Device for producing a dry material film, and method

Abstract

The invention relates to a device (1) for producing a dry material film (M) by evaporating liquid from a liquid sample (P), comprising a container structure (10) having a container (20) with a base section (22) and a circumferential wall section (24), which together delimit a sample space (26) for receiving the sample (P) via a filling opening (28) of the container (20), and having a cover (40) for closing the filling opening (28), wherein at least the container (20) of the container structure (20) has a heatable part (21). The device (1) also has a heating device (50) for heating the heatable part (21), and a supply device (60) which is fluidically connected to the container structure (10) and has an inlet (42) for feeding a gas into the sample space (26) and an outlet (44) for discharging a gas from the sample space (26). The present invention also relates to a method for producing a dry material film (M) from a liquid sample (P).

Description

[0001] Device for producing a dry material film and method

[0002] The present invention relates to a device for producing a dry material film from a liquid sample. The present invention further relates to a method for producing it.

[0003] A dry film of material from a liquid sample must be regularly prepared for analytical procedures. For example, liquid components must be removed from the sample to perform a chemical analysis. These liquid components may include solvents and / or water.

[0004] The object of the invention is to provide solutions for producing a dry material film from a liquid sample. In particular, a device and a method are to be specified. The disadvantages of previously known solutions are to be avoided or at least substantially reduced.

[0005] The above problem is solved according to the invention by the independent claims. Advantageous embodiments are specified in the dependent claims, in the description, and in the accompanying figures.

[0006] A device for producing a dry material film from a liquid sample is proposed. The device comprises:

[0007] • a container structure comprising a container with a bottom section and a circumferential (i.e., a circumferentially closed) wall section, which together define a sample chamber for receiving the liquid sample via a filling opening of the container, and a lid for closing the filling opening, wherein the container structure – and at least the container of the container structure – has a heatable part,

[0008] • a heating device for heating the heatable part (in order to heat a liquid sample contained in the sample chamber), and a supply device fluidically connected to the container structure for supplying a gas into the sample chamber and for removing a gas from the sample chamber.

[0009] In other words, for example, a device is proposed that includes a vessel which can be closed with a lid and into which a substantially liquid sample can be poured or dripped. The device has a heating element with which at least a part or section of the vessel (i.e., the container structure, and at least the container itself) can be heated. Furthermore, the device is designed to introduce gas into and remove gas from the vessel, for this purpose, for example, by including a unit connected to the vessel or its lid.

[0010] The liquid sample (hereinafter also simply referred to as "sample") is preferably any form of liquid or liquid-containing substance; in particular, any form of liquid solution from which a liquid component (e.g., solvent) can be evaporated by heating to obtain a dry residue (e.g., a substance dissolved in the solvent) of the solution. Liquid samples from the medical or pharmaceutical field, such as liquid medications (e.g., cough syrup), are preferred.

[0011] The proposed device enables the removal of liquid from the sample through temperature-assisted evaporation, allowing the remaining material film to settle on the bottom section. The supply system can assist the removal of the (then evaporated) liquid in gaseous form and simultaneously supply fresh gas, such as dry air. Thanks to the device, undesired reactions with gas can be avoided or mitigated, or desired reactions can be induced, for example, by supplying inert or reactive gas. The concept is implemented by selectively heating the container structure, at least in the heated area, so that evaporation can be controlled, gentle, and efficient within the sample chamber. The device enables partial or complete automation of the production of dry material films.Further embodiments of the invention can enhance its advantages. The container structure comprises at least the container and the lid. The container comprises at least the bottom section, the wall section, and the filling opening. Furthermore, at least the container of the container structure—but possibly also other sections of the container structure (such as the lid)—has a heatable part. The heatable part can preferably be provided (at least) by the wall section. Thus, the sample chamber can be surrounded circumferentially by the heatable part, which enables effective heating of the liquid sample. The container is preferably formed in multiple parts. Thus, the individual parts can be manufactured from materials preferred for their respective purposes. Likewise, for example, the wall section and the bottom section can be separated to, for example,to assign a desired heated part to the liquid sample or to simply remove the bottom section for analysis of the dry material film.

[0012] The wall section is provided around the perimeter; thus, it forms a closed perimeter boundary, defining a lateral wall area of ​​the sample chamber. The floor section and the wall section together constitute the sample chamber.

[0013] The wall section can be placed on top of the floor section to form the sample space - e.g., laid on, clamped, pressed on or screwed on (e.g., by means of a screw connection or bayonet connection).

[0014] The wall section can be circular or ring-shaped. The base section can be at least substantially round and / or flat. The base section and / or the wall section can be surfaces of parts or parts themselves.

[0015] The sample can be received in the sample chamber. The sample can be filled into the sample chamber via the filling opening. The sample chamber can be cylindrical, round, or conical, at least substantially and / or partially. The sample chamber can be symmetrical – in particular, rotationally symmetrical or cyclically symmetrical.

[0016] The lid is used to close the container. The lid allows the

[0017] The filling opening or sample chamber must be closed or covered. The lid can, in particular, seal the sample chamber tightly. The lid can abut the wall section, for example, all the way around, especially with a seal arranged between the wall section and the lid. The seal has, for example, a polymer composition, rubber, silicone, FKM or fluoropolymer elastomer or fluororubber, rubber, and / or a mixture thereof. The device can therefore preferably have a seal that is provided between, on the one hand, the container, preferably its wall section, and, on the other hand, the lid, in order to seal the sample chamber on the side of the filling opening against the lid.

[0018] The heating device is designed to heat at least the heatable part. For example, the heating device can heat sections or parts of the container structure. It is, in particular, an electric heating device. The heating device may have or be a source of radiation or electromagnetic radiation. For example, the heating device may generate microwave radiation. The heating device is specifically oriented or directed towards the container or the heatable part of the container for emitting the radiation or microwave radiation. Alternatively, the heating device can also heat the heatable part directly or indirectly in another way; for example, by induction or (direct) heat transfer from a heat source.

