WO2018103851A1

WO2018103851A1 - Device, particularly extraction devices or evaporation device, and method

Info

Publication number: WO2018103851A1
Application number: PCT/EP2016/080282
Authority: WO
Inventors: Reto Gehrig; Ralph Baumgartner; Claudio ZIGERLIG
Original assignee: Büchi Labortechnik AG
Priority date: 2016-12-08
Filing date: 2016-12-08
Publication date: 2018-06-14
Also published as: EP3551309A1

Abstract

The invention relates to a device, particularly an extraction device or evaporation device, comprising at least one receiver for a container (4), at least one heating element for said container (4), at least one light source (1), at least one sensor (2), and an evaluation unit. The light source (1) and/or the sensor (2) are arranged outside of the container (4) such that a light signal (3) generated by the light source (2) and passing through the container can be detected by the sensor (1).

Description

Device, in particular extraction devices or evaporation device and method

The invention relates to devices, in particular extraction devices and / or evaporation devices, a method for cup recognition and / or level detection, a cooler for devices, methods for extraction, a kit comprising a device, a filter assembly for the hydrolysis and a hydrolysis tube / chamber according to the preambles of the independent claims.

In known solid-liquid extractors, for example soxhlet extractors, a solvent is evaporated in a heatable vessel and conducted via a vapor line into an extraction vessel arranged above the vessel. The vessel is intended for Recordin ^¬ me the material to be analyzed. Such extractors have a cooler for condensing the extraction solvent or the solvent. The extract has components of the material to be extracted, which is analyzed after the extraction. This so-called analyte must be protected in order to avoid destruction of the analyte so that the analyte can be ^¬ after extraction completely analy Siert during extraction. Further known extractors are designed, for example, for hot extraction (HE), for example according to the Randall method, or continuous extraction, for example according to the Twisselmann method. Evaporation devices are known, for example, for evaporation according to Kjeldhal. Known extractors lift the vessel from the aluminum block heater to protect the analyte at the end of the extraction to prevent complete evaporation of the solvent by the residual heat of the block and thus dry running of the analyte. This is described for example in WO 97/00109 AI. Is Nachtei ^¬ lig in such extractors that the vessel must be lifted designed and to a complex lifting mechanism is erfor ^¬ sary. It is therefore the object of the invention to overcome the disadvantages of the prior art. In particular, improved extraction devices or evaporation devices are to be provided in which the analyte is protected and thus safer analyzes of the sample are possible. Furthermore, extraction devices are to be provided, the export is traction process efficiently, eg. In terms of Geschwin ^¬ speed and applications of extraction devices or the recovery of solvents. Furthermore, improved filter arrangements are to be provided.

The invention relates to a device, particularly an ex ^¬ traction device or evaporation device comprising at least one seat for a container, at least one heating element ^¬ for the container, at least one light source, at least one sensor and an evaluation unit. The light source and / or the sensor are arranged outside the region for the loading container ^¬ that with the sensor a signal generated by the light source through trespassing through the area for the container light signal is detected. In this way, a device is provided with which the level in the container can be determined optically. The heating element is preferably a heating ^¬ plate, on which the container is positioned. Devices may be Soxhlet Extractors, Hot Extractors, Continuous Extractors or Kjeldahl devices.

The previously described arrangement of light source and sensor is particularly advantageous in the case of an extraction device when an analyte accumulates in the container during extraction. The container is heated during extraction by the heating element to evaporate a solvent. This condenses on a cooling device, drips onto the sample and then collects again in the container. Thus, more and more analyte collects in the container and excess solvent can be discharged from the extraction device. In order to ensure that the desired amount of solvent is always present, ie the residual amount is controllable, and thus to prevent damage to the analyte, in particular by heat, monitoring of the process is made possible with the device according to the invention. Furthermore, can be recovered in such Lö ^¬ solvents. For special applications in the food / feed sector, for example, the determination of fat, such a

Post-drying step eliminated or at least shortened.

Furthermore, the light source and the sensor allow a container recognition, so that it can be detected whether a container is in the device. A procedure is accordingly only started when a container has been positioned in the device.

Furthermore, the device preferably comprises an evaluation unit with which the light signals detected by the sensor can be evaluated and / or processed. In this way, the process can be monitored within a process. The evaluated and / or processed signals can be used for the control and / or regulation of the process. In the evaluation unit Comparative data of extraction processes can be stored as standards / profiles which can be accessed by the process monitoring evaluation unit. The comparison data can be stored in a library in the sense of a collection of comparative data. Likewise, the evaluation unit can learn, ie information from previously performed procedures can be taken into account; that is, a reference can learn who ^¬ so that information, for example, from previously performed processes. with a special solvents can be used as a reference to control / regulation of the process. For process monitoring can be determined whether or not a container has been positioned in the device so that the process, in particular ^¬ sondere the heating is not started. It can also be determined whether a positioned container is full or empty. Accordingly, intermediate states can also be determined, for example, based on the signal change due to rising bubbles in the container, these in each case positionally.

An analyte is understood here and below to mean a substance which is extracted from a sample during the extraction and can subsequently be analyzed in order to characterize or quantify the sample. The analyte in an evaporation device is understood here and below to mean a substance which is evaporated during the evaporation and can subsequently be analyzed.

Furthermore, the light source and / or the sensor can be arranged such that a change in the fill level of the container can be detected. In this way, the progress of the process in the device is monitored. In this case, the light source and / or the sensor can be arranged at the same height. Likewise, they can be arranged at different heights relative to each other. The light source and the sensor can be adjusted horizontally. right, in particular to the heating element, in particular to Heizplat ^¬ te, be arranged to the liquid surface. Alternatively Kgs ^¬ NEN light source and / or the sensor be oblique, in particular to the liquid surface, arranged to allow, for example, an improved bubble detection.

The light source may be configured such that a court ^¬ tetes light signal, in particular pulsed light signal, aussend ^¬ bar is. The light signal can be transmitted continuously or pulsed. Pulsed light signals enable extraneous light suppression.

The light source and the sensor can be arranged such that a light signal emitted by the light source passes through the container and is reflected by a reflector in the direction of the sensor. In this case, the light source, the sensor and the reflector may be arranged such that the light signal reflected by the reflector again passes through the container. So the light signal passes substantially centrally irrespective of the shape of the container, which improves the quality of the Sig ^¬ Nals through the container. The light source and sensor may be arranged nebenei ^¬ Nander in the same plane.

The reflector can be arranged on a protective shield or a protective hood of the device. So it can be detected whether the shield is in position. This may serve to detect a closed or open state of a device. This principle is also independent of the device according to the invention in arrangements of light source, sensor and reflector advantageous. For example, the shield can assume an open and a closed position, wherein in the closed position, the light beam is reflected in the direction of the sensor and in the open position of the light beam is not reflected on the sensor or is not reflected. Such can be detected on the basis of the detected from the sensor Lichtsig ^¬ Nals whether the device is operational. The light source and the sensor can also be arranged such that the light signal passes through a round container eccentrically. By "eccentric passing through" refers here and in the following that the light signal does not meet perpendicularly the wall of the Behäl ^¬ ters, but (in a round container) in an edge region, that is in a distant from the center of the container area. Is Thus, a higher Depth of detail achieved as when the signal passes through the center of the container, which can be explained by the different lateral offset of the light signal due to the different refraction.

"Eccentric" below refers here and in the following that the light signal having an angle equal to 90 ° applies, for example, in a circular container on the wall of the container on ^¬.

The light source and the sensor can be arranged such that the light signal passes through a round container in the middle.

The light source may be a light emitting diode for the exterior of light (LED, light-emitting diode) or a laser diode and / or the sensor to a photodiode or a phototransistor, in particular an IR photodiode or a Photowider ^¬ stand (LDR, light dependent resistor) act. The light source is preferably a laser.

The light source and the sensor are preferably positioned at the same height relative to the area for the container, in particular sondere at a height of 5 to 15 mm, preferably 7.5 to 12.5 mm, particularly preferably 10 mm, above the heating element, insbesonde ^¬ re the heating plate. A light emitted from the light source ^¬ signal applies preferably to the wall of the container in an angular angle equal to 90 °.

