EP1946616B1 - Procede et dispositif de chauffage par micro-ondes d'un materiau d'echantillon - Google Patents

Procede et dispositif de chauffage par micro-ondes d'un materiau d'echantillon Download PDF

Info

Publication number
EP1946616B1
EP1946616B1 EP06828947.9A EP06828947A EP1946616B1 EP 1946616 B1 EP1946616 B1 EP 1946616B1 EP 06828947 A EP06828947 A EP 06828947A EP 1946616 B1 EP1946616 B1 EP 1946616B1
Authority
EP
European Patent Office
Prior art keywords
sample
heating element
microwave
temperature
sample material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP06828947.9A
Other languages
German (de)
English (en)
Other versions
EP1946616A1 (fr
Inventor
Werner Lautenschläger
Martin Metzger
Frank Bismor
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mikrowellen Systeme MWS GmbH
Original Assignee
Mikrowellen Systeme MWS GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mikrowellen Systeme MWS GmbH filed Critical Mikrowellen Systeme MWS GmbH
Publication of EP1946616A1 publication Critical patent/EP1946616A1/fr
Application granted granted Critical
Publication of EP1946616B1 publication Critical patent/EP1946616B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/72—Radiators or antennas
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • H05B6/647—Aspects related to microwave heating combined with other heating techniques
    • H05B6/6491—Aspects related to microwave heating combined with other heating techniques combined with the use of susceptors
    • H05B6/6494—Aspects related to microwave heating combined with other heating techniques combined with the use of susceptors for cooking

