Testing device for testing the tightness of a stopper in a packaging means main part, testing method, and use

Abstract

The invention relates to a testing device (1) for testing the tightness of a stopper (3) in a packaging means main part (5), which together delimit a packaging means volume (15) of a primary packaging means (13), comprising: - a primary packaging means holder (7) which is designed and configured to receive a primary packaging means (13) which is to be tested and which has the packaging means main part (5) and the stopper (3); - a pressure generating device (9) which is designed to apply a test pressure to the stopper (3) on the stopper side (17.1) facing away from the packaging means volume (15) by means of a test gas when the primary packaging means (13) is received in the primary packaging means holder (7), and - at least one gas detection material (11) which is designed such that at least one optical property of the at least one gas detection material (11) changes in the presence of the test gas, the at least one gas detection material (11) being provided on at least one side (17.2) of the sealing portion (2) of the stopper (3), said side facing the packaging means volume (15), when the primary packaging means (13) is received in the primary packaging means holder (7). The invention also relates to a testing method for testing the tightness of a stopper (3) and to the use of a gas detection material (11) in order to test the tightness of a stopper (3).

Description

[0001] 2024-02

[0002] 1

[0003] Vetter Pharma-Fertigung GmbH & Co. KG

[0004] DESCRIPTION

[0005] Test device for testing the tightness of a plug in a packaging base body, test method and use

[0006] The invention relates to a test device for testing the tightness of a plug in a packaging base body, a test method for testing the tightness of a plug in a packaging base body and the use of a gas detection material for testing the tightness of a plug in a packaging base body.

[0007] Primary packaging consists of a base and a stopper, which together define the packaging volume. This volume typically contains a pharmaceutical substance, for example, for injection. The stopper is movable along the central axis of the base such that the pharmaceutical substance is dispensed from the packaging volume via an injection end of the primary packaging when the movable stopper is shifted along the central axis, thus reducing the packaging volume. Such primary packaging is available in a wide variety of sizes, including relatively small sizes with volumes of 1 ml and 2.25 ml. It is known that the stopper in primary packaging is moved by means of a piston rod acting on the stopper, thereby dispensing the pharmaceutical substance.It must be ensured that the stopper fits tightly into the packaging body, preventing contaminants from entering the packaging volume and potentially contaminating the pharmaceutical substance, and conversely, preventing any pharmaceutical substance from leaking out of the packaging volume. Therefore, it is necessary to be able to test the tightness of the stopper within the packaging body cost-effectively, precisely, and—especially with relatively small primary packaging—without mechanical intervention.

[0008] The invention is therefore based on the objective of providing a test device for testing the tightness of a plug in a packaging base body, a test method for testing the tightness of a plug in a packaging base body, and a use of a

[0009] 212221 PCT - KO-HF 2024-02

[0010] 2

[0011] to create gas detection material for testing the tightness of a plug in a packaging base body, whereby the aforementioned disadvantages are reduced, or preferably do not occur.

[0012] The problem is solved by providing the present technical teaching, in particular the teaching of the independent claims as well as the embodiments disclosed in the dependent claims and the description.

[0013] The problem is solved, in particular, by providing a test device for testing the tightness of a plug in a packaging base body, the two components of which together define the volume of a primary packaging. The test device comprises a primary packaging receptacle, a pressure generation device, and at least one gas detection element. The primary packaging receptacle is designed and configured to receive a primary packaging component to be tested, which includes the packaging base body and the plug. The pressure generation device is configured to apply a test pressure, in particular a time-dependent test pressure profile, to the plug on at least one side facing away from the packaging volume using a test gas when the primary packaging is received in the primary packaging receptacle.The at least one gas detection material is configured such that at least one optical property of the at least one gas detection material changes in the presence of the test gas. The at least one gas detection material is arranged on at least one side of a sealing section of the plug facing the packaging volume when the primary packaging is received in the primary packaging receptacle.

[0014] The test device is advantageously simple and compact in design. It allows for a simple and relatively inexpensive way to test the tightness of the stopper in the packaging base. This method advantageously avoids any mechanical impact on the packaging base and the stopper, so that the test device can also be used to test primary packaging with a relatively small volume, particularly 1 ml and 2.25 ml. A change in at least one optical property occurs even when only a relatively small amount of the test gas flows into at least one test volume containing the gas detection material.

[0015] 212221 PCT - KO-HF 2024-02

[0016] 3

[0017] The gas detection material has a specific property. In particular, the test gas acts directly on the reverse side of the plug, specifically on at least one sealing section of the plug, which is opposite the gas detection material. This enables real-time detection of the test gas within the test volume using the gas detection material. Advantageously, complex measurement technology, especially electronic gas measurement technology, can be dispensed with, since the change in at least one optical property is visible to the naked eye.

[0018] In one embodiment, the primary packaging element comprises the packaging body, a plug that is movable, particularly along a central axis of the packaging body, and an injection end, wherein the injection end is arranged, in particular, at one end of the packaging body. The packaging body, together with the movable plug, defines the packaging volume. The plug has an outer diameter that is larger than the inner diameter of the packaging body, so that the plug is pressed against the packaging body when it is inserted into the packaging body as intended. The plug has at least one sealing section. This sealing section completely surrounds the plug along a plug axis that is preferably oriented concentrically to the central axis of the packaging body.In particular, the plug has at least two sealing sections, in particular exactly two sealing sections, or at least three sealing sections, in particular exactly three sealing sections, which are spaced apart from one another along the plug axis. In particular, the plug has a sealing lamella as one sealing section of the at least one sealing section. In particular, the plug has at least two sealing lamellae, in particular exactly two sealing lamellae, or at least three sealing lamellae, in particular exactly three sealing lamellae. In particular, the at least one sealing section, in particular the at least one sealing lamella, is pressed against the packaging base body when the plug is inserted into the packaging base body as intended.In particular, the at least one sealing section of the plug and the packaging base body form a sealing area in which the at least one sealing section, in particular the at least two sealing sections, in particular the at least three sealing sections are pressed against the packaging base body when the plug is inserted into the packaging base body as intended. In particular, the primary packaging material has a sealing area adjacent to the rear of the plug and the 212221 PCT - KO-HF 2024-02.

[0019] 4

[0020] Gas detection material relating to the plug, in particular relating to the pressure chamber opposite at least one sealing section of the plug, into which the test gas flows during a test procedure and applies the test pressure to the plug, in particular directly.

[0021] In one embodiment, at least one gas detection material is arranged within the packaging volume. In particular, the packaging volume is the test volume, also referred to as the packaging volume test volume. Specifically, the plug is inserted so far along the central axis into the packaging body that the plug is in contact with the gas detection material, and in particular rests on the gas detection material, when the primary packaging is received in the primary packaging receptacle and the gas detection material is arranged within the packaging volume.

[0022] In another embodiment, the at least one gas detection material – particularly with respect to the plug axis – is arranged between two, in particular immediately adjacent, sealing sections, especially sealing lamellae, which is also referred to as the sealing section test volume. In particular, a support element is inserted into the packaging volume to prevent displacement of the plug towards the injection end. If the plug has at least three sealing sections, in particular sealing lamellae, a first sealing section of the at least three sealing sections is adjacent to the pressure chamber, and a third sealing section of the three sealing sections is adjacent to the packaging volume. In particular, with respect to the plug axis, a second, in particular a central, sealing section of the at least three sealing sections is arranged between the first and third sealing sections.In particular, at least one gas detection material is arranged between the first sealing section and the second sealing section, which, in particular together with the packaging base body, define a first sealing section test volume, and / or between the third sealing section and the second sealing section, which, in particular together with the packaging base body, define a second sealing section test volume. In particular, two adjacent sealing sections, selected from the first sealing section, the second sealing section, and the third sealing section, together with the packaging base body, form, or in particular define, the sealing section test volume.

[0023] 212221 PCT - KO-HF 2024-02

[0024] 5

[0025] In yet another embodiment, at least one gas detection material is arranged in the packaging volume test volume and additionally in the first sealing section test volume and / or in the second sealing section test volume. In particular, the gas detection material arranged in the packaging volume test volume acts as a support element for the plug.

[0026] In particular, the gas detection material can thus be arranged in several test volumes, selected from the packaging volume test volume and the sealing section test volume, in particular the first sealing section test volume and the second sealing section test volume.

[0027] Due to a leak in the stopper, the test gas can enter the test volume. The test gas can pass between the stopper and the packaging body—bypassing at least one sealing section—and into the sealing section test volume located between two sealing sections. It is also possible that the stopper itself is leaking, particularly porous, allowing the test gas to pass through the stopper into the packaging volume as the test volume, specifically as the packaging volume test volume. Furthermore, it is possible that the test gas passes between the stopper and the packaging body—bypassing all sealing sections—and into the packaging volume as the test volume, specifically as the packaging volume test volume.If the test volume – as a sealing section test volume – is arranged between two adjacent sealing sections, it can be determined, in particular, whether the test gas has flowed past a sealing section of the two sealing sections closer to the pressure chamber and into the sealing section test volume, i.e., whether the sealing area has a leak, or is leaking. If, and especially exclusively, the test volume is the packaging volume, or more specifically, the packaging volume test volume, it can be determined not only whether the test gas has flowed into the packaging volume, but also, and especially, whether the test gas has flowed into the packaging volume as the test volume along the sealing area or through the plug. The change in at least one optical property occurs spatially resolved in the at least one gas detection material, especially if this material is a free-flowing powder or a liquid.Thus, in the event of a test gas leak, it is possible to determine whether the test gas is leaking between the plug and the packaging body - along the sealing area - or through the plug into the packaging volume as the test volume.

[0028] 212221 PCT - KO-HF 2024-02

[0029] 6. If the test gas flows between the stopper and the packaging body into the packaging volume (the test volume), at least one optical property of the gas detection material changes, particularly in the vicinity of the sealing area. If the test gas flows through the stopper into the packaging volume (the test volume), at least one optical property of the gas detection material changes, particularly in the area where the test gas flows through the stopper into the packaging volume (the test volume). The cases described above are also referred to as test gas leakage. In particular, a change in at least one optical property occurs in the case of test gas leakage—that is, in all of the aforementioned cases.

[0030] In one embodiment, the pressure generating device is configured to provide, and in particular generate, a test pressure that differs from ambient pressure, in particular from standard atmospheric pressure of 1013.25 hPa, and which is, in particular, greater than standard atmospheric pressure by a differential pressure. Specifically, the pressure generating device is configured to provide, and in particular generate, a test pressure that differs from ambient pressure of up to 1 MPa, in particular at least 0.1 MPa, in particular at least 0.2 MPa, in particular at least 0.4 MPa, in particular at least 0.6 MPa, in particular at least 0.7 MPa, in particular at least 0.9 MPa, and in particular at most 1.1 MPa, in particular at most 1 MPa. Specifically, the pressure generating device is configured to provide, and in particular generate, the test pressure, and in particular the test pressure profile over time.In the context of this technical teaching, the fact that the pressure generating device provides, and in particular generates, the test pressure means, in particular, that the pressure generating device provides, and in particular generates, the test gas exhibiting the test pressure. It is possible for the pressure generating device to store the test gas at a test gas storage pressure greater than the test pressure, wherein the pressure generating device includes a pressure reducing device designed and configured to reduce the test gas storage pressure to the test pressure. In one embodiment, the pressure generating device comprises a stationary gas storage device or a mobile gas storage device. In particular, the stationary gas storage device is a stationary gas container, especially a stationary gas tank. In particular, the mobile gas storage device is a mobile gas container, especially a gas cylinder.In the context of this technical teaching, a test pressure is understood to be, in particular, an instantaneous pressure of the test gas acting on the back side of the plug. Specifically, see 212221 PCT - KO-HF 2024-02.