When using red light, the signal is in a wavelength region of Wel ^¬ preferably 620-780 nm, more preferably 635-675 nm.

The source may one, in particular pulsed, signal in the infrared range, in particular in a wavelength range of 750 to 950 nm, especially in the range 830-870 nm, emit ^¬. The sensor has a reception range which at least partially encompasses the wavelength range of the emitted signal, and is for example in the range from 600 to 1000 nm, in particular 750 to 950 nm. The use of pulsed signals increases the signal-to-noise ratio (sig). Nal-to-noise ratio) improved, ie achieved a Fremdlichtunterdr- ckung.

The sensor may be associated with a filter, in particular a low-pass filter. This improves the signal-to-noise ratio. The filter may be an active or passive hardware and / or software filter. Here, the hardware side can be provided an RC network and / or software side, a finite impulse response (FIR) or infinite response filters (HR) or a Gelei ^¬ average value. Furthermore, the device can have at least one cooling element, in particular a reflux condenser. The cooling element is preferably arranged above the area for the container. A further aspect of the invention relates to a method for detecting containers and / or filling level detection by means of a device which, in particular, is configured as explained ^above . The method comprises the steps of emitting a light signal from the light source through an area for a container, the light signal preferably passing through the region for the container eccentrically, detecting the light signal by means of the sensor and evaluating the detected signal with ^{¬ means of} the evaluation unit. It has been shown that a light signal which passes eccentrically through the container provides a higher level of detail. It is assumed that this is done on the basis of the refractive ^¬, relation character of the lateral offset of the signal in the edge region of the container. In this way, the process, in particular the extraction process or the evaporation process, can be monitored particularly precisely in order to protect the analyte. By monitoring the process, an analyte is provided which has not been damaged or destroyed by the heat during the process. Furthermore, it is basically possible to check whether a container is in the device. The process and in particular the heater is only started when a container, in particular the richti ^¬ ge container for the implementation of a special method, located in the apparatus. Furthermore, process parameters can be controlled and / or regulated during the process based on the evaluation. These process parameters may be, for example, the heating power of the heating element and / or the cooling capacity of the cooling element. Thus, the method can be controlled and / or regulated in such a way that an extraction that is gentle on the analyte is carried out, or the overall performance of the device is improved. This is particularly advantageous in automated operation. Preferably, the evaluation unit generates information dahinge ^¬ basis whether a container is positioned, whether this is sufficiently filled and whether gas bubbles rise during the extraction. For example, in the use of azeotropic solvents ^¬ convey a constant simmer is set, as indicated for example by rising gas bubbles.

Furthermore, the evaluation unit provides information as to whether the correct solvent for a specific method is in the container. This can be done using a plausibility tests, and from set Prozessparame ^¬ tern and information from the evaluation of the progress of the proceedings is compared with past experience. If the current measured values do not correspond to the expected measured values, for example by comparison with comparative data, then there is no plausibility. The measured values change due to rising bubbles or the decreasing filling level. The refractive index and / or the absorption also change in the course of the process. The process can accordingly be controlled or stopped ^¬ to. The heating power of the heating element can be reduced or he ^¬ increased.

Furthermore, due to the information of the evaluation unit, the heating element can preferably only be started if a

Container has been positioned on the heating element and / or is suffi ^¬ accordingly filled. The controller can thus be designed such that the heating element is turned on when a container is positioned on the heating element and that the heating element is switched off when the level of the container falls below a limit ^¬ value or the container is ent ^¬ removed from the heating element. Optionally, a premature shutdown vorgese ^¬ hen. A further aspect of the invention relates to a device, in particular an extraction device or evaporation device, in particular as explained above, comprising at least one cooling element, a valve and an overflow connected to the valve via a first connection. The valve is arranged on a wall of the device, in particular on a wall of the cooling element, or arranged via a second connection from ^¬ serhalb the cooling element. The first and / or the second connection may be a hose or a tube, preferably made of glass. The second connection can lead as an extension of the first connection through the wall of the cooling element, when the valve is arranged outside the cooling element. The valve is designed in such a way that at least one first open position and one second closed position can be captured. A solvent which condenses on the cooling element is dischargeable through the valve in the first open position and optionally introducible into a container comprising an analyte. The overflow is designed such that solvent which condenses on the cooling element and the valve in the second ge ^¬ closed position is accumulated in the first compound drips off via the overflow. Of course, the dripping does not take place until the volume of pent-up solvent is greater than the volume of the first compound. The overflow is located in the first junction prior to entering a flared funnel positioned above the overflow. The solvent drips onto the sample, which is located below the cooling element. In the first open position, the analyte can be protected by introducing a safety volume into the container formed by the condensed solvent. For this purpose, the solvent, which has been dammed in front of the valve, discharged through the valve in the first open position and introduced into the container as needed. Destruction of the analyte by overheating is thus prevented. A rapid reaction with residual heat of the heating element is possible. By properly switching the valve, the destruction of the analyte can be prevented by overheating towards the end of the process. Furthermore, the arrangement of the

Overflow in the first compound before entering the expanding funnel only a small amount of solvent are stowed on ^¬ . In this way, you can significantly reduce process times, for example in multi-cycle operation. The overflow is positioned higher than the valve.

The valve can be a solenoid valve. Solenoid valves switch very fast. So the valve can be particularly fast rule Zvi ^¬ the two position switch back and forth, so that a quick introduction of the safety volume is optional in the container. The valve can also be a pneumatic valve. The valve can be controlled, in particular with an ^extraction device as explained above. A further aspect of the invention relates to a cooler, in particular for a device as discussed previously, we comprising ^¬ nigstens a cooling element, a valve and connected to the valve via a first connection overflow. The valve is arranged on a wall of the radiator or arranged outside the radiator via a second connection. The first and / or the second connection may be a hose or a tube, preferably made of glass. The second connection can lead as an extension of the first connection through the wall of the radiator, when the valve is located outside the radiator. The valve is configured such that at least a first open position and a second closed position are ingestible. A Lö ^¬ solvents, which condenses on the cooling element, is ausleitbar through the valve in the first open position and optionally in the a container comprising an analyte introduced or optionally in an extraction device in an area, in particular a sample tube of an extraction chamber, comprising a sample introducible. The overflow is designed such that solvent, which condenses on the cooling element and is dammed up on the valve in the second closed position in the first connection, drips off via the overflow. Of course, the dripping does not take place until the volume of pent-up solvent is greater than the volume of the first compound. The overflow is located in the first junction prior to entering a flared funnel positioned above the overflow. The solvent drips onto the sample, which is located below the cooling element. In the first open position of the analyte can be used in the container or in the region of the sample having formed ge be protected ^¬ from the condensed solvent by introducing egg nes safety volume. For this purpose, the solvent which has been dammed in front of the valve is discharged through the valve in the first open position and, if necessary, introduced into the container or in the area having the sample introduced. A destruction of the

Analytes by overheating is thus prevented. A rapid reaction with residual heat of the heating element is possible. Furthermore, the arrangement of the overflow in the first connection before entry into the expanding funnel requires only a small amount of solvent to be dammed up. In this way, you can significantly reduce process times, for example in multi-cycle operation. The overflow is positioned higher than the valve. Another aspect of the invention relates to a method for extraction with an extraction device comprising a cooler comprising a cooling element, such as especially tert previously erläu ^¬, or with a condenser comprising a cooling element such as INS special explained in advance. A valve accumulates in the second closed position on the cooling element condensed solvent ^¬ medium in a compound of the valve and an overflow, which drips over the overflow. Of course, the dripping does not take place until the volume of pent-up solvent is greater than the volume of the first compound. The overflow is located in the connection from the valve and overflow prior to entering a flared funnel positioned above the overflow. The overflow is positioned higher than the valve. Here, the Lö ^¬ solvents dropped on the sample which is located below the Kühlele ^¬ management. The valve remains in the second geschlosse ^¬ NEN position when the extraction in the circulation takes place, that is, solvent evaporates, condenses on the cooling element, is dammed listed, dropwise via the overflow on the sample from the sample in the container, etc. The valve directs in the first open position on the cooling element condensed solvent from and op ^¬ tional in the container comprising the analyte or in the area having the sample a. With the method according to the invention, destruction of the analyte is prevented since, as previously explained, a safety volume of the solvent is introduced into the container or into the region containing the sample and the container dries out and overheats, for example due to the residual heat of the heating element, in particular the heating plate , is prevented. In this way, solvent can be recovered and the analyte can be protected if necessary.

