a result, containers for such products are made of material that is impermeable e.g. glass, such materials being generally rather expensive. It is hence not possible to use cheaper materials such as plastics so high packaging costs are incurred.
• compositions in containers may have to be sterilized under conditions of high temperature or pressure, or once filled under sterile conditions must be robust enough to maintain that sterility. Again, this tends towards higher production costs.
• a method of making ampoules is by Blow-Fill-Seal (BFS), under aseptic conditions, in which the ampoule is formed by extrusion and filled with solution in a multi-part but essentially one-step process. If necessary, and provided the contents are not heat labile, heat sterilization can be used, e.g. ampoules can be sterilised by terminal sterilisation methods, i.e. after the ampoule has been filled and sealed. These methods are well established and accepted by regulatory authorities worldwide.
• BFS Blow-Fill-Seal
• a known problem with existing ampoules is that they allow oxygen, other gases and other volatile compounds into the ampoule and allow water (moisture) to exit. Testing of the contents has revealed that, during storage, contaminants can pass through the plastic of ampoule walls and be absorbed into the formulation. As one specific example, unacceptable amounts of vanillin have been found inside ampoules, leading to failure of the product and refusal of regulatory authorities to licence the ampoules without safeguards against this external contamination.
• the US FDA has recently required that ampoules be over- wrapped by a sealing pouch to avoid contamination of the ampoule contents.
• the pouch material is typically a tri-laminate of paper and/or polymer, aluminum and low density polyethylene (LDP). This pouch is regarded as an acceptable solution.
• Ampoules are typically produced in strips of multiples of single units doses, e.g. fives, tens or thirties. Therefore, a problem with pouches is that if several ampoules are contained within one pouch then as soon as the pouch is opened and the first ampoule used, the remaining ampoules are exposed to the environment and can be contaminated.
• the permeability of the LDP also restricts the labeling of the ampoules, as inks used for direct printing onto ampoules and adhesives used to attach paper labels must be checked carefully to ensure none will penetrate the ampoule and contaminate the contents.
• Some ampoules are topped up with inert gas, e.g. nitrogen. Even in a pouch there is some equilibration of nitrogen with the gases outside the ampoule but inside the pouch. As soon as the pouch is opened more nitrogen will be lost from the ampoule. LDP ampoules are translucent and some photo-sensitive materials when stored in these might be damaged after long-term storage and exposure to light. Pouches offer a partial solution but, again, once the pouch is opened ampoules inside are exposed to light for indefinite periods before being used.
• inert gas e.g. nitrogen.
• LDP tubes are fairly commonly used for cosmetics. But it is necessary to avoid oxygen getting into certain tube contents, e.g. if there are liposomes or other oxygen sensitive contents. LDP and other such materials are as a result not generally acceptable for manufacture of tubes for these cosmetics.
• An object of the present invention is to solve or at least ameliorate the above-identified issues.
• An object of preferred embodiments of the invention is to provide alternative, more preferably improved methods of sealing and / or coating of containers, and containers, in particular ampoules sealed and / or coated by the methods.
• the invention is based upon use of a metal-containing or polymer-containing sealing layer to provide a coating on containers made of plastics material.
• the invention provides an ampoule, comprising a coating of (a) a metal or a metal compound, or (b) a polymer deposited by vapour deposition.
• the invention provides a container for containing liquids, made of plastics material and comprising a coating of metal or a metal compound or of polymer.
• the invention provides a method of reducing moisture egress from a container made of plastics material, comprising applying to an outer surface of the container a coating comprising a metal or a metal compound or of polymer.
• the invention provides a method of sealing a container made of plastics material, comprising applying to an outer surface of the container a coating comprising a metal or a metal compound or of polymer.
• a fourth aspect of the invention provides a method of applying a label to an ampoule, comprising applying a coating of a metal or a metal compound or of polymer to the ampoule and applying the label to the coating.
• the coating can be applied by first providing the plastics layer and then applying the coating onto the layer or by producing, for example by extrusion or otherwise, a plastics layer coated with the coating.
• the coating is of a metal or metal compound, more preferably of metal.
• a coated container of the invention is an ampoule having a coating of a metal or a metal compound.
• the ampoule may be single or one in a strip of ampoules. In use this coating is found to have the effect of sealing the contents of the ampoule, reducing loss of ampoule contents to the outside and reducing contamination of the contents from the outside.
• the ampoule is typically of plastics material, especially polypropylene or polyethylene, low or high density, or other polymer used in manufacture of ampoules or in the drinks industry, e.g. polyethylene terephthalate. Further, the ampoule will typically contain a pharmaceutical agent, such as an inhalation drug or injectable drug, in combination with a pharmaceutically acceptable carrier.
