DE202021107050U1 - Device for extracting volatile substances from sample material - Google Patents

Abstract

A device (100) for extracting volatile substances (E) from sample material (P), comprising
a reaction space (R) with a sample space (20) for receiving the sample material (P),
a heating device (10) for heating the sample material (P) in the sample chamber (20) to form an evaporation gas containing the volatile substances (E) by evaporation,
a fluid inlet (E) which is fluidically connected to the sample space (20) in order to feed process gas into the sample space (20),
a collection space (S) which is fluidically connected to the sample space (20) via a fluid path (23, 24, 60) downstream of the fluid inlet (E) in order to discharge the gases from the sample space (20),
wherein the fluid path (23, 24, 60) has a condenser (60) to condense the evaporation gas into the collection space (S),
wherein the sample space (20), the fluid path (23, 24, 60) and the collection space (S) together form a device space (V), and
wherein the collection space (S) has a fluid outlet (A) with a pressure relief valve (70) which is designed such that gas in the device space (V) can escape to the outside when a defined pressure is exceeded.

Description

The present invention relates to a device for the (preferably microwave-assisted) extraction of volatile substances from sample material, in particular from natural substances such as plants or parts of plants.

The extraction of volatile substances from sample material, in particular from natural substances, is widely used in the fields of pharmacy, medicine, food technology and the like in order to extract volatile substances such as oils from plant material, for example. For example, CBD, THC, and terpenes can be extracted from cannabis plant material, lavender oil from lavender flowers, lemon oil from lemon peel, etc.

Methods for extracting volatile substances from sample material are known, in particular by evaporating the volatile substances, condensing the resulting gas phase and collecting the condensate as an extract (“distillation”). The problem with extraction methods of sensitive sample material is the effect of oxygen on the sample material, which leads to oxidation and can damage the extract to be collected, i.e. the condensate of the volatile substance. However, it can also be desirable to have a targeted reactive effect on the sample material in order to improve the breakdown of the same, which is not possible with conventional methods.

The present invention has been made with the foregoing circumstances in mind, and has an object of providing a volatile matter extracting apparatus which can improve the ability of volatile matter extraction.

This object is achieved by the device according to the invention according to the independent claim. The dependent claims further develop the invention to advantage.

According to the present invention, an apparatus for extracting volatiles from sample material is provided. The device has a reaction space with a sample space for receiving the sample material. Furthermore, the device has a heating device for heating the sample material in the sample chamber to form an evaporation gas containing the volatile substances by means of evaporation. The device also has a fluid inlet which is fluidically connected to the sample space in order to supply process gas into the sample space. Furthermore, the device has a collection space which is fluidically connected to the sample space via a fluid path downstream of the fluid inlet in order to discharge (the) gases (ie in particular at least the vaporization gas and the process gas) from the sample space. The fluid path includes a condenser to condense the vaporization gas into the plenum. The sample space, fluid path, and collection space together form a device space. The plenum has a fluid outlet with a pressure relief valve. The pressure relief valve is designed in such a way that gas in the device space can escape to the outside, i.e. out of the device, if a defined (gas) pressure is exceeded.

According to the invention, “sample material” means all materials that contain volatile substances that can be obtained by means of evaporation. In particular, natural substances such as plant material, e.g. whole plants or parts thereof (e.g. flowers), both in a fresh and in a pre-processed state, such as (freeze-)dried, rehydrated, crushed, etc. are included.

According to the invention, “volatile substances” are understood to mean the components of the sample material that can be obtained by evaporation, e.g. (ethereal) oils.

Extraction can be improved by using a solvent. Water or an organic solvent can be used as the solvent.

The device according to the invention makes it possible to improve the extraction of volatile substances in several respects. First of all, it is possible with the device according to the invention to flush the device space with the process gas before the actual evaporation begins, ie gas (e.g. air) in the device space by introducing a corresponding quantity of process gas to the outside via the pressure relief valve, ie from the device addition, to displace and replace it as far as possible with the process gas. The composition of the gas phase (ie the gas) in the device space can thus be influenced in a targeted manner, for example unwanted oxygen can be flushed out if necessary. Furthermore, the device according to the invention also allows gases formed or released during the evaporation process to be continuously expelled to the outside, in that process gas is fed in via the fluid inlet. Since the gases can only escape to the outside via the pressure relief valve, but cannot enter the device from the environment, only a small volume of released/formed gases has to be expelled, which advantageously leads to low process gas consumption. Furthermore, by increasing the pressure in the device space, the relief valve advantageously causes the dew point in the condenser to be increased, which also improves extraction. Ultimately, the device space can be set to a specific gas composition and maintained at this level, and this with only a small consumption of process gas. Furthermore, the quality, ie in particular the quality of the extracted volatile substances, can be improved, since undesired processes such as oxidation are impeded, while desired processes can be promoted by selecting a suitable process gas. By making it possible according to the invention to specifically influence the gas phase (the gas) in the device, the reaction of the gas with the sample material can be specifically influenced or prevented, so that the quality of the volatile substances can be improved. Furthermore, this advantage is achieved with a particularly low gas consumption, so that the device is at the same time advantageous in terms of its operating costs.

