阅读说明：本技术 用于色谱装置的气液分离器 (Gas-liquid separator for chromatographic apparatus ) 是由 亚历山大·博齐克 于 2018-05-15 设计创作，主要内容包括：本发明描述一种用于色谱装置的气液分离器,包括：a)具有入口喷嘴、碰撞单元和导气单元的分离区；b)具有液体出口的分隔区；以及c)具有气体出口的气体导出区；其中所述分离区通过分离开口与所述分隔区连通,所述入口喷嘴与所述碰撞单元的距离大于所述分离开口的最小线膨胀,并且所述入口喷嘴被设计成使得由所述入口喷嘴导引的气液流可被施加到所述碰撞单元上。此外,本发明描述一种包括本发明的分离器的色谱装置以及一种使用所述分离器的色谱方法。(The present invention describes a gas-liquid separator for a chromatography apparatus comprising: a) a separation zone having an inlet nozzle, a collision unit, and an air guide unit; b) a separation zone having a liquid outlet; and c) a gas lead-out zone having a gas outlet; wherein the separation zone communicates with the separation zone through a separation opening, the inlet nozzle is at a distance from the collision cell greater than the minimum linear expansion of the separation opening, and the inlet nozzle is designed such that the gas-liquid stream directed by the inlet nozzle can be applied to the collision cell. Furthermore, the invention describes a chromatography apparatus comprising the separator of the invention and a chromatography method using said separator.)

1. A gas-liquid separator for a chromatography apparatus comprising:

a) a separation zone having an inlet nozzle, a collision unit, and an air guide unit;

b) a separation zone having a liquid outlet; and

c) a gas lead-out zone having a gas outlet;

characterized in that the separation zone communicates with the separation zone through a separation opening, the inlet nozzle is at a distance from the collision cell which is greater than the minimum linear expansion of the separation opening, and the inlet nozzle is designed such that the gas-liquid stream guided by the inlet nozzle can be applied to the collision cell.

2. The gas-liquid separator according to claim 1, wherein said separation zone does not have a circular cross-section in the region of said inlet nozzle, wherein said separation zone preferably comprises at least three side walls which together with an upper closure member define a space which communicates with said separation zone through said separation opening.

3. The gas-liquid separator of claim 1 or 2, wherein the gas-liquid separator is operable with a gas flow direction in the separation zone substantially parallel to a liquid flow direction.

4. The gas-liquid separator according to at least one of the preceding claims, wherein said separation opening is designed such that the gas flow velocity in said separation zone is reduced.

5. The gas-liquid separator of claim 4, wherein the separation opening has two, three, four or more sub-separation openings, the gas flow rate being reducible by the arrangement of the sub-separation openings.

6. The gas-liquid separator of at least one of the preceding claims, wherein the gas-liquid separator has structure in the separation zone for reducing gas flow.

7. Gas-liquid separator according to at least one of the preceding claims, characterized in that the collision cell is substantially flat and can be regarded as a baffle, wherein this baffle preferably forms one wall of the separation zone and is a side wall of the air guide cell.

8. Gas-liquid separator according to at least one of the preceding claims, characterized in that a deflecting unit is provided in the separation zone, which can apply the aerosol flow to the second collision unit.

9. Gas-liquid separator according to at least one of the preceding claims, characterized in that the collision cell has a surface area with a surface energy in the range of 15 to 120mN/m, particularly preferably in the range of 20 to 80mN/m and especially preferably in the range of 22 to 60mN/m, wherein preferably at least 80%, especially preferably at least 90% of the surfaces of the collision cell have a surface energy in the range of 20 to 80mN/m, especially preferably in the range of 22 to 60 mN/m.

10. The gas-liquid separator of at least one of the preceding claims, wherein the ratio of the entry area of the inlet nozzle disposed in the separation zone to the volume of the separation zone is at 4:1mm ²Per ml to 1:50mm ²In the/ml range, preferably in the 1:1mm range ²Per ml to 1:20mm ²In the/ml range and particularly preferably in the 2:3mm range ²Per ml to 1:5mm ²The/ml range.

11. Gas-liquid separator according to at least one of the preceding claims, wherein the separation zone comprises at least two side walls, preferably at least three side walls, which together with an upper closure and a gas acceleration unit define a space forming the gas guide unit, wherein one of the side walls, the gas acceleration unit or the upper closure is formed as a collision unit, wherein this space communicates with the separation zone through the separation opening, wherein the distance between two opposite side walls is more than half the distance of the inlet nozzle from the collision unit.

12. Gas-liquid separator according to at least one of the preceding claims, characterized in that the ratio of the discharge area of the separation opening to the volume of the gas-liquid separator is at 0.05mm ²Per ml to 6mm ²In the/ml range, particularly preferably in the 0.3mm range ²From ml to 3mm ²In the/ml range and particularly preferably in the range of 0.5mm ²Per ml to 2.0mm ²The/ml range.

13. Gas-liquid separator according to at least one of the preceding claims, characterized in that the inlet nozzle is designed such that the gas-liquid stream guided by the inlet can be applied to the collision cell and the gas-liquid stream guided by the inlet nozzle can be applied to the collision cell at an angle preferably in the range of 50 ° to 130 °, particularly preferably in the range of 70 ° to 110 °.

14. A chromatography device comprising at least one gas-liquid separator according to at least one of claims 1 to 13.

15. A method of separating a gas-liquid mixture, characterized in that a gas-liquid separator according to at least one of claims 1 to 13 or a chromatography device according to claim 14 is used.

Technical Field

The present invention relates to a gas-liquid separator for a chromatography apparatus and a method of separating a gas-liquid mixture.

Background

Supercritical Fluid Chromatography (SFC) has the advantage of being able to separate and chemically analyze, identify and quantify various substances particularly conveniently and reliably. Use of carbon dioxide (CO) in SFC applications ₂) As a liquid, the extraction of the substance is generally carried out at a critical temperature of 31 ℃ or higher and a critical pressure of 74bar or higher.

In order to introduce CO inside the column ₂Or CO ₂The mixture remains in a liquid state and the entire chromatography system must be maintained at a preset pressure level. To this end, a back pressure regulator is usually provided downstream of the chromatography column and downstream of the detector in order to maintain the pressure inside the chromatography system at a preset level.

In practical applications, the SFC technology has the following disadvantages: the mobile phase of the chromatographically separated material cannot be conveniently collected in an open container. Liquid CO ₂Mixture with additional solvent upon exposure to atmospheric pressure, CO ₂It expands and forms an aerosol with the additional solvent. The non-destructive collection of the solvent requires a sufficient gas-liquid separation of the aerosol. In general, the gas can be separated using an inertial separator operating on the cyclone principleThe liquid mixture is separated into a gaseous component and a liquid component. In an inertial separator, the aerosol is introduced tangentially into a conical container. The aerosol spreads on a circular trajectory, so that its liquid particles drift radially outward until hitting the container side wall. Due to the reduced specific mass, the gaseous component is subjected to less inertial forces and can leave the conical container by means of the central submerged tube.

However, SFC can use solvent gradients to separate substances multiple times resulting in aerosol compositions that vary greatly. In CO ₂In mixtures with additional solvents, such as methanol, the methanol fraction can vary, for example, from 10% to 60%. Consequently, the composition and volumetric flow rate of the aerosol may vary accordingly, resulting in a sub-optimal separation rate of the gaseous fraction from the liquid fraction of the aerosol in the cyclone.

Other gas-liquid separation systems, for example, employ collision separation, in which the volumetric flow of the aerosol is directed against a deflector plate, which may be provided by a cuvette, as the case may be. Collision and inertial separators generally require a large volume into which the expanding aerosol can enter. Such larger containers are not optimal in terms of self-cleaning effect, since cross-contamination of aerosol and substances, which in turn are treated by such separators, is possible. In particular, the propagation time difference of the substances must be very large to ensure sufficient separation. In principle, the size and surface of the impact separator can be minimized when working at elevated pressure levels.

For example, test tubes used as deflector plates may be placed in a pressurized environment. In this case, the aerosol can escape from the curved outlet and can hit the side wall of the test tube at a preset angle. It is indeed easier to collect smaller quantities of material by means of such an impact separator.

However, the impact separators operating at elevated pressure levels do not allow large scale automated fractionation.

This results in high operating and installation costs, since only a limited number of test tubes can be handled automatically in the pressure area. In addition, the separation speed is not as fast as in a separator operating at atmospheric pressure.

Disclosure of Invention

In view of the prior art, it is an object of the present invention to provide a gas-liquid separator for a chromatography apparatus that solves the aforementioned problems. Wherein the gas-liquid separator should be as easy and as low cost as possible to manufacture. Furthermore, the volume of the gas-liquid separator should be as small as possible, with reference to the volume flow used for the operation of the chromatography apparatus.

Furthermore, it is an object of the present invention to provide a gas-liquid separator which is capable of perfectly separating liquid from a mixture in the case of large and widely varying aerosol composition differences. Further, the gas-liquid separator should be easy to clean and should have low maintenance work.

It is therefore also an object of the present invention to provide a gas-liquid separator having a particularly high separation efficiency. In particular, it should be possible to remove the gas from the liquid as thoroughly as possible. It is however more important to leave as little liquid content as possible in the gas stream conducted out of the gas-liquid separator in order to ensure as high a yield of purified material as possible. It should be possible to achieve such high separation efficiencies on as different gas-liquid mixtures as possible.