[0019] The supply unit is designed to introduce gas into the sample chamber and to remove gas from the sample chamber. In particular, the supply unit is designed for the simultaneous introduction and removal of gas. This allows, for example, the efficient removal of a vaporized phase of the sample, the introduction of a reaction-promoting or -inhibiting gas, and / or the creation of a negative pressure in the sample chamber.

[0020] The supply system includes, for example, a gas reservoir and / or a connection to a gas source for supplying the gas. The supply system includes, for example, at least one conveying device, in particular a pump, for conveying gas, for example, into and / or out of the sample chamber. Gas can also be supplied via a pressure differential between the gas source and the sample chamber, for example, by creating a negative pressure on the sample chamber side and / or a positive pressure on the gas source side, particularly relative to atmospheric pressure or i bar. A pressure differential can also be used for discharge. A conveying device, in particular a vacuum pump, may be provided to convey gas, for example, to convey it out of or away from the sample chamber, and / or to create a negative pressure in the sample chamber by removing gas.

[0021] The supply system can be connected to the sample chamber via a channel structure and / or one or more supply lines, e.g., hoses and / or pipes. The supply system is specifically connected to the container or the lid.

[0022] The device may include a control unit, for example, for controlling or regulating the heating device and / or the supply device; preferably at least based on measured values ​​from a temperature sensor, described below, for measuring the temperature of the heated part. The control unit may be integrated, at least partially, into the heating device or the supply device, or both.

[0023] The device can have a housing that accommodates the container structure. For example, the heating element can be designed to introduce microwave radiation into the housing. Alternatively or additionally, the heating element can be arranged at least partially or section by section within the housing to provide microwave radiation. The heatable part of the container structure (in particular, at least the container or a section of its wall) preferably comprises a material for absorbing microwave radiation. In this respect, at least the container can be heated very precisely in a section delimiting the sample chamber, which can heat the sample effectively and gently. The housing can be opened and closed. The housing is typically at least partially opaque to microwave radiation, in particular to prevent the escape of introduced microwave radiation.The inside of the housing is preferably at least partially microwave-reflective to increase the effectiveness of the device. The heated part (e.g., the container or the wall section of the container) can have or consist of a black body to absorb microwave radiation. It is possible that other parts or sections of the container structure or the device, in particular at least nothing in the housing, do not have a black body or are free of one. For example, only the container has or forms a black body. This prevents the device from being heated in undesired areas. A black body can absorb microwave radiation surprisingly well and emits radiation particularly effectively, so that, on the one hand, the sample can be heated thoroughly, and on the other hand, a temperature measurement, for example using infrared, can be carried out, especially from the outside of the container.

[0024] The heatable part or the container, or at least the wall section of the container, or a combination thereof, may be made of a material, in particular a rigid or solid and / or non-metallic one. The material preferably comprises a polymer composition containing carbon, preferably graphite, clay, aluminum oxide, silicon carbide, or a mixture thereof. The polymer composition may include a thermoplastic, in particular polytetrafluoroethylene (PTFE). It may be provided that a material heatable by microwave radiation is dispersed, in particular as finely as possible, in another material, for example, graphite in the polymer composition.

[0025] The device may include a temperature sensor for measuring (e.g., determining or recording) the temperature of the heated part. The temperature sensor preferably includes or is an infrared sensor. For example, the temperature sensor may be attached to or directed towards the heated part (e.g., from inside or outside the housing, if present). In particular, the infrared sensor can measure the temperature without contact, where the black body is advantageously well-suited for measurement and provides quite accurate information about the temperature in the sample chamber. For example, overheating or underheating of the sample can be prevented by means of a temperature sensor, especially if the heating device is controlled based on the temperature sensor and / or a user takes the measured temperature into account when adjusting the heating device.The container structure, in particular the container and / or the lid, can be movably mounted. The container structure, or the container and the lid, can be rotatably mounted, preferably about a vertical axis, particularly within the housing. The container can be mounted on a movable, preferably rotatable, base plate of the device. For example, the container can rotate about the vertical axis, particularly on the base plate and / or within the housing. The device can have a drive mechanism, for example, to drive the base plate in order to move or rotate it. The lid can move or rotate with the base plate. The vertical axis can be spaced apart from the container, for example, so that the container moves about the vertical axis like a planet. The container can be fixed in position relative to the base plate, so that, essentially, the base plate is rotatably mounted to allow the container and the lid to rotate with it.This results in a more even heating of at least the part that can be heated, especially in combination with the comparatively long-wave microwave radiation.

[0026] The container can be spring-mounted, for example, on the base plate. For instance, when pressed down, the container can be subjected to a restoring force, for example, by means of a spring acting between the container and the base plate. The container can be mounted to allow movement of one or more millimeters against the spring force. In particular, the container can be spring-mounted against the direction in which the lid is placed to close the sample chamber, preferably along a vertical axis. In this respect, the container can provide a pressing force against the lid when closing. This also allows, for example, a relative inclination between the lid and the container to be easily compensated for, and consequently, the sample chamber to be securely closed with the lid.

[0027] The wall section can be annular. This annular wall section can have a passage, for example, where one side of the passage provides the filling opening and the other side is designed to connect to the bottom section. The wall section can form or comprise the heated part of the container. The wall section can be designed as a heating ring (e.g., as a heated ring element). For example, the wall section can be an injection-molded and / or monolithic part of the container. The wall section can ensure uniform heating of the sample. The sample can be partially shielded against excessively rapid direct evaporation of the liquid. The temperature of the sample can be accurately measured via the wall section.