Furthermore, the valve can be controlled and / or regulated as a function of the detected signal of an arrangement of a light source and a sensor on the container as previously explained. If a lower level in the vessel before or is such a registered, the valve from the first position offe ^¬ NEN can switch to the second closed position and the Cooling element condensed solvent through the overflow into the container with the sample drain.

Alternatively, the valve may switch from the second closed position to the first open position. Condensed and pent-up solvent is then discharged and introduced to protect the analyte in the container or in the area containing the sample. In this way, the progress of the extraction is controlled and / or regulated. Likewise, the extraction can be stopped or terminated.

Another aspect of the invention relates to a device, in particular an extraction device or evaporation device, in particular as explained above, with a cooler and at least one position with a footprint for a container. The cooler has a contact surface for connection of a method-specific glass part, said glass part-specific methodenspe ^¬ has at least one compatible interface on ^¬. The position has at least one height-adjustable Hal- esterification which is designed such that the distance between the stand surface of the container and the contact surface of the cooler can be adjusted such that at least two a are ^¬ brought under ^¬ schiedliche method specific glass components in position.

The adjustment path of the bracket may be ^¬ rich from 200 to 500 mm> 200 mm, particularly in Be.

The footprint of the container may be a heating element, in particular a ceran field.

If the device has more than one position, the distance between the base surface and the contact surface of the respective ligen position can be adjusted by means of the holder so that different method-specific glass parts can be introduced at the different positions. Such Kings ^¬ nen different methods are carried out at different positions. The heating elements of different positio ^¬ nen may additionally be controlled individually and / or regulated. In this way, a device is provided with which several methods can be carried out simultaneously, in parallel, and with which, depending on the choice of method-specific glass parts different methods can be performed simultaneously in the same device. Thus, the processes are simplified and accelerated in the laboratory and increased by hö ^¬ here Unit utilization efficiency. The two or more positions can be heated individually in particular by the respective heating element which is assigned to a position.

The method-specific glass parts are in particular selected from the group comprising

a) glass parts for the methods Soxhlet (Sox), hot extraction (HE), and continuous extraction according to Twisselmann (ECE), as well as

b) Universal glass parts with which all of the above metho ^¬, Soxhlet warm and continuous extraction (CE) to the Continuous extraction by Twisselmann (ECE) can be carried out. In this way, a wide variety of method-specific glass parts can be used.

The holder is preferably attachable to a fastening element of the device and thus in particular height-adjustable.

By means of the positioning of the holder, for example the height of the holder in the device, a coding is preferably carried out. Semi asked. The position of the holder to define the ver ^¬-inverting method-specific pieces of glass at the position of the apparatus and hence the methods to be used at the position of the device.

The height of the holder, which defines the distance between the base surface and the contact surface, can be detected by means of a sensor. In this way it can be checked which metho ^¬ de to be performed at one position.

This can be read out at several predefined possible heights of the holder, a method defining code. For this purpose, it is detected by means of a sensor whether the holder is at one of the predefined heights and at which heights the holder is not located. This makes it possible to determine directly and unambiguously which methods should be carried out at a position.

It is also possible to provide further holders or guides which define further positions of method-specific glass parts. For example, this can be in devices for Soxhlet, ECE and Universal, the height of the interface Zvi ^¬ rule container and the extraction vessel. The co ^¬ dation is so complex because of the second or more additional selectable mounting positions.

The cooler is preferably movable, for example, resiliently mounted on the device. In this way, the cooler can be connected or pressed to method-specific glass parts via a compatible interface. The fastening ^element can be höhenver ^¬ adjustable, for example. By being attached to a lift. Another aspect relates to a kit comprising a Vorrich ^¬ tung, in particular an extraction device or evaporation device, in particular as discussed previously, with ei ^¬ nem cooler comprising a contact surface for connection of a method-specific glass member, the method-specific glass portion comprising at least a compatible interface. The apparatus further includes at least one position on ^¬ took up for containers. The position has at least one hö ^¬ henverstellbare holder, which is designed such that the distance between the base of the container and the contact surface of the radiator is adjustable so that wenigs ^¬ least two different method specific glass parts in the position can be introduced. The kit has method-specific glass parts, the method-specific glass parts have one or more interfaces for connecting method-specific glass parts. The height-adjustable mountings are preferably positionable in a fastening element, preferably a ribbed plate, with a plurality of predefined receptacles, for example at different heights. Has the advantages direction several positions, can, to perform different methods Me ^¬ at different positions, the heating elements of different positions in addition be controlled individually and / or regulated. The method-specific glass parts are designed such that they can be attached to the at least one interface of the positions. In such a way, the user is provided a kit comprising all the components that are necessary for the simultaneous carrying out of differing ^¬ Chen methods in a device. Another aspect of the invention relates to a method with a device, in particular with a device as previously explained or a kit as explained above, wherein the device has a plurality of positions. At least two different schiedliche method specific glass parts are attachable to differing ^¬ chen positions or mounted, and at positions different methods are carried out and / or un ^¬ terschiedliche solvent.

The methods may in particular be selected from the group comprising Soxhlet, for example Soxhlet Standard (Sox st.) And Soxhlet warm (Sox w.), Hot extraction (HE), continuous extraction (CE) and continuous extraction according to Twisselmann (economic continuous extraction, ECE), Kjeldhal.

The different methods can be carried out at the same time. For example, the methods can be started and / or stopped at the same time. Similarly, one method can be started while one method is still running at another position. This allows the user to simultaneously perform different methods as well as efficient use of the device. Empty times of individual positions of the device are thus reduced.

The different methods can be individually controlled and / or regulated at the different positions. Ex ^¬ traction at different positions are controlled so individually and so efficiently used the device. If, for example, an extraction at one position lasts longer, for example due to a complex composition of the sample, a complete extraction independent of the other extraction is possible by means of the individual control and / or regulation. Another aspect of the invention relates to a device, in particular an extraction device or an evaporation ^¬ device, with a receptacle for at least one Lösungsmit ^¬ telauffangbehälter and with a line with a connection for the connection of the solvent effluent of the device and the solvent catcher. In this way, the collecting container is easily accessible in or on the device and is thus advantageously located, for example, in the fume hood of the device.

Preferably, the apparatus in the region of the Lösungsmittelab ^¬ flow to a cooling element for condensing vapors. In this way, a solvent which possibly evaporates in the collecting container is condensed in the collecting container.

The connection can be normalized and is so mountable on standardized Ge ^¬ squirm or counterparts. A preferred thread is GL45.

In the connection one or more solvent drain ^¬ lines can be accommodated. When using multiple solvent drain lines, the same solvent can be collected from processes of different methods and / or positions in the same receiver. This reduces the number of required collection containers. Different solvents can be combined in the collecting container.

The apparatus may comprise a unit for the level measurement and / or level gauge of the solvent capture container to ^¬. In this case, a light barrier comprising a Lichtquel ^¬ le, a sensor and an evaluation unit as previously described may be positioned in the same way on the solvent capture container. In this way it can be determined and displayed whether the collecting container can absorb solvent or this should be changed or emptied. If the collecting container is full, the process can be interrupted and the collecting container can be exchanged. The solvent collecting container may be a bottle, preferably a commercially available laboratory bottle, more preferably a 2 ^liter bottle. Such commercial Laborfla ^¬ rule can be used compared to conventional tanks common laboratory as a collecting container. These are easy to remove from the device or from the device to close and store. The contents of the collection container does not have to like are transferred as with her ^¬ conventional tank into another bottle or. This simplifies the handling as well as the safety, since the collecting container can remain in the chapel.

Another aspect of the invention relates to a filter arrangement for the hydrolysis, eg., The fat extraction from a sample with- means of acid digestion followed by fat extraction from egg ^¬ ner sample, for example. By the Weibull Stoldt method. The filter ^¬ arrangement has a lid with perforation, a filter based on cellulose and a filter protection with perforation. In this case, the filter is arranged in the lid. The filter guard is placed on the filter. Such a filter arrangement has a simpler structure than conventional filter arrangements of a glass frit, kieselguhr, for example celite, and sand

The filter is preferably a resin-impregnated, in particular melamine-impregnated, filter or a plastic-reinforced cellulose filter. Thus, a filter with a particularly good capacity and high chemical resistance is provided.