[0031] 7

[0032] The test pressure along a pressure line path from the pressure generating device to the pressure chamber of the primary packaging is locally constant, since there are no or only negligible local pressure differences due to dynamic flow, especially dynamic pressure components. In particular, several test pressures from different, especially subsequent, points in time constitute the temporal test pressure profile. Specifically, the temporal test pressure profile is either discrete, i.e., exhibits specific test pressure values, or continuous, i.e., exhibits a continuous test pressure profile.

[0033] In one embodiment, the pressure generating device is connected to the pressure chamber via the pressure line path. In particular, the pressure line path runs from the pressure generating device to the pressure chamber.

[0034] In one embodiment – ​​particularly for functional testing of the test device, especially for positive verification of the test device – the test device has a removable capillary element which is designed and configured to connect the pressure chamber to the packaging volume in a pressure-conducting, and in particular fluid-conducting, manner. In one embodiment, the capillary element is arranged in the sealing area, particularly between the packaging base body and the stopper, and particularly past the at least one sealing section, such that the capillary element extends from the pressure chamber to the packaging volume and connects the pressure chamber and the packaging volume in a pressure-conducting, and in particular fluid-conducting, manner.In another embodiment, the capillary element is arranged in the plug, with the capillary element extending through the plug in such a way that it reaches from the pressure chamber to the packaging volume and connects the pressure chamber and the packaging volume in a pressure-conducting, and in particular fluid-conducting, manner. Advantageously, when the capillary element is inserted, applying the test pressure to the plug causes the test gas to enter the packaging volume via the capillary element. If the at least one gas detection material is arranged in the packaging volume, i.e., if the packaging volume is the packaging volume test volume, the presence of the test gas changes the at least one optical property of the at least one gas detection material. This makes it possible to ensure that the test device, and in particular the gas detection material, is functioning correctly.Especially after it has functioned correctly.

[0035] 212221 PCT - KO-HF 2024-02

[0036] If a defect in the test device, in particular in the at least one gas detection material, is detected, the capillary element is removed so that it no longer connects the pressure area and the packaging volume. In particular, the tightness of a plug in a packaging base body can then be tested.

[0037] In the context of this technical teaching, an optical property of the gas detection material is understood to be, in particular, a property that describes an interaction with electromagnetic radiation, especially in the visible spectral range. The at least one optical property is preferably selected from a group consisting of transmission, reflection (directional or diffuse), remission, absorption, and a combination of at least two of these optical properties. In one embodiment, the at least one optical property is a color of the gas detection material, in particular a color perceptible in reflection, wherein the term "color" preferably also includes the property of being white or black, even if these are not colors in the strict physical sense.

[0038] The fact that the gas detection material is configured such that at least one optical property changes in the presence of a test gas is, in other words, referred to as the gas detection material being sensitive to the test gas. Specifically, the gas detection material exhibits sensitivity to the test gas. In particular, the gas detection material is sensitive to the test gas. Specifically, in the presence of the test gas, the gas detection material exhibits a reversible or irreversible color change in the visible spectral range, which can be detected with the naked eye or quantitatively using spectroscopic methods such as UV-Vis or fluorescence spectroscopy.

[0039] The at least one gas detection material is configured such that its at least one optical property changes in the presence of a specific gas, particularly the test gas; this means, in particular, that the gas detection material is tailored to detect a specific gas, especially the test gas. In one embodiment, the gas detection material is chemically configured to react with the specific gas and thereby change its at least one optical property. In one embodiment, the gas detection material has a reactant form, in particular

[0040] 212221 PCT - KO-HF 2024-02

[0041] 9. The gas detection material is defined as a gas detection material characterized by a specific first chemical formula and / or structural formula, and a product form, in particular defined by a specific second chemical formula and / or structural formula, wherein the gas detection material is converted from the reactant form to the product form by reaction with the specific gas, and wherein the reactant form has different optical properties than the product form, in particular a different absorption spectrum. In one embodiment, the color change of the gas detection material is based on a reversible or irreversible chemical redox reaction of an indicator dye or redox dye with the test gas, in particular with a dissociated or otherwise, in particular catalytically, modified form of the gas, for example, dissociated hydrogen.Dissociated hydrogen is produced, for example, in the presence of hydrogen gas through a dissociation of hydrogen, which is catalyzed by a catalytically active substance (for catalyzing the dissociation of hydrogen).

[0042] In one embodiment, the at least one gas detection material has three states or forms, which it assumes depending on the presence and / or history of the presence or concentration of the test gas. A first state or form is hereinafter referred to as the "untouched reactant form"—in particular defined by a specific third chemical formula and / or structure—in which the gas detection material exists before it has first come into contact with the test gas or reacted with the gas for the first time. A second state or form is hereinafter referred to as the "post-reactive reactant form"—in particular defined by the specific first chemical formula and / or structure—in which the gas detection material exists after a first reaction with the test gas and can react further from this state to form the product form.The third state or form is hereinafter referred to as the "product form" and is defined in particular by the specific second chemical molecular and / or structural formula; the gas detection material reaches this state through further reaction with the test gas, starting from the post-reactive reactant form. Advantageously, this embodiment also allows determination of whether the test gas was ever present in the test volume, particularly in the packaging volume, especially in a specific region of the packaging volume, and / or between two sealing sections, particularly if the gas detection material was present in the test volume, especially in the packaging volume, for this period of time.

[0043] 212221 PCT - KO-HF 2024-02

[0044] 10 in particular in the specific area of ​​the packaging volume, and / or between two sealing sections.

[0045] In the context of this technical teaching, the concentration of a test gas is generally understood to mean, in particular, a percentage by volume in vol.%.

[0046] In one embodiment, the reaction from the untreated reactant form to the post-reactive reactant form is irreversible; in particular, this reaction can occur with the elimination of water. In a specific embodiment, the test gas is hydrogen, the untreated reactant form is resazurin, and the post-reactive reactant form is resofurin. Alternatively or additionally, the reaction between the post-reactive reactant form and the product form is reversible. In a specific embodiment, the product form is hydroresofurin, particularly when the post-reactive reactant form is resofurin and the test gas is hydrogen.

[0047] In one embodiment, the at least one gas detection material has a distinct color in each state or form, allowing the states or forms to be distinguished. In one embodiment, the unprocessed reactant form is violet, the post-reactive reactant form is pink, and the product form is white.

[0048] It is possible that a plurality of gas detection material configurations are arranged within the packaging volume. In one embodiment, the different gas detection material configurations can be sensitive to different test gases. Alternatively or additionally, the different gas detection material configurations can be sensitive to different concentrations of a test gas, particularly the same test gas; this means, in particular in one embodiment, that the reaction from the reactant form to the product form takes place at different concentrations of the test gas.

[0049] In one embodiment, the gas detection material can be observed through the packaging body – from the outside – by means of a suitable detection device, for example, by at least one fiber optic cable, a camera, or the like; in particular, this is also possible with the naked eye. This preferably allows for particularly simple monitoring, as well as monitoring from a remote location, or even automated monitoring, and optionally also AI-supported evaluation.

[0050] 212221 PCT - KO-HF 2024-02

[0051] 11

[0052] In the context of this technical teaching, a test configuration is understood to mean, in particular, that a pre-selected plug is inserted into a pre-selected packaging body for testing the tightness of the plug within the packaging body, wherein the gas detection material is arranged in the test volume, in particular in the packaging volume and / or between two sealing sections. In the context of this technical teaching, a test procedure is understood to mean, in particular, that the plug of the test configuration is subjected to a pre-selected test gas at a pre-selected test pressure for a pre-selected test duration.

[0053] According to a further development of the invention, the gas detection material is arranged such that the at least one optical property changes reversibly depending on the concentration of the test gas.

[0054] Advantageously, due to the reversible change in optical properties, a past test gas leak can be detected, and in particular visualized and monitored. Furthermore, it is possible to distinguish between a past test gas leak and a current one. Specifically, it is possible to differentiate whether the gas detection material was in contact with the test gas in the past or is currently in contact with it.

[0055] In the context of the present technical teaching, the fact that the at least one optical property changes depending on the concentration of the test gas means, in particular, that the at least one optical property of the at least one gas detection material changes in a first direction when the concentration of the test gas is present or increases, and changes in a second direction opposite to the first direction when the concentration of the test gas is absent or decreases, i.e., changes back. In one embodiment, the reaction of the reactant form to the product form is a reversible reaction that can proceed in both directions, wherein, in particular, the reactant form reacts to the product form when the test gas is present or its concentration increases, and wherein the product form reacts back to the reactant form when the test gas is absent or its concentration decreases.

[0056] According to a further development of the invention, the gas detection material has supraparticles comprising a particle superstructure consisting of nanoparticles as well as the 212221 PCT - KO-HF 2024-02

[0057] 12

[0058] The particle superstructure contains embedded substances. The nanoparticles are selected from a group consisting of SiO2 nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof. The substances embedded in the particle superstructure contain at least one catalytically active substance for catalyzing hydrogen dissociation and at least one redox dye.

[0059] The superparticle offers the advantage of particularly easy detection of test gas leaks using hydrogen gas as the test gas. It is possible to detect even very small quantities of hydrogen gas in the test volume, especially in the packaging volume and / or between two sealing sections, thus enabling the detection and visualization of even the smallest leaks between the plug and the packaging body.

[0060] In one embodiment, the test gas comprises or consists of hydrogen gas. In the context of this technical teaching, hydrogen gas is understood to mean, in particular, molecular hydrogen, especially as a diatomic molecule, with the symbol H₂. Due to its small atomic size, especially its molecular size, its low mass, and its weak interaction, hydrogen gas is particularly well-suited as a test gas, since it flows into the test volume, especially the packaging volume and / or between two sealing sections, even with a comparatively small leak in the sealing area and / or a small porosity of the plug.If no hydrogen gas flows into the test volume during a test procedure—meaning no change occurs in at least one optical property—it can be assumed that no other gas would have flowed into the test volume even if a different gas, particularly ambient air, especially compressed air, or carbon dioxide, had been used as the test gas. Therefore, if a specific test configuration proved to be leak-tight during a test procedure with hydrogen gas at the test pressure, it can be concluded that this test configuration would also have been leak-tight with other gases, particularly ambient air, especially compressed air, or carbon dioxide.Thus, in particular by using hydrogen gas, a worst-case scenario is tested, since other gases, especially ambient air, especially compressed air, or carbon dioxide, have a larger atomic size, especially molecular size, a greater mass and especially a higher interaction than hydrogen gas.