[0028] In addition to the container itself, the lid of the container structure can also have a heated section. Thus, by heating this section of the lid or the lid itself, infrared radiation can also be directed into the sample chamber from above, further accelerating the evaporation process of the liquid sample within the sample chamber and / or preventing unwanted condensation (e.g., of the evaporated phase) on the inside of the lid.

[0029] An inner wall of the wall section, which defines the sample chamber, can taper towards the base section, preferably conically or spherically. The inner wall can be circumferential or ring-shaped. It can also be funnel-shaped. This facilitates the application of the sample to the base section. Furthermore, this design allows for a relatively large filling opening for easy sample insertion, while a comparatively small base section enables the formation of a dry material film from a small sample quantity.

[0030] The base section can include or be formed from a support disc for the sample. By definition, a disc is a geometric body in the form of a (general) cylinder, in which two dimensions (length and width) are significantly larger than the third dimension (width). The support disc (also referred to as a "support plate" within the scope of the invention) can have any (general) cylindrical shape; for example, a circular cylinder, an elliptical cylinder, a prism (e.g., polygonal or quadrilateral, such as square or rectangular), and the like. The support disc is therefore preferably at least substantially flat or with a thickness that is constant (and small) at least in certain areas, and / or a flat surface facing the sample space. The support disc facilitates, in particular, the easy removal and / or transport of the material film.The base section can further comprise a support body that carries the support disc or plate on a side facing away from the sample chamber (i.e., below the support disc). This ensures the support disc is securely carried and braced against the wall section or the lid. The support body preferably carries the support disc in a detachable manner; consequently, the two parts can preferably be provided in a separable form.

[0031] The base section – preferably the support body – can have a cavity, which may be formed, for example, by a passage through the base section or its support body. The passage may extend along the vertical axis. The cavity may be located below the support disc or directly adjacent to the support disc, for example, to facilitate removal of the support disc. The support disc may cover the cavity or the passage.

[0032] The device may include a pedestal. The pedestal may be associated with the base plate or the container or container structure. In particular, the pedestal may be resilient, for example, by means of a spring. The bottom section may be placed on the pedestal; for example, with the support body. The pedestal may engage the cavity of the bottom section or its support body along the vertical axis and / or opposite the support plate. The container may rest on the pedestal.

[0033] The bottom section and the wall section can be provided in a separable manner. For example, the wall section can be removed from the bottom section, in particular from the support disc and / or the support body. The wall section can be placed on the bottom section to form the sample chamber; preferably, it can be screwed to or bolted to the bottom section (in particular, its support body). The wall section can be fixed to the bottom section, for example, by being pushed on or screwed on. For example, the dry material film can be made more easily accessible in this way, as the bottom section can be separated from the wall section according to the method; and preferably, furthermore, the support disc from the support body.For example, a seal can be provided between the bottom section (preferably at least its support body and / or its support disc) and the wall section, particularly to seal the sample chamber on the bottom section side against the wall section. The seal can be annular. The seal can rest against the wall section and the bottom section (e.g., the support body and / or the support disc) if the wall section is fixed to or mounted on the bottom section. The seal can preferably surround the support disc circumferentially on the outside and, for example, be arranged (e.g., clamped) between the wall section and the support body. The seal prevents the sample from escaping the sample chamber between the wall section and the bottom section. The seal may, for example, have a polymer composition such as rubber, silicone, FKM, or fluoropolymer elastomer.Fluorocarbon rubber, rubber, and / or a mixture thereof.

[0034] The base section, and in particular at least its support disc, can be made of or consist of sapphire, glass, quartz, aluminum oxide, and / or ceramic. For example, the support disc can be made of one or more of these materials. In this respect, the device can accommodate various interchangeable materials for supporting the sample and ultimately as the surface for the material film.

[0035] The filling opening can be formed by an opening or passage in the wall section. The filling opening can be located on the side of the container or wall section facing away from the bottom section. An opening or passage can also be provided on the side of the bottom section, whereby the bottom section or the support disc may adjoin this opening or passage. The opening(s) may be bounded by the wall section.

[0036] The lid can be hood-shaped and / or dome-shaped, particularly to define a reaction chamber together with the sample chamber when it is closed. The lid can be at least substantially hollowed out and / or concave on its inner surface or on a side facing the wall section. The reaction chamber is, in particular, larger than the sample chamber. The lid allows for easy connection of the supply device while simultaneously sealing the filling opening (hood-shaped and / or dome-shaped).

[0037] The lid can have at least one or more inlets or ports for supplying and / or removing a gas. In particular, the lid can have an inlet and / or an outlet. The inlet and outlet can be located side by side. The outlet can be annular. For example, the outlet between a wall of the lid and the inlet can be annular. The outlet can surround the inlet. The outlet can be recessed relative to the inlet. The inlet can project further towards the sample chamber or the base section relative to the outlet, for example, to extract the gas over a wide area in the reaction chamber without immediately extracting the supplied gas again. In particular, the inlet faces the base section and / or the support plate to directly contact the sample. This allows for rapid removal of evaporated liquid.

[0038] The device or supply unit may have a channel structure for guiding gas to the inlet and / or away from the outlet. For example, bores may be incorporated into the lid. The channel structure may be integrated into several sections or parts of the device, such as the lid. The channel structure is designed to guide the gas directly to or from the container or sample chamber, particularly considering that the container may be rotatable, while the supply unit usually is not.

[0039] The lid is preferably movable along a vertical axis, and in particular, guided in a movable manner. The lid can, for example, be guided along the vertical axis, especially to facilitate its removal from or placement on the container.

[0040] The device may have a hood that supports and / or provides the lid.