Another object is to provide a gas-liquid separator in which the substance introduced into the gas-liquid separator separately from the column does not contain impurities due to contamination. For this purpose, it should be possible to flush the gas-liquid separator with as small an aerosol volume as possible. In addition, no encrustation or sticking phenomena should occur in the gas-liquid separator which could contaminate the next fraction. In particular, the substances to be separated should have as small a propagation time difference as possible, but without thereby impairing the separation of the substances to be separated in the gas-liquid separator. Furthermore, the gas-liquid separator should achieve as efficient a separation of the batch material as possible at a predetermined travel time difference.

Another object is to provide a gas-liquid separator which enables to retrofit known HPLC units into SFC units in as simple a manner as possible.

The solution for achieving the above objects and other objects, which, although not explicitly mentioned, can be directly derived or inferred from the context, is a gas-liquid separator for a chromatography apparatus having all the features of claim 1.

Accordingly, the subject of the present invention is a gas-liquid separator for a chromatography apparatus comprising:

a) a separation zone having an inlet nozzle, a collision unit, and an air guide unit;

b) a separation zone having a liquid outlet; and

c) a gas lead-out zone having a gas outlet;

characterized in that the separation zone communicates with the separation zone through a separation opening, the inlet nozzle is at a distance from the collision cell which is greater than the minimum linear expansion of the separation opening, and the inlet nozzle is designed such that the gas-liquid stream guided by the inlet nozzle can be applied to the collision cell.

The invention is primarily intended to improve the separation efficiency of a gas-liquid separator, in particular to separate liquid from aerosol very efficiently. Furthermore, contamination of the substances which are separated in the column and which are introduced into the gas-liquid separator can be reliably avoided. Compared with other gas-liquid separators, the improvement mainly refers to that: a very efficient separation of the batch passing through the gas-liquid separator can be achieved with a preset travel time difference. In addition, in the case where the difference in the propagation times of the substances to be separated is relatively small, excellent separation can be achieved in the gas-liquid separator.

In addition, the gas-liquid separator is low in manufacturing cost and easy to manufacture. Moreover, the gas-liquid separator is low in maintenance and convenient to clean.

In addition, excellent gas-liquid separation can be achieved even at different gas-liquid compositions. In addition, the gas-liquid separator can be used even in the case of a large difference in aerosol volume flow rate without seriously affecting the separation of the aerosol.

Furthermore, it is possible to achieve an automated fractionation which can be scaled to the requirements, without a large investment.

In addition, the complexity and cost of the technical equipment required for SFC analysis can be reduced by the gas-liquid separator.

The invention is based on the following recognition: by providing and designing the separation opening, the collision separation can be improved unexpectedly. Specifically, this can reduce the volume of gas supplied at the time of collision separation, and thus can reduce the total volume of the gas-liquid separator. Whereby the aforementioned separation efficiency can be improved.

The gas-liquid separator of the present invention includes a separation region having an inlet nozzle, a collision unit, and an air guide unit.

The separation zone is preferably designed to enable collision separation. Collision separation means: the droplets in the aerosol are directed onto the collision cell, so that a liquid film can be formed. Wherein the aerosol can be directed in a direct jet from the inlet nozzle onto the collision cell. Furthermore, two or more collision cells can be provided in the separation region, by means of which at least partial gas-liquid separation of the aerosol is achieved. Furthermore, the aerosol may be directed into the separation zone by two or more inlet nozzles, wherein deflection of the aerosol flow may be achieved.

Any object that can be hit by the aerosol stream can be used as a collision cell. For example, the aerosol flow may be directed onto an upper region of the separation zone, for example onto an upper closure of the separation zone. In this case, projections, for example protrusions or the like, can be provided, onto which the aerosol flow is applied, so that the drops guided onto the collision cell do not reflect back or bounce back from the collision cell, but form a film. The collision cell can occupy areas of different sizes inside the separation zone, according to the way described above of introducing the aerosol flow into the separation zone. When a large degree of deflection is induced by the introduction of two or more aerosol streams into the separation zone, the entire inner surface of the upper region of the separation zone can be considered as a collision cell.

The gas-liquid separator utilizes the gravitational force to separate gas and liquid when working. Accordingly, the expression "upper" relates to the orientation of the gas-liquid separator when in operation, whereby gas can flow upwards, whereas "lower" refers to the opposite direction, in which liquid leaves the gas-liquid separator.

In a preferred embodiment, the following settings are possible: the collision cell is substantially flat and can be regarded as a baffle, wherein this baffle preferably forms one wall of the separation zone and is a side wall of the air guide cell. The expression "substantially flat" means: the collision cell or the baffle is not curved but may have a surface structure. In a particular embodiment, the baffle is preferably designed without a surface structure, so that this surface is smooth.

In a preferred embodiment, the collision cell preferably comprises a surface structure, wherein this embodiment is preferred over an embodiment with a smooth surface. The surface structure preferably has elevations and depressions, wherein the height of the elevations, referred to the depressions, is preferably in the range from 0.2mm to 10mm, particularly preferably in the range from 0.8mm to 8mm, and particularly preferably in the range from 1.5mm to 5 mm.

Further, the following settings are possible: the ratio of the height of the projections (with reference to the depressions) to the volume of the gas-liquid separator is preferably in the range of 0.01mm/ml to 10mm/ml, particularly preferably in the range of 0.03mm/ml to 5 mm/ml.

In a further embodiment, the surface structure of the collision cell has grooves, wherein the elevations and depressions of the grooves are preferably oriented in the direction formed by the inlet nozzle and the separation opening or extend parallel to this direction.

By means of the structured surface of the collision cell, which is preferably formed as a groove structure, the volume of the gas-liquid separator can be kept particularly small, thereby improving the separation efficiency. In this case, the substances to be separated can have a relatively small propagation time difference without the separation of the substances to be separated in the gas-liquid separator being impaired thereby. In addition, the separation degree of the liquid from the aerosol can be improved with reference to the volume of the gas-liquid separator.

In another preferred embodiment, the following steps are provided: the collision cell has a curvature or curvature, wherein the radius of curvature is preferably small. The collision cell is here preferably formed as part of the upper closure or as part of the gas acceleration unit, as will also be explained in more detail below.

In a further development of the invention, the crash unit preferably has a surface area with a surface energy of at least 10mN/m, particularly preferably at least 15mN/m and particularly preferably at least 20 mN/m. Preferably, the following settings are possible: the collision cell preferably has a surface area with a surface energy in the range from 15mN/m to 120mN/m, particularly preferably in the range from 20mN/m to 80mN/m and particularly preferably in the range from 22mN/m to 60mN/m, wherein preferably at least 80%, particularly preferably at least 90%, of the collision cell surfaces have a surface energy in the range from 20mN/m to 80mN/m, particularly preferably in the range from 22mN/m to 60 mN/m. This surface energy can be achieved by a corresponding material selection (material used for the production of the crash unit).

Further, the collision cell can have a coated surface area in order to adjust the surface energy, wherein preferably at least 80%, particularly preferably at least 90%, of the collision cell surface is coated.

According to Ownes-Wendt-Rabel&The Kaelble method measures surface energy. For this purpose, a series of measurements was carried out using the Busscher standard series, in which the test liquid used was water [ SFT 72.1mN/m]Formamide [ SFT 56.9mN/m]Diiodomethane [ SFT 50.0mN/m]And α -bromonaphthalene [ SFT 44.4mN/m]The surface energy can be determined using the G40 contact angle measurement system from the company hamburger Kr ü ss, wherein the method of implementation is described in the user's manual of the G40 contact angle measurement system (1993), for the calculation method, reference can be made to a.w.neumann,

die Messmethodik zur Bestimmung

(measurement method for determining the magnitude of interfacial energy), part I, Zeitschrift f ü r Phys. chem. (journal of physical chemistry), volume 41, page 339-352 (1964), and A.W.Neumann,

die Messmethodik zur Bestimmung (measurement method for determining the magnitude of interfacial energy), part II, Zeitschrift f ü r Phys. chem. (journal of Physichemistry), volume 43, pages 71-83 (1964).

In a preferred embodiment, the following settings may be provided: the air flow hits the collision cell and is guided to the second collision cell. By this design, the separation efficiency, in particular the separation of liquid from the aerosol, can be surprisingly improved. Preferably, the aerosol may first be directed onto a first collision cell, e.g. formed by one wall of the separation zone. The gas flow can then be directed onto a second collision cell, which is preferably arranged in the upper region of the separating area, particularly preferably in the upper closure of the separating area.

Further, the following settings are possible: two collision cells are provided in the separation zone, wherein the first collision cell is arranged below the second collision cell. The aerosol is guided first onto a first collision cell arranged below a second collision cell and then onto the second collision cell.

In the separation zone of the gas-liquid separator of the present invention, an inlet nozzle is provided in addition to the collision unit. The aerosol is directed from the inlet nozzle into the gas-liquid separator, in particular into a separation zone of the gas-liquid separator.

As already mentioned in connection with the collision cell, the inlet nozzle is here designed such that the gas-liquid stream guided by the inlet nozzle can be applied to the collision cell.

The shape and type of inlet nozzle is not critical and can be selected by the person skilled in the art within his ability. For example, the inlet nozzle can be designed such that the aerosol is directed onto the collision cell in a very narrow jet. Furthermore, the inlet nozzle can also be designed to direct a conical spray onto the collision cell.

The nozzle can here be flush with the wall of the separation zone or project into the separation zone via a projection. The embodiment with a projection is advantageous if the collision cell is arranged in the upper closure of the separation zone.

Particularly preferably, the inlet nozzle is designed in the form of a simple bore or a simple opening. In a further embodiment, the following can be provided: the inlet nozzle disposed in the separation zone has a substantially circular entry face.