[0061] 212221 PCT - KO-HF 2024-02

[0062] 13

[0063] In one embodiment, it is provided that the at least one catalytically active substance contains or consists of at least one transition metal, wherein the at least one transition metal is optionally selected from a group consisting of iridium, ruthenium, rhodium, gold, palladium, platinum, and mixtures and alloys thereof, wherein the at least one transition metal is further optionally selected from the group consisting of gold, palladium, platinum, and mixtures and alloys thereof.Alternatively or additionally, the at least one catalytically active substance is provided to contain or consist of nanoparticles, which are optionally selected from the group consisting of iridium nanoparticles, ruthenium nanoparticles, rhodium nanoparticles, gold-platinum nanoparticles, gold-palladium nanoparticles, palladium nanoparticles, platinum nanoparticles, and mixtures thereof, wherein the nanoparticles are further optionally selected from the group consisting of gold-platinum nanoparticles, gold-palladium nanoparticles, palladium nanoparticles, platinum nanoparticles, and mixtures thereof. Alternatively or additionally, the at least one catalytically active substance is provided to contain or consist of a sulfonated Wilkinson catalyst.

[0064] In particular, the catalytic activity of the catalytically active substance can be influenced by the catalyst material used, as well as by its size, geometry and concentration, and thus the sensitivity, response time and working range of the supraparticles used for optical indication of the test gas can be specifically adapted.

[0065] In one embodiment, the at least one redox dye is a polyaromatic compound that optionally contains a redox-sensitive chromophore and / or a redox-sensitive fluorophore. Alternatively or additionally, the at least one redox dye is selected from the group consisting of bromothymol blue, methyl red, methyl blue, Evan's blue, methyl orange, Nile blue, dichloroindophenol, methylene blue, resazurin, resorufin, and mixtures thereof. Alternatively or additionally, the at least one redox dye is selected from the group consisting of dichloroindophenol, methylene blue, resazurin, resorufin, and mixtures thereof. Alternatively or additionally, the at least one redox dye undergoes a reversible color change or reversible at least partial decolorization upon reaction with dissociated hydrogen, or an irreversible color change or irreversible at least partial decolorization.

[0066] 212221 PCT - KO-HF 2024-02

[0067] 14

[0068] In one embodiment, the metal oxide nanoparticles are selected from the group consisting of Ce3O4 nanoparticles, TiCh nanoparticles, AhCE nanoparticles, and mixtures thereof.

[0069] In one embodiment, the substances embedded in the particle superstructure additionally contain at least one organic or inorganic acid, optionally selected from the group consisting of hydrochloric acid, sulfurous acid, carbonic acid, acetic acid, phosphoric acid, sulfuric acid, and mixtures thereof, wherein the at least one organic or inorganic acid is optionally sulfuric acid. Alternatively or additionally, the substances embedded in the particle superstructure contain at least one substance for quenching electronic triplet states, optionally selected from the group consisting of ascorbic acid, mercaptoethylamine, cysteamine, diphenylhexatriene, 2,2,6,6-tetramethylpiperidinyloxyl (TEMPO), urea, 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (TROLOX), and mixtures thereof.

[0070] In one embodiment, the at least one gas detection material is in the form of a powder, preferably a free-flowing powder. In another embodiment, the at least one gas detection material is in the form of a fluid. In particular, the fluid is in a liquid state. In yet another embodiment, the at least one gas detection material is contained, in particular fixed.

[0071] In one embodiment, the gas detection material contains 60 to 99.99994 wt%, optionally 80 to 99.99994 wt%, and further optionally 90 to 99.99 wt%, of nanoparticles selected from the group consisting of SiCh nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof, based on the total weight of the gas detection material. Alternatively or additionally, the gas detection material contains 0.00005 to 20 wt%, optionally 0.00005 to 1.0 wt%, of at least one catalytically active substance for catalyzing the dissociation of hydrogen, based on the total weight of the gas detection material. Alternatively or additionally, it is provided that the gas detection material contains 0.00001 to 5 wt.%, optionally 0.00001 to 2 wt.%, of the at least one redox dye, based on the total weight of the gas detection material, wherein the gas detection material optionally additionally contains 0.01 to 40

[0072] 212221 PCT - KO-HF 15

[0073] The gas detection material contains a wt.%, optionally 0.1 to 20 wt.%, of at least one organic or inorganic acid, based on the total weight of the gas detection material. Alternatively or additionally, the gas detection material contains 0.01 to 10 wt.%, preferably 0.1 to 2 wt.%, of at least one substance for quenching electronic triplet states, based on the total weight of the gas detection material.

[0074] In one embodiment, the at least one gas detection material is a powder or a liquid containing or consisting of supraparticles as described in DE 10 2021 211 738 B3.

[0075] According to a further development of the invention, the pressure generating device includes a gas generation device, in particular a gas generation cell, which is designed and configured to generate the test gas.

[0076] The use of a gas generation device makes it advantageous to eliminate the need to store the finished test gas. This significantly reduces, and preferably eliminates, any potential risks associated with storing the test gas. Furthermore, the gas generation device allows the test gas to be produced before the test procedure, particularly immediately beforehand.

[0077] In one embodiment, the gas generation device is designed and configured as an electrochemical gas generation device to produce the test gas by means of a chemical reaction. In particular, the gas generation device comprises a housing in which at least one gas generation cell is arranged. Specifically, the gas generation cell has an anode and a cathode. The gas generation device further comprises two electrical contacts configured to be connected to an external voltage source. Specifically, one contact of each of the two electrical contacts is electrically connected to the anode and one contact of each of the two electrical contacts is electrically connected to the cathode. In particular, the two electrical contacts extend through the housing so that they can be electrically connected to the external voltage source.Connecting the anode and cathode to the external voltage source advantageously allows for a uniform test gas generation rate. In particular, the gas generation cell comprises a first chemical element and a second chemical element as an electrolyte. Specifically, when the gas generation cell is connected to 212221 PCT - KO-HF 2024-02.

[0078] When an electrical resistor is discharged, the test gas is generated in relation to the flowing current. This test gas can escape through at least one outlet opening in the base of the gas generation cell. In one embodiment, the at least one outlet opening is openably closed with a sealing element to prevent drying out and the ingress of atmospheric oxygen into the gas generation cell. In particular, the gas pressure generated by the gas generation cell is sufficient to lift the sealing element from the base and allow the test gas to escape. Specifically, the sealing element is designed as a sticker, wherein the gas pressure generated by the gas generation cell is sufficient to detach an adhesive from the sticker and allow the test gas to escape. In particular, the gas generation device has an adjustable resistance, especially a potentiometer.This makes it advantageously possible to adjust the flow rate and thus the test gas generation rate.

[0079] In one embodiment, the gas generation cell is designed as a button cell. It is possible to arrange several gas generation cells in series, in particular by connecting them one after the other. Specifically, the gas generation cell has an anode on a first side and a cathode on a second side opposite the first side, such that the gas generation cells are connected in series, in particular when they are arranged one after the other, with each anode on a first side in contact with a cathode on a second side.

[0080] In one embodiment, a single gas generation cell is configured to produce a maximum of 10 ml of the test gas per hour, particularly at a gas pressure of at least 2.5 MPa, whereby a total maximum test gas quantity of 140 ml can be produced with a single gas generation cell. In particular, five gas generation cells arranged in series are configured to produce a maximum of 50 ml of the test gas per hour, whereby a maximum test gas quantity of 700 ml can be produced.

[0081] According to a further development of the invention, the gas generation device, in particular the gas generation cell, is designed and configured to produce hydrogen as the test gas.

[0082] The advantage of using the gas generation device is that it is not necessary to store hydrogen gas. Hydrogen gas is highly flammable and 212221 PCT - KO-HF 2024-02

[0083] Hydrogen can form explosive mixtures with air. Furthermore, it can penetrate certain metals and reduce their strength. Using the gas generation device, it is advantageously possible to generate the hydrogen gas only shortly before the testing procedure, particularly immediately beforehand. This reduces, and preferably eliminates, the aforementioned risks associated with storing hydrogen gas.

[0084] In one embodiment, the gas generation cell is designed as an electrochemical gas generation cell, in particular as a mercury-free hydrogen generation cell, comprising a metal anode, an electrolyte, and a gas diffusion electrode, wherein the metal anode comprises zinc as its main component with additives of indium and bismuth, and wherein the electrochemical gas generation cell, calculated on its total weight, contains less than 5 ppm mercury, less than 20 ppm cadmium, and less than 40 ppm lead, wherein the electrolyte comprises additives from each of the following groups of substances: a) corrosion inhibitors, b) surfactants (wetting agents), and c) viscosity modifiers, and wherein i) one or more of the following compounds are used as corrosion inhibitors: benzotriazole, tolyltriazole, tolyltriazole solution, and benzimidazole; ii) surfactants,which are used on the surface of the zinc to limit the reaction nuclei, include one or more of the following compounds: sulfone salts, polyethylene glycols (PEGs), PEG diacid, polyfluoroalcohol ethoxylate, alkyl polyethylene oxide, polyethylene ether, diaminepyridine, phenyldiamine, aminophenol sulfonic acid, 2,4-dinitrophenols, benzidine, fluorosurfactants, hydroxyethyl quinoline, and quaternary ammonium phenolates; and iii) as viscosity-forming agents, include one or more of the following substances: natural substances, such as polyalcohol, cellulose or cellulose derivatives, such as carboxymethyl cellulose (CMC) and agar, and as polymers, polyvinyl alcohol,Teflon (PTFE) and polyacrylic acids. In particular, these substances contribute to a further reduction of zinc self-discharge and spontaneous and uncontrolled hydrogen evolution. Furthermore, the potential difference of local cells can be reduced and the flow properties of the electrolyte favorably influenced. For example, the addition of inorganic and organic acids, such as phosphoric acid, tartaric acid, succinic acid, and citric acid to the electrolyte can improve the hydrogen overpotential and reduce dendrite formation. These additives are typically added to a NaOH / KOH electrolyte containing approximately 0.3 to 0.6 mol of ZnO. The cathode consists mainly of Zn and 212221 PCT - KO-HF 2024-02.

[0085] 18

[0086] ZnO, with woven-in cellulose fibers serving as internal moisture conductors. These fibers form internal electrolyte channels that keep the electrode wet and porous over a long operating period. Wherever electrically insulating and / or material-separating materials are required, polyvinyl alcohol (PVA), polyacrylic acid (PAA), polyethylene (PE), and polypropylene (PP) can be used. The current collector on the cathode side often has a trimetallic composition of Ni / SS304 / Cu tape, with copper located internally in the cap. This tape may have an additional metal coating on the copper side, consisting of tin. The thickness of this tin layer can range from 0.2 to 10 µm and can be applied using various techniques, such as electroless plating, electrochemical plating, or vapor deposition. This additional tin layer may have minor defects, such as...Small pores or cracks can lead to the copper layer of the current collector being exposed to the aggressive alkaline electrolyte. Therefore, the addition of additives is necessary to reduce side reactions resulting from the electrical properties of the copper / electrolyte / zinc system. To improve the uniformity of the tin coating, the coated film can be heated to a temperature close to the melting point of tin, thereby repairing any defects. This leads to the disappearance of small pores and a faster, spontaneous alloying of the tin layer with the copper atoms. This heat treatment can also be combined with a mechanical treatment. Stainless steel or another deep-drawable steel can be used for the positive electrode, which may be further refined with a nickel plating after the forming process.A further advantageous development of the gas evolution cell is achieved when an inner surface of a current collector facing the metal anode is at least partially coated with a Cu / Zn and / or a Cu / Sn and / or a Cu / Zn / Sn alloy. This metal layer can also additionally contain indium. This at least partial coating increases the hydrogen overpotential of the surface, improves the corrosion properties of the current collector, and stabilizes the contact resistance between the electroactive metal anode and the current collector. Particularly reliable and consistent operation of the electrochemical gas evolution cell is achieved when the concentration of indium and bismuth is in the range of 50 to 2000 ppm, preferably in the range of 100 to 1000 ppm. Such a concentration has proven sufficient to ensure the smooth operation of the gas evolution cell.

