JPS61239161A - Device for overpressure thin-layer chromatography - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to an apparatus for performing chromatographic separations by overpressurized thin layer chromatography.

[Conventional technology]

According to the prior art, known devices include a carrier plate covered with an adsorbent layer for receiving the sample to be tested and a softening element on the adsorbent layer or an overlay for pressing the adsorbent layer on a suitable element. and elements forming an enclosed space in which pressure can be generated. The efficiency of separation achieved by overpressure thin layer chromatography can be improved by utilizing the apparatus of the present invention. The advantages offered by column chromatography and its planar variant so-called thin layer chromatography are described, for example, in British Patent Specification No. 157,076.
According to this specification, an apparatus for implementing the method includes an overpressure chamber adjacent to an adsorbent bed. As adsorbent layer, the same organic and inorganic materials can be used in both methods. The adsorbent layer is completely covered by a plastic plate, advantageously made from a soft material, which is generated in an enclosed space by filling it with water, for example, and pressed onto the layer by nine ohms of pressure. . The device is used to suppress the solvent leaving the adsorbent layer, for example by a sealing layer around the adsorbent layer to be associated with this plastic plate. This results in the virtual elimination of vapor spaces, a characteristic of known thin layer chromatography. The vapor phase created above the adsorbent layer is believed to be the source of some disadvantages. The plate carrying the adsorbent layer is sealed on both its lines in order not to leak the eluent/solvent allowed into the adsorbent layer under the influence of the overpressure imparted by the plastic plate, as mentioned above. Should. The migration of the eluent can be prevented by grooves made in the adsorbent layer or by plastic plates pressed onto the surface of the adsorbent layer.

To improve the effectiveness of known overpressured thin layer chromatography techniques, more adsorbent layers can be prepared in-house. In this case, the carrier plates cover each other and form a parallel system with the adsorbent layers on the same side of these plates. A device of this type is shown, for example, in Han Lee Patent Application No. 1335/82, early published in February 1985. The carrier plates should be sealed to each other on their edges by using a suitable sealing medium.

An overpressed closed space can be formed either above or below the bottom carrier plate;
In this case, the carrier plate transmits overpressure within its system. Usually the carrier plate has a system of parallel grooves starting from one of its halves or from the middle of the adsorbent layer, where the eluent can communicate between the adsorbent layers.

Chromatographic separations cannot achieve high efficiency unless the basic conditions for the separation are selected in an appropriate manner. The basic conditions of liquid chromatography are the substance of the adsorbent, the mobile phase-eluent, the temperature of separation, etc. Is temperature important in chromatography? Lame
are chosen very carefully. The desired temperature value is maintained with high accuracy during the separation. To date, practitioners have believed that the role of temperature is unimportant in liquid chromatography. This is clear from the conventions of column chromatography.

Known devices for thin layer chromatography operate practically without taking into account temperature effects. For example, in 1978 in New York, J.C. Touchstone (J-C, T.
ouchstone) and M, F., Dobbins (
M., F. Dobbina) in "The Practice of Thin Layer Chromatography" states on page 304 that the role of temperature is not critical to this method. This statement is self-evident from the fact that in known devices a vapor space is located above the adsorbent layer, and this space has an adverse effect on the conditions of separation at high temperatures. It has been proposed to use high temperatures for heating the chamber during separation, as the detection of different substances is unlikely; It concerns the multi-expansion method using . In a single deployment, the high temperature and the evaporation of the solvent facilitated by it cause many problems due to the closed vapor space above the adsorbent layer, and therefore this separation is often inefficient and Vine is rated as unreliable. Solvent vapors cause loss of accuracy.

Of course, the adsorbent layer can be placed with its temperature in an incubator that ensures a stable temperature value selected by the substance to be separated. This is a known feature of thin layer chromatography development.

In comparison with traditional gas chromatography methods, classical liquid column chromatography lacks speed and efficiency due to the use of large adsorbent particles. Liquid chromatography was developed because chromatography is applicable to only about 20% of all organic substances.