The filter protection may have a coding, in particular one or more cams, for alignment on the lid. In this way, the lid and the filter protection can be aligned relative to each other. The lid and the filter protection can have corresponding perfo ^¬ turing. This achieves a higher efficiency in the hydrolysis. The filter protection can have a, in particular circumferential, web on the underside, so that the filter protection is in contact with the filter only in the outer region of the filter, while the central / central region of the filter is not in contact with the filter protection. This will not damage the filter. A bridge is also understood as a rib. The web helps to waterproofing ^¬ th by pressing.

Another aspect of the invention relates to a sample tube or a sample chamber with a filter arrangement as previously explained.

Another aspect of the invention relates to a particular punched sample holder for extraction. The sample holder has a perforation in the outer area and a central opening. The sample holder is in the use state on the

Glass shoulder of a sample tube an extraction chamber positioned. Reference is made to the explanations to FIGS. 11 and 12. Another aspect of the invention relates to a device, in particular extraction device, in particular as previously explained, wherein the device has a rear wall as a base ^¬ side and protruding leg. The device has a plurality, preferably 2 to 12, more preferably 3 to 10, most preferably 4 to 8, positions, which are arranged in particular ^¬ along the two legs or along one of the two legs. The positions are individually controllable and / or adjustable. The positions have recordings for method-specific glass components. The plurality of positions may be arranged along the legs. When used as intended, the back side (base is the longer base of a trapezoid) of the floor plan is away from the user so that the multiple positions are easily accessible. The shape of the device is also space-saving compared to a device with a linear arrangement of the positions.

The invention will be explained in more detail below with reference to illustrations of exemplary embodiments. Show it:

Fig. 1A: Schematic arrangement of a light source and a Sen ^¬ sors to a container according to the invention the extraction device;

FIG. 1B: Schematic arrangement of a light source and a Sen ^¬ sors to a container with evaluation unit and Steue ^¬ tion;

2 to 6: Schematic arrangements of exemplary embodiments of the extraction device according to the invention;

Fig. 7: A diagram with level measurements of different solvents during the extraction;

Fig. 8: A diagram of a level measurement of cyclohexane during the extraction;

Fig. 9: A diagram of a level measurement of methanol during the extraction; 10A: sectional view (A) of a cooler according to the invention for an extraction device;

10B: a perspective view of a cooler according to the invention for an extraction device;

Fig. IIA: exploded view of a filter arrangement according to the invention; Fig. IIB: A perspective view of the lid of the inventive filter assembly;

Fig. HC: A perspective view of the filter protection of the inventive filter assembly;

Fig. 12: Variants of a sample holder for the inventive

Filter arrangement;

Fig. 13: Schematic representation of a solvent outflow comprising a cooling element;

Fig. 14: Schematic representation of an extraction device having a condenser, evaluation unit, valve sleeve and samples Lö ^¬ sungsmittelabflüssen;

Fig. 15: Schematic representation of an extraction device with holder and interface;

Fig. Schematic representation of method-specific glass share at different positions; Fig. 17: Schematic representation of a ribbed plate for positioning ^¬ tion of method-specific glass parts in positions of the device; Fig. 18: Schematic representation of a holder for the positioning of method-specific glass parts in positions of the device;

Fig. 19: Schematic top view of an extraction device with multiple extraction positions;

Fig. 20: A perspective view of a glass structure for Soxhlet extraction. Figure 1A shows a schematic arrangement of a light source 1 and a sensor 2 to a container 4. A from the light source 1 emitted light signal 3 passes through the container 4 exzent ^¬ driven, ie in an area which is distant from the center M of the container 4 and the central axis MA, which halves the container diameter. The emitted from the light source 1 light signal 3 strikes the wall of the container 4 at an angle not equal to 90 °. During the extraction of the cooking or evaporation process is monitored in the container 4 by an evaluation ^¬ unit (5 in Figure 1B) evaluates the received signal from the sensor 2. The information generated by the evaluation unit can be used for the regulation or control, for example, depending on the signal detected by the sensor, the extraction process. In this case, different control modes can be provided. By way of example, when the temperature falls below a certain level, the power of a heating element (for example heating element 7 in FIG. 14) can be reduced. The light barrier comprises a light source and a sensor. The light source is, for example Balluff STM microSPOT® (Balluff) with Präzi ^¬ sions red light LED L-18 or precision IR-LED and transmits a light signal having a wavelength of 655 nm or 850 nm. The sensor is a photo transistor, for example Balluff Phototransistor FT-18 (Balluff).

Figure 1 B shows a schematic arrangement of a light source 1 and a sensor 2 to a container 4. A from the light source 1 Light emitted signal 3 passes through the container 4 exzent ^¬ driven and strikes the sensor 2. The eccentric passes through the light signal 3 through the container 4 leads to a seitli ^¬ chen offset of the light signal 3 due to the different refraction. Thus, a higher level of detail is achieved than when the light signal 3 passes through the center of the container 4. The emp ^¬ captured signal is averaged over ^¬ for evaluation to the evaluation unit. 5 Here the evaluation of the detected signal takes place. The detected signal can be compared with comparison values and an extraction process can be monitored. The comparative values can choose from a library that is stored in the electronic evaluation unit ^¬ 5, is retrieved, or learned who ^¬. On the basis of the evaluation, the evaluation unit 5 can cause the controller 6 to adapt process parameters, for example to reduce, increase or suspend the heat output of an extraction device. Preferably, a car may be provided extract function, whereby the user merely starts the extraction process and the sensors and Steue ^¬ tion / control automatically performs the process. The Steue ^¬ tion / control, the heating power based on the ausgewerte- th information of the sensor in such a one that the solvent in the container 4 is cooking constant. Figure 2 shows a schematic arrangement of an exemplary embodiment of the inventive device from above, wherein two containers 4 are provided. Each of the light sources and the sensors are arranged on a printed circuit board as a unit 14. The unit 14 is positioned on a copper core 13. The unit 14 is thermally insulated and heat is dissipated by means of the copper core 13. The copper core 13 thus ensures ei ^¬ ne cooling of the heat-sensitive sensors. The unit 14 and the copper core 13 are encapsulated in a glass tube 12. In this case, the glass tube 12 may have two units 14. From the light sources of the units 14 emitted light signals 3 pass through the container 4 eccentric as explained for Figure 1. The glass tubes 12 penetrate a device wall 11 and are connected to a heat dissipation 15. In this way, the glass tube 12 comprising the unit 14 can be set to a desired temperature, so that unwanted heat of the heater is dissipated.

Figure 3 shows a schematic arrangement of another exemplary embodiment of the inventive device from above. Here, the light signal 3, which is emitted by the ^{Lichtquel ¬} le 1 is sent through a light guide 16 in the direction of the container 4. The light signal 3 passes through the container 4 eccentrically (as explained for Figure 1) and enters a light guide 16 which tet the light signal on the sensor 2 leads. Thus, the light source 1 and the sensor 2 need not be arranged in a sectional plane through the container 4. They are freely positionable.

FIG. 4 shows a schematic arrangement of a further exemplary embodiment of the device according to the invention from above. Here, the mirror surfaces 17, 17 ^λ provided. The mirror surface 17 deflects a light signal 3 emitted by the light source 1 onto the container 4. The light signal passes through Container 4 eccentric (as explained for Figure 1) and is deflected by the mirror surface 17 ^λ on the sensor 2. Thus, the light source 1 and the sensor 2 need not be arranged in a sectional plane through the container 4. They may be positioned depending on the geometries of the mirror surfaces 17, 17 ^λ.