[0087] 212221 PCT - KO-HF 19

[0088] The absence of the toxic metals mercury, lead, and cadmium is necessary to restore the effects that would otherwise be lost. To achieve these desired effects, it is particularly advantageous if the particle sizes of indium and bismuth are in the range of 0.5 to 1000 pm, preferably from 1 to 500 pm.

[0089] In one embodiment, the gas development cell is designed as described in EP 2 337 124 Bl.

[0090] In one embodiment, the gas generation cell contains zinc powder and potassium hydroxide solution as the electrolyte. Particularly when the gas generation cell is discharged via an electrical resistor, pure hydrogen gas is produced relative to the flowing current, which can escape through the at least one outlet opening in the base of the gas generation cell. It is possible to additionally connect the anode and the cathode to an external voltage source to establish a uniform test gas generation rate. Specifically, the zinc powder reacts with the potassium hydroxide solution to form zinc oxide.

[0091] According to a further development of the invention, the test device has a pressure sensor which is arranged and set up to detect the test pressure.

[0092] The pressure sensor offers the advantage of monitoring the gas pressure of the test gas, particularly the test pressure, at any given moment. It also allows for the detection of the gas pressure acting on the plug, particularly the test pressure. Furthermore, it enables the detection of multiple test pressures at different, particularly subsequent, points in time, and thus the temporal profile of the test pressure. This allows for the precise detection of the test pressure at which at least one optical property of the gas detection material changes. In particular, it enables the precise detection of the test pressure at which a test gas leak occurs, specifically when the test gas flows into the test volume and the plug is no longer airtight.

[0093] In one embodiment, the pressure sensor is connected to the pressure line path in a pressure-conducting manner. In particular, the pressure sensor is arranged and configured to detect an instantaneous pressure in the pressure line path. In one embodiment, the pressure sensor is configured to generate an electrical pressure signal and to measure the electrical

[0094] 212221 PCT - KO-HF 20

[0095] To transmit a pressure signal to an evaluation device. In particular, the electrical pressure signal contains information about the value of the measured pressure.

[0096] According to a further development of the invention, the test device has a pressure relief valve which is designed to release the test gas.

[0097] The pressure relief valve offers the advantage of allowing the test gas to be released and, in particular, the pressure in the pressure line path, especially in the pressure chamber, to be reduced to a lower pressure than the test pressure, especially to ambient pressure. This simplifies the removal of the primary packaging from the test device after a completed test, since the test gas is first released, and the test device is depressurized, before the primary packaging can be removed from the test device, especially at ambient pressure.

[0098] In one embodiment, the pressure relief valve branches off from the pressure line path. In particular, the pressure relief valve is arranged and configured to open the pressure line path, specifically so that the test gas contained in the pressure line path and especially in the pressure chamber can escape through the pressure relief valve from the pressure line path and especially from the pressure chamber.

[0099] In one embodiment, the test device includes a safety valve designed and configured to automatically release the test gas upon reaching a predetermined pressure threshold, particularly in the pressure line path. Specifically, the pressure threshold is between 0.8 MPa and 1.2 MPa, and more specifically, 1 MPa. In one embodiment, the pressure release valve is configured as the safety valve. In another embodiment, the test device includes a separate safety valve – thus comprising both a pressure release valve and a safety valve.

[0100] According to a further development of the invention, the test device has an injection end sealing element for closing, in particular sealing, an injection end of the primary packaging material. The injection end sealing element is located at the injection end.

[0101] 212221 PCT - KO-HF 21 and closes the injection end, in particular sealing it when the primary packaging material is received in the primary packaging receptacle.

[0102] The injection end sealing element advantageously allows the injection end to be sealed, thereby limiting the packaging volume. For complete limitation, and especially sealing, of the packaging volume, the plug must be properly inserted into the packaging body. Specifically, the injection end sealing element prevents the gas detection material from escaping through the injection end from the packaging volume (the test volume) when the plug is pressurized with the test gas, particularly the test pressure. This makes it possible to pressurize the plug with higher test pressures than would be possible without the injection end sealing element.

[0103] In one embodiment, the injection end sealing element comprises a plastic, in particular an elastic plastic, in particular a rubber, in particular a hard rubber, or is formed from a plastic, in particular an elastic plastic, in particular a rubber, in particular a hard rubber. In particular, the injection end sealing element has an insertion sealing section which is designed and arranged to be inserted section by section into an injection opening of the injection end for sealing purposes. In particular, the insertion sealing section is inserted into the injection opening when the injection end sealing element is intended to close, in particular seal, the injection end.

[0104] According to a further development of the invention, the test device has a transparent splinter protection element, wherein the primary packaging material is partially enclosed by the splinter protection element when the primary packaging material is received in the primary packaging receptacle.

[0105] Advantageously, the splinter protection element shields the primary packaging material, in particular the packaging body, from the environment in which the test device is arranged, and in particular, set up. This advantageously prevents people from being injured by a breaking, and in particular shattering, primary packaging material, especially by splinters of the primary packaging material.

[0106] 212221 PCT - KO-HF 2024-02

[0107] 22

[0108] In one embodiment, the primary packaging material is almost completely, in particular without an injection end, or completely, in particular with an injection end, encompassed by the splinter protection element when the primary packaging material is received in the primary packaging receptacle.

[0109] Preferably, the splinter protection element is designed as a splinter protection sleeve in which the primary packaging material is arranged section by section when the primary packaging material is received in the primary packaging receptacle. In particular, the primary packaging material is arranged almost completely, especially without an injection end, or completely, especially with an injection end, in the splinter protection sleeve.

[0110] In one embodiment, the splinter protection element comprises a transparent plastic, in particular a transparent hard plastic or a shatterproof glass material, or is formed from a transparent plastic, in particular a transparent hard plastic, or a shatterproof glass material.

[0111] According to a further development of the invention, the test device comprises a base body. This base body has a pressure interface and a primary packaging interface. A pressure line connects the pressure interface to the primary packaging interface. The pressure interface is also connected to the pressure generation device. The primary packaging interface is configured to be connected to the primary packaging material via a pressure connection. Preferably, the primary packaging material is connected to the primary packaging interface via a pressure connection when the primary packaging material is held in the primary packaging receptacle.

[0112] The device body is advantageously of a particularly simple and compact design, wherein the pressure generating device is securely connected to the primary packaging material, in particular to the pressure chamber, in a pressure-conducting manner when the primary packaging material is received in the primary packaging receptacle.

[0113] In particular, the pressure line and the pressure line path are congruent in sections, especially identical, particularly from the printing interface to the primary packaging interface.

[0114] 212221 PCT - KO-HF 2024-02

[0115] 23

[0116] In one embodiment, the device base body is formed in one piece, particularly of a single material. Specifically, the device base body has a first side and a second side opposite the first side. In particular, the first side has the printing interface and the second side has the primary packaging interface.

[0117] In one embodiment, the primary packaging interface has an insertion section designed and arranged to be inserted into the primary packaging, in particular into the packaging base body, wherein the insertion section is inserted into the primary packaging, in particular into the packaging base body, when the primary packaging is received in the primary packaging receptacle. In particular, the primary packaging interface has a first sealing element arranged between the device base body and the primary packaging, in particular the packaging base body. In particular, the first sealing element is arranged and designed to seal the primary packaging, in particular the packaging base body, and the device base body against each other. This in particular prevents the test gas from unintentionally escaping between the primary packaging, in particular the packaging base body, and the device base body.In particular, the primary packaging interface has a first pressure line opening that leads into the pressure chamber when the primary packaging is received in the primary packaging receptacle. In one embodiment, the pressure interface has a contact section that is designed and arranged so that the pressure generating device can be attached to the contact section, and in particular, the pressure generating device rests against it. The pressure generating device rests against the contact section, especially during a test procedure. The pressure interface also has a second sealing element that is arranged between the device base and the pressure generating device. The second sealing element is designed and arranged to seal the device base and the pressure generating device against each other.In particular, this prevents the test gas from unintentionally escaping between the pressure generating device and the device base. Specifically, the pressure interface has a second pressure line opening that leads into the pressure generating device when the pressure generating device is in contact with the system section. Specifically, the pressure line connects the first pressure line opening to the second pressure line opening in a pressure-conducting manner.

[0118] 212221 PCT - KO-HF 24

[0119] According to a further development of the invention, the device base body has a secondary interface branching off from the pressure line. This secondary interface is connected to the pressure sensor and / or the pressure relief valve via a pressure-conducting connection.

[0120] Advantageously, the pressure sensor and / or the pressure relief valve can be connected to the pressure line in a particularly simple way.

[0121] In one embodiment, the secondary interface branches off from the pressure line between the printing interface and the primary packaging interface.

[0122] In one embodiment, the secondary interface is connected to the pressure sensor and the pressure relief valve via a pressure-conducting connection, wherein the pressure sensor and the pressure relief valve are connected in parallel. Optionally, the safety valve is also connected in parallel if the test device includes a safety valve that is different from the pressure relief valve. The secondary interface has a first interface port and a second interface port. The pressure sensor is connected to the first interface port via a pressure-conducting connection. The pressure relief valve is connected to the second interface port. If the test device includes a safety valve that is different from the pressure relief valve, the secondary interface has a third interface port, wherein the safety valve is connected to the third interface port via a pressure-conducting connection.Advantageously, the test gas can be released manually via the pressure relief valve or automatically via the safety valve from the pressure line path, especially the pressure chamber.

[0123] According to a further development of the invention, the device base body forms at least one element selected from a group consisting of: the pressure interface, the primary packaging interface, the pressure line and the secondary interface.

[0124] The device base is advantageously simple in design. In particular, the device base is formed as a single piece. This ensures ease of handling. Furthermore, the risk of leaks is significantly reduced compared to a device base composed of several individual parts.

[0125] 212221 PCT - KO-HF 25

[0126] Preferably, the device base body forms the pressure interface, the primary packaging interface, the pressure line, and the secondary interface. In particular, the device base body forms the insertion section.

[0127] According to a further development of the invention, the primary packaging receptacle has a first clamping device which is designed and configured to press the primary packaging against the primary packaging interface, so that the primary packaging is pressure-conductingly connected to the primary packaging interface. Alternatively or additionally, the test device has a second clamping device which is designed and configured to press the pressure-generating device, in particular the gas generation device, especially the gas generation cell, against the pressure interface, so that the pressure-generating device is pressure-conductingly connected to the pressure interface.

[0128] The two clamping devices provide a simple and cost-effective way to attach the primary packaging material and the pressure generation device to the test device as intended and to connect them pressure-conductingly to the interface assigned to it as intended.