Planar methods, especially thin layer chromatography methods, have proven to be very useful due to their advantages. The method is thus simple and extremely economical in terms of time and materials, allowing visual inspection and simultaneously testing of many samples using coagulating reagents. But there are also drawbacks. The disadvantage of this is that it limits the number of separations by the length of the carrier plate and the amount of time required for deployment. The overpressure thin-layer chromatography method ensures rapid and effective separation of mixtures of various organic and inorganic substances, which is performed 5 to 20 times faster than traditional thin-layer methods, but is faster than the aforementioned ones. also requires the use of smaller and more homogeneous adsorbent particles.

This separation is particularly efficient and rapid in many cases.

This method is insufficient when a mixture containing many organic compounds is used, and the separation is weak, making it difficult to separate multiple substances and evaluate the obtained chromatogram.

[Problem that the invention seeks to solve]

The problem that the present invention seeks to solve is the desire to create a method and apparatus that improves the efficiency and rapidity of separations performed by overpressure thin layer chromatography.

The present invention provides that when applying a temperature program during deployment,
It is based on the recognition that autopressure thin layer chromatography can be improved by special methods. Temperature is a very important parameter when the vapor phase is removed, i.e. in this overpressure thin layer chromatography process - contrary to the prevailing belief to date. It is also important that the eluent flows in a predetermined direction under the influence of overpressure; and that this flow rate can be varied with temperature. Based on this recognition, the fundamental feature of the present invention lies not in the application of temperature per se, but in its transformation. Thereby, it is possible to change the order, ie the configuration, of the substances separated in the adsorbent layer. This improves the separation of the different components of the mixture compared to known methods. The faster separation speed ensured by increasing the temperature also allows the adoption of online evaluation methods.

The present invention further demonstrates that the material pressed into the adsorbent layer by higher temperatures absorbs the eluent at conditions other than low temperatures, thereby creating a very confined space with a particular vapor pressure that separates the constituent granules/orders. Based on the fact that the adsorption layer is realized on the adsorbent layer, and the specificity affects the efficiency in an advantageous manner.

[Means for solving problems, and their actions and effects]

The aim of the present invention to solve the above problems is that, compared to known methods of thin layer chromatography, a temperature program is utilized and the temperature is at different points in the space containing the adsorbent layer together with the substance to be separated. The present invention relates to an apparatus embodying an improved overpressure thin layer chromatography method that can be varied according to a timely determined sequence by different methods.

It is therefore an object of the present invention to provide at least one carrier plate installed adjacent to an enclosed space, nine adsorbent layers provided on the surface of this carrier plate, such as a soft plate, in said enclosed space. means for covering the surface of said adsorbent layer under the influence of overpressure generated, a first inlet for delivering a solvent to said adsorbent layer, a second inlet for delivering an overpressure medium to said enclosed space, said adsorbent. The present invention relates to an apparatus including a heating unit for varying the temperature of a layer and a temperature control device for energizing the heating unit.

Preferably, the heating unit has a carrier plate which is plate-shaped and capable of receiving electromagnetic energy from an induction heating unit or heating element arranged parallel to the carrier plate. As with the carrier plate, the number of heating elements may be greater than one, and it is advantageous to arrange them in a parallel system. The carrier plate can also be in contact with a thermal insulation element.

According to the invention, the device of the invention comprises a central microprocessor unit controlling the temperature of the carrier plate and the heating element, which allows the temperature distribution in the adsorbent bed to be varied in time and steric sequence according to a stored program. .

In a further advantageous embodiment of the device according to the invention, the temperature control device controls the temperature of the adsorbent layer, which is connected via a differential amplifier to the input of the comparator, above the first input of the comparator. Contains a temperature sensor to detect. Here, a second input of the comparator amplifier is connected to a series of outputs including a control keyboard and an integrator for programming a central microprocessor unit, the comparator amplifier having a signal level U, on the first input. Signal level U on the second output
Sending a positive high level signal Uc when the signal level Uc is higher than b and sending a positive low level signal when the signal level Ua on the first input is approximately the same as the level Ub of the signal on the second input. , and when the signal at the first input is at a level Ua lower than the level Ub of the signal at the second input, it sends a signal at a negative level Uc, and the other input of the comparator is connected to the top of the level shift unit. The output of the comparator is connected to the output of the mustard oscillator, and the output of the comparator is connected to a power switch forming the control output of the temperature control device.