Further, the following settings are possible: the inlet nozzle disposed in the separation zone had an inlet diameter at 0.05mm ²To 20mm ²In the range of 0.5mm, preferably ²To 15mm ²In the range, particularly preferably 0.5mm ²To 10mm ²In the range and particularly preferably in the range of 0.8mm ²To 5mm ²The area of entry of the range. In another embodiment, the following can be provided: the inlet nozzle disposed in the separation zone had an inlet diameter at 2mm ²To 40mm ²In the range of preferably 4mm ²To 20mm ²In the range and particularly preferably in the range of 5mm ²To 15mm ²The area of entry of the range. In case several inlet nozzles are used, this value relates to the size of a single inlet nozzle.

If the inlet nozzle is designed in the form of a bore, the bore preferably has a diameter in the range from 0.3mm to 5mm, preferably from 0.5mm to 4mm, particularly preferably from 0.8mm to 3mm, particularly preferably from 1mm to 2mm and/or particularly preferably from 2mm to 3 mm. In case several inlet nozzles are used, this value relates to the size of a single inlet nozzle.

Further, the following settings are possible: the ratio of the inlet area of the inlet nozzle provided in the separation zone to the volume of the gas-liquid separator was 0.01mm ²From ml to 1mm ²In the/ml range, preferably in the range of 0.04mm ²Per ml to 0.4mm ²In the/ml range, particularly preferably in the 0.08mm range ²Per ml to 0.25mm ²In the/ml range and particularly preferably in the range of 0.08mm ²Per ml to 0.17mm ²The/ml range. In the case of several inlet nozzles, this value relates to the sum of the areas of all the inlet nozzles used.

Further, the following settings are possible: the ratio of the entry area of the inlet nozzle arranged in the separation zone to the volume of the separation zone is 1:3mm ²Per ml to 1:50mm ²In the/ml range, preferably in the 1:5mm range ²Per ml to 1:20mm ²In the/ml range and is particularly preferredThe land is selected at 1:7mm ²Per ml to 1:15mm ²The/ml range. In another embodiment, the following can be provided: the ratio of the entry area of the inlet nozzle arranged in the separation zone to the volume of the separation zone is 4:1mm ²Per ml to 1:50mm ²In the/ml range, preferably in the 1:1mm range ²Per ml to 1:20mm ²The/ml range and particularly preferably lies in the range from 2:3mm2/ml to 1:5mm 2/ml. In the case of several inlet nozzles, this value relates to the sum of the areas of all the inlet nozzles used.

One or several inlet nozzles may be provided in the separation zone. In the case of several inlet nozzles, these are preferably oriented in parallel. The gas-aerosol mixture is preferably introduced into the separation zone from exactly one inlet nozzle, preferably onto a collision cell located in the separation zone.

In another preferred embodiment, the separation zone comprises two or more inlet nozzles, wherein the inlet nozzles are preferably arranged such that the flow of the gas-aerosol mixture is directed onto different parts of one collision cell or onto different collision cells. The two or more inlet nozzles are preferably designed such that the gas-liquid streams directed by the two or more inlet nozzles are aligned with each other, so that these gas-liquid streams would at least partially meet if no collision cell were present. Accordingly, in this preferred embodiment with two or more inlet nozzles, the collision cell or collision cells are preferably arranged between the two or more inlet nozzles.

In another preferred embodiment, the separation zone comprises two or more inlet nozzles, wherein these inlet nozzles are preferably arranged such that the flow velocity of the gas-aerosol mixture is reduced in the upper region of the separation zone. Accordingly, it is preferable to set as follows: the gas-liquid streams directed by the two or more inlet nozzles are aligned with one another. In this preferred embodiment, for example, part of the side walls of the separating zone preferably form the respective collision cell. By this design, the separation efficiency, in particular the separation of liquid from the aerosol, can be surprisingly improved. Here, two or more inlet nozzles may be arranged such that the air flow can be attenuated to the greatest extent. Further, the following settings are possible: two or more inlet nozzles are aligned with one another but the gas-liquid streams are slightly offset from one another so that, although the gas streams are attenuated, this attenuation of the gas streams is not maximized. The impairment of the air flow is here dependent on the original velocity vector of the air flow including the original direction of the air flow.

Further, the following settings are possible: the inlet nozzle is designed such that the gas-liquid stream guided by the inlet can be applied to the collision cell and the gas-liquid stream guided by the inlet nozzle can be applied to the collision cell at an angle preferably in the range from 50 ° to 130 °, particularly preferably in the range from 70 ° to 110 °. In particular, this angle can be determined by the direction in which the inlet nozzle is directed at the collision cell. These data relate to the angle at which the primary jet of aerosol is directed onto the collision cell. The shape of the aerosol jet is not critical per se, as long as collision separation is achieved. In this case, the droplets of the aerosol should be joined by hitting the collision cell and preferably form a film. Therefore, the inlet nozzle should be chosen such that the droplets of the aerosol do not become too small.

In a preferred embodiment, two collision cells are provided in the separation zone, wherein the inlet nozzle directs the gas flow onto the first collision cell as described above. Any known means may be used to divert the flow of air onto the second collision cell. For example, the deflection at the first collision cell can be achieved by a corresponding angle and/or a corresponding shape of the first collision cell. In a preferred embodiment, the following settings are possible: a deflector unit is provided, by means of which the aerosol flow is guided onto the second collision unit. The deflecting unit preferably has at least three separating surfaces, so that the air flow is guided from the inlet of the inlet nozzle through the outlet opening onto the second collision unit. Hereby, the deflector element preferably forms a gap, the bottom of which may be U-shaped or V-shaped, and which has two opposite side faces and an end face which preferably serves as the first collision element, so that a space is defined between the inlet of the inlet nozzle and the first collision element. The inlet nozzle preferably guides the aerosol flow or the gas flow parallel to the bottom of the interspace, so that the aerosol flow or the gas flow hits the end face formed as a first collision cell. The aerosol flow is then guided through the recess or the outlet opening of the deflector unit onto the second collision unit. In a preferred embodiment, the deflection of the gas flow is preferably directed upwards at an angle preferably in the range from 50 ° to 130 °, particularly preferably in the range from 70 ° to 110 °, with reference to the direction of the aerosol flow directed from the inlet nozzle onto the first collision cell. Preferably, the flow velocity of the aerosol flow is limited by this embodiment, wherein the air flow reflected back from the first collision cell, in particular from the end face of the deflector unit, preferably from the interspace, is first aligned with the aerosol flow directed from the inlet nozzle into the deflector unit, preferably into the interspace.

Further, the following settings are possible: the outlet opening of the deflection unit or of the recess, which is preferably arranged in the separating zone, has a diameter of 0.1mm ²To 60mm ²In the range of 1.5mm, preferably ²To 40mm ²Range and particularly preferably at 3mm ²To 20mm ²The discharge area of the range.

Preferably, the following settings are possible: the discharge area of the outlet opening of the deflector element or of the recess is at least as large as the inlet area of the inlet nozzle. Preferably, the area ratio of the outlet opening of the deflector element or of the recess, which is preferably arranged in the separation zone, to the inlet area of the inlet nozzle arranged in the separation zone is in the range from 20:1 to 1:1, preferably in the range from 15:1 to 3:2 and particularly preferably in the range from 5:1 to 2: 1.

Further, the following settings are possible: the deflector element or the recess arranged in the separating zone preferably has a width in the range from 0.3mm to 8mm, preferably from 0.8mm to 5mm and particularly preferably from 1.5mm to 4 mm. The width of the deflector element or gap is the maximum distance between at least two opposing sides.

Further, the following settings are possible: the deflector element or the recess preferably arranged in the separating zone has a length in the range from 1mm to 60mm, preferably from 5mm to 40mm and particularly preferably from 10mm to 30 mm. The length of the deflector element or gap is the distance between the surface formed as a collision element and the inlet nozzle.

Further, the following settings are possible: the deflector element or the recess arranged in the separating zone preferably has a height in the range from 0.5mm to 40mm, preferably from 1.5mm to 30mm and particularly preferably from 5mm to 20 mm. The height of the deflector element or the recess is the distance between the bottom of the deflector element or the recess and the discharge opening.

The gas-liquid separator has a separation opening arranged between the separation zone and the dividing zone, so that there is a through-flow connection of gas and liquid between these zones. Preferably, the inertial separation is achieved by a separation opening. That is, the liquid propagating downwards in the form of a liquid film on the collision unit and/or the gas guiding unit is separated from the gas by inertia. Wherein the gas is preferably accelerated by the liquid such that the liquid is transferred into the separation zone at a higher velocity than without the gas acceleration. In this case, the liquid film preferably rests in the form of a film on a wall of the separating zone, which is preferably designed as part of the collision cell and/or the gas conducting cell, and is transferred directly into the separating zone without leaving this wall adjoining the separating zone. In contrast to the liquid phase, the gas phase does not adhere to the walls but can be discharged upwards and transferred into a gas discharge zone. In contrast, the liquid is discharged into the separation zone and leaves the gas-liquid separator through a liquid outlet provided in the separation zone.

The shape of the separation opening is not critical as long as the above-described function of the separation opening is achieved. However, it is preferably set as follows: the separating opening has a discharge surface which is gap-shaped or has several openings arranged in parallel, which may be U-shaped, V-shaped or circular, for example.

According to the invention, the distance of the inlet nozzle from the collision cell is greater than the minimum linear expansion of the separation opening. The distance between the inlet nozzle and the collision cell is derived from the distance traveled by the aerosol from the inlet nozzle to the hitting collision cell. The minimum linear expansion of the separation opening relates to the width or length of the separation opening, wherein the planar expansion up to the edge of the separation opening is related to the plane between the separation zone and the separating zone which results in the separation opening having the smallest area. The length of the longest expansion of the separation opening is determined in this plane of the separation opening, so that the shortest length of the separation opening perpendicular to the longest expansion of the separation opening can then be measured. This minimum linear expansion can also be considered herein as the width of the separation opening.