Definitions

  • the present invention relates to a method for heating sample material with introduction of microwaves, as well as a device with a microwave chamber for heating sample material.
  • Such methods and apparatus for treating sample material are known per se from laboratory technology.
  • such devices serve to heat sample material as part of chemical analysis to trigger evaporation events.
  • microwave space For irradiation of the "microwave space” or “treatment space” is usually provided a microwave radiator or microwave transmitter in the form of a magnetron.
  • the microwave space is usually provided with metallic inner walls that reflect microwave radiation due to their material properties. So it may be a "microwave oven” so far.
  • the intensity of the microwave radiation emitted by the microwave radiator can usually be changed, for example "infinitely", so that influence on the energy input into the microwave space can be taken in this way.
  • the absorption of microwaves by an at least partially microwave-absorbing body is dependent on the intensity of the microwave radiation impinging on it, so that by varying the intensity of the microwave irradiation Influence on the temperature behavior of this body can be taken.
  • Sample containers or “containers” are usually provided for receiving sample material. These containers are placed with the sample material introduced therein into the treatment or microwave space, where they are then exposed to microwave irradiation.
  • sample material is itself (at least partially) microwave-absorbing, it will heat upon microwave irradiation by absorbing this radiation.
  • a device can thus serve in particular for a treatment of microwave-absorbing sample material.
  • the sample material is not or only slightly microwave-absorbing, it can be provided that the sample material is heated indirectly, for example by the sample container consists of microwave-absorbing material. In the case of microwave irradiation, heating of the container thus occurs and the heat produced there is then passed on to the sample material in the container by heat conduction or possibly also by convection.
  • the term “indirect heating” of the sample material is intended to express that the sample material itself is not or only slightly microwaveable and the heating takes place at least predominantly by absorbing heat from the environment.
  • the "environment” may in particular be a solid, such as a sample container in which the sample material is located, and / or a gaseous Environment, so for example air, which surrounds the sample material in the microwave space.
  • the term "insignificant microwave-absorbing" for the sample material is furthermore intended to express the fact that the above-described heating effects by heat absorption from the environment in the case of a microwave entry into the microwave space dominate over an optionally occurring absorption-induced heating of the sample material itself.
  • indirect heating element is understood as meaning an at least partially microwave-absorbing body which can transfer heat (directly or indirectly via an intermediate body) to the sample material via heat conduction.
  • At least partially is intended to mean that the indirect heating element is at least warmed more strongly with microwave irradiation than the sample material, so that therefore a heat flow from the heating element in the direction of the sample material is formed.
  • sample material of a known mass is heated or heated in such a way that evaporation or combustion processes occur, through which a portion of the sample material is released into the environment or burns up or burns.
  • the mass of the remaining sample material is less than the mass of the original sample material. Subsequently, this remaining mass of the sample material is then determined.
  • the temperature of the sample material in a predetermined manner changes, so that the temperature in the treatment process at least temporarily a predetermined or pre-recorded temperature curve, or "temperature curve” follows.
  • This curve can also be referred to as the "setpoint curve” or "reaction curve”.
  • a device for evaporating treatment which has a microwave space.
  • Containers are provided for receiving sample material, wherein the containers may consist of a microwave-absorbing material, so that indirect heating of the sample material via the containers is made possible.
  • the containers may according to this prior art of plastic material, such as PTFE Teflon (polytetrafluoroethylene) exist and are particularly intended as a pressure-stable container.
  • plastic material such as PTFE Teflon (polytetrafluoroethylene) exist and are particularly intended as a pressure-stable container.
  • a "heat build-up" in the region of the sample material is caused by the pot-like shape of the container.
  • the air (or more generally the corresponding gas mixture) in the container is thus heated, for example by the heat radiation of the container into the interior of the container.
  • This "heat accumulation” has the consequence that a corresponding adjustment of the temperature of the sample material is generally noticeably delayed when the irradiated microwaves are reduced. This also precludes a precise control of the sample material temperature according to a predetermined reaction curve.
  • the detection of the temperature of the sample material as z. B. by infrared measurement from the prior art, for. B. from the mentioned EP 0 592 654 B2 known per se, does not change anything in the principles or effects described above.
  • the temperature measured in this way makes it possible to determine with hindsight what time course the temperature of the sample material has taken.
  • a precise and reliable control of the temperature profile requires, first of all, that the temperature of the sample material be fast and can be selectively changed. This is contrary to the above effects.
  • the object of the present invention is to specify a method and a device for treating, in particular, no or only insignificantly microwave-absorbing sample material using microwave irradiation, with which or with which the time profile of the temperature of the sample material can be better controlled.
  • a method of heating sample material comprising the steps of: placing the sample material in a microwave space relative to a heating element of microwave absorbing material such that the heating element does not substantially extend beyond the level of the sample material and the sample material is in direct or indirect bathleitcard to the heating element.
  • the entry of microwaves for heating the heating element is provided.
  • the heating element in the microwave chamber heats up due to its microwave-absorbing properties. Due to the politiciansleittures then the thus transferring heat from the heating element to the sample material and thus heating the sample material.
  • the heating element does not extend at least substantially above the level of the sample material, it is achieved that, after a reduction in the intensity of the microwave radiation radiated into the microwave space, no further heat emission from heat stored in the heating element ("postheating") from the side or takes place above the sample material. As a result, the temperature of the sample material can adjust more quickly with microwave reduction.