Figure 5 shows a schematic arrangement of another exemplary embodiment of the inventive device from above. The light source 1 and the sensor 2 are arranged on a device wall 11 or directly on the printed circuit board (PCB) in the interior. A light signal 3 emitted by the light source 1 passes through the container 4 eccentrically (as explained for FIG. 1) and impinges on a reflector 18 which reflects the light signal 3 onto the sensor 2 (a reverse arrangement is possible). On the side facing away from the light source 1 of the Re ^¬ reflector 18, a shield 19 is positioned, which shields the light signal 3 from the environment. Alternatively, the reflector itself may be configured as a shield. Such Müs ^¬ sen the light source 1 and the sensor 2 can not be arranged flat by the container 4 in an interface. They are positionable depending on the dimensions of the reflector 18 and its distance from the light source 1 and the sensor 2. The light source 1, the sensor 2 and the reflector 18 can also be arranged such that the light beam reflected by the reflector 18 again passes through the container 4.

The reflector 18 may be arranged on a protective shield or a protective hood of the device. So it can be detected whether the shield is in position. This can serve to detect a closed or open state of a device by means of the positions of the protective shield or the protective hood. Figure 6 shows a schematic arrangement of another exemplary embodiment of the inventive device from above. In this case, a light emitted from the light source 1

Light signal 3 from a solvent in the container 4 and / or deflected from the edge region of the container 4 to the sensor 2. The

Light signal 3 does not pass through the container 4, but penetrates into the outer region of the container 4 and is deflected ^¬ . The position of the light source 1 and the sensor 2 are comparatively freely selectable, in particular height-adjustable. For containers 4 that are not made of glass, trans ^¬ parente viewing window can be provided. The light source 1 and the sensor 2 can be selectively arranged so that the signal hits the viewing window at specific angles. This is advantageous in aluminum containers with one or more viewing windows.

FIG. 7 shows a diagram with level measurements of different solvents during the extraction. The solvents in detail are deionized water, petroleum ether

40/60, ethanol, chloroform, cyclohexane, dichloromethane, acetone

Diethyl ether, dimethylformamide, n-heptane, n-hexane, isopropanol, methanol, toluene, benzene, methyl ethyl ketone, tetrahydrofuran, xylene. Compare these measurements the levels by means of light ^¬ barrier in various solvents in an extraction apparatus B-811 (Buchi). Under beaker detection is understood here and below also level measurement. The fill level measurements can be stored as default values in a library of an evaluation unit (see FIG. 1B). From the library, comparison values for an extraction method can be selected and used for comparison with the extraction process, or the method can be regulated based on the determined process parameters. This allows you to choose from many options. The light barrier comprises a light source and a sensor. The light source is eg Balluff STM chip microSPOT® (Balluff) and sends a light signal with a wavelength of 655 nm. The sensor is a phototransistor, eg Balluff STM (Balluff). The height of the light barrier, ie both the light source and the sensor, is at 10 mm height of the container and is horizontal to the heating plate, on which the container containing the solvent center, and the solvent surface is positioned. The filling height at the beginning of the extraction was 15 mm.

The extraction device (FIG. 1B) used for beaker detection has a cooler 21 with cooling element 22, overflow 23, drip-off nose 24, valve 25 and outflow 26, as explained below for FIG.

The diagram of FIG. 7 shows a plateau at 15 mm at the beginning of the extraction and falling fill levels for the measured solvents in the course of the extraction. The filling level is reduced almost as far as 0 mm (see Figures 8 and 9). The rising signal at the right end of the diagram in Figs. 8 and 9 is the point at which, due to the opening of the valve 25 (see Fig. 10), solvent stored at the valve 25 runs back into the container to protect the analyte the region of the extraction device comprising the sample is running. The valve 25 can be opened before the filling height reaches 0 mm. This is dependent on the solvent and especially relevant for volatile solvents. In the fat extraction is to ensure that the level of the solvent does not drop to 0 mm as long as the tempera ^¬ ture is so high that the fat could burn. FIGS. 8 and 9 each show a diagram of a level measurement of a solvent. In Figure 8, cyclohexane was used. In FIG. 9, methanol was used. Both graphs show the rise of the signal (in V) of the sensor at the right end of the graph. This corresponds to the filling of the container Be ^¬ and thus the increase of the level due to the in ^¬ leading a security volume, which was accumulated upstream ^¬ the valve. If an emptying of the container is detected, the valve opens and initiates the safety volume of the solvent with the purpose of protecting the analyte, in the container or in the region of the extraction device comprising the sample.

Figure 10A shows a cooler 21 having a cooling element 22 in the form of a double reflux condenser, an overflow 23 and ei ^¬ NEN drip nose 24. A spiral-radiator may be used equally. During extraction, the cooler 21 is positioned over a sample and a container (see Figure 4 in Figure 1) having solvent. During the extraction, evaporated solvent condenses on the cooling element 22 and flows off. On the wall of the radiator 21, a solenoid valve 25 is provided, wel ^¬ ches in the closed position of the cooling element 22 in a flared funnel-collecting (30), which is disposed above the overflow 23, collected effluent in a compound 29 between the Overflow 23 and the solenoid valve 25 dammed. Alternatively, the solenoid valve 25 may be arranged from ^¬ serhalb the radiator 21. The overflow 23 is disposed hö ^¬ forth as the valve 25. The solenoid valve 25 is before ^¬ preferably a three-way valve having two outputs.

The widening funnel catch 30, which is arranged above the overflow 23 and shown in FIG. 10A, as well as the overflow 23, can be designed as one piece with the cooler 21, as shown here. forms his. Here, the funnel trap 30 can be completely be ^¬ reinforces circumferentially or at certain points in the region of the wall of the cooler 21st Alternatively, the overflow 23 may be attached to a nozzle and positioned substantially centrally of the radiator 21.

The first outlet is connected to a recovered solvent collector. The second outlet is connected to the container, which is positioned below the reflux condenser to catch the extract. If the accumulated in the CLOSED position ^¬ Senen solvent exceeds the height of the overflow 23, the solvent drips on the drip nose 24 from the below-positioned sample. The solvent dissolves the analyte from the sample and is collected in the container positioned below the sample. A continuous extraction is carried out by the evaporated again in the container extract or the solvent evaporated, condensed and dripping from ^¬ drip as previously explained. This results in a closed circuit. In the open position of the solenoid valve 25, solvent is passed through the solenoid valve 25 and discharged through the drain 26. In order to protect an analyte, if, for example, the level of the container positioned below the cooler 21, in which the analyte is located, sinks too much, the pent-up solvent is reintroduced into the container (through the second outlet of the valve). There is introduced a Vo ^¬ lumen into the vessel so that the analyte does not dry out ^¬ and / or is destroyed by heat, but is diluted at the same time not unduly. Alternatively, the volume is introduced into the region of the extraction device comprising the sample. The introduced solvent enters, in particular flows or drips, from there into the container in order to protect the analyte. Optionally, the pent-up solvent can be released through the valve in the open position (and through the first outlet). passage) for the recovery of the solvent in a collecting container.

As an alternative to a three-way valve, a two-way valve may be provided having an outlet. Here, it is dammed in the closed position and solvent discharged solvent in the offe ^¬ NEN position. The two-way valve may be connected downstream of a switch, which controls the introduction of the Lö ^¬ solvents in a region of the device, for example. The sample chamber or container comprising the analyte, or in the solvent capture container. The two-way valve and optionally the switch can be controlled or regulated on the basis of the signals of an arrangement of light source and sensor as described above.

FIG. 10B shows a perspective view of a cooler according to the invention for an extraction device as previously described for FIG. 10A. At the position of the solenoid valve 25 may alternatively be provided in the radiator of Figures 10A and 10B, a connection nipple, so that an external valve, for example via a hose or a tube, preferably a glass tube, connect to the connection nipple.

FIG. 11A shows an exploded view of a filter arrangement 31 according to the invention comprising a sample sleeve 32, a filter cover 33, a filter 34 and a filter protection 35. In the application situation, the filter 34 is inserted in the filter cover 33. On the filter 34, the filter protection 35 is positio ^¬ ned, which protects the filter 34 from mechanical stress. The filter protection 35 has an outer circumferential web on the bottom. The jetty is located outside only on the filter 34. The central / central region of the filter is thus not in contact with the filter protection 35.