If the separating opening is gap-shaped, the separating opening preferably has a gap width (minimum linear expansion) in the range from 0.1mm to 1.5mm, particularly preferably from 0.3mm to 1.0mm and particularly preferably from 0.4mm to 0.7 mm. In the case of a circular or oval separating opening, the gap length depends on the circumference, wherein these values can preferably lie in the range from 5mm to 120mm, particularly preferably in the range from 10mm to 60 mm.

If the separating opening is gap-shaped, the separating opening preferably has a gap width (minimum linear expansion) in the range from 0.1mm to 3.0mm, particularly preferably from 0.3mm to 2.0mm and particularly preferably from 0.4mm to 1.5mm in a further embodiment. In the case of a circular or oval separating opening, the gap length depends on the circumference, wherein these values in a further embodiment can preferably lie in the range from 5mm to 150mm, particularly preferably in the range from 10mm to 80 mm.

In the case of a non-circular or non-oval separation opening with a gap shape, preferably characterized by two ends, the length of the separation opening is preferably in the range from 3mm to 80mm, preferably in the range from 5mm to 50mm, particularly preferably in the range from 15mm to 30 mm.

The dimensions mentioned above apply accordingly if the separating opening is realized by several openings arranged in parallel and which can be, for example, U-shaped, V-shaped or circular, wherein these openings preferably have a width (minimum linear expansion) in the range from 0.1mm to 1.5mm, particularly preferably from 0.3mm to 1.0mm and particularly preferably from 0.4mm to 0.7 mm. In a further embodiment, the openings can preferably have a width (minimum linear expansion) in the range from 0.1mm to 3.0mm, particularly preferably from 0.3mm to 2.0mm and particularly preferably from 0.4mm to 1.5 mm.

The gap width, which is the minimum linear expansion of the gap opening that can be considered as the transition plane from the separation zone to the separation zone, is measured perpendicular to the gap length or gap circumference. This transition plane has minimal two-dimensional expansion in the transition region from the separation zone to the separation zone.

The separation opening preferably has a diameter of at least 10mm ²To 120mm ²In the range, particularly preferably 15mm ²To 60mm ²Range and particularly preferably at 15mm ²To 40mm ²The discharge area of the range. In another embodiment, the separation opening may have a diameter at 10mm ²To 180mm ²In the range, particularly preferably 15mm ²To 120mm ²In the range and particularly preferably in the range of 30mm ²To 100mm ²The discharge area of the range. Further, the following settings are possible: the ratio of the discharge area of the separation opening to the volume of the gas-liquid separator was 0.05mm ²Per ml to 2mm ²In the/ml range, particularly preferably in the 0.1mm range ²From ml to 1mm ²In the/ml range and particularly preferably in the 0.3mm range ²Per ml to 0.8mm ²The/ml range. In another embodiment, the following can be provided: the ratio of the discharge area of the separation opening to the volume of the gas-liquid separator was 0.05mm ²Per ml to 6mm ²In the/ml range, particularly preferably in the 0.3mm range ²From ml to 3mm ²In the/ml range and particularly preferably in the range of 0.5mm ²Per ml to 2.0mm ²The/ml range.

The spatial shape of the separation zone is not critical and can be adjusted as desired. The key is to form the gas guide unit in the separation zone. The gas guiding unit causes a change in the flow velocity of the gas such that the velocity of the gas in the region of the inlet nozzle is smaller than the velocity of the gas in the region of the separation opening. Since the volume flow rate can be regarded as constant when the aerosol composition is the same, this means that the aerosol is first introduced into a relatively large space, which then narrows, so that the flow velocity increases.

Hereby, the separating zone may for example be circular in cross-section, wherein the cross-section preferably narrows in a wedge shape, for example from the inlet nozzle towards the separating opening.

In a preferred embodiment, the separating zone does not have a circular cross section in the region of the inlet nozzle, wherein the separating zone preferably comprises at least three side walls which together with the upper closure element define a space which communicates with the separating zone via the separating opening. Such an embodiment of the separation zone not comprising a circular cross-section, but comprising an angular cross-section, in particular a triangular, quadrangular, pentagonal or hexagonal cross-section, particularly preferably a rectangular cross-section, is easier to manufacture with the required accuracy, wherein the volume of the gas-liquid separator can be better adapted to the requirements. In particular, a gas-liquid separator suitable for particularly small volume flows can also be provided. Unlike gas-liquid separators having a circular cross-section, gas-liquid separators having a non-circular cross-section (preferably an angular cross-section) may have exactly one inlet nozzle, but without the occurrence of areas of insufficient wetting of the gas-liquid mixture.

Preferably, the following settings are possible: the gas guiding unit has at least two substantially flat side walls, which can be regarded as gas guiding plates, wherein these gas guiding plates preferably form the walls of the separation zone. The two substantially flat side walls may extend towards each other, thereby forming a wedge shape.

Further, the following settings are possible: the gas guiding unit has at least two side walls, wherein at least one of the side walls is curved so as to form a concave shape such that the two side walls can extend towards each other, wherein the distance between the side walls in an upper region of the separation zone, which upper region is formed in the vicinity of the inlet nozzle, is larger than the distance between the side walls in a lower region of the separation zone, which lower region is formed in the vicinity of the separation opening, wherein the decrease in distance decreases from the upper region towards the lower region.

Preferably, the following settings are possible: the gas conducting unit has a gas accelerating unit which, together with at least one side wall, preferably at least two side walls, brings about a change in the gas flow rate.

In another embodiment, the following steps can be provided: the cross section of the gas guiding unit decreases at least locally from the inlet nozzle in the direction of the separation opening, preferably in the region towards the separation opening, so that the plane perpendicular to the flow direction of the gas-liquid mixture becomes smaller, wherein this decrease is preferably continuous, so that preferably at least two of the side walls of the gas guiding unit form a wedge in longitudinal section.

In another embodiment, the following steps can be provided: the separation zone comprises an upper closure, wherein this upper closure comprises a curvature or an angle, wherein the highest point of the curvature or the angle is preferably arranged centrally so as to lie on a line with the inlet nozzle, which line is parallel to the gas flow direction or the liquid flow direction, i.e. to the direction of the gas inlet-liquid outlet-opening, wherein the upper closure preferably transitions into the two side walls such that the transition between the side walls and the upper closure is curved.

In a preferred embodiment, two collision cells are provided in the separation zone, wherein the inlet nozzle directs the gas flow onto the first collision cell as described above. Among these, in a preferred embodiment, the following can be provided: the second collision cell is arranged in the region of the upper closure. Accordingly, the aerosol is preferably guided by the deflector unit from the first collision unit onto a second collision unit arranged in the upper closure.

In a further development of the invention, the following can be provided: the separating zone comprises at least four side walls which together with the upper closing part define a space forming the air guide unit, wherein one of the side walls is formed as a collision unit, wherein this space communicates with the separating zone through the separating opening. In this embodiment, in which the separation zone comprises at least four side walls, which together with the upper closure element define a space, the following can preferably be provided: the distance between the two opposing side walls is greater than half the distance between the inlet nozzle and the collision cell. In this embodiment, in which the separation zone comprises at least four side walls, which together with the upper closure element define a space, the following can preferably be provided: the ratio of the distance between the two opposing side walls to the distance of the inlet nozzle from the collision cell is in the range from 0.8 to 8, particularly preferably in the range from 0.9 to 6, particularly preferably in the range from 1.0 to 4 and particularly preferably in the range from 1.2 to 2. In particular, these values relate to the two opposite side walls having the greatest distance.

In a further development of the invention, the following can be provided: the separation zone comprises at least two side walls, preferably at least three side walls, which together with the upper closing part and the gas acceleration unit define a space forming the gas guide unit, wherein one of said side walls, the gas acceleration unit or the upper closing part forms a collision unit, wherein this space communicates with the separation zone through the separation opening. In this embodiment, in which the separation zone comprises at least two side walls and a gas acceleration unit, said side walls and said gas acceleration unit together with the upper closure member define a space, it is preferably provided that: the distance between the two opposing side walls is greater than half the distance between the inlet nozzle and the collision cell. In this embodiment, in which the separation zone comprises at least two side walls and a gas acceleration unit, said side walls and said gas acceleration unit together with the upper closure member define a space, it is preferably provided that: the ratio of the distance between the two opposing side walls to the distance of the inlet nozzle from the collision cell is in the range from 0.8 to 8, particularly preferably in the range from 0.9 to 6, particularly preferably in the range from 1.0 to 4 and particularly preferably in the range from 1.2 to 2. In particular, these values relate to the two opposite side walls having the greatest distance.

Further, the following settings are possible: the inlet nozzle is arranged in the upper region of the separation zone, particularly preferably in the upper third of the separation zone, wherein this direction results from the arrangement of the inlet and the liquid outlet, whereby the inlet nozzle is arranged above the liquid outlet.

In addition to the separation zone described above, the gas-liquid separator of the present invention has a separation zone. As previously mentioned, the phases are separated in a separation zone, wherein the separation zone has a liquid outlet through which the liquid phase can be extracted from the gas-liquid separator. The gas phase is introduced into the gas lead-out zone. Hereby, the separation zone communicates with the gas lead-out zone through the opening and is in flow contact with the gas lead-out zone.

Preferably, the following settings are possible: the compartment with the liquid outlet comprises a bottom, which preferably comprises a curvature, arc, angle or other shape that creates an end-tapering effect, wherein the liquid outlet is arranged in the deepest region of the bottom.