The device proposed by the invention imparts a temperature change to the adsorbent layer, thereby improving the separation of different components of a mixture containing organic and inorganic compounds. Improved separation efficiency
To improve the reliability of chromatographic evaluations based on the abrasher thin layer a-r togelafy method.

〔Example〕

The present invention will now be described in further detail with reference to the accompanying drawings, in which preferred embodiments of the invention are shown.

According to the invention, the device is developed in FIG. 1 to include one or more carrier plates 3 disposed on the clamps 12 or other suitable elements capable of rigidly supporting the elements of the device. The carrier plate 3 is covered from at least one side by an adsorbent layer 2 and is in thermal contact with a heating unit that allows the temperature of the adsorbent layer 2 to be varied over time and, if necessary, in a steric sequence. device AIC
As shown in Figure t41, the heating unit includes two plate-shaped heating bodies 4 charged with electric current.

One of the heating bodies 4 is arranged above the adsorbent layer 2 separated by an insert plate 9 made of soft material. A further heating element 4 is arranged below the carrier plate 3.

It is self-evident that these heating bodies 4 are advantageously parallel to the carrier plate 3 and have a controlled power. If a temperature hierarchy is desired, these heating bodies can be divided into independent sections each connected to a controlled power source.

The low heating element 4 rests on the plate 11 fitted in a clamp 12 in which a thermally insulating layer can be used between the plate 11 and the heating element 4. A first inlet 16 communicates with the adsorbent bed 2 for delivering the solvent/eluent to the appropriate location. Above the upper heating body 4 there is a 10 (gray) laterally restricted by a closure plate 14 and between which an OIJ song is used for sealing.
There is a closed space 1 axially limited by. This closed space 1 can maintain the overpressure occurring therein by passing a suitable overpressure medium, such as water or gas, through the second inlet 15. Under the influence of the overpressure effectively generated in the closed space 1 by the liquid deck, the upper heating body 4 is pressed onto the adsorbent layer 2 from above the insert plate 9 . The heating element 4 is connected by conductors 17 to the respective inputs and outputs of the temperature control device 24 . The heating body 4 described above can be divided into a plurality of parts, and temperature sensing means are connected to them or to respective regions of the adsorbent layer 2,
The temperature control device 240 is connected to the input section and the output section to separate them. The heating element 240 segment is advantageous as an element of control power, which is the basis for varying the temperature in the environment of the adsorbent layer 2 with a predetermined time and three-dimensional program. Under the influence of the solvent introduced onto the first inlet 16, the sample carried onto the surface of the adsorbent layer 20 is separated, and the separation can be evaluated by the detector 19. In the case of on-line evaluation, the detector 19 includes detection means arranged on both edges of the carrier plate 3. When the evaluation is carried out off-line, the detector 19 is completely independent on the device A and the carrier plate 3 is removed from the device for evaluation.

The temperature control device 24 is controlled by the divided portions of the heating body.
Adsorbent layer 2, which usually allows temperature control by adjusting the charged power. The mutual arrangement of carrier plate 3 and heating element 4 is possible in various ways. One of the possibilities is that the substrate 7 on top of the thermally insulating layer 5/this is e.g. the plate 11
It is possible to adjust the heating element 4 on /. The heating body 4 is covered on its opposite side by a carrier plate 3 having an adsorbent layer 2 . A suitable soft plate above the adsorbent layer 2 carries the overpressure from the enclosed space 1 (FIG. 2). As shown in FIG. 3, the two heating bodies 4 and the carrier plate 3 form a sandwich structure, in which the closed space 1 is located on one side of one of the heating bodies 4, i.e. the low heating body. 4 can be provided above or below. The other heating elements are supported by a heat insulating plate 6, which together with the substrate 7 is clamped by suitable elements.

DETAILED DESCRIPTION OF THE INVENTION The device proposed by the present invention can be used effectively with multiple carrier plates 3. The first possibility is
As shown in the figure, the carrier plate 3 is arranged with the adsorbent layer 2 oriented in the same direction and there are heating bodies 4 between them and/or above and below. The heating elements 4 are again subjected to overpressure from the closed space 1 , and one heating element 4 is supported by an insulating grate 6 arranged on the substrate 7 .