• a pharmaceutical agent such as an inhalation drug or injectable drug
• the sealing is not required to be complete but is preferred to be such that after testing for the periods required e.g. in the case of ampoules to satisfy the regulatory authorities that the contents are adequately protected so that no further steps such as provision of external overwrapping by pouches are imposed.
• the coating may hence cover at least 50% of the outer surface area of the ampoule, or at least 70%, 80%, 90% or 95% of the outer surface area of the ampoule. Very preferably substantially all of the outside of the ampoule is coated.
• the coating material can be selected from a wide variety of metals and metal compounds which can be coated onto e.g. the ampoule.
• the coating can comprise aluminium, copper, carbon, chromium, silver, zirconium, tantalum, tungsten, titanium, cobalt, gold, palladium, platinum, and their alloys, including steel, and their compounds, including compounds of metals with gases, for example carbon nitride, tin oxide, indium oxide, silicon dioxide.
• gases for example carbon nitride, tin oxide, indium oxide, silicon dioxide.
• the coating preferably comprises aluminium, titanium, chromium, silver, copper, or a mixture or alloy of the aforesaid.
• Particularly preferred coatings comprise or consist of aluminium, titanium, chromium or tetrahedral amorphous carbon.
• Suitable coating methods include physical vapour deposition, e.g. by sputtering, and arc deposition. Sputter coatings optionally also have a UV lacquer to protect the coating and improve adhesion.
• Sputtering deposition is performed in a vacuum chamber where atoms, generally argon atoms, are ionized and accelerated to strike a target material, say aluminium. Coating material enters the vapour phase through a physical process rather than by a chemical or thermal process. The argon atoms dislodge aluminium atoms when they strike the target, then these ejected aluminium atoms strike the container to be coated, and this process applies a dense coating.
• Argon (Ar) ions can be created in an ion gun which then imparts kinetic energy and directs the ions toward the target to be sputtered, or in a plasma that contains Ar+ and electrons.
• Chemical vapour deposition or CVD is a generic name for a group of processes that involve depositing a solid material from a gaseous phase and is similar in some respects to physical vapour deposition (PVD). PVD differs in that the precursors are solid, with the material to be deposited being vaporised from a solid target and deposited onto the substrate. Whilst CVD may in some instances be suitable for the invention, generally the high temperatures required restrict the material that can be coated. CVD may also be too costly for large-scale manufacture of one-use products such as ampoules.
• an ion-containing plasma is created in a vacuum between an anode and a target, usually the cathode.
• a filtered cathode arc ions from the plasma are steered towards the substrate via a filter designed to remove neutral particles such as macroparticles. The ions deposit on the surface, forming the coating.
• the filtered vacuum cathode arc can apply coatings at lower temperatures, even lower than sputter coaters, below 70 degrees C and down to room temperatures, and is hence particularly suitable for temperature sensitive substrates such as plastics. Though, plastics which can withstand temperatures up to around 120 degrees C can be coated using sputter techniques. Metal or carbon or alloy coatings can be made using the filtered cathode arc, also compounds using introduction of reactive gas into the coating chamber near the substrate.
• Filtered cathode vacuum arc technology is described further in US patents 6,761,805, 6,736,949, 6,413,387 and 6,031,239, the contents of which are incorporated herein by reference.
• the coating is applied by physical vapour deposition or arc deposition.
• aqueous cleaning is generally sufficient.
• the articles to be coated is made of or comprises polymer such articles can be cleaned using known procedures except that more careful handling may be required.
• polymers may absorb water which must later be removed to achieve vacuum coating adhesion. The coating may adhere without any treatment in which case even aqueous washing can be omitted.
• the articles will likely remain clean for only a short period unless in a special environment, such as a dry nitrogen-purged container or in a UV/ozone chamber.
• a cleaning and/or surface preparation station as part or in juxtaposition to the coating station.
• a further consideration is that newly formed or moulded polymer, as in the blow-fill-seal process typically used for ampoule formation may not require any surface preparation for adequate adhesion of the coating to be obtained.
• ampoules can be prepared by forming the ampoule and applying the coating to the ampoule.
• a known method of forming ampoules is by blow-fill-seal (BFS), and the coating step can conveniently be added to the ampoule production line immediately after the BFS step and prior to packaging and/or labeling.
• BFS blow-fill-seal
• the ampoules typically contain from about ImL to about 5mL (extractable volume) of solution.
• a suitable depth is of at least 20 nm, preferably at least 50 nm, and also suitably up to 50 microns, preferably up to 20 microns.