Further, the following settings are possible: the liquid outlet is provided in the lower region of the separation zone, particularly preferably in the lower third of the separation zone, wherein this direction results from the arrangement of the inlet nozzle and the liquid outlet, whereby the inlet nozzle is arranged above the liquid outlet.

In another embodiment, the following can be provided: the inner surface of the compartment has a surface area with a surface energy in the range of 15mN/m to 120mN/m, particularly preferably in the range of 20mN/m to 80mN/m and particularly preferably in the range of 22mN/m to 60mN/m, wherein preferably at least 80%, particularly preferably at least 90%, of the compartment surfaces have a surface energy in the range of 20mN/m to 80mN/m, particularly preferably in the range of 22mN/m to 60 mN/m. Preferably, the difference between the surface energy of the inner surface of the separation zone and the surface energy of the inner surface of the separation zone may be at least 10mN/m, preferably at least 30mN/m, wherein these values relate to a maximum or a minimum value, whereby the difference is maximal.

Further, the following settings are possible: the separation zone has a cross section in the region of the inlet nozzle which is at least 80%, preferably at least 90%, of the largest cross section of the separation zone, wherein said cross section is related to a plane perpendicular to the collision cell and perpendicular to the main striking point-opening direction of the gas-liquid mixture.

The gas lead-out zone is for discharging the gas phase from the gas-liquid separator, and thus the gas lead-out zone comprises a gas outlet.

The gas outlet region is preferably designed such that the gas velocity at the gas outlet is maximum, preferably the gas velocity increases in the gas flow direction from the separating region towards the gas outlet. Thereby, a suction effect can be produced, so that the gas-liquid separator can be operated stably with low maintenance. Furthermore, the volume of the gas-liquid separator can be reduced without degrading other properties of the gas-liquid separator, such as separation performance.

Thus, in contrast to the separation zone, the space decreases from the separation zone towards the gas outlet. Accordingly, the cross section preferably tapers from the separating region in the direction of the gas outlet.

In a further development of the gas-liquid separator, the following can be provided: the area of an imaginary plane perpendicular to the direction from the separation zone to the gas outlet decreases from the separation zone in the direction of the gas outlet, wherein this decrease is preferably continuous, wherein preferably the gas guiding unit forms a side wall of the gas lead-out zone and in longitudinal section this side of the gas guiding unit forms a wedge with the other side wall of the gas lead-out zone.

Further, the following settings are possible: the gas outlet is provided in the upper region of the gas lead-out zone, particularly preferably in the upper third of the gas lead-out zone, wherein this direction results from the arrangement of the inlet nozzle and the liquid outlet, whereby the inlet nozzle is arranged above the liquid outlet.

Further, the following settings are possible: the inner surface of the gas discharge zone has a surface area with a surface energy in the range of 10mN/m to 40mN/m, wherein preferably at least 80%, particularly preferably at least 90%, of the surface of the gas discharge zone has a surface energy in the range of 10mN/m to 30 mN/m.

Further, the following settings are possible: the separation zone is arranged above the separation zone and the gas lead-out zone is arranged above the separation zone, wherein this direction results from the arrangement of the inlet nozzle and the liquid outlet, whereby the inlet nozzle is arranged above the liquid outlet.

Furthermore, the following can be provided: the separation zone is arranged above the separation zone and the gas lead-out zone is arranged above the separation zone, wherein this direction results from the arrangement of the inlet nozzle and the liquid outlet, whereby the inlet nozzle is arranged above the liquid outlet.

Further, the following settings are possible: the volume ratio of the separating zone to the separating zone is preferably in the range from 4:1 to 1:10, preferably in the range from 2:1 to 1:6 and particularly preferably in the range from 1:1 to 1: 3.

Further, the following settings are possible: the volume ratio of the separating zone to the separating zone is preferably in the range from 6:1 to 1:6, preferably in the range from 4:1 to 1:4 and particularly preferably in the range from 2:1 to 1: 2.

In another embodiment, the following can be provided: the volume ratio of the separation zone to the gas outlet zone is preferably in the range from 10:1 to 1:10, preferably in the range from 5:1 to 1:5 and particularly preferably in the range from 2:1 to 1: 2.

Further, the following settings are possible: the volume ratio of the separating zone to the gas discharge zone is preferably in the range from 10:1 to 1:4, preferably in the range from 6:1 to 1:2 and particularly preferably in the range from 3:1 to 1: 3.

Further, the following settings are possible: the height of the separation zone is preferably in the range from 1cm to 100cm, particularly preferably in the range from 5cm to 20 cm.

Further, the following settings are possible: the width of the separation zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 1.5cm to 10 cm.

Further, the following settings are possible: the depth of the separation zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 1.5cm to 10 cm.

Further, the following settings are possible: the distance of the inlet nozzle from the collision cell is in the range from 3mm to 60mm, particularly preferably in the range from 6mm to 40mm and particularly preferably in the range from 10mm to 25 mm.

Further, the following settings are possible: the height of the separating zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 2cm to 5 cm.

Further, the following settings are possible: the width of the separating zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 1.5cm to 10 cm.

Further, the following settings are possible: the depth of the separating zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 1.5cm to 10 cm.

Further, the following settings are possible: the height of the gas discharge zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 2cm to 5 cm.

Further, the following settings are possible: the width of the gas discharge zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 1.5cm to 10 cm.

Further, the following settings are possible: the depth of the gas discharge zone is preferably in the range from 0.5cm to 20cm, particularly preferably in the range from 1.5cm to 10 cm.

Further, the following settings are possible: the ratio of the height of the separating zone to the height of the separating zone is preferably in the range from 1:2 to 10:1, particularly preferably in the range from 1:1 to 7:1 and particularly preferably in the range from 3:1 to 6: 1.

Further, the following settings are possible: the ratio of the height of the separating zone to the height of the gas discharge zone is in the range from 2:1 to 1:10, particularly preferably in the range from 1:1 to 1:7 and particularly preferably in the range from 1:3 to 1: 6.

Preferably, the direction of flow of the gas in the separation zone of the gas-liquid separator is substantially parallel to the direction of flow of the liquid. In this region, the gas pressure directs the gas-liquid mixture downward. In the separation zone, the direction of flow of the gas is deflected so as to be different from the direction of flow of the liquid. The liquid flows substantially downwards, while the gas flows upwards in the separation zone and the gas outlet zone.

According to the above and the following embodiments, the flow directions of the gas and the liquid are not parallel throughout the separation zone, but mainly in the lower region of the separation zone, preferably in the lower third of the separation zone, wherein this direction results from the arrangement of the inlet and the liquid outlet, whereby the inlet nozzle is arranged above the liquid outlet.

In a further preferred embodiment, the following can be provided: the gas-liquid separator is constructed such that the gas flow velocity is reduced after the separation opening, in particular in the separation zone, by special measures. For this purpose, structures can be provided in the separating zone, such as deflecting plates or deflecting grids, which prevent the gas from encountering the liquid present in the separating zone.

The separation opening is preferably designed such that the gas flow rate is reduced. Further, the following settings are possible: the separation opening has two, three, four or more sub-separation openings, by the arrangement of which the gas flow rate can be reduced. In particular, there may be two, three, four or more sub-separation openings in an arrangement that reduces the gas flow rate. Preferably, the gas flow rate in the horizontal direction is reduced by at least 5%, particularly preferably by at least 15% and particularly preferably by at least 30%, wherein these numbers relate to the initial value of the flow rate. The above-mentioned values can be determined, for example, by means of corresponding flow tests, wherein these values can also be obtained by means of simulation calculations. These values are preferably obtained by measuring the degree of reduction of the amount of liquid carried by the gas.

Preferably, the sub-separation openings are arranged substantially symmetrically in order to attenuate the air flow in the horizontal direction. If there are 2, 4, 6 or more sub-openings, these are correspondingly arranged oppositely, or in case there are 3, 5 sub-openings, the sub-openings are arranged in a triangle or pentagon, so that the gas passing through the separation openings flows in horizontal direction towards each other, thereby reducing the gas flow rate.

The sub-separation openings are here preferably arranged symmetrically, wherein the axis of symmetry or plane of symmetry is parallel to the flow direction of the gas and liquid in the separation zone. There is one point or mirror symmetry depending on the number of sub-split openings. The term "substantially symmetrical" means: effectively impairing the gas flow rate in the separation zone. This symmetry is preferably defined by the geometry of the sub-separation openings and/or the geometry of the air guide unit. In the case of two sub-separation openings, the area ratio of the sub-separation openings is preferably in the range from 2:1 to 1:2, particularly preferably in the range from 1.5:1 to 1:1.5, particularly preferably in the range from 1.2:1 to 1: 1.2. If three or more sub-separation openings are present, these values apply correspondingly to different pairs of sub-separation openings, so that the ratio of the area of the largest sub-separation opening to the area of the smallest sub-separation opening is preferably at most 2:1, preferably at most 1.5:1 and particularly preferably at most 1.2: 1.

Here, the gas-liquid separator may have one, two or more separation zones each having an inlet nozzle, a collision unit and an air guide unit. In a preferred embodiment, the following settings are possible: the gas-liquid separator comprises exactly one inlet nozzle with a collision cell and the gas guiding cell is divided into two, three or more zones each comprising a (sub-) separation opening. In another embodiment, the following steps can be provided: the gas-liquid separator comprises several separate separation zones each having exactly one inlet nozzle comprising a collision cell, wherein the separation openings of the different (sub-) separation zones communicate with exactly one separation zone. In a further preferred embodiment, the following can be provided: the gas-liquid separator comprises two or more inlet nozzles with collision cells, which inlet nozzles, as mentioned before, are designed such that the gas-liquid streams directed by the two or more inlet nozzles are aligned with each other, and the gas-directing cell is divided into two, three or more regions each comprising a (sub-) separation opening. In this way, the gas flows guided by different (sub-) separation openings are guided into the same compartment and the flow rates of the gases decrease with respect to each other.