[0129] In one embodiment, a clamping device, selected from the first clamping device and the second clamping device, is designed and configured to clamp an associated insertion element, selected from the primary packaging material and the pressure-generating device, in particular to clamp it to the test device, especially the device base body. In particular, the clamping device has a clamping element that is configured to be displaced between a clamped position, in which the insertion element is clamped to the test device, and a loose position, in which the insertion element is released, in particular not clamped to the test device. In particular, the first clamping device has a first clamping element, and the second clamping device has a second clamping element.

[0130] In one embodiment, the primary packaging material is pressed against the device base body, in particular against the first sealing element, by means of the first clamping device. In particular, the pressure generating device is pressed against the device base body, in particular against the second sealing element, by means of the second clamping device.

[0131] 212221 PCT - KO-HF 2024-02

[0132] 26

[0133] According to a further development of the invention, the first clamping device comprises two guide elements, two first fastening elements, and a first retaining element. The two guide elements are attached to the device base body on two opposite sides of the primary packaging interface. The first retaining element has a packaging contact section for the primary packaging, which is designed such that the packaging base body abuts the packaging contact section section when the primary packaging is received in the primary packaging receptacle. The first retaining element has two first guide element recesses for the guide elements, which are designed such that the first retaining element can be slid onto the two guide elements by passing one guide element of each of the two guide element recesses through a first guide element recess.In this arrangement, a first fastening element of each of the two first fastening elements is designed and configured to be connected to a guide element of each of the two guide elements in such a way that the first retaining element can be moved towards the device base body by means of the first fastening element. The packaging base body is arranged between the first retaining element and the device base body, so that the primary packaging is pressed against the primary packaging interface and pressure-conductingly connected to the primary packaging interface when the packaging base body is in contact with the packaging system section as intended and the two first fastening elements are connected to the two guide elements as intended.

[0134] The first clamping device is advantageously simple and cost-effective in design. In particular, readily available mechanical components are used for this device. This makes it possible to replace defective components easily, as they are relatively easy to obtain. Furthermore, the test device can be scaled to a certain extent, especially for testing the leak tightness of primary packaging materials of varying sizes.

[0135] In the context of this technical teaching, the fact that the packaging base body is in contact with the packaging system section as intended means in particular that the packaging base body is connected to the base body with its end, especially its injection end.

[0136] 212221 PCT - KO-HF 2024-02

[0137] 27

[0138] The packaging material assembly section is in contact with the primary packaging element when the primary packaging is received in the primary packaging receptacle. In particular, the packaging material assembly section is designed and arranged such that it corresponds to an outer shape of the packaging base body, especially the base body end, particularly the injection end. Specifically, the packaging material assembly section has a negative form of the outer shape of the packaging base body, especially the base body end, particularly the injection end. Advantageously, this ensures that the primary packaging is in particularly secure and reproducible contact with the first retaining element, especially the packaging material assembly section.In particular, the first clamping device is designed to press the packaging base body against the device base body, in particular the primary packaging interface, with a predetermined sealing force, in particular such that the packaging base body and the device base body, in particular the primary packaging interface, are sealed to each other.

[0139] In the context of the present technical teaching, the fact that the two first fastening elements are connected to the two guide elements as intended means in particular that the two first fastening elements are positively connected to the two guide elements and in particular push the first retaining element towards the device base body, in particular exert a force on the first retaining element that acts in the direction of the device base body.

[0140] In one embodiment, a guide element of the two guide elements, in particular both guide elements, is each designed as a threaded rod element. Specifically, the device base body has a threaded bore on each of the two opposite sides of the pressure interface, each bore being designed and configured so that a threaded rod element can be screwed into it. Specifically, a threaded rod element is screwed into each threaded bore. Specifically, a first fastening element of the two first fastening elements, in particular both first fastening elements, is each designed as a threaded nut element, in particular as a knurled screw element.In particular, a threaded rod element of the two threaded rod elements and a threaded nut element of the two threaded nut elements are designed to correspond to each other, so that the threaded nut element can be screwed onto the threaded rod element. In particular, the first retaining element is a first retaining plate 212221 PCT - KO-HF 2024-02.

[0141] 28 formed, in particular the first two guide element recesses are each formed as a first through hole.

[0142] According to a further development of the invention, the first retaining element has a sealing element assembly section for the injection end sealing element, which is designed such that the injection end sealing element rests against the sealing element assembly section when the primary packaging material is received in the primary packaging receptacle. The first retaining element and the first two fastening elements interact in this respect and are configured to press the injection end sealing element against the injection end for sealing.

[0143] Advantageously, the sealing element assembly ensures that the injection end sealing element rests securely and reproducibly against the first retaining element. In particular, the injection end is reliably sealed, and the packaging volume is reliably and reproducibly limited and sealed. For complete limitation and sealing of the packaging volume, the plug must be properly inserted into the packaging body. The sealing element assembly also prevents the primary packaging, especially the packaging body, from tilting when the two first fastening elements are tightened. Furthermore, it ensures that the injection end sealing element rests firmly against the injection end and closes it, sealing it completely.In particular, the sealing element system section is designed and arranged in such a way that it corresponds to the injection end sealing element, in particular to an outer shape of the injection end sealing element.

[0144] Alternatively or additionally, the first retaining element has a protective element mounting section for the splinter protection element, which is designed such that the splinter protection element rests against the protective element mounting section when the primary packaging is received in the primary packaging receptacle. The first retaining element and the first two fastening elements work together and are designed to press the splinter protection element against a splinter protection element mounting surface of the test device. In one embodiment, the second retaining element has the splinter protection element-

[0145] 212221 PCT - KO-HF 2024-02

[0146] 29

[0147] The device base has a mounting surface. In another embodiment, the device base body has the splinter protection element mounting surface.

[0148] Advantageously, the protective element assembly ensures that the splinter protection element rests securely and reproducibly against the first retaining element. This improves the shielding of the environment in which the test device is located, and in particular, where it is set up. It also advantageously prevents injuries to persons from a breaking, especially shattering, primary packaging material, particularly from splinters of the primary packaging material. In particular, the protective element assembly prevents the splinter protection element from tilting when the two first fastening elements are tightened. This ensures, in particular, that the splinter protection element is held securely.

[0149] In one embodiment, the protective element assembly section is designed and arranged in such a way that it corresponds to the splinter protection element, in particular to an outer shape of the splinter protection element.

[0150] According to a further development of the invention, the first clamping device comprises two secondary fastening elements and a secondary retaining element. The secondary retaining element has a recess for the primary packaging material, configured such that the base body of the packaging material can be inserted section by section through the recess until a collar of the base body abuts a stop on the secondary retaining element and blocks further insertion. The secondary retaining element also has two secondary guide element recesses for the guide elements, configured such that the secondary retaining element can be slid onto the two guide elements by inserting one guide element of each of the two guide elements through a secondary guide element recess of the second guide element recess.Each of the two second fastening elements has a second fastening element designed and configured to be connected to a guide element of each of the two guide elements, in order to press the second holding element towards the device base body by means of the second fastening element. The collar is positioned between the second holding element and the device base body, so that the collar rests against the device base body.

[0151] 212221 PCT - KO-HF 2024-02

[0152] 30 is compressed when the primary packaging material is passed through the packaging material recess as intended and the two second fastening elements are connected to the two guide elements as intended.

[0153] Advantageously, the primary packaging is better supported by improved storage on the test fixture, particularly on the fixture base. This ensures that the collar of the packaging base is pressed particularly reliably and firmly against the fixture base, especially against the primary packaging interface, and particularly against the first seal. This seals the primary packaging, especially the packaging base, and the primary packaging interface, especially the pressure line, against each other.

[0154] In the context of the present technical teaching, the fact that the primary packaging material is passed through the packaging recess as intended means in particular that the packaging base body with the injection end is passed through the packaging recess to such an extent that the collar of the packaging base body abuts the stop of the second retaining element and blocks further passage.

[0155] In the context of the present technical teaching, the fact that the two second fastening elements are connected to the two guide elements as intended means in particular that the two second fastening elements are positively connected to the two guide elements and in particular push the second retaining element towards the device base body, in particular exert a force on the second retaining element that acts in the direction of the device base body.

[0156] In one embodiment, a second fastening element of the two second fastening elements, in particular both second fastening elements, is each designed as a threaded nut element, in particular as a knurled screw element. In particular, a threaded rod element of the two threaded rod elements and a threaded nut element of the two threaded nut elements are configured to correspond to each other, so that the threaded nut element can be screwed onto the threaded rod element. In particular, the second retaining element is designed as a second retaining plate, wherein in particular the two second guide element recesses are each configured as a second through-hole.

[0157] 212221 PCT - KO-HF 2024-02

[0158] 31

[0159] According to a further development of the invention, the second clamping device comprises two guide fastening elements and a third retaining element. The third retaining element rests against the pressure-generating device on a side facing away from the device base. The two guide fastening elements each connect the third retaining element to a counter-retaining element, selected from the first retaining element, the second retaining element, and a fourth retaining element, the fourth retaining element resting against a side of the device base facing away from the pressure-generating device. The two guide fastening elements, the third retaining element, and the counter-retaining element are designed and configured to change the distance between the third retaining element and the counter-retaining element such that the pressure-generating device is pressed against the pressure interface by the third retaining element.

[0160] The second clamping device is advantageously simple and cost-effective in design. In particular, readily available mechanical components are used for this second clamping device. This makes it possible to replace defective mechanical components without significant effort, as these are relatively easy to obtain. Furthermore, the test device can be scaled to a certain extent, especially to accommodate pressure generation devices, particularly gas generation devices, of varying sizes for supplying, and especially generating, the test gas.

[0161] In one embodiment, a guide fastening element of the two guide fastening elements, in particular both guide fastening elements, is each designed as a second threaded rod element. In particular, the third retaining element is designed as a third retaining plate. In particular, the third retaining element has a pressure generation device assembly section that is designed and configured to bear against the pressure generation device. In particular, the

[0162] The pressure generating device assembly section is designed in a ring-shaped, circular, or annular form. In particular, the pressure generating device assembly section has a pressure ram element designed and arranged to be pressed against the pressure generating device and thus press the pressure generating device against the device base body. In particular, the third retaining element has, on the two opposite sides of the pressure generating device assembly section 212221 PCT - KO-HF 2024-02

[0163] 32 each has a second threaded bore, each designed and configured so that a second threaded rod element can be screwed into the second threaded bore. In particular, a second threaded rod element is screwed into a second threaded bore in each case. In particular, the counter-holding element has two third threaded bores, each designed and configured so that the second threaded rod element can be screwed into the third threaded bore in each case. In particular, a second threaded rod element is screwed into the third threaded bore in each case.

[0164] In one embodiment – ​​where the fourth retaining element is selected as the counter-retaining element – ​​the fourth retaining element has a clamping section designed and arranged to abut the device base body, the first retaining element, or the second retaining element. In particular, the fourth retaining element has two third threaded bores on each of the two opposite sides of the clamping section, each designed and configured so that the second threaded rod element can be screwed into the third threaded bore.

[0165] In one embodiment, a retaining element, selected from the first retaining element, the second retaining element, the third retaining element, and the fourth retaining element, comprises or is formed from a plastic. In particular, the retaining element comprises or is formed from a composite material. In particular, the retaining element comprises a reinforcing element, especially a reinforcing core.