In principle, all (process) gases or (process) gas mixtures with which the extraction process can be advantageously influenced come into consideration as process gases. The process gas is preferably an inert gas (also referred to as an inert gas) or a reactive gas or a mixture of the gases mentioned. Inert (process) gases or (process) gas mixtures prevent oxidation or other reactions. Reactive (process) gases or (process) gas mixtures make it possible, for example, to improve the digestion of the sample material and/or to bring about desired reactions. Reactive (process) gases or (process) gas mixtures can have an oxidative and/or reductive character.

Furthermore, the process gas can preferably comprise argon or hydrogen or a mixture of argon and hydrogen. The process gas is preferably an argon/hydrogen mixture. If hydrogen is present, the proportion of hydrogen in the process gas can preferably be less than or equal to 5% by volume, more preferably between 0.1% by volume and 5% by volume. Each intermediate value is also expressly disclosed. The use of an argon/hydrogen mixture is particularly preferred, so that the process gas has both a reductive and an inert character at the same time. In particular, the process gas is suitable for influencing the sample material, but without being combustible. The use of argon or a mixture of argon and hydrogen can also make it easier to evacuate the gas from the sample chamber, since argon has a higher density than air.

The heating device may preferably be a microwave heating device. Thus, the heating device can be set up to generate microwave radiation; this preferably by means of one or more magnetron(s).

By irradiating the sample space with microwave radiation, a particularly targeted input of energy is possible, as a result of which the sample material can be heated in a targeted manner, i.e. locally and after its energy input, in a targeted manner to form the vaporization gases. A change in the volatile substances can be avoided through the targeted energy input, which further improves the quality of the extraction. Furthermore, the sample material can be heated evenly, which improves the yield and thus also the extraction.

The fluid inlet can preferably have a feed line, which preferably extends into the sample chamber. In the process, it can particularly preferably extend as far as the sample material or directed towards the sample material.

By supplying the process gas via a supply line, the targeted entry of process gas into the sample chamber is possible. In the particularly preferred case that this supply line extends into the sample chamber, the process gas can be supplied in a targeted manner to a sample material located therein and particularly preferably introduced directly onto the surface of the sample material, whereby the effect of the process gas can be increased. This can be particularly advantageous in the case of low-density process gases or process gas mixtures.

The fluid inlet can preferably have a valve that opens only towards the sample space or device space, in particular a non-return valve, via which the process gas can be supplied.

As a result, it can be prevented in a simple manner that (process) gas can escape from the device through the fluid inlet during the introduction of the process gas. The efficiency of the extraction can thus be further improved since the consumption of process gas can be minimized by preventing unwanted losses.

The device can also preferably have a process gas source which is fluidically connected to the fluid inlet in order to feed process gas into the sample space or device space.

In this way, any desired process gas can be made available in sufficient quantity for the process. It is also easy to switch between different process gases or simply combine them to form a gas mixture on site.

The device can also preferably have a process gas pump for conveying a process gas via the fluid inlet into the sample space or device space; preferably from the process gas source.

The process gas can thus be introduced into the system in a simple manner and preferably in an easily controllable manner.

The device can also preferably have a sample container which forms or has the sample space. Consequently, the interior delimited by the sample container has or forms the sample space.

A defined sample space can thus be provided, into which the sample material can be accommodated in a simple manner and from which it can be removed again. Process gas and the heating source (e.g. microwaves) can also be introduced in a targeted manner through the defined sample space.

The sample container can preferably be detachably provided in the reaction space.

Consequently, the sample chamber can be easily removed via the sample container for removing and receiving sample material from the device or the reaction chamber. It is also possible in this way to select the sample chamber appropriately matched to the sample material (e.g. type, quantity, etc.) and the process gas to be used and, if necessary, the heating device.

The sample container can preferably have a handle element, preferably a ring element surrounding the sample space or the sample container on the outside, for lifting the sample container.

A simple means for handling the sample container is provided with the grip element. If this is designed as a ring element, it can also be easily grabbed for particularly safe handling.

The reaction space can preferably have positioning structures which interact with the sample container, preferably an alignment element or centering element of the same, which is particularly preferably formed by its gripping element or ring element, in order to position the sample container in a defined manner, preferably centering it.

A defined position of the sample container can thus be achieved by means of the positioning structures. The sample container can thus be aligned in a defined manner with respect to the heating device, for example, in order to bring about effective heating of the sample material in the sample chamber.

The device can also preferably have a drive unit for rotatably driving the sample space, preferably the sample container, in the reaction space.

In this way, a particularly homogeneous heating of the sample material can be achieved.

The drive unit can preferably have a turntable. This can accommodate the sample space and more preferably the sample container. In this case, in a particularly preferred embodiment, the turntable can have the positioning structures.

Thus, a simple but effective means for providing the sample material or the sample space or the sample container in a rotatable manner can be provided.

The sample space, preferably the sample container, can preferably have a cover for selectively opening the sample space to receive and remove sample material. The cover can be opened, for example, by lifting it off the reaction space or sample space or sample container.