[0041] The hood can be understood as a holder for the lid. The channel structure can extend at least partially through the hood. The hood is specifically designed to move and / or guide the lid along the vertical axis. The hood can have a guide, in particular one or more guide rods, for example, to provide a positive fit between the base plate and the hood, which is particularly releasable and acts at least with respect to movements about the vertical axis. The hood can be placed onto the base plate via the guide, in particular by transmitting torque. The guide can ensure that the hood is placed in the correct position or in only one rotational position.

[0042] The hood can have several sections or parts. In particular, the hood has a first section and a second section, preferably rotatable about the vertical axis relative to the first section, which includes the lid. The channel structure can extend through both sections or through the first and second sections. For example, the second section can be located on the side of the container, particularly to move with the container. The first section can be located opposite the container and / or the base plate. The first section can be essentially stationary. A coupling area can be provided between the first and second sections, allowing relative movement. The channel structure can be sealed in the coupling area.

[0043] Several container structures can be provided. The container structures can be arranged in a fixed position relative to one another, i.e., at least in the direction or plane perpendicular to the vertical axis (i.e., evenly distributed around the vertical axis). For example, the hood, in particular the second section of the hood, supports all the lids of the container structures, and / or the base plate supports all the containers of the container structures. The hood can be configured to move all the lids, preferably simultaneously, along the vertical axis. This allows several samples to be heated simultaneously in the device to produce material films. For example, at least or more than two, for example three, four, five, six, seven, eight, nine, ten or more, and up to twenty container structures are provided.The container structures can be arranged, for example, in a star shape and / or at regular intervals around the vertical axis. The supply system can be configured to provide a negative pressure in the sample chamber or reaction chamber. Negative pressure means that the pressure is below ambient pressure. Specifically, the negative pressure is below 500 mbar, below 250 mbar, below 100 mbar, or below 50 mbar. This allows the boiling point of the liquid in the sample to be effectively lowered if necessary.

[0044] The supply system can be configured to introduce a gas, such as air, a reactive gas, or an inert gas like oxygen, nitrogen, argon, or a mixture thereof, into the sealed and, in particular, vacuum-operated sample chamber in a controlled manner. In this respect, the supply system can create a vacuum by extracting gas and simultaneously supply new gas. This can lower the boiling point of the liquid, enabling the material film to be produced at a lower temperature and / or more quickly. This can be gentler on the sample.

[0045] The base plate has a diameter of, for example, 500 mm or less. Preferably, a diameter of at least 50 mm and / or at most 400 mm is provided. The radius can accordingly be half the diameter.

[0046] The base section and / or the support disc has a diameter of, for example, 40 mm or less. Preferably, a diameter of at least 10 mm and / or at most 30 mm is provided.

[0047] The wall section, particularly in an area adjacent to the base section, has an inner diameter of, for example, 10 mm or less. Preferably, an inner diameter of at least 6 mm and / or at most 8 mm is provided. The wall section preferably has a wall thickness of at most 5 mm and / or at least 1 mm, more preferably a wall thickness of 3 mm ± 1 mm. Furthermore, a method for producing a dry material film from a liquid sample is proposed. The method can be carried out using the apparatus described herein. The method particularly comprises:

[0048] • Providing the device according to the invention, and preferably afterwards

[0049] • Filling the sample chamber with a liquid sample (preferably a solution), for example with a volume of at least 0.05 ml and / or at most 2 ml, in particular with a volume of at least 0.1 ml and / or at most 1 ml,

[0050] • Closing the sample chamber with the lid,

[0051] • Heating at least the heatable part of the container structure or the container itself,

[0052] • Heating the sample in the sealed sample chamber using the heated, heatable part of the container and evaporating the liquid from the liquid sample to form the dry material film on the bottom section, and

[0053] • Supplying a gas into the sample chamber and / or removing a gas from the sample chamber, at least during the heating of the liquid sample.

[0054] In other words, for example, the use of the device described here is claimed, wherein the sample is placed in the container, the container is sealed, the heatable part of at least the container is heated, and the supply device provides gas exchange. Furthermore, a vacuum can be applied to the container or the sample chamber and / or a specific gas can be supplied, particularly in a controlled manner.

[0055] In this process, the heatable part (i.e., at least the container or part of the container) is heated to a temperature of, for example, 100 °C ± 50 °C.

[0056] The gas supplied can be air, a reaction gas, an inert gas, or a mixture thereof. This allows for targeted control over any reactions of the sample and / or the removal of the liquid. The removal process can include the removal of the vaporized liquid and, in particular, the supplied gas. For example, the vaporized liquid is pumped or extracted alone or together with the gas.

[0057] A negative pressure can be created in the sample chamber, at least during heating. For example, the gas contained in the sample chamber can be at least partially pumped out, which can create the negative pressure. The amount of gas removed via the outlet can be greater than the amount of gas supplied via the inlet, which can also create the negative pressure.

[0058] After the formation of the dry material film, the sample chamber can be opened to expose the dry material film. Furthermore, preferably after opening the sample chamber, the bottom section containing the dry material film can be removed and / or separated from the wall section. Additionally, preferably after opening the sample chamber, the wall section can be removed from the bottom section. Finally, preferably after opening the sample chamber, the carrier disc containing the dry material film can be removed and / or separated from the bottom section (e.g., removed and / or separated from the wall section).It is possible that the container can be removed from the device after opening, for example in order to handle the dry material film separately from the rest of the device, in particular to analyze it.

[0059] It may be provided that the heating device is controlled depending on a temperature measured at the container, in particular by means of an infrared sensor.

[0060] Further embodiments and advantages of the present invention are described below with reference to the figures in the accompanying drawings. These show:

[0061] Fig. 1 shows a device in a sectional view with the sample chamber open, and Fig. 2 shows the device in a sectional view with the sample chamber closed.