The gas-liquid separator is preferably constructed such that the gas flow velocity in the separation zone is minimized in order to prevent liquid present in the lower region of the separation zone from being entrained or absorbed. In preferred embodiments in which two, three, four or more sub-separation openings are provided, these sub-separation openings are preferably of correspondingly symmetrical design. Thus, in a preferred embodiment having two separation openings, the separation openings are preferably substantially equally large and arranged opposite to each other, so as to minimize the gas flow. The meaning of "substantially" is preferably: the gas flow rate ratio is preferably in the range from 2:1 to 1:2, in particular in the range from 1.5:1 to 1:1.5, particularly preferably in the range from 1.2:1 to 1: 1.2. If three or more sub-separation openings are present, these values are correspondingly adapted to the different pairs of sub-separation openings, so that the ratio of the gas flow rate of the largest sub-separation opening to the gas flow rate of the smallest sub-separation opening is preferably at most 2:1, preferably at most 1.5:1 and particularly preferably at most 1.2: 1.

In particular, the gas flow rate may be calculated from the discharge area of the sub-separation openings, taking into account the geometry of the gas guiding unit. The gas flow rate of the separation openings can be determined by the flow rate at which chromatography is carried out, wherein the discharge area of the separation openings has to be taken into account.

In embodiments having two or more sub-separation openings, which can be considered as separation openings as a whole, the above and below dimensional data, for example with respect to area, length, width, etc., apply accordingly, wherein the term "separation opening" can be understood as a totality of sub-separation openings.

A particularly preferred embodiment has exactly one or two separating zones comprising an inlet nozzle, a collision cell and an air guide cell, wherein exactly two (sub-) separating openings are provided. This solution can be produced particularly simply by machining, preferably by milling from a block of material, preferably made of plastic. The side walls are preferably formed by cover plates which are connected to the milled material block by means of pressure, for example by screwing. By simply removing the screws and the cover plate, the gas-liquid separator can be reliably cleaned.

In a preferred embodiment, a deflector element, preferably a gap, is provided in the separation zone, wherein the inlet nozzle directs the gas flow onto the first collision element, wherein in this embodiment, as previously described, the gas flow velocity in the separation zone is preferably further minimized in order to prevent liquid present in the lower region of the separation zone from being entrained or absorbed. Among these, in a particularly preferred embodiment, the following can be provided: the second collision cell is arranged in the region of the upper closure part such that the deflection cell directs the air flow onto the region in the upper closure part. Particularly preferably, the second crash unit is designed as an intrados. The shape of the intrados is irrelevant here.

In this particularly preferred embodiment, in which the second crash unit is designed as an intrados, the following can be provided: the separation zone comprises an upper closure, wherein this upper closure comprises more than one curvature or angle, whereby a deeper point is provided between two higher points in the upper region, wherein the deeper point of curvature or angle is preferably centrally arranged so as to lie on a line with the inlet nozzle, which line is parallel to the gas flow direction or the liquid flow direction, i.e. from top to bottom can be imagined, wherein the upper closure preferably transitions into the two side walls such that the transition between the side walls and the upper closure is at least doubly curved.

The configuration of the intrados or the design of the embodiment in which more than one curvature or angle is provided in the upper closure is not particularly limited and can be adapted accordingly according to other technical solutions. For example, the following settings may be provided: the height of the intrados is preferably in the range from 1mm to 30mm, particularly preferably in the range from 2mm to 15mm and particularly preferably in the range from 3mm to 10 mm. The height of the intrados refers to the distance between the highest point of the upper closure and the deepest point of the upper closure between the side walls.

Further, the following settings are possible: the distance between the outlet opening of the deflector unit (preferably the recess) and the closest point of the intrados (to which the deflector unit preferably directs the gas flow) is preferably in the range from 0.8mm to 25mm, particularly preferably in the range from 1.5mm to 20mm and particularly preferably in the range from 2mm to 10 mm.

The embodiments described above and below with two or more sub-separation openings are particularly preferred over other solutions, wherein the surprising finding is that: the amount of liquid carried by the gas can thereby be kept very small. This improvement is particularly suitable in the case of large differences in the liquid composition of the solvent mixture used for chromatography. This embodiment is therefore particularly suitable for performing gradient chromatography, as described in detail above and below, in which the composition of the solvent in liquid form at room temperature and pressure and the composition of the fluid in gaseous form at room temperature and pressure are subject to drastic changes.

The aforementioned preferred properties of the gas-liquid separator require the definition of different regions which are in flow contact with each other, since the mixture consisting of gas and liquid phases is conducted through the separation zone into a separation zone, in which the liquid is separated from the gas phase and the gas is transferred into the gas lead-out zone. The separating opening separates the separating zone from the separating zone, wherein the plane in which the ends of the separating opening lie defines the transition to the separating zone.

The transition between the separating zone and the gas discharge zone is likewise delimited by an opening, which is however comparatively large compared to the separating opening. This opening is defined by the following plane: the plane is arranged at the level of the separation opening and extends perpendicular to the direction of the gas flow direction of the gas-liquid mixture in the separation zone, or parallel to the flow direction of the gas phase as soon as the gas phase passes from the separation zone over the separation opening into the separation zone or is parallel to the liquid level during operation. The plane defined by the expansion of the opening is selected such that it forms the smallest area between the separating zone and the gas discharge zone, wherein this plane touches the separating opening and runs substantially parallel to the bottom of the separating zone or, in operation, to the liquid level.

Further, the following settings are possible: the ratio of the entry area of the inlet arranged in the separation zone to the distance of the inlet from the collision cellAt 5:1mm ²From mm to 1:10mm ²In the range of/mm, preferably 2:1mm ²From mm to 1:5mm ²/mm。

The gas-liquid separator of the present invention may be made of any known material as long as it satisfies the requirements in terms of solvent and physical conditions. It is preferable to use a transparent material through which the separation process can be seen so that failure analysis can be performed promptly when a coating is formed or the like occurs.

The gas-liquid separator may be made of metal, mineral glass, preferably designed to be acid and base resistant, and/or plastic, preferably solvent resistant, such as fluoropolymer, Polyetheretherketone (PEEK) or similar materials.

The gas-liquid separator preferably has a volume in the range from 20ml to 100ml, particularly preferably in the range from 20ml to 70ml, particularly preferably in the range from 20ml to 50 ml. In the case of a substantially cuboidal shape, which can be designed as an arc or dome, for example, in the upper and/or lower region of the gas-liquid separator bounded by the inlet nozzle and the liquid outlet, the height of the gas-liquid separator is preferably in the range from 8cm to 150cm, particularly preferably in the range from 10cm to 12cm, wherein the height is defined by the linear expansion in the gas flow direction (i.e. from the inlet nozzle to the liquid outlet). The width and depth of the gas-liquid separator are preferably in the range of 15mm to 60mm, particularly preferably in the range of 15mm to 25mm, respectively.

Preferably, the following settings are possible: the gas-liquid separator is not cylindrical and preferably has a substantially cuboidal basic structure with an arcuate upper cover portion and an arcuate lower cover portion.

The gas-liquid separator of the present invention may be constructed and manufactured in any manner. According to a preferred embodiment, the gas-liquid separator may be designed to be detachable, i.e. to be assembled and disassembled in a single piece. This allows the gas-liquid separator to be easily cleaned when it is soiled. For example, a substantially cuboidal base body can be produced with suitable recesses, to which cover parts are attached in a screwed manner as side walls. As mentioned before, the side walls serving as cover part may assume the function of the collision cell and/or be part of the air guiding cell. In this embodiment, a further section of the side wall of the gas conducting unit, which preferably further forms the gas discharge zone, can be fixed by form fit, welding (preferably laser welding), adhesive bonding or the like into a substantially cuboidal base body with suitable recesses, so that the above-described regions, in particular the at least one separating zone, the at least one separating zone and the at least one gas discharge zone, are produced. The gas-liquid separator is preferably manufactured by machining, preferably by milling from a block of material, preferably consisting of plastic. The side walls are preferably formed by cover plates which are connected to the milled material block by means of pressure, for example by screwing. As described hereinbefore and hereinafter, the gas-liquid separator can be reliably cleaned by simply removing the screws and the cover plate.

Generally, the gas-liquid separator may operate at atmospheric pressure. However, in order to avoid the accumulation of relatively large amounts of liquid (e.g. methanol), the gas-liquid separator can be operated with a back-pressure regulator at moderate internal counter-pressures, e.g. in the range of 0.1bar to 4 bar. Hereby the following settings can be set: the chromatography apparatus is provided with a back pressure regulator after the gas outlet, which is preferably adjustable in the range of 1bar to 4bar overpressure (2 bar to 5bar absolute), preferably 2bar to 3bar overpressure. However, the liquid component collected via the separating zone and supplied via the liquid discharge channel enables an automated fractionation operable at atmospheric pressure. Full automatic fraction collection can also be achieved for SFC analysis by means of a gas-liquid separator and in a comparable manner by means of a conventional HPLC apparatus.

Since the separation zone of the gas-liquid separator and the inner walls and components in the separation zone are wetted substantially continuously, not only is a self-cleaning effect achieved, but a lower degree of cross-contamination of the sample is also achieved. Another advantage is that the gas-liquid separator causes relatively little peak broadening in the synthetic chromatogram.

According to another aspect, the present invention also provides a conversion kit capable of converting a High Performance Liquid Chromatography (HPLC) system to an SFC system. Such a kit comprises at least one gas-liquid separator as described above. The kit preferably contains other components, such as a heat exchanger or a back pressure regulator, as described below, to convert the HPLC apparatus into an SFC system.