A possible arrangement of ponds containing two carrier plates 3 is shown in FIG. In FIG. 5, the heating element 4 is arranged between the carrier plates 3, i.e. the heating element 4 is separated from the C adsorbent layer 2 by the carrier plate 3 or otherwise the adsorbent Layer 2 faces heating body 4 .

In this latter case, the structure containing adsorbent 1-2 is
It is closed by carrier plate 3. Closed space 1
generates overpressure from the first side of the heating element 4,
And the insulation grate 6 supports it on the substrate 7.

The heating unit of device A of the invention can cooperate with an induction heating system. In this case, the temperature control device 24 energizes the induction heating unit, which is combined with a metal carrier plate 25 (FIG. 6) and supported by the support grate 8. Under the influence of induction heating, the carrier plate 25 and the adsorbent layer 2 covering it from at least one side are warmed up.

The carrier plates 3 and 25 can be constructed in multiple parts, as described above. The materials are glass, ceramic,
It can be an aluminum or terephthalate based polymer. The closed space is arranged from at least one side of the heating unit. The carrier plate 3 is rectangular/square or rectangular, but may also be pond-shaped. For online evaluation, it is preferred to use a carrier plate 3 with at least one straight edge.

A typical carrier plate 3 has a thickness of 0.1 to 5.0 m. The higher the thickness of the carrier plate, the higher the power required due to temperature conditions and the higher the stiffness of the carrier plate.

The choice depends on the given conditions and is routine for skilled workers.

In the device proposed by the invention, a closed space 1 with overpressure generally means a water pocket. This is because it seems to be the best bath solution for safety reasons. On the other hand, pressurized air can guarantee the same effect. Carrier plate 3 includes substrate 7 and plate 10.1
1 and clan f12 must have a tight fit against overpressure.

The adsorbent layer 2Fi may consist of organic and inorganic materials. Examples include silica dal, aluminum oxide, cellulose scraps, and synthetic resins. It is self-evident that these examples do not exclude all possibilities.

The material pressed onto the adsorbent layer 2 of the carrier plate 3 to deliver overpressure, for example the insertion grate 9, usually consists of a polytetrafluoroethylene terephthalate based polymer, polyethylene or aluminum foil. This material is selected depending on the conditions of the chromatographic separation. The aluminum foil can serve as a stretchable layer to separate the adsorbent layer 2 from the enclosed space.

The insulating part of the device of the invention is generally asbestos, but it is obvious that any other suitable material could be used.

Other examples of materials used to make the device according to the invention offer only some preferred possibilities and, based on the known conditions of chromatographic development, the skilled worker can select a suitable material for the pond.

In the device according to the invention it is preferred to use a rectangular carrier plate 3 on which the adsorbent layer 2 is surrounded on three sides by a sealing layer 20 (FIGS. 7.8.9 and 10). , adsorbent layer 2
Above there is an entry point 21 and a charging point 23. These points 2
1.23 is positioned depending on the development conditions, and the seal layer 20
The adsorbent layer 201 may be disposed on the edge of the adsorbent layer 201 opposite the free end 18 that does not carry or in the center thereof. As a matter of course,
Other possible positions are also possible. The inlet section 21 receives the eluent and the charging point 23 (starting point) deposits it. Oats-de-Vtsher is adsorbent layer 3. A release agent flows through the groove 22 on the carrier plate 2, in which case the eluent can move in this groove in the direction of the edge 18 of the carrier plate 3, as indicated by the arrow in the figure. During this movement, the sample separates into its components.

In the case of on-line development, the eluent reaches the edge 18 with its constituents and can then be detected by a suitable device, for example an ogtoelectronic detector. This detection is the basis of the generated signal sent to the detector 19. As shown in FIGS. 7 and 8, the carrier plate 3 can be used for one-dimensional measurements evaluated by on-line methods. If the evaluation is carried out by offline methods,
The components separated on the adsorbent Jii2 move over different distances, and the distance range depends on the components obtained by separation and the deployment conditions. The distance between the charging point 23 (starting point) and the component spot is the basis of the evaluation.