[0062] Figures 1 and 2 show a device 1 for producing a dry material film M (see Figure 2) by evaporating liquid from a liquid sample P in a sectional view parallel to a vertical axis Y. The device 1 is shown only partially and essentially to the left of the vertical axis Y.

[0063] Fig. 1 shows the device with the container 20 open and sample P filled therein, and Fig. 2 shows the device 1 with the container 20 closed, wherein the sample P is essentially present as a dry material film M according to the method.

[0064] The device 1 comprises a container structure 10 with the container 20 and a lid 40 for closing the container 20 or its filling opening 28. The container 20 is preferably mounted on a base plate 3 of the device 1. Furthermore, the device 1 preferably has a hood 4 which supports the lid 40 and is designed to move the lid 40 along the vertical axis Y, in particular guided movement; see, for example, the difference between Fig. 1 and Fig. 2.

[0065] The container 20 has a bottom section 22 and a circumferential wall section 24, which together define a sample chamber 26 of the container 20. The sample chamber 26 is designed to receive the sample P via the filling opening 28 of the container 20. The lid 40 is designed to close the filling opening 28. The lid 40 can abut against a seal 25b of the container 20, or a seal 25b can be provided between the two.

[0066] At least the container 20 of the container structure 10 – preferably also the lid 40 thereof – has a heatable part 21. The heatable part 21 (here, for example, formed by the wall section 24) is preferably made of a material having a polymer composition containing carbon, preferably graphite, for example, PTFE with carbon. Variants with or made of a polymer composition or plastic, clay, aluminum oxide, and / or silicon carbide are also conceivable. The device 1 has a heating element 50 for heating the heatable part 21. The device 1 can further have a temperature sensor 52 for determining or detecting a temperature of the heatable part 21, wherein the temperature sensor 52 is particularly preferably an infrared sensor. The temperature sensor 52 preferably points directly towards the heatable part 21.The heating device 50 can generate microwave radiation to heat at least the heatable part 21, in particular by introducing it into a housing 2 of the device 1. Alternatively, the heating device 50 can also heat the heatable part 21 directly or indirectly in another way; for example, by induction or direct heat transfer from a heat source.

[0067] The temperature of the heated part 21 can be determined or measured via the temperature sensor 52, which allows, for example, conclusions to be drawn about a (maximum) temperature in the sample chamber 26 in order to monitor the heating of the sample P and to regulate or control the heating device 50 accordingly.

[0068] The device 1 comprises a supply unit 60 fluidically connected to the container structure 10, with an inlet 42 for supplying gas into the sample chamber 26 and an outlet 44 for removing gas from the sample chamber 26. The supply unit 60 preferably includes a pump 61, in particular a vacuum pump for generating a vacuum. Dashed lines indicate the fluidic connections of a gas supply 62 (e.g., comprising a gas reservoir and / or a connection to a gas source) of the supply unit 60 for supplying gas into the system (i.e., the container structure 10, the hood 4, or the sample chamber 26) and a gas discharge 63 (e.g., comprising the pump 61) of the supply unit 60 for removing gas from the system.

[0069] The device 1 preferably includes a control unit 7 that can control and / or regulate the heating device 50 and the supply device 60; and likewise, if present, further components of the device 1, such as a drive for the base plate 3.

[0070] The device 1 preferably comprises the housing 2 accommodating the container structure 10, wherein the heating device 50 is configured for introducing microwave radiation into the housing 2, and wherein the heatable part 21 comprises a material for absorbing microwave radiation. The heatable part 21 preferably consists of, or comprises, a black body for absorbing microwave radiation.

[0071] The container structure 10, in particular the container 20 and the lid 40, is preferably movably or rotatably held about the vertical axis Y, particularly within the housing 2. This is preferably achieved in the present case by holding or mounting the base plate 3 movably or rotatably about the vertical axis Y within the housing 2. In the present case, the base plate 3 is driven, for example, by means of the drive of the device 1. The housing 2 can be opened and closed. The housing 2 is typically at least partially opaque to microwave radiation.

[0072] The container 20 is preferably resiliently mounted on the base plate 3 along the vertical axis Y, opposite to the mounting direction Yi of the lid 40 for closing the sample chamber 26. More precisely, the bottom section 22 is, by way of example, placed on a resilient pedestal 36. A spring 32, acting between the container 20 and the base plate 3, particularly of the pedestal 36 of the device 1, is arranged. A spring force ensures that the container 20 is pre-tensioned towards the lid 40, for example, to allow for tolerance compensation of the container 20 in the direction of the vertical axis Y and with respect to the hood 4.

[0073] The wall section 24 is preferably ring-shaped. The wall section 24 preferably forms or includes the heatable part 21. The wall section 24 is preferably formed as a heating ring (i.e., a heatable ring element). An inner wall 25 of the wall section 24, which delimits the sample chamber 26, preferably tapers conically towards the bottom section 22.

[0074] The bottom section 22 preferably includes a support disc 23 for supporting the sample P. The bottom section 22, and in particular at least its support disc 23, preferably comprises sapphire, glass, quartz, aluminum oxide and / or ceramic. The bottom section 22 can further include a support body 29 which supports the support disc 23 on a side facing away from the sample chamber 26 (here: bottom) – preferably detachably.

[0075] Below the support disc 23, a cavity 34 is provided as an example. The cavity 34 is formed in the base section 22, or here in the support body 29. The cavity 34 extends as a passage along the vertical axis Y. The platform 36 engages the cavity 34 along the vertical axis Y and opposite the support disc 23. The container 20 can be removed from the platform 36 along the vertical axis Y when the device 1 is open (see Fig. 1).