The gas-liquid separator is mainly applied in chromatographic apparatuses designed for supercritical liquid chromatography.

Such a system is for example used in combination with supercritical CO ₂And a solvent (e.g., methanol). Accordingly, a chromatography apparatus designed for supercritical liquid chromatography has at least one storage vessel for a solvent and at least one storage vessel for a supercritical fluid (e.g., CO) ₂) The storage container of (1). Generally, fluid is withdrawn from a reservoir and transferred by at least one pump into a mixing element in flow communication with a chromatography column. The pump and/or the mixing element and the chromatography column can be provided with a temperature control device in order to be able to establish the predetermined temperature. For this purpose, in particular, a heat exchanger can be provided. The addition of the mixture to be separated, in particular of the substance to be purified, can be carried out by known means, such as injectors, which are preferably arranged in a conduit for introducing the solvent to the mixing element.

The fluid leaving the chromatography column is preferably at least partially provided to a detection or analysis unit. For example, the detection or analysis unit includes, but is not limited to, a UV detector and/or a mass spectrometer.

A back pressure regulator and preferably a heat exchanger are generally provided after the chromatography column and preferably after the detection or analysis unit. The aerosol leaving the heat exchanger is preferably subsequently supplied to the gas-liquid separator of the present invention.

Depending on the type of gas, the gas phase of the aerosol can be captured and treated, or for example in the use of CO ₂In this case, it may be released into the surrounding environment.

The liquid phase of the aerosol is preferably collected in a fraction collector. The collected fraction is particularly preferably automatically collected as the main fraction, the excess solvent then being disposed of or disposed of. The connecting line between the liquid outlet of the gas-liquid separator and the fraction collector may preferably be designed such that the residue of the gas phase (preferably CO) ₂Residue) can escape through this connection. For this purpose, semipermeable plastics can be usedMaterials such as polytetrafluoroethylene, AF 2400 (commercially available from DuPont) is particularly preferred.

The SFC chromatography system can preferably be operated at a volume flow in the range from 10ml/min to 450ml/min, particularly preferably in the range from 50ml/min to 300ml/min and particularly preferably in the range from 100ml/min to 250 ml/min. Further, the following settings are possible: the SFC chromatography system can preferably be operated at a volume flow of at least 10ml/min, particularly preferably at least 50ml/min and particularly preferably at least 100 ml/min.

Another subject of the invention is a method for separating a gas-liquid mixture using a gas-liquid separator according to the invention or a chromatography apparatus having a gas-liquid separator according to the invention.

When separation is performed using a supercritical fluid, it is preferable to use a gas that can be relatively easily converted into a supercritical state. Preferred gases having these characteristics include, but are not limited to, carbon dioxide (CO) ₂) Ammonia (NH3), freon, xenon, among which carbon dioxide (CO) ₂) Is particularly preferred.

Further, the following settings are possible: the process of the invention uses inorganic or organic solvents which are liquid under conventional separation conditions, in particular at 25 ℃ and atmospheric pressure (1023 mbar). Among them, depending on the type of compound to be isolated or purified, polar or non-polar solvents may be used.

Preferably, the following settings are possible: the gas-liquid mixture to be converted into the supercritical state comprises a polar solvent and a gas selected from CO ₂NH3, freon, xenon, preferably CO ₂. The polar solvent is preferably an alcohol, preferably methanol, ethanol or propanol, hexane, a mixture comprising dichloromethane, chloroform, water (preferably up to 3 vol%, otherwise miscibility gaps occur), an aldehyde or a ketone, preferably methyl ethyl ketone; esters, preferably ethyl acetate; or an ether, preferably tetrahydrofuran.

In the case of using a polar solvent, it is preferable to set as follows: the collision cell has a surface area with a surface energy in the range of 35 to 100mN/m, particularly preferably in the range of 50 to 80 mN/m.

Further, the following settings are possible: the gas-liquid mixture to be converted into the supercritical state comprises a nonpolar solvent and a gas selected from the group consisting of CO ₂NH3, freon, xenon, preferably CO ₂. The non-polar solvent is preferably an aliphatic hydrocarbon, preferably hexane, cyclohexane, heptane, octane; aromatic hydrocarbons, preferably benzene, toluene, xylene; esters, preferably ethyl acetate; or an ether, preferably tetrahydrofuran.

In the case of using a nonpolar solvent, it is preferable to set: the collision cell has a surface area with a surface energy in the range of 10 to 40mN/m, particularly preferably in the range of 15 to 30 mN/m.

In a preferred embodiment of the method, the chromatography apparatus comprises a back pressure regulator which can be used to regulate the pressure in the gas-liquid separator, wherein the following can be provided: the pressure regulation is selected according to the solvent content of the gas-liquid mixture, which regulation can preferably be designed such that: when the solvent content is higher, a higher pressure is set in the gas-liquid separator.

Drawings

The preferred embodiments of the present invention will be described below by way of example with reference to the four drawings, but the present invention is not limited thereto. Wherein:

FIG. 1 is a schematic longitudinal sectional view of a gas-liquid separator of the present invention,

FIG. 2 is a schematic cross-sectional view of a gas-liquid separator of the present invention,

figure 3 is a schematic top view of a gas-liquid separator of the present invention,

FIG. 4 is a schematic longitudinal sectional view of another embodiment of the gas-liquid separator of the present invention,

FIG. 5 is a schematic longitudinal sectional view of another embodiment of the gas-liquid separator of the present invention,

FIG. 6 is a schematic longitudinal sectional view of another embodiment of the gas-liquid separator of the present invention,

FIG. 7 is a schematic longitudinal sectional view of another embodiment of the gas-liquid separator of the present invention,

fig. 8 is a schematic longitudinal sectional view of the embodiment of the gas-liquid separator of the present invention shown in fig. 7, wherein the sectional plane is rotated by 90 deg. with respect to the sectional plane shown in fig. 7,

FIG. 9 is a schematic longitudinal sectional view of another embodiment of the gas-liquid separator of the present invention,

FIG. 10 is a schematic of a chromatography system having a gas-liquid separator of the present invention.

Detailed Description

Fig. 1 depicts a gas-liquid separator 10 of the present invention in longitudinal cross-section.

Gas-liquid separator 10 includes a separation zone 12 having an inlet nozzle 14, a collision cell 16, and an air guide cell 18. The gas conducting unit 18 is formed by the collision cell 16, which is here formed as a baffle, of the gas accelerating plate 20 and the other two side walls, which are not shown in longitudinal section. The figure shows in particular the here wedge-shaped form of the separation zone 12, which causes the gas to be accelerated from the region of the inlet nozzle 14 towards the separation opening 22.

The crash unit 16, which is formed here as a baffle, can have a structured surface or a smooth surface. The gas acceleration plate 20 can be flat or slightly concave from the direction of the inlet nozzle 14 toward the separation opening 22, so that the distance between the baffle 16 and the gas acceleration plate 20, which is visible here, decreases less. Separation region 12 is upwardly bounded by upper closure member 24.

Gas-liquid separator 10 includes a separation region 26 having a liquid outlet 28, wherein separation region 26 communicates with separation region 12 through separation opening 22 such that separation region 12 is in flow contact with separation region 26.

The crash unit 16 formed as a baffle here forms the side wall of the separating zone 26. The bottom of the gas-liquid separator 10 is formed by the lower closure of the separation zone 26. This bottom may be designed such that the liquid outlet 28 is arranged at the deepest part of the bottom.

The side wall 32 of the gas discharge region 30 and the two side walls not shown in longitudinal section form the further boundary of the separating region together with the opening 34 provided between the gas discharge region 30 and the separating region 26 and the separating opening 22.

In the separating zone 26, the gas phase is separated from the liquid phase, wherein the gas is preferably accelerated by the gas conducting unit 18 in the direction of the separating opening 22, so that the liquid is diverted in the direction of the bottom of the separating zone 26.

The gas phase is introduced into the gas outlet region 30 through an opening 34 provided between the gas outlet region 30 and the separating region 26. The gas discharge area 30 is designed here such that the gas is accelerated in the direction of a gas outlet 35 arranged in the gas discharge area 30.

The rear wall of the gas acceleration plate 20 forms a corresponding wedge shape together with the side wall 32 projecting into the separating region, wherein an edge of the gas acceleration plate 20 is connected to the side wall 32.

FIG. 2 shows a schematic cross-sectional view of the gas-liquid separator 10 of the present invention wherein like reference numerals describe like components.

The side walls 36, 38 of the gas-liquid separator 10, which are not shown above, are particularly shown. Furthermore, a supply line 40 for aerosol and a discharge line 42 for gas are shown.

It can further be seen that in this embodiment the collision cell 16 formed as a baffle has a grooved surface structure.

FIG. 3 shows a schematic top view of the gas-liquid separator 10 of the present invention wherein like reference numerals describe like components. The figures show in particular the preferred design of the lower closure 44 of the separating zone 26 and of the upper closure 24 of the separating zone 12, which are each designed in the form of an arc here.

Fig. 4 depicts the gas-liquid separator 50 of the present invention in longitudinal section.

The gas-liquid separator 50 includes a separation region 52 having an inlet nozzle 54, a collision cell 56, and an air guide cell 58. The gas conducting unit 58 is formed by a gas accelerating unit 60, two side walls 62a, 62b and another bottom and top wall, not shown in longitudinal section. The drawing shows in particular the here wedge-shaped form of the separating zone 52, which causes the gas to be accelerated from the region of the inlet nozzle 54 towards the separating opening 64.