  • the microwave radiation on the way between the transmitter, so z. B. the magnetron and the heating element is not weakened by absorption. This also causes a particularly rapid response of the temperature change of the heating element due to a change in the irradiance.
  • the heating element can be manufactured with comparatively low cost of materials, so that it has a correspondingly small heat capacity.
  • a particularly rapid heating and cooling or general temperature adaptation of the heating element and thus also of the sample material as a function of a change in intensity of the irradiated microwaves is possible.
  • the temperature of the sample material can be adapted very quickly when the intensity of the irradiated microwave irradiation changes.
  • the tracking of a setpoint curve is therefore possible with much greater accuracy and faster response.
  • a so-called “hysteresis-free” regulation of the temperature of the sample material is effected, whereby under “hysteresis” here the Residue of the temperature adaptation of the sample material to be understood against a change in the microwave irradiation. In other words, the duration of the temperature adjustment is thus shifted to zero.
  • the heating element must therefore not extend "substantially" beyond the level of the sample material. It must therefore be ensured that above this level, a corresponding space is created without heating element.
  • the ratio between a first vertical extension between the support level of the sample material and the level of the upper limit of the heating element to a second vertical extent between this upper limit of the heating element and the upper limit of the microwave space a predetermined value, for example "1 : 1 "or” 1: 2 "may not exceed.
  • sample support or “sample holder” is understood to mean a means for holding the sample material in the microwave space.
  • this means may be designed for example as a “support”, in the sense of “plate” or the like, ie with a substantially flat surface on which the sample material can be easily applied, or but as a “receptacle” in the sense that an edge is provided on a corresponding support, which secures the applied sample material against lateral breakage.
  • the “sample support / sample holder” can be a “sample plate” with a flat surface or a plate-shaped sample holder, for example, which differs from the sample plate by a certain edge elevation.
  • a “sample plate” is suitable, for example, for solid sample material, while, for example, for a rather viscous sample in this sense, a “sample recording” is suitable.
  • the inventive method can be advantageously designed by the sample material is placed on a sample support / sample holder in the microwave space. This makes it possible to keep the upper half space around the sample material free of solids. Through this free space formed the formation of a heat accumulation is avoided. This also contributes to the shortening of the reaction time in the temperature adjustment of the sample material due to a change in the intensity of the irradiated microwave radiation. This of course applies to any solid, regardless of its microwave absorbing property. In particular, therefore, for example, no "pot-shaped" body, for example in the form of side walls of a sample container, must be provided around the sample material. (Also for this clearance, an indication of a minimum vertical extent could be made in analogy to the above statements.)
  • the sample material may be in direct contact with the heating element or in indirect.
  • a sample support / sample holder itself may be provided as a heating element, on which the sample material is arranged directly.
  • the heat conduction takes place directly between the heating element in the form of the sample support / sample holder and the sample material.
  • the contact area over which the heat conduction takes place is in this case comparatively large (so to speak "maximum") because it extends over the entire contact surface of the sample material.
  • the sample material is arranged in the microwave space on a sample support / sample holder made of essentially microwave transparent material.
  • the shape of the sample support / sample holder can be optimized independently of the heating element, ie in particular achieve a corresponding increase in surface area for the sample material to be recorded.
  • this sample support / sample holder made of substantially microwave-permeable material on which the sample material is arranged, this sample support / sample holder on the other hand is in direct or indirect varnishleitcard with the heating element, so that the sample material is in indirect politiciansleitcard to the heating element ,
  • the heating element can thereby be optimized independently of the sample support / sample holder in terms of its heat capacity, so in particular be dimensioned such that in the sense of the above representations a particularly rapid temperature adjustment is possible.
  • the heating element can be provided below the sample support / sample holder and the sample support / sample holder can be easily arranged on the heating element, for example.
  • the size of the contact surface for heat conduction are chosen practically freely, so that in this way the heat conduction effect can be influenced.
  • the contact surface between the sample support / sample holder and the heating element can advantageously be made approximately annular.
  • the heat at a heat output of the heating element only short propagation paths back to the sample material, so that the heating takes place quickly.
  • the "unwanted" after-heating effect is comparatively low, since the contact surface and therefore the heat-conducting effect are comparatively small due to the annular design.
  • the material of the sample support / sample holder is "substantially" microwave permeable in the sense that the heating of the heating element in microwave irradiation is noticeably faster than the heating of the sample support / sample holder.
  • the sample support / sample holder is intended to rapidly transfer the heat absorbed via the contact surface to the sample material, so that to that extent a material with a good heat-conducting property is particularly well suited.
  • a sample support / sample holder may be provided, which consists at least partially of glass fiber and / or quartz fiber material.
  • the temperature of the sample material or the heating element or the sample support / sample holder is detected. Further advantageously, the temperature detection is carried out during the microwave entry into the microwave space repeatedly. On the basis of this temperature measurement, a temperature curve can be made. Because of the fast Temperature adjustment can be assumed in a detection of the temperature of the heating element that this temperature is virtually representative of the temperature of the sample material.
  • the intensity of the microwave irradiation is then regulated as a function of the detected temperature.
  • an air flow takes place in the microwave space. This allows, for example, removal of moisture or solvent vapors.