[0166] In one embodiment, the fourth retaining element rests directly against the device base. In another embodiment, the fourth retaining element rests indirectly against the device base by means of the second retaining element and / or the second fastening elements. In yet another embodiment, the fourth retaining element rests directly against the first retaining element. In still another embodiment, the fourth retaining element rests against the first fastening elements.

[0167] In one embodiment, the test device includes a control device configured and set up to perform the test procedure. In particular, the control device is configured and set up to perform the test procedure described below. In one embodiment, the control device is connected to the pressure generating device and / or the pressure sensor, in particular via data transmission, in particular 212221 PCT - KO-HF 2024-02

[0168] 33. Control-connected. In particular, the test device has a display device which is designed and configured to display information to a user. In one embodiment, the information includes at least one value selected from a group consisting of: an instantaneous pressure, in particular a test pressure, a target test pressure, an actual test pressure, a voltage, in particular a gas generation device, a current, in particular a gas generation device, a resistance, in particular a gas generation device, and a duration, in particular a test pressure build-up time and a test pressure duration. In particular, the display device is data-connected to the control device and configured to display the at least one value.

[0169] In one embodiment, the test device has an input device that is connected to the control device, in particular via data transmission and control interaction. Specifically, the input device makes it possible to execute the test process in response to user input via the control device.

[0170] In one embodiment, the test device has an outer housing. In particular, the outer housing has a housing opening that is designed and configured to be selectively opened and closed.In particular, at least one component is arranged in the outer housing, which is selected from a group consisting of: the primary packaging receptacle, the pressure generating device, in particular the gas generation device, in particular the gas generation cell, the at least one gas detection material, the primary packaging, in particular the packaging base body and the plug, the pressure sensor, the pressure relief valve, in particular the safety valve, the injection end sealing element, the splinter protection element, the device base body, in particular its pressure interface and / or its primary packaging interface and / or its secondary interface, the first clamping device, the second clamping device, the control device, and the display device.

[0171] The task is also solved by creating a test procedure for verifying the tightness of a plug in a packaging base body, which together define the packaging volume of a primary packaging. The test procedure comprises the following steps: arranging a gas detection material on at least one part of the packaging volume.

[0172] 212221 PCT - KO-HF 2024-02

[0173] 34. The side of a sealing section of the plug facing away from the packaging volume is tested, wherein the gas detection material is configured such that at least one optical property of the gas detection material changes in the presence of a test gas. The plug is pressurized with the test gas on at least one side facing away from the packaging volume. A change in the at least one optical property of the gas detection material is then checked. The test method offers the advantages already explained in connection with the test device. In particular, the aforementioned steps take place in precisely this sequence.

[0174] In one embodiment, the test method additionally comprises the step of inserting the plug to be tested into the packaging body so that the packaging body, together with the packaging body, defines the test volume containing the gas detection material, in particular the packaging volume test volume and / or the sealing section test volume. This step is specifically performed as the first step. In particular, the plug is inserted so far into the packaging volume that it comes into contact with the gas detection material, in particular resting on the gas detection material if it is arranged within the packaging volume, or that the plug rests on the support element.

[0175] In one embodiment, the test method additionally includes the step of inferring a tightness between the plug and the packaging base body based on a change in the optical properties of the gas detection material. In particular, this step is performed as the last step, especially after the aforementioned steps.

[0176] In one embodiment, the change in at least one property of the gas detection material is checked by monitoring the color change of the gas detection material.

[0177] According to a further development of the invention, the plug is subjected to the test pressure by means of the test gas for a predetermined test duration, in particular the test pressure duration.

[0178] It is advantageous to be able to precisely detect at which test pressure and test duration at least one optical property of the gas detection material changes for a specific test configuration. In particular, it is thus possible to precisely detect at which test pressure and test duration a test gas leak occurs, specifically when the test gas flows into the test volume, particularly into the packaging volume and / or between two sealing sections, and specifically when the seal of the plug in a specific test configuration is no longer tight.

[0179] In one embodiment, the test duration comprises the test pressure build-up time and the test pressure exposure time. The test pressure build-up time is, in particular, the time required to increase the instantaneous test pressure—especially the actual test pressure—from the ambient pressure to a predetermined target test pressure. The test pressure exposure time is, in particular, the time during which the plug is exposed to the test gas, which has an actual test pressure corresponding to the predetermined target test pressure.

[0180] In one embodiment, the test pressure build-up time, particularly during the generation of the test gas by means of the gas generation device, especially the gas generation cell, is from 35 to 55 minutes, more specifically from 40 to 50 minutes, and more specifically from 43 to 45 minutes. In particular, a test pressure of 0.4 MPa to 0.6 MPa, and more specifically 0.5 MPa, is generated. In particular, the gas generation device, especially the gas generation cell, is operated with a voltage of U = 2.4 V, a resistance of R = 100 ohms, and a current of I = 45 mA.In another embodiment, if the test gas is provided by means of a stationary gas storage device or a mobile gas storage device, the test gas is provided significantly faster, especially if the test gas is stored at the test gas storage pressure, which can be reduced relatively quickly to the test pressure, in particular the target test pressure, by means of the pressure reducing device.

[0181] In one embodiment, the test pressure duration is longer than a possible injection duration for a subsequent injection of the pharmaceutical substance stored in the same or a similar primary packaging. In particular, it is possible to determine a safe injection duration at a specific injection pressure based on the time of change in the optical properties of the gas detection material and the test pressure acting on the stopper during a subsequent injection of the pharmaceutical substance stored in the same or a similar primary packaging. Specifically, the test pressure duration corresponds to the subsequently intended injection duration multiplied by...

[0182] 212221 PCT - KO-HF 2024-02

[0183] 36 with a factor of 2 to 4, in particular 2.5 to 3.5, in particular 3. In one embodiment, the test pressure duration is from 15 seconds to 45 seconds, in particular from 20 seconds to 40 seconds, in particular from 25 seconds to 35 seconds, in particular 30 seconds.

[0184] In one embodiment, the test pressure, in particular the actual test pressure, is at least 0.1 MPa, in particular at least 0.2 MPa, in particular at least 0.4 MPa, in particular at least 0.6 MPa, in particular at least 0.7 MPa, in particular at least 0.9 MPa, and in particular at most 1 MPa. In particular, an instantaneous pressure acting on the plug, especially starting from the ambient pressure, is increased to the test pressure, in particular the target test pressure. In one embodiment, the test pressure, in particular the actual test pressure, is kept constant during the test period. In another embodiment, the test pressure, in particular the actual test pressure, is increased or decreased at least once during the test period.

[0185] According to a further development of the invention, the testing method is carried out using a testing device according to the invention or a testing device according to one or more of the embodiments described above. The advantages already explained above are particularly advantageously realized in this way.

[0186] The embodiments described and statements made in connection with the test device according to the invention also relate, mutatis mutandis, to the test method according to the invention and vice versa.

[0187] The problem is also solved by using a gas detection material, configured such that at least one optical property of the gas detection material changes in the presence of a test gas, to test the tightness of a plug in a packaging base. The advantages of this use are particularly evident in the context of the test device and the test method already explained.

[0188] The embodiments described and statements made in connection with the test device and the test method according to the invention also relate, mutatis mutandis, to the use according to the invention and vice versa.

[0189] 212221 PCT - KO-HF 2024-02

[0190] 37

[0191] According to a further development of the invention, the gas detection material comprises supraparticles consisting of a particle superstructure made up of nanoparticles and substances embedded in the particle superstructure. The nanoparticles are selected from a group consisting of SiCE nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof. The substances embedded in the particle superstructure contain at least one catalytically active substance for catalyzing hydrogen dissociation and at least one redox dye.

[0192] The invention will be explained in more detail below with reference to the drawing. The drawing shows:

[0193] Figure 1 shows a schematic first representation of an embodiment of a test device for testing the tightness of a plug in a packaging base body,

[0194] Figure 2 shows a schematic second representation of the embodiment of the test device from Figure 1.

[0195] Figure 3 shows a schematic third representation of the embodiment of the test device from Figure 1.

[0196] Figure 4 shows a schematic first representation of a gas generation device of the test device of Figure 1.

[0197] Figure 5 shows a schematic representation of gas development cells of the gas development device of Figure 4.

[0198] Figure 6 shows a schematic representation of a process flow diagram of a test procedure for testing the tightness of a plug in a packaging base body, and

[0199] Figure 7 shows a schematic representation of the plug that is inserted into the packaging base body.

[0200] Fig. 1 shows a schematic first representation of an embodiment of a test device 1 for testing the tightness of a plug 3 in a packaging base body 5, which together limit a packaging volume 15.

[0201] The test device 1 comprises a primary packaging receptacle 7, a pressure generation device 9, and at least one gas detection material 11.

[0202] 212221 PCT - KO-HF 2024-02

[0203] 38

[0204] The primary packaging receptacle 7 is designed and configured to receive a primary packaging element 13 to be tested, which comprises the packaging base body 5 and the plug 3. The pressure generation device 9 is configured to apply a test pressure, in particular a time-dependent test pressure profile, to the plug 3 on at least one side 17.1 facing away from the packaging volume 15 by means of a test gas when the primary packaging element 13 is received in the primary packaging receptacle 7. The at least one gas detection material 11 is configured such that at least one optical property of the at least one gas detection material 11 changes in the presence of the test gas. Here, the at least one gas detection material 11 is located on at least one side 17.2 of a sealing section 2 of the plug 3 facing the packaging volume 15 (see Figure 7), in this case within the packaging volume 15 as test volume 4, in particular as packaging volume-test volume 4.1, arranged when the primary packaging material 13 is received in the primary packaging receptacle 7. It is also possible that the at least one gas detection material 11 is arranged between two sealing sections 2, in particular sealing lamellae, in a sealing section test volume 4.2, cf. Figure 7.

[0205] The gas detection material 11 is configured such that at least one optical property changes reversibly depending on the concentration of the test gas. The gas detection material 11 comprises supraparticles consisting of a particle superstructure made up of nanoparticles and substances embedded within this superstructure. The nanoparticles are selected from a group consisting of SiO₂ nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof. The substances embedded within the particle superstructure contain at least one catalytically active substance for catalyzing hydrogen dissociation and at least one redox dye.

[0206] The pressure generating device 9 is designed and configured as a gas generation device 19, which has several gas generation cells 25, to generate hydrogen as the test gas.

[0207] The primary packaging receptacle 7 has a first clamping device 21.1, which is designed and configured to press the primary packaging 13 against a primary packaging interface 23 (see Figure 2) so that the primary packaging 13 is pressure-conductingly connected to the primary packaging interface 23. Additionally, the test device 1 has a second

[0208] 212221 PCT - KO-HF 2024-02

[0209] 39

[0210] Clamping device 21.2, which is designed and configured to press the pressure generating device 9, in particular the gas generating device 19, against a pressure interface 27 (see Figure 2), so that the pressure generating device 9 is connected to the pressure interface 27 in a pressure-conducting manner.