An easily accessible sample space can thus be provided. In particular, with such an embodiment of the sample space, it is possible to easily remove the sample material from the reaction space or the device or to take it up. If a detachable sample container is provided, the sample container can be easily removed for receiving and removing sample material. Overall, the handling of the device can be improved.

Preferably, at least part of the fluid path and preferably also of the collection space can be connected to the cover in such a way that they are moved or lifted together with the cover when the sample space is opened; for example, can be raised from the sample container. For this purpose, the cover is preferably provided in a movable but stationary manner in the device, while—if present—the sample container can be removed. Thus, the remaining components of the device do not have to be dismantled before removing the cover in order to access the sample chamber or to remove the sample container. Overall, so the Handling of the device can be further simplified and improved.

Preferably, the device can also have an actuator, by means of which the cover can be selectively opened.

Thus, it is possible to automate the opening of the lid. This simplifies the removal of the sample container. Overall, the handling of the device can thus be further simplified and improved.

The device can also preferably have a collection container, preferably in the form of a separator, which in turn has the collection space.

Thus, the plenum can be easily provided and managed.

The collection space can preferably have a return line for returning a condensed solvent phase, preferably a water phase, into the sample space.

It is thus possible to create a circulation of the solvent in the device, in that condensed and separated solvent is fed back into the sample chamber, where it is then available again for dissolving the volatile substances. In principle, all suitable substances can be used as solvents, in particular water, but also hydrocarbons, alcohols, etc. In this way, the effectiveness of the extraction can be increased and the consumption of solvents and the required heating power can be reduced.

The return line can preferably be arranged in such a way that it prevents a gas flow through the return line when the solvent phase is present.

It is thus possible to shut off the collection space from the sample space in a gas-tight manner via the solvent phase on one side, for example by using a separator with an overflow, so that a gas flow can only take place through the fluid path. As a result, the volume of the gas phase in the device space can be reduced, which further reduces the consumption of process gas. Furthermore, it can be ensured in this way that the direction of flow of the gas in the device space is adjusted from the sample space to the pressure relief valve via the fluid path, which improves the effect of the displacement of undesired gases in the device space.

The return line can preferably run at least partially coaxially with the feed line.

On the one hand, this simplifies the structure, since only one opening is required in the sample space in order to introduce the process gas and recycled solvent phase into it. Furthermore, the temperature of the process gas and the returned solvent phase can already equalize before entry into the sample chamber, which leads to improved thermal stability of the process.

At least part of the return line and part of the fluid path between sample space and condenser can be identical or run together.

In this way, the structure of the system can be further simplified; comparable to the advantages described in the previous feature.

The device can preferably further have a temperature sensor for measuring a temperature in the device space.

It is thus possible to monitor the state of the extraction process and to take appropriate corrective measures if a predetermined critical temperature is exceeded; for example to reduce the heating output. In this way, the release of unwanted substances can be prevented and ultimately a high quality of the extracted volatile substances can be guaranteed. Furthermore, it can be prevented in this way that an excessive increase in pressure associated with increased temperature would lead to an excessive amount of gas escaping from the pressure relief valve, which further improves the quality of the extraction.

The temperature sensor can preferably have a sample temperature sensor which is assigned to the sample space for measuring a temperature of the sample material. This can be, for example, an infrared sensor directed towards the sample space.

Thus, the temperature in the sample chamber and in particular of the sample material can be monitored in order to prevent the release of unwanted substances and ultimately to ensure a high quality of the extracted volatile substances. As will be explained below, the heating device for process control, for example, can be controlled or regulated in this way.

The temperature sensor may preferably be a control temperature sensor for measuring a temperature in the device space downstream of the Condenser, preferably in the area of the fluid outlet have.

Thus, the temperature in the device space and particularly preferably in the area of the fluid outlet can be monitored. In this way, it can preferably be prevented that an excessive increase in pressure associated with increased temperature would lead to an excessive amount of gas escaping from the pressure relief valve. Thus, the quality of the extraction can be further improved.

The pressure relief valve can preferably have or carry the control temperature sensor.

Thus, the structure of the device can be further simplified. If the control temperature sensor is carried by the pressure relief valve, its exact positioning can be simplified and its removal, which may be necessary, for example for maintenance purposes, can be simplified.

The pressure relief valve can preferably be or have a gravimetric valve.

In this way, a valve that is also permanently accurate can be provided. In principle, other pressure relief valves, for example with spring elements, are also conceivable.

The defined pressure in the device space can basically correspond to any desired overpressure compared to the environment. In particular, the defined pressure may depend on the nature of the process, the design of the device, the volumes of the sample space, fluid path and collection space, as well as the device space as a whole, and many other factors. The defined pressure is preferably 5 to 800 mbar above ambient pressure, more preferably 10 to 400 mbar above ambient pressure. In this way, the dew point in the condenser can be increased in a targeted and defined manner, which further improves the extraction.

The device can preferably also have a control unit for controlling an extraction process by means of the device. The control unit preferably serves to control the heating device and/or the fluid inlet and, if present, also the process gas pump and/or the actuator and/or the drive unit.

In this way, an extraction process can preferably be carried out automatically and with particularly high accuracy.

The control unit can preferably be set up in such a way to control the device on the basis of at least one of the temperature sensors.