  • a device for heating sample material which has a microwave chamber and a sample support / sample receptacle arranged therein for receiving the sample material. Furthermore, the device has a microwave-absorbing heating element which is in direct or indirect heat-conducting contact with the sample support / sample holder. In this case, the heating element does not substantially extend beyond the level of the sample support / sample holder or, if appropriate, of the sample material located thereon.
  • the sample support / sample holder and the heating element may be formed in one piece or in two pieces.
  • a two-piece embodiment is generally advantageous, because in this case simply different materials can be selected for the heating element and for the sample support / sample holder.
  • the sample support / sample holder consists of a substantially microwave transparent material.
  • a material can be selected for the sample support / sample holder, which conducts the heat comparatively well (because of the above shown connections) and also as inert as possible, so that undesirable reactions with the resting sample material can be virtually excluded.
  • a material can be selected which stores comparatively poor heat, that is, has a comparatively low heat capacity, so that even a decrease in temperature or a reduction in temperature increase can take place particularly rapidly and thus supports a fast and easily controllable temperature control becomes.
  • a material for this example glass fiber and / or quartz fiber is particularly well.
  • the sample support / sample holder is at least partially made of a material which has the following properties: (i) it is chemically inert as far as possible so as not to undesirably interact with the resting sample material, (ii) it is as intended in the treatment Temperature range heat resistant, and (iii) for the reasons given above, it is good heat conducting at low heat capacity.
  • the said glass fiber and / or quartz fiber material is particularly suitable.
  • the sample support / sample holder and the heating element in the microwave space are arranged freely such that the sample support / sample holder is at least substantially laterally and not surrounded by microwave-absorbing material.
  • a change in the intensity emitted by the magnetron results in a corresponding change in the microwave radiation incident on the heating element directly, that is to say in particular without a time delay and without weakening. This also favors a particularly rapid response of the temperature behavior when changing the microwave radiation.
  • the microwave radiation coming from the microwave radiator can penetrate unattenuated into the material of the sample plate holder and in this way cause particularly rapid heating.
  • the heating element should be arranged in the microwave space so that its surface is at least partially directly exposed to the microwave radiation, either directly from the microwave radiator or example once (almost lossless) has been reflected on one of the inner walls of the microwave space.
  • a free space is advantageously formed in the microwave space in the upper half-space around the sample material so that no heat accumulation can form.
  • the material for the heating element care should be taken in the sense of the above statements that the material has correspondingly appreciable absorption properties with respect to microwave radiation. At very low or too low absorption capacity of the material, the desired rapid heating effect can not form, because then the heating of the heating element is too slow in microwave irradiation.
  • the absorbent properties depend on various factors, such as: B. in particular from the material itself, from the Wavelength (or wavelengths) of the incident radiation and of the temperature.
  • the heating element consists of a semiconductor material or of an insulator material with finely distributed conductive material, preferably at least partially of silicon carbide.
  • This material is very temperature resistant, for example, system temperatures between room temperature and 1400 ° C can be achieved.
  • the heating element consists of an inert material.
  • the heating element is at least substantially sleeve-shaped or ring-shaped or cylindrically shaped. This allows for a total material-saving design a good and stable support surface for the sample support / sample holder and also allows to design the contact surface for heat conduction of suitable size.
  • An approximately annular contact surface as it results in a substantially annular or sleeve-like or cylindrical shape of the heating element, is particularly advantageous because in this case, the heat flow must cover only relatively short propagation paths to the entire volume of the sample support / sample holder to penetrate. This in turn allows a particularly rapid spread of heat.
  • the sample support / sample holder is approximately circular in horizontal section and the contact surface between the heating element and the sample support / sample holder is provided annularly, this ring being substantially centric with respect to the sample support / sample holder and having an average radius which approximately half the radius of the sample support / sample holder corresponds.
  • the heating element is conically shaped at least in its lower region. For example, it can be tapered downwards, so that on the one hand, a comparatively stable support surface for the sample support / sample holder can be formed and, on the other hand, insertion into a receiving opening of a magazine or the like is particularly easy.
  • the heating element is designed as a crucible sleeve.
  • the device further comprises a temperature measuring device for detecting the temperature of sample material located on the sample support / sample holder and / or for detecting the temperature of the sample support / sample holder and / or for detecting the temperature of the heating element.
  • the temperature measuring device comprises an infrared sensor.
  • the temperature can be detected quickly without contact.
  • the temperature profile can be controlled virtually without loss of time.
  • the temperature quasi-permanent so for example in short time intervals, are detected, which is particularly in connection with the possible rapid temperature change advantage.
  • the results of such a temperature measurement can support a particularly reliable control of the temperature profile act, in particular, because any deviations from setpoints, an immediate countermeasure in the form of a change in the intensity of the microwave radiation can take place.
  • the device further comprises a means for generating an air flow in the microwave space.
  • the means may comprise, for example, a suction device for removing moisture and / or steam, for example solvent vapor, from the treatment space.
  • a suction device for removing moisture and / or steam, for example solvent vapor, from the treatment space.
  • the suction device generates a corresponding air flow for shielding the treatment space for this purpose.
  • the device has a "sample tray” arranged in the microwave space or a "magazine” or the like for receiving the heating element.