Separation can also be performed by two-dimensional methods. In this case,
Separation first takes place in the direction of the closure string 26 and then
This is done in the direction of the pond closure string 27 perpendicular to the first closure string. FIG. 9 shows offline evaluation. The two-way deployment can be determined by means of the carrier grate 30 edge 18 and a closure cord 26 with a hollow section created by cutting some portion of the sealing layer 20 (FIG. 10 shows the online evaluation). conduct). During the two-dimensional development, a first solvent is used, the remainder of which may be removed by a suitable inert gas, and then a second solvent allows separation in the other direction.

Due to the lack of a large vapor space above the carrier plate 3, there is no need to take into account the negative influence of the bath medium on the subsequent development. During development, the temperature of the adsorbent layer 2 can be varied according to a predetermined nine-gram.

The temperature control device 24 in FIG. 11 is a heating element 4 of the present invention.
Alternatively, it is combined with a metal carrier plate 25, and the combination is a temperature sensor 31 or a temperature sensor system 31 provided for detecting the temperature of the component part of the adsorbent layer 2.
Configure. The temperature control device 24 regulates the power of the heating element 4 or the amount of electromagnetic charge delivered to the metal carrier plate 25, and the cooperation of these two units allows a feedback circuit according to FIG. 12. In this case, the unit 5 for determining the reference signal, ie the unit for programming the change in temperature, is connected to the comparator and through it to the amplifier! , and to the output of the amplifier C and to a signal type unit) d which constitutes a thyristor or other suitable element for regulating the output. The signal-forming unit) d provides its signal to the intervention unit 2, thereby providing means flc for ensuring temperature regulation of the device according to the invention in accordance with the requirements. The last unit is connected via a feedback network L to a comparator which generates a signal corresponding to the input signal difference. A comparative example can be implemented, for example, on the basis of platinum thermocouples. A preferred embodiment of the feedback system shown in FIG. 10 is the temperature control device 24 of FIG.

The temperature of the adsorbent layer 2 is determined by the temperature sensor 31 as described above.
at one or more points during the chromatographic development.

The output of the temperature sensor is connected via a differential amplifier 32 to a temperature disgray 33 and then to a comparator 45 with hysteresis.
and similarly comparative increase Ill? ! It is connected to the first inlet section of the vessel 39. Comparison amplifier 39 is a logic circuit element that generates an output signal of Uc level, which is a positive high level, a positive low level, or a negative level depending on the signal level sent to its input. It has at least a first input for receiving a U level signal, a second input for receiving a Ub level signal, and produces at its output a Ue level signal.

Level Ue is a positive high level when U is greater than Ub, decreases when the difference between levels U and Ub is smaller, and is relative when these two levels are the same or nearly the same. to a low positive level. Level U0 becomes negative when U is smaller than Ub.

A second input of the comparator amplifier 39 is an input means for a control key dart 34 or pond, a central microgrocer unit 35 connected to a second temperature display gray 38, and an optical switch 3.
6 and an integrator 37. In this case, optical switch 36 is used to couple integrator 37 and central microprocessor unit 35 without electrical contact. temperature disgray 33
is the temperature detected in the adsorbent layer 2, and the second temperature display 38 is the central microprocessor unit 35.
Shows the value programmed by . A control keyboard 34 or other suitable input means is provided for programming the central microprocessor unit.

The output of the comparator amplifier 39 is connected to the input of a comparator 40 for receiving the Uc level signal, this comparator 40
has a second input for receiving the Ud level signal generated by the level shifting unit 42 from the oscillator 41, which oscillator is preferably a sawtooth generator. The output of the comparator 40 which transmits the U, 7 Pel signal is a power source which generates a signal for controlling the heating element 4 associated with the heating unit of the apparatus 11A, e.g. Connected to switch 430 input. A comparator 45 with hysteresis is connected to a rerice (relmlm) 46, which
6 opens the passage under the conditions given to the current sent from the power supply unit 47.゛Temperature control device 2 that requires power supply
4 other units are connected to power supply means 48.