The control or regulation based on at least one of the temperature sensors (ie at least sample temperature sensor and/or control temperature sensor) ensures a particularly accurate and effective extraction process.

• - Aufnehmen des Probenmaterials in einem Probenraum eines Reaktionsraumes,
• - Zuführen von Prozessgas in den Probenraum über einen Fluid-Einlass,
• - Erhitzen des Probenmaterials zur Bildung eines die flüchtigen Stoffe aus dem Probenmaterial enthaltenen Verdampfungsgases mittels Verdampfung,
• - Abführen der Gase aus dem Probenraum über einen Fluidpfad,
• - Kondensieren des abgeführten Verdampfungsgases in einen Sammelraum (S), wobei der Probenraum, der Fluidpfad und der Sammelraum zusammen einen Vorrichtungsraum bilden, und
• - bei Überschreiten eines definierten Drucks in dem Vorrichtungsraum, Entweichen des in dem Vorrichtungsraum befindlichen Gases nach außen über ein Überdruckventil eines Fluid-Auslasses des Sammelraumes.

According to the invention, there is also provided a method for extracting volatiles from sample material. This is preferably carried out using the device according to the invention. The method according to the invention includes:

• - Picking up the sample material in a sample space of a reaction space,
• - supply of process gas into the sample chamber via a fluid inlet,
• - heating the sample material to form a vaporization gas containing the volatile substances from the sample material by means of evaporation,
• - discharge of the gases from the sample chamber via a fluid path,
• - condensing the evacuated evaporation gas into a collection space (S), wherein the sample space, the fluid path and the collection space together form a device space, and
• - When a defined pressure in the device space is exceeded, the gas in the device space escapes to the outside via a pressure relief valve of a fluid outlet of the collecting space.

The defined pressure in the device space results as already described above, and can consequently correspond to any desired excess pressure compared to the environment. In particular, the defined pressure may depend on the nature of the process, the design of the device, the volumes of the sample space, fluid path and collection space, as well as the device space as a whole, and many other factors. The defined pressure is preferably 5 to 800 mbar above ambient pressure, more preferably 10 to 400 mbar above ambient pressure.

The sample space can preferably be formed by a sample container, which can be optionally removed from the reaction space to receive the sample material.

When the sample container is inserted into the reaction space, the sample container can be fitted with positioning structures of the reaction space preferably interact in such a way that the sample container is positioned or centered in a defined manner in the reaction space.

The sample space, preferably the sample container, can preferably be moved and more preferably rotated at least during the heating of the sample material in the reaction space.

The device space can preferably be flushed before the heating of the sample material by supplying the process gas via the fluid inlet via the pressure relief valve.

The heating can preferably be done by means of microwaves.

The process gas can preferably be supplied during all or part of the extraction process.

The process gas can preferably be supplied in an amount per minute which essentially corresponds to the volume of the device space, preferably 1/4 to 2/1 of the volume of the device space, more preferably 1/2 to 3/2 of the volume of the device space.

The step of supplying process gas and/or the step of heating the sample material can preferably be controlled as a function of a temperature in the device space or the collection space and/or a temperature of the sample material.

The collection space can preferably have a return line via which a condensed solvent phase, preferably a water phase, is returned to the sample space, the return line being arranged in such a way that it prevents a gas flow through the return line when the solvent phase is present.

The process gas can preferably be at least partially a reductive, oxidative or inert gas, preferably a gas mixture containing argon, particularly preferably a non-combustible gas mixture containing argon and hydrogen.

The advantages and preferred further developing aspects of the method result analogously to those of the device already explained. For the sake of clarity, repeated reproduction is therefore dispensed with.

With the method according to the invention it is also possible to improve the extraction analogously to the device. The gas phase in the device space can therefore be influenced in a targeted manner before and during the evaporation, with the process gas consumption being able to be reduced. Furthermore, the quality of the recovered volatiles can be improved.

• 1 ein Ausführungsbeispiel einer erfindungsgemäßen Vorrichtung.

These and other aspects and advantages also result from the following description and the single figure. However, the following description and figure have no restrictive effect. Furthermore, individual features can be detached and combined with other features as desired, insofar as this is covered by the scope of the independent claims and does not create any contradictions. It shows

• 1 an embodiment of a device according to the invention.

An exemplary embodiment of a device 100 according to the invention for extracting volatile substances X from sample material P is shown in 1 shown.

The device has a reaction space R. The reaction space R in turn has a sample space 20 for receiving the sample material P. FIG. The entire reaction space R can serve as a sample space 20 . However, it is also conceivable that the sample space 20 forms only part of the reaction space R. The sample space 20 can form a fixed or integral part of the reaction space R. It is also conceivable for the sample chamber 20 to be detachable. In the exemplary embodiment shown, the device has a sample container 21 which forms or has the sample space 20 . The sample container 21 is preferably provided in the reaction space R in a detachable manner. The sample space 20 or the sample container 21 is preferably made of glass, PTFE or another at least partially microwave-transparent material.