  • This magazine can be provided in particular for receiving a plurality of heating elements.
  • the magazine for this purpose have at least one receiving opening for insertion of the heating element.
  • a conical shape of the heating element is advantageous in this respect, because it can be easily inserted from above into such a receiving opening.
  • the magazine can be made of a microwave-transparent material.
  • the magazine is rotatably arranged in the treatment room.
  • the heating element is generally guided through areas of space, which are more or less permeated by microwave radiation, so that a total of uniform heating is ensured.
  • the microwave space is advantageously protected on the inside with an insulating material.
  • This can be provided, for example, to protect a microwave metal housing.
  • the insulating material is advantageously microwave transparent and, for example, mounted directly on metallic inner walls of the microwave space.
  • a device for heating sample material comprises a microwave space and a microwave-permeable crucible arranged in the microwave space for receiving the sample material. Furthermore, the device comprises a microwave-absorbing sleeve for receiving the crucible.
  • the sleeve may be provided as a heating element in the sense of the above statements.
  • a device for heating sample material has a microwave space and a sample tray which is arranged in the microwave space.
  • the sample tray may be provided for example in the form of a magazine.
  • the sample tray has at least one defined parking space for a heating element.
  • the parking space may be provided for example by an opening or "receiving opening" in the sample tray.
  • the heating element consists of microwave-absorbing material and is designed for direct or indirect contacting with the sample material.
  • the heating element is adjustable in the at least one defined parking space, for example from above.
  • the heating element consists of a semiconductor material.
  • the device comprises a temperature measuring device for direct or indirect detection of the temperature of the sample material.
  • the temperature measuring device is connected to a control and data unit, and the sample plate is rotational position-coded via the control and data unit, so that the detected temperature can be assigned to the heating element.
  • the heating element may be provided in the form of a crucible, a sleeve or a crucible sleeve.
  • a method of heating sample material comprising the steps of: arranging the sample material with respect to at least one Heating element of microwave-absorbing material such that the sample material is in direct or indirect réelleleitcard to the at least one heating element; Setting the at least one heating element, for example from above in a designated space of a sample tray; Arranging the sample tray, the at least one heating element and the sample material in a microwave space; and introducing microwaves to heat the at least one heating element.
  • the heating element consists of a semiconductor material.
  • the temperature of the sample material is detected directly or indirectly with a temperature measuring device.
  • the temperature measuring device is connected to a control and data unit, and the sample plate is rotational position-coded via the control and data unit, so that the detected temperature is assigned to the at least one heating element.
  • Fig. 1a shows a schematic cross section through a heating element, which is designed according to this embodiment as a crucible sleeve 2 and a sample support / sample holder in the form of a "sample plate” or a “sample carrier” 5, which is located on top of the crucible sleeve 2 and serves for placing sample material 1 ,
  • the heating element also serves as a "sample plate holder”.
  • the crucible sleeve 2 is in Fig. 1a in a receiving opening 20 of a (only partially shown) magazine 4 recorded or inserted.
  • Fig. 1b shows a crucible-shaped heating element 2 ', which may be formed conically at least externally.
  • the Sample material 1 can be used directly, or, for example, indirectly, ie, by inserting a temperature-shaped mat 21, for example of glass fiber.
  • the magazine 4 in this case represents a sample tray and through the receiving opening 20 in the magazine 4 and the sample tray, a defined parking space for the crucible sleeve 2 and the heating element in the magazine 4 and in the sample tray is formed.
  • the heating element or the example. Outside slightly conical crucible sleeve 2 is adjustable or usable from above into the receiving opening 20 according to this embodiment.
  • the heating element is brought in another way in the intended position on the parking space, for example by lateral insertion.
  • the receiving opening may for example be provided in the form of a U-shaped recess extending inwardly from the edge of the sample tray.
  • the crucible sleeve 2 consists of a microwave-absorbing material, the sample carrier 5 of an at least substantially microwave-transparent material. Cup sleeve 2 and sample carrier 5 are provided in a (in Fig. 1 not shown) microwave space or treatment room, which is part of a device for treating sample material.
  • the treatment room can be irradiated with a microwave radiator, so for example with a magnetron.
  • the crucible sleeve 2 If the crucible sleeve 2 is exposed to microwave irradiation in the treatment room, it heats up due to its microwave-absorbing property. The heat is transmitted through the annular contact or contact surface with the sample carrier 5 by conduction of heat to the latter, so that the sample carrier 5 is heated and in turn the heat to a on the sample carrier 5 resident sample 1 forwarded.
  • the system is thus particularly suitable for sample material 1, which itself is not or only slightly microwaveable.
  • the crucible sleeve 2 thus consists of a microwave-absorbing material, for example of a ceramic material with embedded therein electrically conductive material, for example of silicon carbide. It is advantageous if the material has comparatively "good" microwave-absorbing properties, because then a rapid increase in temperature upon irradiation can take place. This is particularly advantageous in terms of the possibility of a rapid temperature control, by changing the intensity of the microwave irradiation in the treatment room. For example, it can be provided that at least 50% of the microwave radiation used in the treatment in question is absorbed by the crucible sleeve 2.
  • the sample carrier 5 can contribute to the enlargement of the surface in the arrangement according to the invention, so that the support surface of the sample carrier 5 can be adapted exactly to the amount of the provided sample material 1. According to the above representations, it is favorable in terms of the choice of the material of the sample carrier 5, to choose a material that conducts the heat well and reacts quickly when reducing the heat, so has a relatively low heat capacity. In addition, of course, the material must withstand the intended temperature range of the system accordingly. For example, this glass and / or quartz fiber material is particularly suitable.