The lid 33 having the filter 34 and the filter protection 35 is connected to the sample sleeve 32 by an external thread 40 at the

Sample sleeve 32 and an internal thread screwed to the cover 33, so that the filter 34 and the filter protection 35 are arranged in the lower end of the sample tube 32. The filter protection 35 has cams 36 for positioning the filter protection on the cover 33. The cover 33 has corresponding receptacles 44 for the No ^¬ cken 36. In this way, the filter protection 35 is positioned so that the perforations 42 of the filter protection 35 and the perforation ^¬ tion 43 of the cover 33 are in line (see Figure IIB with a side view of the lid 33 of the inventive filter assembly and Figure HC with a side view of the filter protection 35th the filter arrangement according to the invention). In this way, the sample sleeve 32 is permeable to solvent ^¬ tel, which drips example of a positi ^¬ onierten in the sample tube sample. In the application situation, for example, the sample is positioned in the sample sleeve 32 of the filter arrangement 31 with a sample holder 37a (see FIG. The sample sleeve 32 is positioned in the sample situation in the sample holder 37 a, wherein the sample holder 37 a, the upper outer shoulder of the sample sleeve 32 contacted.

FIG. 12 shows three variants of a punched sample holder 37a, 37b, 37c. The sample holder 37a is suitable for the inventive filter arrangement 31 (see FIG. The sample holders have a central opening 38 and a perforation 39 in the outer area. The sample holder 37a holds in the application situation, a glass sample tube, eg., The sample sheath 32 (see FIG. ^¬ Fi gur HA). The sample holders 37b, 37c hold in the application situation, for example, a paper tube containing the sample. FIG. 13 shows schematically a solvent drain 54 of an extraction device. In a region of the solvent drain 54, a cooling element 55 is positioned. The cooled solvent is introduced into the solvent receiver 52. Solvent that may be evaporated in the receiver 52 is cooled and condensed by the cooler 55. The cooling element 55 acts as a vapor barrier. The cooling element 52 is positioned in a receptacle 51 of the extraction device. The solvent catcher 52 is positioned in a receptacle of the extraction device (not shown). Optionally, the solvent catcher 52 may also be positioned adjacent to or on top of the extraction device. A connection 53 is provided for the connection of the cooling element 55 and the solvent collecting container 52. The connection is preferably nor ^¬ mized so-standard laboratory bottles can be used as container.

Figure 14 shows schematically an extraction device. A light source 1 sends a light signal 3 through a container 4. The container 4 is positioned on a heating plate 7. The light signal strikes the wall of the container at an angle not equal to 90 °, passes at least partially through the container 4 and impinges on the sensor 2. The signal received by the sensor 2 is evaluated by the evaluation unit 5. The evaluation unit 5 comprises a controller 6, which stands in connection with the heating plate 7 and a cooler 21 for controlling or regulating it. An extraction process can therefore be controlled by means of the evaluation of the detected signals, in particular automatically controlled or regulated.

In the container 4 is a solvent for the extraction of a sample 45, which is above the container 4 in a sample sleeve 31 is located. The sample tube 31 is positioned in an extraction chamber 46. For the design of the sample tube, reference is made to the description of Figures IIA, IIB, HC and 12. By means of the heating plate 7, the solvent is heated and rises in the extraction device as a solvent vapor. At the radiator 21, which is positioned over the sample tube 31, the solvent condenses and is discharged to a valve 25 which is in a first open position or accumulated on the valve 25, which is in a second closed position so that it drips onto sample 45. For the operation of the valve reference is made to the descriptions of Figures 10A and 10B. The valve is a three-way valve with two outputs. Solvent may be passed into a solvent effluent 54 via the first exit 27 and passed into a solvent receiver 52. In a region of the Lösungsmittelab ^¬ flow 54ist positioned a cooling element 55, which condenses the evaporated solvents in the collection container on ^¬ 52nd The Küh ^¬ lelement 55 acts as a vapor barrier. , This is particularly advantageous in the use of volatile solvents, so that a high recovery rate of the solvent is achieved.

The cooling element 55 has a standardized connection 53, with which the cooling element 55 is connected to the collecting container 52 (see description of FIG. The standardized connection 53 allows the use of commercially available laboratory bottles as a collecting container. These can be easily removed from the extraction device, sealed and stored. The collection container 52 need not be like conventional fixed tanks are emptied, but can simply by an empty receptacle, for example, a commercial laboratory ^¬ bottle with a standardized counterpart, be replaced. Solvent may be introduced into the container 4 via the second outlet 28, in particular to protect an analyte at a low level of the container 4. The residual heat of the heating plate 7 can damage the analyte towards the end of the extraction. In order to protect the analyte, the controller 6 can on the basis of the processed signals from the evaluation unit 5 ver ^¬ cause that solvent via the second output 28 of the valve 25 are introduced into the sample tube 31 when a low level is detected in the container 4.

Figure 15 shows schematically an extraction device with the extraction positions E1, E2. The extraction position E1, E2 each have a container 4, which is positioned on a heating plate 7, which represents the footprint. In the container 4 is solvent for the extraction of a sample 45, which is located in the sample tube 31 above the container 4. The sample tube 31 is positio ^¬ ned in an extraction chamber 46. The extraction chamber 46 is disposed ^λ 62 to the container 4 by means of an interface. In addition, a cut is ^¬ point 62 between the extraction chamber 46 and a condenser 21 which is located above the sample tube 31, is provided. With the aforementioned interfaces method-specific glass parts can be easily attached to an extraction position El, E2. The interface 62 is aligned at a höhenverstell ^¬ ble holder. The interface 62 ^λ or the glass parts, which form the interface 62 ^λ , are guided by a height-adjustable guide. The holder and the guide are adjustable along the height H. By adjusting the height of the holder, the distance between the contact surface of the cooler with the extraction chamber 46 and the heating plate 7 is adjusted. The cooler 21 is resiliently suspended and can ^{¬ style} with the extraction chamber a sealing connection to the Form interface 62. The interface 62 ^λ forms a sealing connection between the extraction chamber 46 and the container 4. For closing the interfaces, or the glass parts at the interfaces, a lift may be provided. The lift pressed while the contact areas of individual glass parts Anei ^¬ Nander. This allows the simple introduction of methodenspe ^¬-specific glass articles to an extraction position E1, E2. The contact areas of individual pieces of glass may be used as cuts out forms ^¬ or be provided with gaskets. The features of the extraction device of Figure 15 may be implemented in an extraction device such as shown in Figure 14.

FIG. 16 shows various method-specific glass parts for an extraction device according to the invention. Are shown in four extraction positions (El, E2, E3, E4) glass assemblies for the methods Soxhlet (abbreviated Sox in El), continuous ex ^¬ traction after Twisselmann (abbreviated ECE in E2), and Heissext- ROUP (E4). In E3 there are universal glass superstructures, with which the previously mentioned methods as well as the continuous extraction (CE) and Soxhlet warm up to the continuous extraction according to Twisselmann are feasible (abbreviated U in E3). In extraction position El, a glass structure for extraction according to Soxhlet is shown comprising a heating element 7, here a cerium-anfeld, a holder 61 and a guide 61 which are arranged along the height H. Furthermore, the interfaces 62, 62 ^λ between method-specific glass components comprising sawn container Bl, principal glass are ( "Sox") and illustrated cooler K. The Posi ^¬ tion of the arrayed holder 61 defined by the distance between the contact surface of the cooler with the main glass (Sox ) to the heating ^¬ element 7, the method-specific glass parts to be used and The position of the interface 62. The interface 62 is formed by the contact surface of the radiator and the contact surface of the main glass "Sox." An O-ring can be provided as a seal The guide 61 ^λ guides the glass parts in the lower part of the position Guide 61 ^λ may alternatively be formed as a second holder.

In extraction position E2 the main glass is a Twisselmann glass (ECE). The Twisselmann glass is shorter than the main glass for Soxhlet extraction in extraction position El. Therefore, the holder 61 is positioned at E2 lower than in Extraktionspo ^¬ sition El. The position of the interface 62 is defined accordingly and is used to connect the radiator K with the main ^¬ glass (Twisselmann, ECE).