[0076] The bottom section 22 and the wall section 24 are preferably provided in a separable manner. To form the sample chamber 26, the wall section 22 is preferably placed on the bottom section 22 – preferably at least on its support body 29 and / or the support disc 23 – and is in particular fixed and / or screwed onto the bottom section 22 or the support body 29. The filling opening 28 is preferably formed by an opening 30 in the wall section 24. The filling opening 28 is preferably provided on a side of the container 20 or the wall section 24 facing away from the bottom section 22 and is preferably bounded by the wall section 24.

[0077] A (further) seal 25a of the device 1 is preferably provided between, on the one hand, the bottom section 22 (preferably at least its support body 29 and / or its support disc 23) and, on the other hand, the wall section 24, in order to seal the sample chamber 26 on the side of the bottom section 22 against the wall section 24. The seal 25a can preferably, as shown, circumferentially surround the support disc 23 on its outer surface. Furthermore, as described, the seal 25b can preferably be provided between, on the one hand, the container 20 – preferably its wall section 24 – and, on the other hand, the lid 40. The seals 25a and 25b are, by way of example, each designed as annular cord seals.

[0078] The lid 40 is preferably hood- or dome-shaped in order to define a reaction chamber 27 together with the sample chamber 26 when it is closed, see Fig. 2. The lid 40 preferably has at least one access point for supplying or removing a gas, more precisely an inlet 42 and an outlet 44. The outlet 44 is annular and surrounds the inlet 42.

[0079] The device 1 or the supply unit 60 can have a channel structure 46 for guiding gas to the inlet 42 and away from the outlet 44.

[0080] The lid 40 is preferably movable along the vertical axis Y, for example to close or open the sample chamber 26.

[0081] Preferably, the device 1 comprises several of the described container structures 10, which are arranged here in a fixed position relative to one another, with the hood 4 preferably supporting all lids 40 and designed to move all lids 40 simultaneously along the vertical axis Y. The container structures 10 are preferably arranged (preferably uniformly) around the vertical axis Y. In Figures 1 and 2, the remaining container structures 10 are omitted for the sake of simplicity. A comparison of Figures 1 and 2 shows that the hood can be moved along the vertical axis Y to selectively open and close the containers 10.

[0082] The hood 4 preferably has a guide 5, in this case several guide rods. The guide 5 provides, for example, a releasable positive fit between the base plate 3 and the hood 4, which is effective at least with respect to movements about the vertical axis Y. The hood 4 can be placed onto the base plate 3 via the guide 5, transmitting torque. The guide rods can engage in the base plate 3, in particular, only in one rotational position. The guide 5 ensures that the hood 4 can only be placed on the base plate 3 in one rotational position or with a corresponding alignment between the container 20 and the lid 40.

[0083] The hood 4 preferably has a first section 4.1 and a second section 4.2 rotatable relative to the first section 4.1, with the lid 40, wherein the channel structure 46 extends through both sections 4.1 and 4.2. When the container structures 10 are rotated about the vertical axis Y, the second section 4.2 rotates along with them, while the first section 4.1 does not. During the movement, gas can be passed between sections 4.1 and 4.2 via the channel structure 46, in particular between sample chamber 26 or reaction chamber 27 and the supply unit 60. The supply unit 60 is preferably configured to provide a negative pressure or a vacuum below 100 mbar, for example, a negative pressure of 50 mbar, particularly in sample chamber 26 or reaction chamber 27.The supply unit 60 is preferably configured to supply a gas, e.g. air, reaction gas and / or inert gas, to the sealed and negatively pressurized sample chamber 26 or reaction chamber 27 in a controlled manner.

[0084] The base plate 3 preferably has a diameter of, for example, 500 mm or less. The radius R of the base plate 3 is preferably 250 mm or less. The support disc 23 preferably has a diameter Di of 15 mm. The wall section 24, particularly in an area adjacent to the base section, preferably has an inner diameter of 10 mm. The wall section 24 preferably has a wall thickness of at least 1 mm at the sample chamber 26.

[0085] A device 1 for producing a dry material film M by evaporating liquid from a liquid sample P, preferably for evaporating liquids containing dissolved substances, e.g., pharmaceutical products, is shown and described. The vapors are extracted, and the dried substances are deposited on the base section 22 (preferably the carrier disk 23) as a carrier material. The removal of the resulting vapors is preferably achieved by the supply device 60 with at least one pump. The supply device 60 can simultaneously be used to reduce the boiling points by means of reduced pressure or under vacuum and, if necessary, to supply inert gas in order to prevent substance changes, in particular degradation, by atmospheric oxygen and / or heat. Reaction gas can also be supplied if this is advantageous for the process. The residue of the sample P as a dry material film M on the base section 22 or...Here on the carrier disk 23, the process is used to identify the substance or substance mixture of sample P, for example, using spectroscopic methods such as Fourier-transform infrared spectroscopy (FTIR), in particular ATR technique (attenuated total reflection), or chromatography such as high-performance liquid chromatography (HPLC), in particular HPLC-MS (MS = mass spectrometry), or other methods. The advantage of this method is the ability to process one or more samples P. The temperature and preferably also the vacuum can be controlled.

[0086] The apparatus 1 shown can be used to carry out a process, in particular for producing a dry material film M from a liquid sample P. In the process, the apparatus 1 is first provided. The process includes, in particular, filling the liquid sample P, preferably through the filling opening 28, into the sample chamber 26. The sample P can have a volume in the range of at least 100 microliters, at least 200 microliters, or at least one milliliter up to at least several milliliters. If the apparatus 1 has several container structures 10, several samples P can be filled into the several container structures 10.

[0087] After filling, the sample chamber 26 is to be closed with the lid 40, followed by heating at least the heatable part 21; for example by introducing microwave radiation through the heating device 50 into the housing 2.