The temperature control device 24 ensures the regulation of the temperature according to the nologram to be placed in the device A by means of a control mate 34 cooperating with a central micronolocessor unit 35. This nologram can be determined from the adsorbent layer 2 according to FIG.
and the temperature change of the carrier plate 3 can be realized. This change means a temperature change over time t. The basic value of this temperature is T.

, which is the uppermost ML T on the intermediate values T1 and TZ with respective values of the characteristic gradients βl, β2 and β3
Descend towards s. Naturally, the nologram means determine different shapes and possible slopes. The lines associated with the temperature range may be non-linear if desired.

During operation of the temperature control device shown in FIG. 11, it is generally sufficient for the temperature to rise to a maximum of 90.degree. This temperature measurement is guaranteed with an accuracy of ±1°C. The temperature repeatability is approximately 0.5°C.

During this measurement, the rate of temperature change is preferably selected in the range from 20°C to 20°C/min. Temperature control unit 24
, a comparator amplifier 39 generates a signal Uc based on the above-mentioned temperature conditions, ensuring the heating intensity by the difference between the set temperature and the measured temperature and determining the temperature of the carrier plate 3 or the adsorbent layer 2. Turn off the power when the temperature is higher than the scheduled program temperature. The output of comparator 40 is increased.

The level signal is a rectangle whose width and distance are based on the temperature difference, that is, the input signal of the comparator 40! Consists of russ.

If the temperature of the adsorbent layer 2 is higher than the programmed temperature, a signal is generated thereby stopping the heating.

Hysteresis, Rerice 46 and High Power Unit 47
The comparator 45 has a protection function.

A comparator 45 with hysteresis provides an output signal if the temperature detected in the adsorbent layer 2 is higher than the maximum value allowed for the system, for example due to a fault in the electrical circuit. In this case, the rerice 46 closes the contact part,
And the current delivered by the high power unit 47 reliably interferes with the current path of the device A and its heating unit.

The temperature sensor 31 preferably consists of a firing unit and a current generator, the sensor element of which is provided in one branch of the generator being associated with the carrier plate 3 and the adsorbent layer 2. These elements can also be mechanically coupled. The final bath liquid ensures a high level of thermal coupling.

The above central microprocessor unit has optical switch 3
(well-known unit connected to three integrators via 6) 80
80 or 8085. This is because grounding is not required in this case. The power switch 43 is, for example, a Darlington circuit.
ton circuit).

Preferably, the heating element 4 is a circuit board with string-like channels for dissipating energy. A portion of this passage can be used to detect temperature.

During the analysis evaluated by the off-line method, a separation diagram for nicotine alkaloids according to FIG. 14 can be obtained. Here the influence of temperature can be observed. Repressor R
f increases in value with increasing temperature, contrary to known thin layer chromatography, which is characterized by an undesirable decrease in this cage. Nicotine alkaloids can typically be separated into five components that migrate through different distance ranges under the influence of different temperature programs, as shown in FIG. This temperature program is selectively determined.

For example, glograms (1) and (V) can be evaluated very well, ensuring chromatography, and the separation in these cases is very good. If a pond program is chosen, a separation is obtained in which several compounds occupy the same location and are very close to each other (f program LI [[ and V)].

The device for thin layer chromatography according to the present invention costs $1□
It ensures effective separation of different substances and expands the possibilities offered by overbred thin layer chromatography.

From the above description, it can be seen that the device of the invention may use a heating element, a carrier plate and an adsorbent layer similar to that described above, as well as a temperature control device for different program regulation having a circuit arrangement similar to that described above. should be obvious. A device of this construction is within the scope of the claims and depends on the given conditions and the components of the mixture to be separated.