The device 100 also has a heating device 10 for heating the sample material P in the sample space 20 to form an evaporation gas containing the volatile substances X by means of evaporation. The heating device 10 is particularly preferably a microwave heating device. In this case, the reaction space R or at least the sample space 20 is designed as a microwave space. The microwave heating device is set up to generate microwave radiation, preferably by comprising magnetrons (not shown). In principle, however, the heating device 10 can also be another, e.g. conventional, heating device 10 and can have, for example, heating mats, heating cartridges, heating lamps and the like.

The device 100 also has a fluid inlet E, which flows with the sample chamber 20 is connected to feed process gas into the sample space 20. As already described, (process) gases or (process) gas mixtures, in particular with an inert, reductive and/or oxidative character, are preferably suitable as the process gas.

As in 1 shown, the fluid inlet E can have a feed line 51 which can extend into the sample chamber 20 - here into the sample container 21 - and particularly preferably up to the sample material P or towards the sample material P. The fluid inlet E can have a valve 50 that only opens toward the sample chamber P, in particular a check valve 50 or another type of one-way valve, via which the process gas can be supplied.

The process gas can be provided via a process gas source Q, for example. This can, as in 1 is shown schematically, be fluidically connected to the fluid inlet E in order to supply the process gas into the sample chamber 20 in this way. The device 100 can also have a process gas pump F for conveying a process gas via the fluid inlet E into the sample chamber 20; this preferably from the aforementioned process gas source Q.

The device 100 also has a collection space S, which is fluidically connected to the sample space 20 via a fluid path 23, 24, 60 downstream of the fluid inlet E in order to discharge (the) gases from the sample space 20. The fluid path 23, 24, 60 has a condenser 60 in order to condense the evaporation gas in the collection space S. In the exemplary embodiment shown, the device 100 has a collection container 80 which in turn has the collection space S. The collection container 80 is designed here, for example, in the form of a separator, in which the condensed volatile substances (hereinafter also referred to as extract X) separate out over the solvent phase L as a phase of lower density. The solvent phase L is preferably a water phase, which collects in a preferably present outlet part 81 of the collection space S or collection container 80 . For example, the condensed phases X, L and in particular the extract X can be removed via a tap 84 . It is also shown that the collection space S or the collection container 80 can be selectively cooled by means of an optional cooler 83 .

The sample chamber 20, the fluid path 23, 24, 60 and the collection chamber S together form a device chamber V. In the example shown, the fluid path 23, 24, 60 is formed by a return line 23 to be described in more detail, a return line 23 and the condenser 60 connecting tube 24, and the condenser 60. In principle, the fluid path can be formed by any fluidic connection and spaces.

The collecting space S has a fluid outlet A with a pressure relief valve 70, which is designed in such a way that gas in the device space V can escape to the outside when a defined pressure is exceeded. The pressure relief valve 70 may preferably include or be a gravimetric valve. The defined pressure in the device space V can basically correspond to any desired overpressure compared to the environment. The defined pressure is preferably 5 to 800 mbar above ambient pressure, more preferably 10 to 400 mbar above ambient pressure.

The sample container 21 can have a handle element for lifting the sample container 21 . This handle element can, as in 1 shown, preferably be formed by a ring element 25 surrounding the sample chamber 20 or the sample container 21 on the outside.

The reaction space R can also have positioning structures 33 . These are designed in such a way that they interact with the sample container 21 or an alignment element thereof in order to position the sample container 21 in the reaction space R in a defined manner. The alignment element is preferably formed by the grip element or ring element 25 . Centering is preferred, with the alignment element 25 then being designed as a centering ring.

The device 100 can also, as in 1 shown, have a drive unit 32 for driving the sample chamber 20, preferably the sample container 21, in the reaction chamber R in a rotatable manner. In this way, the input of thermal energy into the sample material P can be equalized. For this purpose, the drive unit 32 can preferably have a motor, for example in a gear compartment 30 of the device 100 . The drive unit 32 can preferably have a turntable 31 in order to rotatably drive the sample chamber 20 by rotating the turntable 31 . For this purpose, the turntable 31 can particularly preferably accommodate the sample container 21 . If the positioning structures 33 described above are present, the turntable 31 can preferably have these positioning structures 33, as is shown in 1 is shown as an example.

In order to position or center the sample space 20 or sample container 21, the alignment element (e.g. grip element or ring element) 25 can be arranged so that it can slide, preferably vertically, along the sample space 20/sample container 21 not be. Thus, the sample space 20 or the sample container 21 can first be positioned in the reaction space R—for example on the turntable 31 . By sliding or pushing down the alignment element 25, the latter can be brought into operative contact with the positioning structures 33 in order to position or center the sample chamber 20 or the sample container 21 in a correspondingly defined manner.

As also in 1 is shown, the sample chamber 20 or the sample container 21 can have a cover 22 for selectively opening the sample chamber 20 for receiving and removing sample material P. A seal is preferably provided between the cover 22 and the sample container 21 , which seals off the sample space 20 from the outside and here also from the reaction space R.