In extraction position E3, a so-called universal glass U between container Bl and cooler K is positioned in contrast to the extraction ^¬ positions El and E2. The holder 61, the guide 61 ^λ and the interfaces 62, 62 ^λ are configured accordingly as previously explained. Due to the long Universal ^¬ U glass, the holder is positioned in a high position 61st The universal glass U optionally has another Heizele ^¬ ment 7 ^λ. The heating element 7 ^λ is used to bring the solvent ^¬ medium in the extraction chamber to boiling temperature. Ascending solvent condenses on cooler K and drips off.

In extraction position E4, a glass structure for hot extraction is shown. In this case, a container B2 is positioned on a heating element 7, here a ceramic field. The container B2 is arranged via an interface 62 directly to the radiator K. Un ^¬ terschied to those described for the extraction positions El, E2, E3 constructions, the hot extraction did not require a major glass, in which a sample to be extracted is positioned. The sample is rather positioned in the container B2. Accordingly, in the extraction position E4, a holder 61 is shown, which defines the height of the interface 62 between the container B2 and the radiator K. Since no main glass but only a longer container B2 is used in E4, the holder 61 is arranged lower than in the extraction positions El, E2, E3. In summary define the positions, or the height, the

Holder 61 and optionally the guide 61 ^λ designed as two ^¬ te holder in the extraction positions El, E2, E3 or the holder 61 in the extraction position E4, the usable method-specific glass parts and thus the corresponding feasible methods at an extraction position. The height of the holder 61, which defines the distance of the contact cushions of the radiator and the heating element 7, is preferably 241.5 mm for hot extraction, 301.5 mm for Twisselmann continuous hot extraction, 421.5 mm for Soxhlet extraction and 421.5 mm for extraction Universal glass 466.5 mm.

The positioning of the holder 61 is a coding, so that by the choice of the position of the holder 61 is directly and clearly derivable, which method can be performed at an extraction position. This can be done solely by reading the height of the holder 61 by means of one or more sensors based on the position of the holder 61. The sensors may be electrical contact switches or part of an optical system comprising, for example, a light source. Likewise, the sensor may be a sound or Hall sensor. Capacitive or inductive ^{configurations} are possible. Alternatively, the guide 61 may additionally be used alone or ^λ and a coding by represent the same principle as described for the holder 61.

Figure 17 shows a ribbed plate 71 as a fastener for the positioning of brackets and guides along the height of an extraction position as described for example in Figure 16. In the device according to the invention, the ribbed plate is arranged behind the position. The ribbed plate 71 has at different heights in pairs per height two receptacle 72, 72 ^λ , which are designed for receiving ^{korrespondie ¬ end} designed pin. By means of the savings ^¬ 72, 72 ^λ brackets and guides can be arranged on the ribbed plate 71. Likewise, a plurality of brackets and guides can be arranged at different positions, ie heights of the ribbed plate 71. The ribbed plate 71 may be configured as a sheet metal construction.

Figure 18 shows a top view of an exemplary holder 61 for placement in a ribbed plate (see ribbed plate 71 of Figure 17). The bracket 61 includes pins 73, 73 ^λ at which the recording of the rib plate (see FIG. Pickup 72, 72 ^λ in Fig. 17) are correspondingly designing. By means of the pins 73, 73 ^λ , the holder 61 is positioned in the recesses 72, 72 ^λ at a height of the ribbed plate. Furthermore, the esterification Hal- on spigots 74, 74 74 ^{λ λ,} which are te ^¬ such ausgestal that method-specific glass components can be included in the centering. The centerings can have plastic inserts for protecting the glasses. The holder 61 is provided for three parallel extraction positions. Of course, the holder may also have fewer or more centerings. FIG. 19 shows a schematic plan view of a device 81 according to the invention with a plurality of positions E1, E2, E3, E4, E5, E6 for method-specific glass parts. The trapezoidal ^device has a rear wall 82, which points away from the user in the application situation, for example in laboratory operation. In this way, the individual extraction positions, which are arranged on the legs 83.83 ^{λ of} the rear wall 82, are equally accessible to the user, so that method-specific glass parts can be easily attached or removed. Furthermore, this embodiment is advantageous since space is saved in comparison to a linear arrangement of the positions in which the positions are lined up next to one another.

Figure 20 shows a glass structure for Soxhlet extraction. The Glausaufbau has a cooler 21, an extraction chamber 46 and a container 4.

The cooler 21 has a cooling element 22 in the form of a double reflux condenser, an overflow 23 and a drip-off nose 24. Single-spiral coolers can be used equally. The cooler 21 is positioned over the extraction chamber 46 and the container 4 having solvent. During Soxhlet extraction, vaporized solvent from vessel 4 rises via riser 48 and condenses on cooler 21. The solvent condensed on cooler 21 drains off. On the wall of the radiator 21, a solenoid valve 25 is provided, which accumulates in the closed position of the cooling element 22 collected in the collecting effluent solvent and discharges solvent in the open position. The valve is preferably a three-way valve having two outputs.

When the solvent accumulated in the closed position exceeds the height of the overflow 23, the solvent drips via the Abtropfnase 24 to the positioned below in the sample tube 32 sample. The solvent dissolves the analyte from the sample. If the solvent exceeds the height of the sample tube 32, it runs down outside on the sample tube 32 and flows via the outlet 49 into the container 4. A continuous one

Extraction is carried out by re-evaporating, condensing and draining the extract or solvent collected in the container, as explained above. The result is a geschlosse ^¬ ner circuit.

The method-specific glass parts (4, 21, 46) are ^λ interconnected via the interfaces 62 and 62nd The interface 62 is formed by a ball flange in the lower portion of the radiator 21, a pan in the upper portion of the extraction chamber 46 and an O-ring 47. Such can be misalignments and

Manufacturing inaccuracies of the glass parts are compensated. The interface 62 is formed by a ball flange in the lower region of the extraction chamber 46, a pan in the upper region of the container 4 and an O-ring 47 ^λ . In this way, skew positions and production inaccuracies of the glass parts can be compensated.

The first outlet of the valve is connected to a recovery tank for recovered solvent. The second outlet of the valve is connected to the container 4, which under the

Reflux condenser is positioned to catch the extract. If the solvent accumulated in the closed position exceeds the height of the overflow 23, the solvent drips off via the drip nose 24 to the sample positioned underneath. The solvent dissolves the analyte from the sample and is collected in the container 4 positioned below the sample. A continuous extraction is carried out by the evaporated again in the container 4 extract or the solvent evaporated, condensed and dripped as previously explained. This results in a closed circuit. In the open posi- tion of the solenoid valve 25 solvent is passed through the Mag ^¬ netventil 25 and discharged through the drain.

In order to protect an analyte, if, for example, the level of the positioned below the radiator 21 container 4, in which the analyte is to greatly drops, the pent Lö ^¬ solvents is again introduced into the container 4 (through the second outlet of the valve ). A volume is introduced into the container so that the analyte does not dry out and / or be destroyed by heat, but at the same time is not excessively diluted. Alternatively, the volume is introduced into the region of the extraction device comprising the sample. The introduced solvent enters, in particular flows or drips, from there into the container in order to protect the analyte. Optionally, the pent-up solvent may pass through the valve in the open position (and through the first outlet) for the

Recovery of the solvent are passed into a collecting container.

On the container 4, an arrangement of a light source and a sensor as described above can be arranged (cf., for example, Figures 1 to 6). The control of a process can be done based on the detection. For this purpose, an evaluation unit may be provided which evaluates the detected light signals and controls or regulates the process, for example by means of regulation or control of the heating element (which is located below the container 4) and / or the valve. If a low level is detected in the container 4, the valve 25 can change to the open position and dammed up solvents. tel are introduced into the container 4 to protect the analyte. If a low level in the container 4 is detected, the power of the heating element can also be reduced in order to protect the analyte.

Alternatively, a 2-way valve may be provided, which may be configured as explained for Fig. 10.

Claims

claims

1. Device, in particular extraction device or evaporation device, comprising

at least one receptacle for a container (4), at least one heating element (7) for the container (4), at least one light source (1),

at least one sensor (2),

an evaluation unit (5),

wherein at least the light source (1) and / or the sensor (2) outside the range for container (4) are arranged so that with the sensor (2) from the light source (1) he generated by the area ^¬ for the container ( 4) passing light signal (3) can be detected.

2. Apparatus according to claim 1, characterized in that the light source (1) and / or the sensor (2) are angeord ^¬ net such that a change in the level of the container (4) can be detected.