[Brief explanation of the drawing]

FIG. 1 is a cross-sectional view of a preferred embodiment of the device according to the invention when using one carrier plate; FIG. 2 is a cross-sectional view of an array of carrier plates with an adsorbent layer and a heating element; FIG. A cross-sectional view of an array of carrier plates with a layer of adsorbent between two heating bodies, FIG.
h2′o”″”■Nail 66”1O1l[[! 9゛,: 5th
The figure shows a cross-sectional view of an arrangement with two carrier plates and a heating element for heating the two adsorbent layers; FIG. 6 shows an inductively heated carrier plate arranged between two closed spaces. 7 is a plan view of a carrier plate for line expansion used in online evaluation; FIG. 8 is a plan view of a carrier plate for two-way expansion used in online evaluation; Figure 9 is a plan view of a carrier plate for two-dimensional deployment used in online evaluation; Figure 10 is a plan view of a carrier plate for two-dimensional expansion used in online evaluation; Temperature used in the device according to the invention □ Block diagram of a preferred embodiment of the control device,
Figure 12 shows the temperature control panel used in the device of the present invention.
The working diagram of the unit, Figures 13A, B, 0 is a diagram showing some possibilities of temperature control used to control the heating unit, and Figure 14 is a diagram showing the possibility of controlling the heating unit. Includes 10 samples
0R4/Rf means a suppressor and indicates a separation state obtained by giving different values of / ■4
, is a schematic diagram. A... Apparatus, 1... Closed space, 2... Adsorbent layer,
3... 1゛Carrier Great, 4.
... Heating body, 6 ... Insulation brace, 7
... Board, 15... Second entrance, 16... First person
□ Port, 19...Detector, 20...Seal/i, 21...Entrance point, 22-...Groove, 23...
Charging point, 24...Temperature control device, 25...Carrier plate, 31...Temperature sensor, 32...
Differential amplifier, 33...temperature diss. Play, 34... Control keyboard, 35... Central micro processor unit, 36... Optical switch, 3
7... Integrator, 38... Second temperature display, 3
9...Comparison amplifier, 40...Comparator, 41...Shining oscillator, 42...Level shift unit), 43...
- Power switch, 44... Power oscillator, 45... Comparator, 46... Relisu, 47... High power supply unit, 48... Power supply means. (Continued from page 1) Inventor: Gisela Belsarne Hanga IJ
-Country, 1082 Petri 44) Inventor Sandor Meszaros Country of Hungary, 114874/BeIe Inventor Ildeiko Falka Hungary! J
- Country y 2013 Syune Tompa) Inventor Atteira Nagy Hungary,
1144) Inventor Lasja Sepesi Hungary,
1111) Inventor Las Lovida, Hungary, 1023 Rem Utsza 22) Inventor Emil Minčović, Hungary, 2000 eter 4) Inventor Gabor Kemeny, Hungary, 111
210/a) Inventor Zoltanne Baranyi Hungary, 1144 Italy 10
Budapest, Irei Utza Budapest, Fuogarasi Utzapomaz, Samoka Utza 2 Futapest, Feredi Utza Abdapest, Zenta Utza 5 Budapest, Arpad Hueyedesentendre, Basarhelyika.

Claims (1)