Preferably, at least part of the fluid path 23, 24, 60 and preferably also of the collection space S is connected to the cover 22 in such a way that they are moved or lifted together with the cover 22 when the sample space 20 is opened; are preferably lifted here together with the cover 22 from the sample container 21 . It is shown that all attachments, i.e. elements 23, 24, 60, 70, 80 can be connected to the cover 22, with the return line 23 in the illustrated embodiment being mechanically connected to the collection space S and this being mechanically connected to the condenser 60 . In principle, other configurations are also conceivable. For example, the elements to be moved or lifted can be connected and movable via a common frame or a common housing.

The device 100 preferably also has an actuator 40, such as a linear motor 40, by means of which the cover 22 can be selectively opened, ie preferably lifted. The actuator 40 can be stationarily connected to a housing G of the device. If at least part or all of the fluid path 23, 24, 60 is connected to the cover 22, as described above, the actuator 40 can displace all of these connected attachments, including the cover 22, and thus open the cover 22 without first having to manually remove said attachments Need to become. In the event that the sample chamber 20 or the sample container 21 is rotatably accommodated in the device 100, it is preferred that the attachments such as the return line 23 do not rotate, but that a corresponding sliding seal is provided, e.g. between the cover 22 and the return line 23 is.

Said return line 23, 82 can preferably be provided in order to connect the collection space S to the sample space 20 for the return of the condensed solvent phase L, preferably the water phase L, to the latter. As in 1 shown, the return line 23, 82 is arranged in such a way that it prevents a gas flow through the return line 23, 82 when the solvent phase L is present. This is in the embodiment shown 1 achieved in that a part 82 of the return line 23, 82 is oriented obliquely upwards from the downstream to the upstream end, so that the solvent phase L can collect in it and run into the sample chamber 20 via another part 23 of the return line 23, 82. Thus, the return line 23, 82 as a whole is permeable for the solvent phase L, but not for the gas phase. However, other means of achieving this function are also conceivable, such as the use of a siphon or the use of special valves.

As in 1 As shown, the return line 23, 82 may be at least partially (23) coaxial with the feed line 51, for example the feed line 51 running as a smaller diameter tube in the return line 23 as a larger diameter tube. Both tubes 23, 51 can be held in one another, for example with a plug 52, for example on the side of the fluid inlet E. The plug 52 can accommodate the check valve 50 here, for example.

At least part of the return line 23 and part of the fluid path 23 between sample chamber 20 and condenser 60 can, as in 1 shown to be identical.

The fluid path 23 preferably extends out of the sample chamber 20 through the cover 22 or the sample container 21 . Likewise, the feed line 51 can extend through the cover 22 or the sample container 21 into the sample chamber 20 . Furthermore, the return line 23 can also extend through the cover 22 or the sample container 21 into the sample chamber 20 . For this purpose, the cover 22 or the sample container 21 has a corresponding passage opening 26 . A seal is preferably provided in the through-opening in order to appropriately seal the line or path 23, 51 running through the cover 22 or the sample container from the cover 22 or the sample container 21. In the case of the rotatable provision of the sample space 20, this can involve the above-described sliding seal.

The device 100 can preferably also have a temperature sensor 11, 71 for measuring a temperature in the device space V. The temperature sensor can preferably be a control temperature sensor 71 for measuring a temperature in the device space V downstream of the condenser 60, preferably in the region of the fluid outlet A. In this case, the pressure relief valve 70 preferably has the control temperature sensor 71, which is preferably directed into the device space V and which can preferably measure the temperature in the collection space S here. Furthermore, the temperature at the fluid inlet E can be determined with a further temperature sensor (not shown) provided for this purpose. It is also possible to determine the temperature in the sample chamber 20 with a preferably contactless sensor 11, such as an infrared sensor 11. For this purpose, the temperature sensor can preferably have a sample temperature sensor 11, which is assigned to the sample chamber 20 for measuring a temperature of the sample material P

The device 100 preferably also has a control unit. Such is basically well known and is therefore for the sake of clarity in the 1 not shown. The control unit is preferably used for the ((partially) automated) control of an extraction process by means of the device 100, preferably the heating device 10 and/or the fluid inlet E (e.g. the valve 50) and, if present, also the process gas pump F and /or the actuator 40 and/or the drive unit 32.

The control unit is preferably set up in such a way to control the device 100 on the basis of at least one of the temperature sensors 11, 71. For example, the control unit can be set up in such a way that it receives measured temperature values from the temperature sensors 11, 71 and regulates the heat output of the heating device 10 as a function of predetermined process parameters in order to optimally control the extraction process. If present, that control unit can also control the actuator 40 in order to enable the sample material P to be removed, for example via the sample container 21 . If present, the control unit can also control the drive 32 e.g. for driving the turntable 31 in rotation. The process gas pump F, if present, can also be controlled via the control unit for the defined and process-dependent supply of process gas. It is also conceivable to control the fluid inlet E, for example via its valve 50, in order to control a process gas supply in a defined manner.

A method according to the invention for extracting volatile substances X from sample material P, preferably by means of a device 100 of the present invention, is described below.

First, the sample material P is received in the sample space 20 of the reaction space R, for example filled into the sample space 20 . The sample chamber 20 can be formed by the sample container 21 described above, which is then used to hold the sample material P and can be removed from the reaction chamber R as required. When optimally inserting the optional sample container 21 into the reaction space R, the sample container 21 preferably interacts with positioning structures 33 of the reaction space R such that the sample container 21 is then positioned or centered in the reaction space R in a defined manner.