In the present embodiment, the separation zone 52 is divided into two sub-zones 52a, 52b, which communicate with the separation zone 66 through respective sub-separation openings 64a and 64 b.

In the present exemplary embodiment, the collision cell 56 is formed in the region of the gas acceleration cell 60, which connects the two partial regions 60a, 60b of the gas acceleration cell 60 in an arc-shaped manner at this point and partially separates the partial regions 52a, 52b of the separation region 52. The inlet nozzle 54 directs the gas-liquid mixture onto the collision cell 56. Thereby creating a gas stream that is parallel to the direction of flow of the liquid in separation region 52. The gas acceleration unit 60 has two partial regions 60a, 60b, which, in the direction of the separating opening 64 from the inlet nozzle 54, cause a reduction in the distance between the gas acceleration unit 60 and the side walls 62a, 62b, wherein the partial regions 60a, 60b of the gas acceleration unit 60 can be flat or slightly concave. Separation region 52 is upwardly bounded by upper closure 68.

The gas-liquid separator 50 includes a separation region 66 having a liquid outlet 70, wherein the separation region 66 communicates with the separation region 52 through the separation opening 64 or two sub-separation openings 64a and 64b such that the two sub-regions 52a, 52b of the separation region 52 are in flow contact with the separation region 66.

The bottom of the gas-liquid separator 50 is formed by the lower closure of the separation zone 66. This bottom may be designed such that the liquid outlet 70 is arranged at the deepest part of the bottom.

The gas discharge area 72 is formed by the gas acceleration unit 60 and two walls, not shown in longitudinal section, together with an opening 74 provided between the gas discharge area 72 and the separating area 66.

In the separating zone 66, the gas phase is separated from the liquid phase, wherein the gas is preferably accelerated by the gas conducting unit 58 in the direction of the separating opening 64, so that the liquid is diverted in the direction of the bottom of the separating zone 66. In the present embodiment, the two sub-flows introduced into the separation zone 66 through the sub-separation openings 64a, 64b are directed towards each other such that the velocities of the sub-flows are minimized in the separation zone. The amount of liquid entrained in the gas stream can be greatly reduced by this design.

The gas phase is introduced into the gas discharge zone 72 through an opening 74 provided between the gas discharge zone 72 and the separation zone 66. The gas discharge area 72 is designed here such that the gas is accelerated in the direction of a gas outlet 76 arranged in the gas discharge area 72.

The rear side of the aforementioned gas acceleration unit 60 is formed here in a corresponding shape that narrows upwards.

The embodiment shown in fig. 4 can be milled very simply from a plastic block. By retaining material, a back wall not shown in fig. 4 can be produced, wherein by a corresponding milling depth or material removal depth, the volume of the above-mentioned region or sub-region can be obtained. The upper side can be provided by a plate, for example a glass plate, which presses the milled plastic block from above. The compression may be achieved, for example, by screwing. The corresponding holes are designated herein by reference numeral 78. The plate forming the upper side is preferably fastened by means of a recess, which can be regarded as a groove, arranged in a stepped manner along the region and the sub-region. This stepped gap is designated herein by reference numeral 79.

Fig. 5 depicts the gas-liquid separator 80 of the present invention in longitudinal cross-section. The gas-liquid separator 80 shown in fig. 5 is equivalent in structural design to the gas-liquid separator 50 shown in fig. 4, wherein the same or similar components have the same reference numerals. The gas-liquid separator 80 includes a separation region 52 having an inlet nozzle 54, a collision cell 56, and an air guide cell 82. The gas guide unit 82 is formed by a gas acceleration unit 84, two side walls 62a, 62b, and another bottom wall and a top wall, which are not shown in longitudinal section.

Specifically, the main differences are: the gas acceleration cell 84 is sharply divided into two sub-regions 84a and 84b, whereas the gas acceleration cell 60 of the embodiment shown in fig. 4 is curved in the collision region. The nozzle is guided here onto an impact region 56, which can be formed relatively flat, so that the connection point of the two partial regions 84a and 84b is flattened.

Fig. 6 depicts in longitudinal section a gas-liquid separator 90 according to the invention. The gas-liquid separator 90 shown in fig. 6 is equivalent in structural design to the gas-liquid separator 80 shown in fig. 5, wherein the same or similar components have the same reference numerals. The gas-liquid separator 90 includes a separation region 52 having two inlet nozzles 94a, 94b, a collision cell 56, and an air guide cell 82.

Specifically, the main differences are: the two inlet nozzles 94a, 94b direct the aerosol from both sides onto the air guide unit 82 or onto the two sub-regions 82a, 82b of the air guide unit 82. It will be clear to the person skilled in the art that the closure 68 with the air guide unit 82 facing upwards can be divided by a dividing wall into two separate zones which are actually separated, without the flow in the region of the separating zones changing significantly.

Fig. 7 depicts the gas-liquid separator 100 of the present invention in longitudinal cross-section. The gas-liquid separator 100 shown in fig. 7 is equivalent in structural design to the gas-liquid separator 50 shown in fig. 4, wherein the same or similar components have the same reference numerals. The gas-liquid separator 100 includes a separation zone 52 having an inlet nozzle 102 and an air guide unit 58. In the present embodiment, the collision cell is formed by a ceiling wall not shown in fig. 7.

Specifically, the main differences are: the collision cell is formed by a ceiling wall, not shown in the figure, onto which the gas is first directed after entering the gas-liquid separator 100 through the inlet nozzle 102. The deflection unit 104 directs the air flow onto an upper closure member 106, which in this embodiment has an intrados 108. The deflector element 104 is formed here by a recess in the gas acceleration element 110, which connects the two partial regions 110a, 110b of the gas acceleration element 110 in an arc-shaped manner at this point and partially separates the partial regions 52a, 52b of the separating region 52.

Accordingly, the upper enclosure 106, in particular the region of the intrados 108, may be considered as a second collision cell, as a portion of the aerosol may undergo further collision separation. The intrados 108 help to stabilize the gas flow so that the aerosol flow or gas flow is directed directionally into the two sub-regions 52a, 52b of the gas guide unit.

Fig. 8 shows the gas-liquid separator 100 depicted in fig. 7 in a longitudinal view, wherein the sectional plane depicted is perpendicular to the view presented in fig. 7. The plane shown in the figure shows the tip of the intrados 108 and a cross-section of the liquid outlet 70. Top wall 112 and bottom wall 114 are particularly shown. The line 116 represents the bottom area of the deflector element 104 and the line 118 represents the tip of the intrados 108. The dashed lines 120, 122 indicate material grooves forming the deflection unit 104, and the dashed line 124 indicates the upper region of the gas discharge area 72, in which the gas is guided together and transferred into the gas outlet 76.

Fig. 9 depicts the gas-liquid separator 130 of the present invention in longitudinal cross-section. The gas-liquid separator 130 shown in fig. 9 is equivalent in structural design to the gas-liquid separator 50 shown in fig. 4, wherein the same or similar components have the same reference numerals. The gas-liquid separator 130 includes a separation region 52 having two inlet nozzles 134a, 134b, two collision units 136a, 136b, and an air guide unit 52.

Specifically, the main differences are: the two inlet nozzles 134a, 134b direct the aerosol onto opposite sides of the side walls 62a, 62b, which are formed at the respective locations as collision cells 136a, 136b, wherein the jet of the inlet nozzle 134a is directed at the collision cell 136a, which can be considered as part of the side wall 62 b. Here, the two inlet nozzles 134a, 134b can be slightly displaced in the horizontal direction or in the vertical direction.

As previously described with reference to fig. 4, the embodiment shown in fig. 5 to 9 can likewise be milled out of a plastic block, wherein the upper side can be provided by a plate (e.g. a glass plate) which presses the milled-out plastic block from above. Furthermore, all embodiments may accordingly be provided by casting or the like.

Fig. 10 schematically shows a chromatography system 200 with a gas-liquid separator 230 of the invention, which is suitable for supercritical liquid chromatography.

Such a system is described below using supercritical CO2 as an example, with methanol as an exemplary solvent. Of course, systems using other solvents (preferably organic solvents) or other supercritical fluids have similar structures.

As shown in fig. 10, each fluid is provided in a storage vessel, specifically, a gas is provided in a storage tank 202 that is continuously used in a supercritical state, a solvent is provided in a storage tank 204, and the gas and the solvent can be delivered from the storage tanks 202, 204 to other components of the apparatus by pumps 206, 208, respectively. In the system 200 described herein, a preliminary stage 210, 212, which may be liquid tempering, is preferably provided in each fluid supply conduit. In addition, a smoothing of the pressure fluctuations indicated by the pump can be provided. Accordingly, this preliminary stage may be formed as a heat exchanger or a pump, for example. An addition unit 214, for example an ejector, may preferably be provided in the solvent line, through which the mixture to be separated is introduced into the system 200 before the CO2 and solvent are introduced into the mixer 216 and provided by the mixer to the chromatography column 218.

In the present system 200, two analysis units are connected downstream of the chromatography column 218, for which purpose a sample lead-out unit 220 is connected to a mass spectrometer 222 and, after the sample lead-out unit, a UV detector 224 is provided. A back pressure regulator 226 disposed in the tubing maintains the pressure required to maintain the fluid in a supercritical state. A heat exchanger 228 is provided after the back pressure regulator 226 to prevent the aerosol from freezing during pressure reduction. Next, the aerosol is directed into the gas-liquid separator 230 of the present invention, wherein the gas is discharged out of the device through outlet 232.

The liquid is directed into a fraction collector 234 and fractionated therein. The solvent contained in these samples may be removed from the fractionated samples.

The features of the invention disclosed in the above description and in the claims, the drawing and the examples can be used both individually and in any combination to realize various embodiments of the invention.