[0088] Heating can be carried out for a period of at least 0.1 minutes, 1 minute, 2 minutes, 3 minutes or more.

[0089] During heating, the base plate 3, and thus the container structure 10 along with the sample P, can be rotated about the vertical axis Y. In this way, the samples P are heated very uniformly by the microwave radiation. During rotation, the container structures 10 can pass the temperature sensor 52 (i.e., its measuring range).

[0090] By means of the heated, heatable part 21, the sample P is heated in the sealed sample chamber 26, and consequently the liquid from the liquid sample P evaporates to form the dry material film M on the bottom section 22. The process includes, at least during the heating of the liquid sample P—and if necessary, also before or after heating the liquid sample P—the introduction of a gas into the sample chamber 26 or the reaction chamber 27 and / or the removal of the gas from the sample chamber 26 or the reaction chamber 27.

[0091] In this process, it is preferably provided that the supplied gas is air, a reaction gas, or an inert gas. The discharge can include the removal of both the vaporized liquid and the supplied gas.

[0092] In this process, a negative pressure is preferably generated in the sample chamber 26 or in the reaction chamber 27, at least during heating. Furthermore, the process can be carried out, or the supply unit 60 can be operated, such that the amount of gas discharged via the outlet 44 is greater than the amount of gas supplied via the inlet 42.

[0093] After the formation of the dry material film M, the sample chamber can be opened to expose the dry material film M.

[0094] Optionally, the container 20 and / or the bottom section 22 (or at least its support disc 23) with the dry material film M can be removed. It is also possible to separate the bottom section 22 with the dry material film M from the wall section 24; preferably, to separate the support disc 23 with the dry material film M from the bottom section 22.

[0095] The material film M can be placed on an AT-R crystal of an IR spectrometer for identity determination.

[0096] Alternatively or additionally, the material film M can be washed out of container 10 and transferred to a measuring system. The material film M can then be identified and measured.

[0097] The dry material film M can thus be easily and directly examined using further methods, such as infrared spectroscopy or chromatography to separate the individual components. For separating the individual components using chromatography, the dry material film M (i.e., the residue of the vaporized sample P) can be suspended in a solvent (e.g., a transport liquid or gas), which simultaneously serves as the mobile transport phase for the respective chromatography method.

[0098] The device can therefore be used to produce a dry material film M by evaporating liquid from a liquid sample P, particularly in the medical or pharmaceutical field.

[0099] Device 1 could be used in the field of plastics engineering, for example with plastics containing plasticizers. Device 1 could also be used in the field of biology, for example in plant material extraction.

[0100] The device 1 can be scaled in size, for example to fill larger or smaller samples into the sample chamber 26.

[0101] The present application is not limited by the embodiments provided it is covered by the subject matter of the following claims.

[0102] Reference symbol list

[0103] device

[0104] Housing

[0105] Base plate

[0106] Hood -1, 4-2 section

[0107] guide

[0108] Container structure 0 Container 1 Heated section 2 Bottom section 3 Support plate 4 Wall section 5a, 25b Seals 6 Sample chamber 7 Reaction chamber 8 Filling opening 9 Support body 0 Opening 2 Spring 4 Cavity 0 Lid 2 Inlet 4 Outlet 6 Channel structure

[0109] Heating system

[0110] Temperature sensor (infrared sensor) 0 Supply unit 1 (vacuum) pump 2 Gas supply

[0111] Gas discharge

[0112] Control unit P probe

[0113] Y axis

[0114] Yi placement direction

[0115] R radius (base plate)

[0116] Diameter (carrier disc)

[0117] D2 inner diameter (wall section)

Claims

Claims 1. Device (1) for producing a dry material film (M) by evaporating liquid from a liquid sample (P), comprising • a container structure (10) comprising a container (20) with a bottom section (22) and a circumferential wall section (24), which together define a sample chamber (26) for receiving the sample (P) via a filling opening (28) of the container (20), and a lid (40) for closing the filling opening (28), wherein at least the container (20) of the container structure (10) has a heatable part (21), • a heating device (50) for heating the heatable part (21), and • a supply device (60) fluidically connected to the container structure (10) with an inlet (42) for supplying a gas into the sample chamber (26) and an outlet (44) for removing a gas from the sample chamber (26).

2. Device (1) according to the preceding claim, wherein the bottom section (22) has or is formed a support disc (23) for supporting the sample (P).

3. Device (1) according to the preceding claim, wherein the bottom section (22) further comprises a support body (29) which supports the support disk (23) on a side facing away from the sample chamber (26), preferably detachably.

4. Device (1) according to one of the preceding claims, wherein the bottom section (22) and the wall section (24) are provided in a separable manner.

5. Device (1) according to one of the preceding claims, wherein the wall section (22) for forming the sample chamber (26) is placed on the bottom section (22), wherein preferably the wall section (22) for forming the sample chamber (26) is screwable to the bottom section (22), in particular its support body (29) if present.

6. Device (1) according to one of the preceding claims, further comprising a seal (25a) which is provided between, on the one hand, the bottom section (22), preferably at least its support body (29) and / or its support disc (23) if present, and on the other hand, the wall section (24) in order to seal the sample chamber (26) on the side of the bottom section (22) against the wall section (24), wherein the seal (25) preferably surrounds the support disc (23), if present, on its outer circumference, and / or further comprising a seal (25b) which is provided between, on the one hand, the container (20), preferably its wall section (24), and on the other hand, the lid (40) in order to seal the sample chamber (26) on the side of the filling opening (28) against the lid (40).

7. Device (1) according to the preceding claim, wherein the bottom section (22), in particular at least its support disc (23) if present, comprises or consists of sapphire, glass, quartz, aluminium oxide and / or ceramic.