Then the process gas is fed into the sample space 20 via the fluid inlet e. The process gas can be fed in, for example, in an amount per minute which essentially corresponds to the volume of the device space V, preferably ¼ to 2/1 of the volume of the device space V, more preferably ½ to 3/2 of the volume of the device space V. The process gas can preferably be at least partially a reductive, oxidative or inert gas, more preferably a gas mixture with an argon fraction, particularly preferably a non-combustible gas mixture with an argon and hydrogen fraction.

Then, the sample material P is heated to form an evaporation gas containing the volatile matter X from the sample material P by evaporation. The heating is particularly preferably carried out by means of microwaves. The sample space 20, preferably the sample container 21, is preferably moved or rotated at least during the heating of the sample material P in the reaction space R, in order to bring about a homogeneous heating of the sample material.

The supply of process gas and/or the heating of the sample material P is preferably controlled as a function of a temperature in the device space V or the collection space S and/or a temperature of the sample material P.

The device space V described above is preferably purged before the sample material P is heated by the supply of the process gas via the fluid inlet E via the pressure relief valve 70 .

The gases from the sample chamber 20 are discharged via the fluid path 23, 24, 60. The discharged evaporation gas is condensed into the plenum S, wherein the sample space 20, the fluid path 23, 24, 60 and the plenum S together form the device space V described above. If a defined pressure is exceeded in the device space V, the gas in the device space V escapes to the outside via the pressure relief valve 70 of the fluid outlet A of the collection space 80.

The pressure relief valve 70 may preferably include or be a gravimetric valve. The defined pressure in the device space V can basically correspond to any desired overpressure compared to the environment. The defined pressure is preferably 5 to 800 mbar above ambient pressure, more preferably 10 to 400 mbar above ambient pressure.

The process gas is preferably supplied during all or part of the extraction process.

The collection space S preferably has the return line 23, 82, via which the condensed solvent phase L, preferably a water phase L, can be returned to the sample space 20. The return line 23, 82 is preferably arranged in such a way that it prevents a gas flow through the return line 23, 82 when the solvent phase L is present. It is preferred to fill the collecting space S with a predetermined amount of solvent L before the start of the heating or the evaporation process, particularly preferably with such an amount (e.g. 200-300 ml) that the gas flow through the return line 82 is prevented. The filling can be done by removing the overpressure valve 70 and filling in the solvent L through the corresponding opening 72 .

With the device 100 according to the invention and the method according to the invention, it is thus possible in particular to flush the device space V with process gas before the start of the evaporation process, but also—and this with particularly low process gas consumption—to displace gas produced during the evaporation process by means of replenished process gas. In this way, the quality of the resulting extract X or of the condensed evaporation gas phase containing the volatile substances X can be ensured at any time during the extraction.

As an independent aspect, the present invention also relates to a device 100 for extracting volatile substances X from sample material P. The device 100 has a reaction chamber R with a sample chamber 20 for receiving the sample material P, and a heating device 10 for heating the sample material P in the sample chamber 20 to form an evaporation gas containing the volatile substances X by means of evaporation. The sample chamber 20 is formed by a sample container 21 which is arranged in the reaction chamber R in a detachable manner. Furthermore, the reaction space R has positioning structures 33 which interact with an alignment element 25 of the sample container 21 in order to position the sample container 21 in the reaction space R in a defined manner, preferably to center it.

In this case, the alignment element 25 can be arranged such that it can be moved or slid vertically along the sample space 20 or sample container 21 . Thus, the sample chamber 20 or the sample container 21 can first be positioned in the reaction chamber R--for example on the turntable 31 described above. By sliding or pushing down the alignment element 25, the latter can be brought into operative contact with the positioning structures 33 in order to position or center the sample chamber 20 or the sample container 21 in a correspondingly defined manner.

The alignment element 25 can be designed as a gripping element for gripping and handling or lifting the sample container 21 and/or the ring element surrounding the sample chamber 20 or the sample container 21 on the outside.

The device 100 can also have the rotary plate 31 described above, which in turn can have the positioning structures 33 .

The device of this independent aspect can also have all the other features of the device 100 described above, as are also exemplified in FIG 1 are shown.

The present inventions are not limited by the exemplary embodiments described above, insofar as they are covered by the subject matter of the following claims. In particular, the optional features of the exemplary embodiments can be combined with one another as desired, and the features of the exemplary embodiments can be combined with one another and exchanged in any way.