  • sample carrier 5 and crucible sleeve 2 it is furthermore advantageous if a material which is as inert as possible is chosen in order to prevent undesired interactions with the sample material 1 to be treated. Also in this regard, the specific materials exemplified as silicon carbide and glass / quartz fiber are advantageous.
  • a temperature range of the system can be handled, which is for example between room temperature and 1400 ° C.
  • the upper limit of this temperature range is particularly particularly influenced by the special choice of the material of the crucible sleeve 2.
  • a schematic representation of the device according to the invention is shown.
  • a magazine 4 or “sample plate" with receiving openings 20, in the crucible sleeves can be used.
  • the magazine can be part of a sample changer or sample changer system.
  • crucible sleeves 2 and a sample plate 5 are shown. In practice, of course, it may be provided to provide in each of the receiving openings 20 of the magazine 4 in each case a crucible sleeve 2 with a sample plate 5 arranged thereon.
  • the sample carrier 5 and the crucible sleeve 2 are arranged so freely in the treatment space 70 that the microwave radiation generated by the microwave emitter 7 is not weakened by microwave-absorbing material on the way to the crucible sleeve 2.
  • the crucible sleeve 2 is free of any microwave-absorbing parts, for example in a lateral and upper region.
  • the sample material 1 is arranged in the microwave space 70 on the sample plate 5 and this on the crucible sleeve 2, which serves as an indirect heating element.
  • the magnetron 7 is turned on, so that microwaves are irradiated into the microwave space 70. Due to the absorption property of the crucible sleeve 2, the latter heats up and, via the annular contact surface, transfers the heat to the sample plate 5. This heats up quickly due to their good heat-conducting properties and in turn transfers the heat to the sample material 1.
  • the temperature of the crucible sleeve 2 is reduced rapidly due to the comparatively low heat capacity thereof.
  • the transfer of heat to the sample plate 5 via the comparatively small, annular contact surface also reduces rapidly, which in turn leads to the temperature of the sample material correspondingly adapting rapidly.
  • the magazine 4 is thus located in a treatment or microwave space 70 into which microwave radiation can be radiated by means of a magnetron 7.
  • the bottom 75 of the treatment chamber 70 has two access openings 71, 72, wherein the first access opening 71 is provided for the passage of a balance 3, more precisely for the corresponding support of a receiving surface 35 of the balance 3 and the second passage opening 72 for a holder 74 of Magazine 4.
  • a motor 61 is provided for rotating the magazine 4 via its holder 74.
  • this motor 61 is mounted on a mounting plate 63 which is mounted vertically movable via a parallel guide 66.
  • Another motor 60 is provided for driving an eccentric disk 62, wherein the eccentric disk 62 acts from below against the mounting plate 63, thereby forming the mounting plate 63 and thus also the magazine 4 are height adjustable. In this way, a lifting system is formed. Through this lifting system, the magazine 4 from the in Fig.
  • control unit 65 which is connected via data lines to the motors 60, 61 and also the balance 3. Furthermore, the control unit 65 is integrally connected to a data system 40, for example, so that a control and data unit is formed.
  • the control data which relate to the motor 61, in particular contain information about the rotational position of the sample tray 4 and thus information about which crucible sleeve 2 is currently at which rotational position and thus, for example, on the balance 3 or its bearing surface 35 , Thus, this information is used for sample identification by means of rotational position coding.
  • the control data related to the motor 60 provide information about the height adjustment of the sample tray 4 and thus information related to a weighing operation of the crucible sleeve 2 with the balance 3.
  • an infrared temperature sensor 80 is provided. The temperature measurement can take place for example on the weighing position of the crucible sleeve 2 or in the immediate vicinity thereof.
  • the temperature sensor is inserted in a recess 81 of the metallic wall 90 of the microwave space housing.
  • the temperature sensor can be arranged laterally at the level of a crucible wall and thus measure the temperature of the coating indirectly via the crucible temperature.
  • the temperature sensor can also be arranged above a crucible (see reference numeral 80 ') so as to be directed directly to sample material and thus to directly detect the sample temperature.
  • the temperature sensor 80 is also connected to the control and data unit, so that the measured temperature values are available there as well.
  • the various crucibles are therefore rotated past the laterally arranged temperature sensor ("measurement while driving by"), the response time of the sensor being matched to the rotational speed and the crucible size.
  • the rotational speed is in a range of 5 to 20 rpm.
  • a fast IR sensor with a response time of, for example, 50 ms to 100 ms is preferably used.
  • at least one part 82 of the evaluation electronics is preferably arranged in the sensor cable 83.
  • each temperature measurement can be assigned to a particular sample and in time successive samples are stored to a temperature curve 69 of a sample and optionally displayed on a screen 67.
  • a curve can be used to control the temperature to a desired temperature curve by adjusting the microwave power and / or for quality control.
  • a sample position can be moved in front of the temperature sensor before the MW treatment.
  • the user can then label this sample position by means of the display device 67 and an input device (keyboard, touch screen, etc.) 68.
  • the treatment space 70 may be protected by a microwave permeable insulating layer 90.
  • a (not shown) suction device may be provided.
  • moisture and / or solvent vapors can be sucked out of the treatment space 70 by generating a corresponding air throughput.
  • the procedure can advantageously be as follows: In addition to the temperature, the weight change of the corresponding sample material 1 is detected at short time intervals, in each case with the balance 3. From the tare weight of the crucible sleeve 2 and the Proberivras 5 and the weight losses due to volatile components of the sample material can then be a graphical and tabular evaluation of the volatilizing shares are created. On this basis, a particularly high quality Quality control can be achieved because unforeseen events, such as splashing etc. of sample material are directly visible and an accurate measurement of the sample temperature is possible.
  • the device is also suitable for direct drying when a Probenmateriel is used, which is itself microwave-absorbing.
  • microwave-absorbing crucible sleeves 2 instead of microwave-absorbing crucible sleeves 2, it is also possible to manufacture the sample tray or the magazine 4 from a microwave-absorbing material.
  • the crucible sleeves 2 can also be used together with standard crucibles which are inserted into the crucible sleeves.
  • standard crucibles made of microwaveable material can also be used in this case.