8. Device (1) according to the preceding claim, comprising a housing (2) accommodating the container structure (10), wherein the heating device (50) is designed for introducing microwave radiation into the housing (2), wherein the heatable part (21) comprises a material for absorbing microwave radiation.

9. Device (1) according to the preceding claim, wherein the heatable part (21) for absorbing microwave radiation comprises or consists of a black body.

10. Device (1) according to the preceding claim, wherein the heatable part (21) or the container (20) or at least the wall section (24) of the container (20) is made of a material which comprises: • a polymer composition comprising carbon, preferably graphite • Sound, • Aluminum oxide, and / or • Silicon carbide.

11. Device (1) according to one of the preceding claims, further comprising a temperature sensor (52) for determining or detecting a temperature of the heated part (21), wherein the temperature sensor (52) preferably comprises or is an infrared sensor.

12. Device (1) according to one of the preceding claims, wherein the container structure (10), in particular the container (20) and the lid (40), is movably, preferably rotatably about a vertical axis (Y), in particular in the housing (2).

13. Device (1) according to one of the preceding claims, wherein the container (20) is mounted on a movable, preferably rotatable, base plate (3) of the device (1).

14. Device (1) according to one of the preceding claims, wherein the container (20) is resiliently mounted opposite a placement direction (Yi) of the lid (40) for closing the sample chamber (26), preferably along one or the vertical axis (Y), preferably on the base plate (3).

15. Device (1) according to one of the preceding claims, wherein the wall section (24) is formed in an annular shape.

16. Device (1) according to one of the preceding claims, wherein the wall section (24) has or forms the heatable part (21), and / or wherein the wall section (24) is formed as a heating ring.

17. Device (1) according to one of the preceding claims, wherein the lid (40) of the container structure (10) further comprises the heatable part (21).

18. Device (1) according to one of the preceding claims, wherein an inner wall (25) of the wall section (24) limiting the sample chamber (26) tapers towards the bottom section (22), preferably conical or spherical. 19- Device (1) according to one of the preceding claims, wherein the filling opening (28) is formed by an opening (30) of the wall section (24).

20. Device (1) according to one of the preceding claims, wherein the filling opening (28) is provided on a side of the container (20) or wall section (24) facing away from the bottom section (22), preferably limited by the wall section (24).

21. Device (1) according to one of the preceding claims, wherein the lid (40) is designed in a hood or dome shape to limit a reaction chamber (27) together with the sample chamber (26) when the sample chamber (26) is closed.

22. Device (1) according to one of the preceding claims, wherein the lid (40) has at least one access point, in particular the inlet (42) and / or the outlet (44), for supplying or removing a gas.

23. Device (1) according to one of the preceding claims, wherein the device (1), in particular the supply device (60), has a channel structure (46) for guiding gas to the inlet (42) and / or away from the outlet (44).

24. Device (1) according to one of the preceding claims, wherein the outlet (44) is annular and / or surrounds the inlet (42).

25. Device (1) according to one of the preceding claims, wherein the lid (40) is movable along one or the vertical axis (Y).

26. Device (1) according to the preceding claim, comprising a hood (4) which supports the cover (40) and is designed to move the cover (40) along the vertical axis (Y).

27. Device (1) according to the preceding claim, wherein the hood (4) has a first section (4.1) and a rotatable section relative to the first section (4.1). second section (4.2) with the cover (40), in particular wherein the channel structure (46) extends through both sections (4.1, 4.2).

28. Device (1) according to one of the preceding claims, comprising several of the container structures (10), which are preferably arranged in a fixed position relative to each other, further preferably around a vertical axis (Y).

29. Device (1) according to one of the three preceding claims, wherein the hood (4) supports all covers (40) and is designed to move all covers (40) preferably simultaneously along the vertical axis (Y).

30. Device (1) according to one of the preceding claims, wherein the supply device (60) is configured to provide a negative pressure below 500 mbar, in particular a negative pressure below 250 mbar or 100 mbar, and / or wherein the supply device (60) is configured to supply a gas to the sealed and pressurized sample chamber (26) in a controlled manner, for example air or a reaction gas or an inert gas, such as oxygen, nitrogen, argon, air or a mixture thereof.

31. Device (1) according to one of the preceding claims, further comprising a control unit (7) which is configured to control the heating device (50) and / or the supply device (60), preferably at least on the basis of measured values ​​from the temperature sensor (52).

32. Method for producing a dry material film (M) from a liquid sample (P), comprising • Providing a device (1) according to any one of the preceding claims, • Pouring a liquid sample (P) into the sample chamber (26), • Closing the sample chamber (26) with the lid (40), • Heating at least the heatable part (21), • Heating the sample (P) in the sealed sample chamber (26) by means of the heated heatable part (21) and evaporating the liquid from the liquid sample (P) to form the dry material film (M) on the bottom section (22), and • Supplying a gas into the sample chamber (26) and / or removing a gas from the sample chamber (26) at least during the heating of the liquid sample (P).

33. Method according to the preceding claim, wherein • the supplied gas is air, a reaction gas or an inert gas, and / or • the removal process includes: removal of the evaporated liquid and, in particular, the supplied gas.

34. Method according to one of the two preceding claims, wherein a negative pressure is generated in the sample chamber (26) at least during heating and / or the amount of gas discharged via the outlet (44) is greater than the amount of gas supplied via the inlet (42).

35. Method according to any one of the three preceding claims, comprising • After the formation of the dry material film (M): Opening the sample chamber (26) to expose the dry material film (M), and / or • Removing the bottom section (22), preferably at least the support disc (23) if present, with the dry material film (M), and / or separating the bottom section (22) with the dry material film (M) from the wall section (24), preferably separating the support disc (23) if present, with the dry material film (M) from the bottom section (22).

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