[0211] The first clamping device 21.1 has two guide elements 29, two first fastening elements 31.1, and a first retaining element 33.1. The two guide elements 29 are attached to a device base body 35 on two opposite sides of the primary packaging interface 23. The first retaining element 33.1 has a packaging contact section 37 (see Figure 2) for the primary packaging 13, which is designed such that the packaging base body 5 abuts the packaging contact section 37 section by section when the primary packaging 13 is received in the primary packaging receptacle 7. Here, the first retaining element 33.1 has two first guide element recesses 39.1 (see Figure 2) for the guide elements 29, which are designed such that the first retaining element 33.1 can be pushed onto the two guide elements 29 by passing one guide element 29 of the two guide elements 29 through a first guide element recess 39.1 of the two first guide element recesses 39.1 is passed through. A first fastening element 31.1 of each of the two first fastening elements 31.1 is formed and configured to be connected to a guide element 29 of each of the two guide elements 29 such that the first retaining element 33.1 can be moved towards the device base body 35 by means of the first fastening element 31.1. The packaging base body 5 is arranged between the first retaining element 33.1 and the device base body 35, so that the primary packaging 13 is pressed against the primary packaging interface 23 and is pressure-conductingly connected to the primary packaging interface 23 when the packaging base body 5 is in intended position against the packaging system section 37 and the two first fastening elements 31.1 are in intended position to be connected to the two guide elements 29.

[0212] The first clamping device 21.1 further comprises two second fastening elements 31.2 and a second retaining element 33.2. The second retaining element 33.2 has a packaging recess 41 (see Figure 2) for the primary packaging 13, which is designed such that the packaging base body 5 can be passed through the packaging recess 41 212221 PCT - KO-HF 40 section by section until a collar 43 (see Figure 2) of the packaging base body 5 abuts a stop 45 of the second retaining element 33.2 and blocks further passage. Here, the second retaining element 33.2 has two second guide element recesses 39.2 for the guide elements 29, which are designed such that the second retaining element 33.2 can be pushed onto the two guide elements 29 by passing one guide element 29 of the two guide elements 29 through a second guide element recess 39.2 of the two second guide element recesses 39.2.Each of the two second fastening elements 31.2 is designed and configured to be connected to a guide element 29 of the two guide elements 29, in order to press the second retaining element 33.2 towards the device base body 35 by means of the second fastening element 31.2. The collar 43 is arranged between the second retaining element 33.2 and the device base body 35, such that the collar 43 is pressed against the device base body 35 when the primary packaging material 13 is passed through the packaging material recess 41 as intended and the two second fastening elements 31.2 are connected to the two guide elements 29 as intended.

[0213] The second clamping device 21.2 has two guide fastening elements 47 and a third retaining element 33.3. The third retaining element 33.3 rests against the pressure generating device 9 on a side 17.3 facing away from the device base body 35. The two guide fastening elements 47 each connect the third retaining element 33.3 and a fourth retaining element 33.4 as a counter-retaining element 34, with the fourth retaining element 33.4 resting against a side 17.4 of the device base body 35 facing away from the pressure generating device 9 – indirectly by means of the second fastening elements 31.2 and the second retaining element 33.2. The two guide fastening elements 47, the third retaining element 33.3 and the counter-retaining element 34 are designed and configured to change the distance between the third retaining element 33.3 and the counter-retaining element 34 such that the pressure generating device 9 is held by the third retaining element 33.3 is pushed against the print interface 27.

[0214] 212221 PCT - KO-HF 41

[0215] The test device 1 includes a display device 28, which is configured to display information to a user. The test device 1 can also be arranged in an outer housing, which is not shown here.

[0216] Fig. 2 shows a schematic second representation of the embodiment of the test device 1 of Figure 1 in an exploded view, in particular in a disassembled, especially dismantled state, wherein the second clamping device 21.2 is not shown.

[0217] Identical and functionally equivalent elements are provided with the same reference symbols in all figures, so that reference is made to the preceding description in each case.

[0218] The test device 1 has an injection end sealing element 49 for closing, in particular sealing, an injection end 51 of the primary packaging material 13. The injection end sealing element 49 rests against the injection end 51 and closes the injection end 51, in particular sealing it, when the primary packaging material 13 is received in the primary packaging material receptacle 7.

[0219] The test device 1 has a transparent splinter protection element 53, wherein the primary packaging material 13 is partially enclosed by the splinter protection element 53 when the primary packaging material 13 is received in the primary packaging receptacle 7.

[0220] The test device 1 comprises the device base body 35. The device base body 35 has the pressure interface 27 and the primary packaging interface 23. A pressure line 55, shown in dashed lines, connects the pressure interface 27 to the primary packaging interface 23 in a pressure-conducting manner. The pressure interface 27 is also pressure-conductingly connected to the pressure generation device 9. The primary packaging interface 23 is configured to be pressure-conductingly connected to the primary packaging 13. Preferably, the primary packaging 13 is pressure-conductingly connected to the primary packaging interface 23 when the primary packaging 13 is received in the primary packaging receptacle 7. In particular, the primary packaging interface 23 has a first sealing element 24, especially an O-ring, which is arranged between the device base body 35 and the packaging base body 5.

[0221] 212221 PCT - KO-HF 2024-02

[0222] 42 is designed to seal the primary packaging material 13, in particular the packaging material base body 5, and the device base body 35 to each other.

[0223] The device base body 35 has a secondary interface 57 branching off from the pressure line 55. The secondary interface 57 is connected to a pressure sensor 59 and to a pressure relief valve 61 via a pressure-conducting connection (see Figure 3).

[0224] The device base body 35 forms the printing interface 27 in this case, which

[0225] Primary packaging interface 23, pressure line 55 and secondary interface 57.

[0226] The first retaining element 33.1 has a sealing element section 63 for the injection end sealing element 49, which is designed such that the injection end sealing element 49 rests against the sealing element section 63 when the primary packaging 13 is received in the primary packaging receptacle 7. The first retaining element 33.1 and the first two fastening elements 31.1 work together and are designed to press the injection end sealing element 49 against the injection end 51 for sealing.

[0227] The first retaining element 33.1 has a protective element mounting section 64 for the splinter protection element 53, which is designed such that the splinter protection element 53 rests against the protective element mounting section 64 when the primary packaging material 13 is received in the primary packaging material receptacle 7. The first retaining element 33.1 and the first two fastening elements 31.1 work together and are designed to press the splinter protection element 53 against a splinter protection element mounting surface 66 of the test device 1. In this case, the second retaining element has the splinter protection element mounting surface 66.

[0228] Fig. 3 shows a schematic third representation of the embodiment of the test device 1 from Figure 1 in a view rotated about a vertical axis compared to Figure 2, with the second clamping device 21.2 not shown. Furthermore, the primary packaging material 13 and the gas detection material 11 are not shown.

[0229] The test device 1 includes the pressure sensor 59, which is arranged and configured to detect the test pressure. The test device 1 also includes the pressure relief valve 61, which

[0230] 212221 PCT - KO-HF 2024-02

[0231] 43 is configured to release the test gas. The test device 1 further includes a safety valve 65, which is designed and configured to release the test gas when a predetermined pressure threshold is reached. In this case, the pressure release valve 61 and the safety valve 65 are different valves. It is also possible that the pressure release valve 61 and the safety valve 65 are the same valve.

[0232] Fig. 4 shows a schematic first representation of the gas generation device 19 of the test device 1 of Figure 1 in a disassembled, in particular dismantled, state.

[0233] The gas generation device 19 has a housing 67 in which several gas generation cells 25 are arranged. Furthermore, the gas generation device 19 has an adjustable resistor 69, which in this case is designed as a potentiometer. The gas generation cells 25 are each designed and configured to generate the test gas.

[0234] The gas generation device 19 further comprises two electrical contacts 70, which are configured to be connected to an external voltage source (not shown). This allows a uniform test gas generation rate to be set.

[0235] Fig. 5 shows a schematic representation of the gas generation cells 25 of the gas generation device 19 from Fig. 4. The gas generation cells 25 are shown removed from the device housing 67, which is not shown. The adjustable resistor 69 is also not shown.

[0236] The gas generation cells 25 are designed as button cells, arranged one behind the other and connected in series. Each gas generation cell 25 has an anode 71 on a first side 18.1 and a cathode 73 on a second side 18.2 opposite the first side 18.1. Except for one outwardly facing anode 71 and one outwardly facing cathode 73, each anode 71 on a first side 18.1 is in contact with a cathode 73 on a second side 18.2, thus realizing the series connection.

[0237] Fig. 6 shows a schematic representation of a process flow diagram of a test procedure for testing the tightness of a plug 3 in a packaging base body 5, which together

[0238] 212221 PCT - KO-HF 2024-02

[0239] 44 limit the packaging volume 15 of the primary packaging 13. The following test procedure is preferably carried out using a test device 1 according to Figures 1 to 3.

[0240] The test procedure comprises the following steps: First step Sl : Arranging a gas detection material 11 on at least one side 17.2 of a sealing section 2 of the plug 3 facing the packaging volume 15, wherein the gas detection material 11 is arranged such that at least one optical property of the gas detection material 11 changes in the presence of a test gas.

[0241] Second step S2: Applying the test gas to the plug 3 on at least one side 17.1 facing away from the packaging volume 15 at a test pressure.

[0242] Third step S3: Check for a change in at least one optical property of the gas detection material 11.

[0243] The test procedure in this case additionally includes the optional steps shown in dashed lines:

[0244] Zeroth step SO – temporally prior to the first step Sl: Insertion of the plug 3 to be tested into the packaging base body 5, such that it, together with the packaging base body 5, delimits the test volume 4 containing the gas detection material 11, in particular the packaging volume test volume 4.1 and / or the sealing section test volume 4.2. In particular, this step takes place as the first step. In particular, optionally, the plug 3 is inserted so far into the packaging volume 15 that it comes into contact with the gas detection material 11, in particular, rests on the gas detection material 11 if this is arranged in the packaging volume 15 as packaging volume test volume 4.1, or the plug 3 rests on a support element (not shown).

[0245] Fourth step S4 - occurring after the third step S3: Conclusion regarding a tightness between the plug 3 and the packaging base body 5 depending on a change in the optical properties of the gas detection material 11. In particular, this step takes place as the last step.

[0246] In particular, the steps are carried out in the following order: zeroth step SO, first step Sl, second step S2, third step S3, fourth step S4.

[0247] 212221 PCT - KO-HF 2024-02

[0248] 45

[0249] By carrying out the present test procedure, the gas detection material 11, which is configured such that at least one optical property of the gas detection material 11 changes in the presence of the test gas, is used to test the tightness of the plug 3 in the packaging body 5. The gas detection material 11 optionally comprises supraparticles consisting of a particle superstructure made up of nanoparticles and substances embedded in the particle superstructure. The nanoparticles are selected from a group consisting of SiO2 nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof. The substances embedded in the particle superstructure contain at least one catalytically active substance for catalyzing hydrogen dissociation and at least one redox dye.

[0250] Figure 7 shows a schematic representation of a plug 3 which is inserted into the packaging base body 5, which is only shown in sections.

[0251] The plug 3 has several sealing sections 2, including a first sealing section 2.1, a second sealing section 2.2, and a third sealing section 2.3. The first sealing section test volume 4.2.1 is located between the first sealing section 2.1 and the second sealing section 2.2 and is delimited by the plug 3 together with the packaging base body 5. The second sealing section test volume 4.2.2 is located between the second sealing section 2.2 and the third sealing section 2.3 and is delimited by the plug 3 together with the packaging base body 5.