• the coating depth may also be at least 100 nm and up to 10 microns.
• an ampoule is made of plastics material and comprises a coating of aluminium applied by sputter coating. More specifically, the ampoule contains a solution of an inhalation pharmaceutical in a pharmaceutically acceptable carrier.
• blow-fill-seal technology is used to obtain ampoules containing 2.5mL of a formulation containing salbutamol in saline.
• the ampoules are made from LDP and exit the filling apparatus in strips of 10.
• the strips are coated with an external coating of aluminium, applied using a sputter coater, to a depth of approximately 300 run, giving a shiny metallic look.
• the ampoules are packaged in the usual way though not overwrapped. Patients are given the ampoules in strips and tear off one ampoule at a time. The remaining ampoules are kept in a (now reduced size) strip until the next ampoule is removed and used, and so on until all ampoules are used.
• an ampoule is made of plastics material, comprises a coating of aluminium, chromium or titanium applied by sputter coating or filtered cathode arc and contains a solution of an injectable pharmaceutical in a pharmaceutically acceptable carrier.
• the solution may for example be water for injection or saline for injection. Typical volumes are 30ml or less, 25ml or less, 20ml or less, 15ml or less or 10ml or less.
• the ampoules can be manufactured in strips of 5, 10, 15 or more, as for other embodiments of the invention, to be torn off and used when required.
• a plastic ampoule is coated with a layer of titanium, applied by sputter coating, to a depth of about 150 nm.
• a plastic ampoule is coated with tetrahedral amorphous carbon to a depth of about 100 nm.
• the invention in certain embodiments relates more generally to containers for containing liquids, made of plastics material and comprising a coating of metal or a metal compound.
• containers can be made of polymer comprising polyethylene or polypropylene and further can have a maximum filled volume of up to 100ml, preferably up to 50ml, more preferably up to 20ml.
• the containers are useful for liquids containing volatile substances which would otherwise permeate plastics containers to an unacceptable degree.
• Also provided by the present invention are a method of reducing moisture egress from a container made of plastics material, comprising applying to an outer surface of the container a coating comprising a metal or a metal compound, and a method of sealing a container made of plastics material, comprising applying to an outer surface of the container a coating comprising a metal or a metal compound.
• the coating and its application are further and preferably as described with respect to the above embodiments of the invention.
• a further specific method of the invention is for sealing an ampoule, wherein the ampoule comprises from 0.5ml to 10ml of an inhalation pharmaceutical or an injectable pharmaceutical (e.g. water or saline for injection) in a pharmaceutically acceptable carrier, comprising applying to the ampoule a coating of a metal or a metal compound over at least 70% of the outer surface of the ampoule.
• an injectable pharmaceutical e.g. water or saline for injection
• a further method of the invention is a method of applying a label to an ampoule, comprising applying a coating of a metal or a metal compound to the ampoule and applying the label to the coating.
• the label can be attached to the coated ampoule using adhesive.
• the label can also be sprayed or printed onto the coated ampoule, e.g. ink sprayed onto the coated ampoule.
• the inventions in its varying embodiments offers a number of advantages, some or several or all of which may be seen in any given embodiment.
• the ampoules are sealed by the invention; reducing the loss e.g. of moisture and reducing contamination from the outside. Because of the shape of the ampoules, the process effectively seals each ampoule individually although ampoules may still be made in strips of say 5, 10, 30 etc. This is an improvement upon packaging a strip of ampoules in a pouch, as now when an ampoule is removed from the strip the remaining ampoules remain substantially sealed - contrast this with when a pouch containing many ampoules is opened and all become exposed to the environment.
• Ampoules coated according to the invention with a metallic coating have, in addition, a striking appearance.
• the coating has been found to be continuous, non-flaky and resistant to abrasion such as rubbing.
• the coating applied comprises a polymer, applied or deposited using a vapour deposition method.
• Methods for vapour deposition of polymer films are described for example in US patents 6,022,595; 4,013,532; 4,673,588; and 4,921,723, the contents of which are incorporated herein by reference.
• a specific method for applying a coating of poly para xylylene is described for example in Medical Device Technology, January/February 2006, ppl0-l l.
• an ampoule of an embodiment of the invention comprises a coating of a polymer deposited by vapour deposition.
• the coating can be or comprise poly para-xylylene, and polymer coatings of the invention are suitably applied by chemical vapour deposition.
• the ampoules may be made by forming the ampoule and applying the coating to the ampoule.
• the ampoules may in particular contain a solution of an inhalation pharmaceutical or an injection pharmaceutical in a pharmaceutically acceptable carrier.