[Claims] 1. At least one carrier plate 3 provided adjacent to the closed space 1; an adsorbent layer 2 provided on the surface of the carrier plate 3; means for covering the surface of said adsorbent layer 2 under the influence of pressure, a first inlet 1 for delivering a solvent to said adsorbent layer 2;
6, comprising a second inlet 15 for sending an overpressure medium into the closed space 1, further comprising a heating unit for changing the temperature of the adsorbent layer 2 and a temperature control device for supplementing the heating unit; An apparatus for overpressure thin layer chromatography, characterized in that the control output of the temperature control device 24 is associated with the heating unit. 2. The apparatus according to claim 1, wherein the heating unit includes a plate-shaped heating body 4 provided parallel to the carrier plate 3 and adjacent to the adsorbent layer 2. 3. The device according to claim 1 or 2, comprising a heat insulating element provided adjacent to the carrier plate 3 on the opposite side from the heating unit. 4. The heating unit includes at least two plate-shaped heating bodies 4
and a carrier plate 3 arranged in parallel between the heating element and the heating element.
An apparatus according to any one of claims 1 to 3, comprising: 5. At least two carrier plates 3 and a heating body 4 between the carrier plates, the heating body 4 forming part of the heating unit.
4. The device according to any one of items 4 to 4. 6. The device according to any one of claims 1 to 5, comprising at least two heating bodies 4 and at least two carrier plates 3 arranged in parallel forming part of the heating unit. Device. 7. The device according to claim 1, comprising a metal carrier plate (25) cooperating with an induction heating unit for energizing the adsorbent layer (2). 8. at least one carrier plate 3 provided adjacent to the closed space 1; an adsorbent layer 2 provided on the surface of the carrier plate 3; means for covering the surface of the adsorbent layer 2; a first inlet 1 for delivering solvent to the adsorbent layer 2;
6, comprising a second inlet 15 for sending an overpressure medium into the closed space 1, a heating unit for varying the temperature of the adsorbent bed, and a temperature control device 24 for energizing the heating unit, A central microprocessor in which a control device 24 is connected by each of its inputs and outputs to the heating unit divided into a plurality of parts for varying the temperature of the adsorbent layer 2 in a programmed spatial and temporal sequence. An apparatus for overpressure thin layer chromatography, characterized in that it has a unit 35. 9. Comparison amplifier 39 via differential amplifier 32 for the temperature control device 24 to detect the temperature of the adsorbent layer 2
has a temperature sensor 31 connected to an input of a comparator 40 through a first input of the comparator 39, a second input of which comparator 39 has a control keyboard 34 for programming a central microprocessor unit 35 and an integrator. The comparator amplifier 39 is connected to an output section consisting of a continuous member having a comparator 37 in which the signal U_a at the first input is connected to the signal U_a at the second output.
When the signal U_a at the first input is at a higher level than the signal U_b at the second input, a positive high level signal is output; When the level is lower than the input signal U_b, a negative level signal is sent. Vessel 4
9. The device according to claim 8, wherein the output 0 is associated with the power switch 43 and forms the control output of the temperature control device 24. 10. The power supply 43 is re-licensed 46 by its input part.
, the relice 46 is connected via one input to a comparator with hysteresis 45 combined with the first inlet of the comparator amplifier 39 and via another input to a high power supply unit 47. 10. The device according to claim 9, wherein the apparatus is 11. Apparatus according to claim 9 or 10, wherein said continuous member comprises an optical switch 36 between said central microprocessor unit 35 and said specifier. 12. At least one carrier plate 3 provided adjacent to the closed space 1; at least one adsorbent layer 2 provided on the surface of the carrier plate 3; influence of overpressure occurring within the closed space 1; means for covering the surface of the at least one adsorbent layer 2 below, a first inlet 16 for delivering solvent to each of the adsorbent layers 2, a second inlet 15 for delivering an overpressure medium to the enclosed space 1;
, a heating element 4 arranged parallel to the carrier plate 3
, and a temperature control device 24 for energizing the heating body 4 , the temperature control device 24 having an input and an output, respectively, in a space determined by a program stored in a central microprocessor unit 35 . Apparatus for overpressure thin layer chromatography, characterized in that it has a central microprocessor unit 35 connected to a plurality of divided heating elements 4 in order to vary the temperature of the adsorbent layer 2 in time sequence. 13. The temperature control device 24 connects the comparison amplifier 3 via the differential amplifier 32 to detect the temperature of the adsorbent layer 2.
9 and a temperature sensor 31 connected to an input of a comparator 40, the second input of which is connected to a control keyboard 34 for programming said central microprocessor unit 35. The comparator amplifier 39 is connected to the output of a continuous member having an integrator 37, and the comparator amplifier 39 has a first input signal U_a and a second output signal U_a.
When the signal U_a at the first input is at a higher level than the signal U_b at the second input, a positive high level signal is output, and when the signal U_a at the first input is at almost the same level as the signal U_b at the second input, a positive low level signal is output. When the level is lower than the second input signal U_b, a negative level signal is sent, and the other input section of the comparator 40 is connected to the output section of the tension oscillator 41 via the level shift unit 42, 13. The apparatus of claim 12, wherein the output of the comparator (40) is coupled to a power switch, the output of the power switch forming a control output of the temperature control device (24). 14. The power supply 43 is re-licensed 46 by its input section.
, the relice 46 is connected via one input to a comparator with hysteresis 45 coupled to the first input of the comparison amplifier 39 and via another input to a high power supply unit 47. 13. The device of claim 12, being connected. 15. The apparatus of claim 13, wherein said continuous member includes an optical switch 36 between said central microprocessor unit 35 and said integrator 37.