[0252] A sealing section 2, selected from the first sealing section 2.1, the second sealing section 2.2 and the third sealing section 2.3, has in particular a side 17.2 facing the packaging volume 15 and a side 17.1 facing away from the packaging volume 15. In particular, the plug 5 itself also has, in particular additionally, a side 17.2 facing the packaging volume 15 and a side 17.1 facing away from the packaging volume 15.

[0253] The packaging volume 15 is also shown as packaging volume test volume 4.1. The at least one gas detection material 11 – not shown here – can be arranged in at least one, in particular in at least two, in particular in three, test volumes 4, selected from the packaging volume test volume 4.1, the first sealing section test volume 4.2.1 and the second sealing section test volume 4.2.2. In the embodiment of 212221 PCT - KO-HF 2024-02

[0254] 46

[0255] Figures 1 to 3 show that at least one gas detection material 11 is arranged in the packaging volume test volume 4.1.

[0256] 212221 PCT - KO-HF

Claims

2024-02 47 REQUIREMENTS 1. Test device (1) for testing the tightness of a plug (3) in a packaging base body (5), which together define a packaging volume (15) of a primary packaging (13), comprising: - a primary packaging receptacle (7) designed and equipped to receive a primary packaging (13) to be tested, comprising the packaging body (5) and the plug (3); - a pressure generating device (9) which is configured to apply a test pressure to the plug (3) on at least one side (17.1) facing away from the packaging volume (15) by means of a test gas when the primary packaging (13) is received in the primary packaging receptacle (7), and - at least one gas detection material (11) which is arranged such that at least one optical property of the at least one gas detection material (11) changes in the presence of the test gas, wherein the at least one gas detection material (11) is arranged on at least one side (17.2) of a sealing section (2) of the plug (3) facing the packaging volume (15) when the primary packaging (13) is received in the primary packaging receptacle (7).

2. Test device (1) according to claim 1, wherein the gas detection material (11) is arranged such that the at least one optical property changes reversibly depending on a concentration of the test gas.

3. Test apparatus (1) according to one of the preceding claims, wherein the gas detection material (11) comprises supraparticles comprising a particle superstructure consisting of nanoparticles and substances embedded in the particle superstructure, wherein the nanoparticles are selected from a group consisting of SiCE nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof, and wherein the substances embedded in the particle superstructure include at least one catalytically active substance for catalyzing a dissociation of hydrogen and at least one redox dye. 212221 PCT - KO-HF 2024-02 48 4. Test apparatus (1) according to one of the preceding claims, wherein the pressure generating device (9) comprises a gas generation device (19), in particular a gas generation cell (25), which is designed and configured to generate the test gas.

5. Test apparatus (1) according to claim 4, wherein the gas generation device (19), in particular the gas generation cell (25), is designed and configured to generate hydrogen as the test gas.

6. Test device (1) according to one of the preceding claims, comprising a pressure sensor (59), wherein the pressure sensor (59) is arranged and configured to detect the test pressure.

7. Test device (1) according to one of the preceding claims, comprising a pressure relief valve (61), wherein the pressure relief valve (61) is configured to release the test gas.

8. Test device (1) according to one of the preceding claims, comprising an injection end sealing element (49) for closing an injection end (51) of the primary packaging material (13), wherein the injection end sealing element (49) rests against the injection end (51) and closes the injection end (51) when the primary packaging material (13) is received in the primary packaging material receptacle (7).

9. Test device (1) according to one of the preceding claims, comprising a transparent splinter protection element (53), wherein - the primary packaging material (13) is partially enclosed by the splinter protection element (53) when the primary packaging material (13) is received in the primary packaging material receptacle (7), preferably - the splinter protection element (53) is designed as a splinter protection sleeve in which the primary packaging material (13) is arranged section by section when the primary packaging material (13) is received in the primary packaging material receptacle (7).

10. Test device (1) according to one of the preceding claims, comprising a device base body (35), wherein 212221 PCT - KO-HF 2024-02 49 - the device body (35) has a pressure interface (27) and a primary packaging interface (23), wherein a pressure line (55) connects the pressure interface (27) to the primary packaging interface (23) in a pressure-conducting manner, wherein - the printing interface (27) is connected to the printing device (9) in a pressure-conducting manner, wherein - the primary packaging interface (23) is set up to be pressure-conductingly connected to the primary packaging (13), wherein preferably the primary packaging (13) is pressure-conductingly connected to the primary packaging interface (23) when the primary packaging (13) is received in the primary packaging receptacle (7).

11. Test device (1) according to claim 10, wherein the device base body (35) has a secondary interface (57) branching off from the pressure line (55), wherein - the secondary interface (57) is connected to the pressure sensor (59) and / or to the pressure relief valve (61) in a pressure-conducting manner.

12. Test device (1) according to claim 10 or 11, wherein the device body (35) forms at least one element selected from a group consisting of: the print interface (27), the primary packaging interface (23), the print line (55) and the secondary interface (57).

13. Test device (1) according to one of claims 10 to 12, wherein - the primary packaging receptacle (7) has a first clamping device (21.1) which is designed and configured to press the primary packaging (13) against the primary packaging interface (23) so that the primary packaging (13) is pressure-conductingly connected to the primary packaging interface (23), and / or - the test device (1) has a second clamping device (21.2) which is designed and configured to press the pressure generating device (9), in particular the gas generating device (19), against the pressure interface (27) so that the pressure generating device (9) is connected to the pressure interface (27) in a pressure-conducting manner. 212221 PCT - KO-HF 2024-02 50 14. Test device (1) according to claim 13, wherein the first clamping device (21.1) comprises two guide elements (29), two first fastening elements (31.1) and a first retaining element (33.1) exhibits, wherein - the two guide elements (29) are attached to the device base body (35) on two opposite sides of the printing interface (27), wherein - the first retaining element (33.1) has a packaging material attachment section (37) for the primary packaging material (13) which is designed such that the packaging material base body (5) abuts the packaging material attachment section (37) section by section when the primary packaging material (13) is received in the primary packaging material receptacle (7), - the first retaining element (33.1) has two first guide element recesses (39.1) for the guide elements (29) which are designed such that the first retaining element (33.1) can be pushed onto the two guide elements (29) by each guide element (29) of the two guide elements (29) through a first guide element recess (39.1) of the two first guide element recesses (39.1) is carried through, whereby - each of the first fastening elements (31.1) of the two first fastening elements (31.1) is designed and equipped to be connected to one of the two guide elements (29) such that the first retaining element (33.1) can be moved towards the device base body (35) by means of the first fastening element (31.1), wherein - the packaging base body (5) is arranged between the first retaining element (33.1) and the device base body (35) so that the primary packaging (13) is pressed against the primary packaging interface (23) and is pressure-conductingly connected to the primary packaging interface (23) when the packaging base body (5) is in contact with the packaging system section (37) as intended and the two first fastening elements (31.1) are connected as intended to the two guide elements (29).

15. Test device (1) according to claim 14, wherein - the first retaining element (33.1) has a sealing element assembly section (63) for the injection end sealing element (49), which is designed such that the 212221 PCT - KO-HF 2024-02 51 The injection end sealing element (49) rests against the sealing element assembly section (63) when the primary packaging (13) is received in the primary packaging receptacle (7), wherein the first retaining element (33.1) and the first two fastening elements (31.1) interact and are configured to force the injection end sealing element (49) against the injection end (51) for closure, and / or wherein - the first retaining element (33.1) has a protective element assembly section (64) for the splinter protection element (53) which is designed such that the splinter protection element (53) rests against the protective element assembly section (64) when the primary packaging material (13) is received in the primary packaging material receptacle (7), wherein the first retaining element (33.1) and the two first fastening elements (31.1) cooperate and are arranged to press the splinter protection element (53) against a splinter protection element contact surface (66) of the test device (1).

16. Test device (1) according to claim 14 or 15, wherein the first clamping device (21.1) has two second fastening elements (31.2) and a second retaining element (33.2), wherein - the second retaining element (33.2) a packaging recess (41) for the primary packaging (13) which is designed such that the The packaging base body (5) can be passed section by section through the packaging recess (41) until a collar (43) of the packaging base body (5) abuts a stop (45) of the second retaining element (33.2) and blocks further passage, wherein - the second retaining element (33.2) has two second guide element recesses (39.2) for the guide elements (29), which are designed such that the second retaining element (33.2) can be pushed onto the two guide elements (29) by passing one guide element (29) of the two guide elements (29) through a second guide element recess (39.2) of the two second guide element recesses (39.2), wherein - each of the two second fastening elements (31.2) is formed and configured to be connected to each of the two guide elements (29) in order to push the second retaining element (33.2) towards the device base body (35) by means of the second fastening element (31.2), wherein 212221 PCT - KO-HF 2024-02 52 - the second retaining element (33.2) is arranged between the first retaining element (33.1) and the device base body (35), wherein - the collar (43) is arranged between the second retaining element (33.2) and the device base body (35) so that the collar (43) is pressed against the device base body (35) when the primary packaging material (13) is passed through the packaging material recess (41) as intended and the two second fastening elements (31.2) are connected to the two guide elements (29) as intended.

17. Test device (1) according to one of claims 13 to 16, wherein the second clamping device (21.2) has two guide fastening elements (47) and a third retaining element (33.3), wherein - the third retaining element (33.3) rests on the pressure generating device (9) on a side (17.3) facing away from the device base body (35), wherein - the two guide fastening elements (47) each connect the third retaining element (33.3) and a counter-retaining element (34), selected from the first retaining element (33.1), the second retaining element (33.2) and a fourth retaining element (33.4), wherein the fourth retaining element (33.4) rests against a side (17.4) of the device base body (35) facing away from the pressure generating device (9), wherein - the two guide fastening elements (47), the third retaining element (33.3) and the counter-retaining element (34) are designed and configured to change the distance between the third retaining element (33.3) and the counter-retaining element (34) such that the pressure generating device (9) is forced against the pressure interface (27) by the third retaining element (33.3).

18. Test method for testing the tightness of a plug (3) in a packaging body (5) which together limit a packaging volume (15) of a primary packaging (13), comprising: - Arranging a gas detection material (11) on at least one side (17.2) of a sealing section (2) of the plug (3) facing the packaging volume (15), wherein the 212221 PCT - KO-HF 2024-02 53 The gas detection material (11) is configured such that at least one optical property of the gas detection material (11) changes in the presence of a test gas; - Applying the test gas to the plug (3) on at least one side (17.1) facing away from the packaging volume (15) at a test pressure; - Check for a change in at least one optical property of the gas detection material (11).

19. Test method according to claim 18, wherein the plug (3) is subjected to the test pressure by means of the test gas for a predetermined test duration.

20. Test method according to claim 18 or 19, wherein the test method is carried out using a test device (1) according to any one of claims 1 to 17.

21. Use of a gas detection material (11) configured such that at least one optical property of the gas detection material (11) changes in the presence of a test gas, for testing the tightness of a plug (3) in a packaging base body (5).

22. Use according to claim 21, wherein the gas detection material (11) comprises supraparticles comprising a particle superstructure consisting of nanoparticles and substances embedded in the particle superstructure, wherein the nanoparticles are selected from a group consisting of SiCE nanoparticles, metal oxide nanoparticles, polymer nanoparticles, and mixtures thereof, and wherein the substances embedded in the particle superstructure include at least one catalytically active substance for catalyzing a dissociation of hydrogen and at least one redox dye. 212221 PCT - KO-HF

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