Landscapes

  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Devices For Use In Laboratory Experiments (AREA)

Claims (21)

  1. Dispositif à micro-ondes pour le chauffage d'un matériau d'échantillon (1), comprenant
    - une chambre à micro-ondes (70),
    - un plateau (4) à échantillon disposé dans la chambre à micro-ondes (70), ledit plateau à échantillon présentant au moins un emplacement (20) défini pour un élément chauffant (2), ledit élément chauffant (2) étant constitué d'un matériau absorbant les micro-ondes et étant prévu pour un contact direct ou indirect avec le matériau d'échantillon (1), et ledit élément chauffant (2) pouvant être ajusté dans l'emplacement ou les emplacements (20) définis,
    caractérisé en ce que
    - l'élément chauffant (2) est constitué d'un matériau semi-conducteur,
    - le dispositif à micro-ondes comprend un capteur de température infrarouge (80) pour la détection directe ou indirecte de la température du matériau d'échantillon,
    - le capteur de température infrarouge (80) est relié à une unité de commande et de données, et
    - le plateau (4) à échantillon est à codage de position angulaire par l'intermédiaire de l'unité de commande et de données,
    - de manière à pouvoir associer la température détectée à l'élément chauffant (2).
  2. Dispositif selon la revendication 1,
    caractérisé en ce que
    l'élément chauffant (2) peut être introduit dans l'emplacement par en haut, ou peut être posé dressé sur l'emplacement.
  3. Dispositif selon la revendication 1 ou 2,
    caractérisé en ce que
    l'élément chauffant se présente sous la forme d'un creuset ou d'une douille.
  4. Dispositif selon l'une des revendications précédentes,
    caractérisé en ce que
    l'élément chauffant (2) est au moins partiellement constitué de carbure de silicium.
  5. Dispositif selon l'une des revendications précédentes,
    caractérisé en ce que
    l'élément chauffant (2) est constitué d'un matériau inerte.
  6. Dispositif selon l'une des revendications précédentes,
    caractérisé par
    un substrat d'échantillon / logement d'échantillon (5),
    l'élément chauffant (2) présentant une surface de contact (85) pour la mise en contact thermique avec le substrat d'échantillon / logement d'échantillon (5).
  7. Dispositif selon la revendication 6,
    caractérisé en ce que
    le substrat d'échantillon / logement d'échantillon (5) présente une face supérieure plane pour recevoir le matériau d'échantillon (1).
  8. Dispositif selon la revendication 6 ou 7,
    caractérisé en ce que
    le substrat d'échantillon / logement d'échantillon (5) est constitué d'un matériau essentiellement perméable aux micro-ondes.
  9. Dispositif selon l'une des revendications 6 à 8,
    caractérisé en ce que
    le substrat d'échantillon / logement d'échantillon (5) est au moins partiellement constitué d'un matériau en fibres de verre et/ou en fibres de quartz.
  10. Dispositif selon l'une des revendications 6 à 9,
    caractérisé en ce que
    le substrat d'échantillon / logement d'échantillon (5) est constitué d'un matériau inerte.
  11. Dispositif selon l'une des revendications précédentes,
    caractérisé par
    un moyen (3) de détection du poids du matériau d'échantillon (1).
  12. Dispositif selon l'une des revendications précédentes,
    caractérisé par
    un dispositif de levage pour un déplacement vertical relatif entre le plateau (4) à échantillon et l'élément chauffant (2).
  13. Dispositif selon l'une des revendications précédentes,
    caractérisé par
    un moyen de débit d'air dans la chambre à micro-ondes (70).
  14. Dispositif selon l'une des revendications précédentes,
    caractérisé en ce que
    la chambre à micro-ondes (70) présente une couche isolante (90) en matériau perméable aux micro-ondes.
  15. Procédé de chauffage de matériau d'échantillon (1), comprenant les étapes suivantes :
    - disposition du matériau d'échantillon (1) par rapport à au moins un élément chauffant (2) en matériau absorbant les micro-ondes, de manière à mettre le matériau d'échantillon (1) en contact thermoconducteur direct ou indirect avec l'élément ou les éléments chauffants (2),
    - ajustement de l'élément ou des éléments chauffants (2) dans un emplacement (20) d'un plateau à échantillon (4) prévu à cet effet,
    - disposition du plateau à échantillon (4) de l'élément ou des éléments chauffants (2) et du matériau d'échantillon (1) dans une chambre à micro-ondes (70), est
    - application de micro-ondes pour chauffer l'élément ou les éléments chauffants (2),
    caractérisé en ce que
    - l'élément chauffant (2) est constitué d'un matériau semi-conducteur,
    - la température du matériau d'échantillon est détectée directement ou indirectement par un capteur de température infrarouge (80),
    - le capteur de température infrarouge (80) est relié à une unité de commande et de données, et
    - le plateau (4) à échantillon est à codage de position angulaire par l'intermédiaire de l'unité de commande et de données,
    - de manière à pouvoir associer la température détectée à l'élément ou aux éléments chauffants (2).
  16. Procédé selon la revendication 15,
    caractérisé en ce que
    le plateau (4) à échantillon est constitué d'un matériau essentiellement perméable aux micro-ondes.
  17. Procédé selon la revendication 15 ou 16,
    caractérisé en ce que
    lors de l'étape « disposition du matériau d'échantillon », le matériau d'échantillon (1) est mis en place sur un substrat d'échantillon / logement d'échantillon (5) et le substrat / le logement (5) d'échantillon est mis en contact thermoconducteur direct avec l'élément chauffant (2).
  18. Procédé selon l'une des revendications 15 à 17,
    caractérisé en ce que
    la température du matériau d'échantillon (1) et/ou de l'élément chauffant (2) est détectée.
  19. Procédé selon la revendication 18,
    caractérisé en ce que
    l'intensité du rayonnement micro-ondes est réglée en fonction de la température détectée.
  20. Procédé selon l'une des revendications 15 à 19,
    caractérisé en ce que
    le poids du matériau d'échantillon (1) est déterminé.
  21. Procédé selon l'une des revendications 15 à 20,
    caractérisé en ce que
    de l'air est refoulé dans la chambre à micro-ondes (70).
EP06828947.9A 2005-11-07 2006-11-07 Procede et dispositif de chauffage par micro-ondes d'un materiau d'echantillon Active EP1946616B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102005053017 2005-11-07
DE102006014065A DE102006014065B4 (de) 2005-11-07 2006-03-27 Verfahren und Vorrichtung zum Erwärmen von Probenmaterial mit Mikrowellen
PCT/EP2006/010664 WO2007051653A1 (fr) 2005-11-07 2006-11-07 Procede et dispositif de chauffage par micro-ondes d'un materiau d'echantillon

Publications (2)

Publication Number Publication Date
EP1946616A1 EP1946616A1 (fr) 2008-07-23
EP1946616B1 true EP1946616B1 (fr) 2016-03-23

Family

ID=37622039

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06828947.9A Active EP1946616B1 (fr) 2005-11-07 2006-11-07 Procede et dispositif de chauffage par micro-ondes d'un materiau d'echantillon

Country Status (3)

Country Link
EP (1) EP1946616B1 (fr)
DE (1) DE102006014065B4 (fr)
WO (1) WO2007051653A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2931941B1 (fr) * 2008-06-02 2011-03-25 Renault Sas Dispositif d'assistance a la pesee d'un filtre a l'aide d'une balance.
US8640357B2 (en) * 2009-03-23 2014-02-04 Hasan Huseyin Engin Laboratory type quick film drying oven
DE102012007468A1 (de) * 2012-04-13 2013-10-17 Forschungszentrum Jülich GmbH Probenhalter zum Aufheizen einer Probe durch Strahlung aus einer Strahlungsquelle