3. Apparatus according to claim 1 or 2, characterized in that the light source (a) emits a directed light signal (3), in particular pulsed light signal.

4. Apparatus according to claim 1 or 2, characterized in that the light source (1) and the sensor (2) are angeord ^¬ net such that the light signal (3) the container (4) eccentrically ^¬ passes.

5. Device according to one of the preceding claims, characterized in that the light source (1) is a light emitting diode (LED) or a laser diode and / or the sensor (2) is a Pho- to diode or a phototransistor, in particular an IR photodiode or a photoresistor (LDR), is.

Device according to one of the preceding claims, characterized in that the sensor (2) associated with a filter, in particular a low-pass filter.

Device according to one of the preceding claims, characterized in that the extraction device has at least one cooling element (22).

Method for detecting containers and / or level detection, in particular by means of a device according to one of claims 1 to 7, comprising the steps

Emitting a light signal (3) from a light source (1) through an area for a container (4), the light signal (3) preferably passing through the area for the container (B) eccentrically,

Detection of the light signal (3) by means of the sensor (2), evaluation of the detected signal by means of an evaluation unit (5).

A method according to claim 8, characterized in that process parameters controlled on the basis of the evaluation

and / or regulated.

Device, in particular extraction apparatus or evaporation apparatus, in particular according to one of claims 1 to 7, comprising at least one cooling element (22), a valve (25) and connected to said valve via a first Ver ^¬ compound (29) overflow (23), wherein the valve (25) is arranged on a wall of the device, in particular on a wall of the cooling element (22), or via a second connection outside the device is angeord ^¬ net, wherein the valve (25) is configured such that at least a first open position and a second closed position is einnehmbar, wherein a ^{Lösungsmit ¬} tel, which condenses on the cooling element (22) through the valve (25) is dischargeable in the first open position and optionally in a container comprising an analyte and / or in a region of the device comprising the sample is introduced, and wherein the overflow (23) is formed such that solvent, which on cooling element

(22) condenses, is dammed at the valve (25) in the second closed ^¬ nen position in the first connection (29) and dripped over the overflow (23), wherein the overflow

(23) is disposed in the first junction (29) prior to entry into a flared funnel (30) positioned over the overflow (23).

Apparatus according to claim 10, wherein the valve (25) is a solenoid valve or a pneumatic valve.

Cooler (21) for a device, in particular extraction ^¬ device or evaporation device, in particular according to one of claims 1 to 7, comprising at least one Küh ^¬ lelement (22), a valve (25) and one with the valve via a first connection (29 ), wherein the valve (25) is angeord ^¬ net on a wall of the radiator or via a second connection outside the device is arranged, wherein the valve (25) is configured such that at least a first open Positi ^¬ on and a second closed position is ingestible, wherein a solvent which kon ^¬ condenses on the cooling element (22) through the valve (25) is in the first open ausleitbar Posi ^¬ tion and optional comprehensive in a container send an analyte and / or into a region of the device comprising the sample is introduced, and wherein the overflow (23) is formed such that solvent which condenses on the cooling element (22), on the valve (25) in the second closed position in the first connection (29) is dammed and dripped over the overflow (23), wherein the overflow (23) in the first connection (29) before entering a widening funnel (30), which over the overflow (23) positioned is, is arranged.

Method for extraction with a device, in particular according to claim 10 or 11, or a cooler, in particular according to claim 12, wherein a valve (25) in the second closed position on a cooling element (22) condensed solvent in a compound (29) of the Valve (25) and an overflow (23) accumulates, which drips over the overflow (23), wherein the overflow (23) in the Ver ^¬ bond (29) of the valve (25) and the overflow (23) before entering is disposed in a flared funnel (30) positioned over the overflow (23),

wherein the valve (25) in the first open position on the cooling element (22) discharges condensed solvent and optionally introduces the sample into the container comprising the analyte and / or into a region of the device.

14. The method of claim 13, wherein the valve (25) is controlled and / or regulated in dependence on the detected signal. Device, in particular extraction device or evaporation device, in particular according to one of claims 1 to 7, 10 or 11 with

a cooler having a contact surface for connecting a method-specific glass part, wherein the method-specific glass part has at least one com ^¬ patible interface (62, 62 ^λ ), and

at least one position (E) with a base for a container (4),

wherein the position (E) has at least one height-adjustable holder, which is configured such that the distance between the base of the container (4) and the contact surface of the radiator is adjustable so that we ^¬ least two different method-specific glass parts in the position (E ) can be introduced.

The device of claim 15, wherein the method specific glass parts are selected from the group comprising

a) glass parts for the methods Soxhlet, hot extraction (HE) and continuous extraction by Twisselmann (ECE) and b) Universal glass parts with which all of the foregoing Me ^¬ methods, Soxhlet warm and continuous extraction (CE) except for the continuous extraction by Twisselmann ( ECE) are feasible.

Kit comprising one

Device, in particular extraction device or

Evaporation device, with

a cooler having a contact surface for connecting a method-specific glass part, wherein the method-specific glass part has at least one compatible interface (62, 62 ^λ ), and at least one position (E) with receptacles for containers (4), wherein the position (E) has at least one height-adjustable holder which is designed such that the distance between the standing surface of the container (4) and the contact surface ^{¬ of} the cooler such is adjustable, that at least two different methodpezifi ^¬ cal glass parts in the position (E) can be introduced;

and

method-specific pieces of glass, wherein the glass parts methodenspezi ^¬ fishing one or more interfaces (62, 62 ^λ) have for the connection of method-specific glass components.

Method with an apparatus, in particular according to claim 15 or 16 or a kit according to claim 12, with several positions (El, E2), wherein at least two different methods of specific glass components at different positio ^¬ NEN (El, E2) are attachable or attached, and wherein different methods are used at the positions and / or different solvents are used.

The method of claim 18, wherein the methods are selected from the group comprising

Soxhlet standard (Sox st.),

Soxhlet warm (Sox w.),

Hot extraction (HE),

continuous extraction according to Twisselmann (economic continuous extraction, ECE),

continuous extraction (continuos extraction, CE), Kj eldhal. The method of claim 18 or 19, wherein the different ^¬ extraction methods are carried out simultaneously.

Method according to one of claims 18 to 20, wherein the un ferent extraction methods at the different extraction positions (El, E2) are individually controlled and / or regulated.

Device, in particular extraction apparatus or evaporation apparatus, in particular according to one of claims 1 to 7, 10, 11, 15 or 16, with a receptacle (51) for at least one solvent capture container (52) and with a connection (53) for connecting the solvent ^¬ outflow (54, 54 ^λ ) of the device and the solvent ^¬ catch container (52).

The apparatus of claim 22, wherein the device in the region of a solvent effluent (54, ^λ 54) comprises a Kühlele ^¬ element (54) for condensing vapors.

Apparatus according to claim 22 or 23, wherein one or more solvent drain lines are receivable in the port. 25. Device according to one of claims 22 to 24, wherein the device has a unit for the level measurement and / or level indicator of the solvent collecting container (52). 26. Device according to one of claims 22 to 25, wherein the solvent collecting container (52) is a bottle, preferably a commercially available laboratory bottle.

27. Device according to one of claims 22 to 26, wherein the terminal (53) is normalized.

28. A hydrolysis filter assembly (31) comprising a lid (33) with perforation, a cellulose-based filter (34) and a perforated perforated filter guard (35), the filter (34) in the lid (33 ), and wherein the filter guard (35) is disposed on the filter (34).

29. The filter assembly (31) of claim 28, wherein the filter

(34) is a resin impregnated, in particular melamine-soaked, filter.

30. Filter arrangement (31) according to claim 28 or 29, wherein the filter protection (35) has a mechanical coding, in particular one or more cams (36), for alignment on the cover (33).

31. Filter arrangement (31) according to any one of claims 28 to 30, wherein the cover (33) and the filter protection (35) corresponding perforations (42, 43).

32. Filter assembly (31) according to any one of claims 28 to 31, wherein the filter protection (35) on the underside has a preferably circumferential web.

33. Hydrolysis tube or hydrolysis chamber with a filter arrangement (31) according to one of claims 28 to 32.