• the invention also provides a method of reducing moisture egress from a container made of plastics material, comprising applying to an outer surface of the container a coating comprising polymer using a vapour deposition method, such as by chemical vapour deposition.
• the invention also provides a method of sealing an ampoule, wherein the ampoule comprises from 0.5ml to 10ml of an inhalation pharmaceutical or an injection pharmaceutical in a pharmaceutically acceptable carrier, comprising applying to the ampoule a polymer coating using a vapour deposition method over at least 70% of the outer surface of the ampoule, and also provides a method of applying a label to an ampoule, comprising applying a coating of polymer to the ampoule using a vapour deposition method and applying the label to the coating.
• the method applies generally to packaging used where the contents would be damaged by loss of or contamination by gases and other volatiles, for example, vitamins, flavours, perfumes etc.
• the invention provides packaging which is of plastics material, e.g. LDP, and cheaper than glass, trilaminates, ceramics etc.
• Fig. 1 shows a view from the front of a strip of ten ampoules coated with aluminium according to the invention
• Figs. 2 and 3 shows the strip of Fig. 1 with one ampoule being detached; and Fig. 4 shows a view from the front of a strip of ten ampoules coated with titanium according to the invention.
• a strip of 10 ampoules made from low density polyethylene was prepared using a standard blow-fill-seal apparatus, each ampoule containing 3ml of salbutamol solution. The ampoules were inspected visually to confirm correct filling of contents and manually to confirm they were all intact.
• the strip of ampoules was introduced into a filtered cathode arc coating machine fitted with an aluminium target. The machine was closed and pumped down to operating vacuum. The coating operation was begun and continued until the coating thickness monitor indicated a thickness of 300 nm. The coating was stopped, the vacuum released and the chamber opened.
• the coated ampoules (1) are shown in Figures 1-3.
• the ten ampoules exited the coating chamber intact - Fig. 1 and have a head (3) which in use is twisted to break the neck (2) to release the contents.
• the resultant coated ampoules had a shiny, metallic appearance, being completely coated with a thin layer of aluminum.
• the aluminum coating was continuous over the whole surface of the ampoules, was smooth and without noticeable defects. The coating was firmly adhered to the ampoules and did not detach and resisted rubbing.
• a single ampoule (4) was detached from the strip of 10 - See Fig. 2 - without tearing of the coating at the junction (5) between the detached ampoule and the remaining strip of nine ampoules.
• the integrity of the ampoules was tested and it was confirmed they remained intact and contained the same volume of solution as prior to being coated.
• the contents of four ampoules were tested independently using an atomic absorption based method to determine whether there had been contamination by aluminium. In each separate test, an aluminium content of less than 1 ppm was recorded, beyond the lower limit of the detection method, confirming that the aluminium content of the solution inside the ampoule after coating was essentially nil in each case. These results confirmed that the ampoule wall had not been breached during the coating process.
• a strip of 5 ampoules was made from low density polyethylene using a standard blow-fill-seal apparatus, each ampoule containing 3ml of saline solution. The ampoules were inspected visually to confirm correct filling of contents and manually to confirm they were all intact.
• the strip of ampoules was introduced into a filtered cathode vacuum arc apparatus fitted with a titanium target. The machine was closed and pumped down to operating vacuum. The coating operation was begun and continued until the coating thickness monitor indicates a thickness of 300 nm. The coating was stopped, the vacuum released and the chamber opened.
• the resultant coated ampoules (6) are shown in Fig. 4 and were found to have a shiny appearance, being substantially completely coated with a thin layer of titanium, the coating being slightly duller than the aluminum coating of Example 1.
• the invention hence provides coated plastic containers and methods of obtaining the same.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Health & Medical Sciences (AREA)
• Materials Engineering (AREA)
• Engineering & Computer Science (AREA)
• Life Sciences & Earth Sciences (AREA)
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• Animal Behavior & Ethology (AREA)
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• Inorganic Chemistry (AREA)
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• Medical Preparation Storing Or Oral Administration Devices (AREA)

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• 2006
  • 2006-02-09 CZ CZ20070614A patent/CZ2007614A3/cs unknown
  • 2006-02-09 WO PCT/GB2006/000433 patent/WO2006085063A1/en not_active Ceased
  • 2006-02-09 EP EP06701876A patent/EP1846587A1/en not_active Withdrawn
  • 2006-02-09 CA CA002597282A patent/CA2597282A1/en not_active Abandoned
  • 2006-02-09 AU AU2006212081A patent/AU2006212081B2/en not_active Ceased
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• 2007
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