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4566804A (en) * 1982-12-16 1986-01-28 Cem Corporation Apparatuses, processes and articles for controllably heating and drying materials by microwave radiation
DE4023483A1 (de) * 1989-08-03 1991-02-07 Sartorius Gmbh Vorrichtung zur trockensubstanzbestimmung
CA2061790A1 (fr) * 1991-03-01 1992-09-02 Robert N. Revesz Methode de fabrication de contenants pour cendrage
DE4223116A1 (de) * 1992-04-30 1993-11-04 Mikrowellen Labor Systeme Vorrichtung zur verdampfungsbehandlung von vorzugsweise fluessigen stoffen, insbesondere reagenzstoffen, oder zum aufbereiten oder analysieren von probenmaterial
JPH0917566A (ja) * 1995-06-30 1997-01-17 Suzuki Motor Corp マイクロ波加熱用の試料保持平板加熱体
DE19543401A1 (de) * 1995-11-21 1997-05-22 Mikrowellen Systeme Mws Gmbh Vorrichtung zur Wärmebehandlung einer Probe durch die Bestrahlung mit Mikrowellen
DE19827465A1 (de) * 1998-06-19 1999-12-23 Mikrowellen Systeme Mws Gmbh K Vorrichtung zum Behandeln von Stoffen in wenigstens einem Gefäß
US6227041B1 (en) * 1998-09-17 2001-05-08 Cem Corporation Method and apparatus for measuring volatile content

Also Published As

Publication number Publication date
EP1946616A1 (fr) 2008-07-23
DE102006014065A1 (de) 2007-05-10
WO2007051653A1 (fr) 2007-05-10
DE102006014065B4 (de) 2007-10-04

Similar Documents

Publication Publication Date Title
EP0592654B1 (fr) Dispositif pour traiter par evaporation des substances de preferance liquides, notamment des substance reactives, ou bien pour preparer ou analyser des prelevements
DE4143541C2 (de) Vorrichtung zum Extrahieren von Proben mittels eines Lösungsmittels bei erhöhter Temperatur
DE60201330T2 (de) Instrument für mikrowellenunterstützte chemische synthese versehen mit stationärer abstimmung
EP3059076A1 (fr) Procede et dispositif destines a fabriquer un objet tridimensionnel
EP1946616B1 (fr) Procede et dispositif de chauffage par micro-ondes d'un materiau d'echantillon
DE3512457C1 (de) Vorrichtung zu Untersuchungen mit der Methode der Hochdruck-Duennschicht-Chromatographie
DE4243597C2 (de) Mikrowellenleistungs-Erfassungsvorrichtung
EP3165910A1 (fr) Procédé et dispositif d'examen photothermique d'un échantillon
EP1125177B1 (fr) Procede et dispositif pour le sechage de materiaux
DE102015214414B4 (de) Verfahren und System zur Ermittlung biologischer Eigenschaften von Proben
DE3818697C2 (fr)
DE4206109C2 (de) Verfahren und Vorrichtung zur Aufbereitung fester Proben mit Hilfe pyrolytischer Verdampfung für eine Analyse mittels eines Massenspektrometers oder eines Gaschromatographen
WO2020109317A1 (fr) Procédé de détermination du volume d'un liquide
DE4400815A1 (de) Verfahren und Vorrichtung zum Einbetten eines Gegenstandes, insbesondere eines Probematerials, in eine Einbettmasse
DE1489750B2 (de) Strahlungsdetektor zum sichtbarmachen und betrachten von un sichtbaren strahlen
DE19744502C2 (de) Probenaufnahmekammer für ein Röntgenpulverdiffraktometer
DE69734153T2 (de) Verfahren und vorrichtung zur chemischen analyse mit abbildung durch thermische rastermikroskopie
DE1295956B (de) Verfahren und Vorrichtung zum UEberziehen von koernigem Material durch Vakuumaufdampfen
DE3204873C2 (de) Vorrichtung zum automatischen Zuführen einer Probe in den Graphitrohrofen eines Atomabsorptionsspektrometers
Beccaglia et al. Analysis of arsenic and calcium in soil samples by laser ablation mass spectrometry
DE1901099C3 (de) Verfahren und Vorrichtung zur Untersuchung von Stoffproben
EP2574903A1 (fr) Appareil de mesure destiné à la détermination de l'humidité gravimétrique
EP1642648A1 (fr) Dispositif et proeédé pour regler la temperature d'un liquide
EP3577095B1 (fr) Procédé et dispositif pour la dessiccation d'une matière explosive
DE19930742A1 (de) Vorrichtung zur physiko-chemischen Modifizierung von Materialproben mittels eines Elektronenstrahls

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20080318

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): DE GB

17Q First examination report despatched

Effective date: 20081009

DAX Request for extension of the european patent (deleted)
RBV Designated contracting states (corrected)

Designated state(s): DE GB

REG Reference to a national code

Ref country code: DE

Ref legal event code: R079

Ref document number: 502006014840

Country of ref document: DE

Free format text: PREVIOUS MAIN CLASS: H05B0006640000

Ipc: H05B0006720000

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

RIC1 Information provided on ipc code assigned before grant

Ipc: H05B 6/72 20060101AFI20151007BHEP

Ipc: H05B 6/64 20060101ALI20151007BHEP

INTG Intention to grant announced

Effective date: 20151026

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): DE GB

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 502006014840

Country of ref document: DE

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 502006014840

Country of ref document: DE

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20170102

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20191126

Year of fee payment: 14

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20201107

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20201107

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20231127

Year of fee payment: 18