Claims (30)

Device (100) for extracting volatile substances (E) from sample material (P), having a reaction space (R) with a sample space (20) for receiving the sample material (P), a heating device (10) for heating the sample material (P) in the sample chamber (20) for forming a vaporization gas containing the volatile substances (E) by means of evaporation, a fluid inlet (E) which is fluidically connected to the sample chamber (20) in order to feed process gas into the sample chamber (20), a collection chamber (S), which is fluidically connected to the sample chamber (20) via a fluid path (23, 24, 60) downstream of the fluid inlet (E) in order to discharge the gases from the sample chamber (20), the fluid path (23, 24, 60) has a condenser (60) to the evaporation gas in the collecting space (S), wherein the sample space (20), the fluid path (23, 24, 60) and the collecting space (S) together form a device space (V), and wherein the collecting space (S) has a fluid outlet (A ) having a pressure relief valve (70), which is designed such that in the device space (V) located gas can escape to the outside when a defined pressure is exceeded. Device (100) according to claim 1 , wherein the process gas is an inert gas or a reactive gas or a mixture of said gases. Device (100) according to claim 1 or 2 , wherein the process gas comprises argon or hydrogen or a mixture of argon and hydrogen, the proportion of hydrogen in the process gas, if present, preferably being less than or equal to 5% by volume, more preferably 0.1% by volume to 5% by volume. % amounts to. Device (100) according to any one of the preceding claims, wherein the heating device (10) is a microwave heating device. Device (100) according to any one of the preceding claims, wherein the fluid inlet (E) has a feed line (51) which preferably extends into the sample chamber (21). Device (100) according to any one of the preceding claims, wherein the fluid inlet (E) has a valve (50) opening only towards the sample chamber (20), in particular a non-return valve (50), via which the process gas can be supplied. Device (100) according to any one of the preceding claims, further comprising a process gas source which is fluidically connected to the fluid inlet (E) in order to feed process gas into the sample chamber (20). Device (100) according to any one of the preceding claims, further comprising a process gas pump for conveying a process gas, preferably from the process gas source, via the fluid inlet (E) into the sample chamber (20). Device (100) according to any one of the preceding claims, furthermore having a sample container (21) which forms or has the sample space (20). Device (100) according to claim 9 , wherein the sample container (21) is detachably provided in the reaction space (R). Device (100) according to claim 9 or 10 wherein the sample container (21) has a handle element, preferably a sample chamber (20) or the sample container (21) surrounding the ring element (25) on the outside, for lifting the sample container (21). Device (100) according to one of claims 9 until 11 , wherein the reaction space (R) has positioning structures (33) which interact with the sample container (21), preferably an alignment element of the same, which is particularly preferably formed by its grip element or ring element (25), in order to position the sample container (21) in the reaction space (R) to position defined, preferably to center. Device (100) according to any one of the preceding claims, further comprising a drive unit (32) for rotatably driving the sample chamber (20), preferably the sample container (21), in the reaction chamber (R). Device (100) according to Claim 13 , wherein the drive unit (32) has a turntable (31) which preferably receives the sample container (21), wherein the turntable (31) preferably has the positioning structures (33). Device (100) according to any one of the preceding claims, wherein the sample chamber (20), preferably the sample container (21), has a cover (22) for selectively opening the sample chamber (20) for receiving and removing sample material (P). Device (100) according to claim 15 , wherein at least part of the fluid path (23, 24, 60) and preferably also of the collection space (S) are connected to the cover (22) in such a way that they move together with the cover (22) when the sample space (20) is opened or be raised. Device (100) according to claim 15 or 16 , Preferably further comprising an actuator (40) by means of which the cover (22) can be opened selectively. Device (100) according to any one of the preceding claims, further comprising a collection container (80), preferably in the form of a separator, which comprises the collection space (S). Device (100) according to one of the preceding claims, wherein the collection space (S) has a return line (23, 82) for returning a condensed solvent phase (L), preferably a water phase (L), into the sample space (20). Device (100) according to claim 19 , wherein the return line (23, 82) is arranged in such a way that it prevents a gas flow through the return line (23, 82) when the solvent phase (L) is present. Device (100) according to claim 3 as well as one of claim 19 or 20 , wherein the return line (23, 82) is at least partially coaxial with the supply line (51). Device (100) according to one of claims 19 until 21 , wherein at least part of the return line (23) and part of the fluid path (23) between the sample chamber (20) and condenser (60) are identical. Device (100) according to any one of the preceding claims, further comprising a temperature sensor (11, 71) for measuring a temperature in the device space (V). Device (100) according to Claim 23 , wherein the temperature sensor has a sample temperature sensor (11) which is assigned to the sample chamber (20) for measuring a temperature of the sample material (P). Device (100) according to Claim 23 or 24 , wherein the temperature sensor comprises a control temperature sensor (71) for measuring a temperature in the device space (V) downstream of the condenser (60), preferably in the region of the fluid outlet (A). Device (100) according to Claim 25 , wherein the pressure relief valve (70) has or carries the control temperature sensor (71). Device (100) according to any one of the preceding claims, wherein the pressure relief valve (70) is or comprises a gravimetric valve. Device (100) according to any one of the preceding claims, wherein the defined pressure in the device space (V) is 5 to 800 mbar above the ambient pressure, preferably 10 to 400 mbar above the ambient pressure. Device (100) according to any one of the preceding claims, further comprising a control unit for controlling an extraction process by means of the device (100), preferably the heating device (10) and/or the fluid inlet (E) and, if present, also the process gas pump (F) and/or the actuator (40) and/or the drive unit (32). Device (100) according to claim 29 as well as one of Claims 23 until 26 , wherein the control unit is set up to control the device (100) on the basis of at least one of the temperature sensors (11, 71).

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