Vaccum Degassing Using Electroactive Material
20220168670 · 2022-06-02
Inventors
Cpc classification
B01D71/70
PERFORMING OPERATIONS; TRANSPORTING
B01D69/02
PERFORMING OPERATIONS; TRANSPORTING
B01D2259/816
PERFORMING OPERATIONS; TRANSPORTING
B01D2313/903
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
A degasser for at least partially degassing a gas-containing liquid, in particular for a sample separation device, includes a liquid accommodation volume for accommodating the gas-containing liquid during degassing, a negative pressure chamber in which a negative pressure, compared to the liquid accommodation volume, is to be generated, a gas permeable membrane separating the liquid accommodation volume from the negative pressure chamber and arranged so that ultrasound forces at least part of gas of the gas-containing liquid to move through the membrane by a combination of the negative pressure and the ultrasound, and an ultrasound source including an electroactive material and configured for generating ultrasound for actuating the gas-containing liquid and/or the gas permeable membrane.
Claims
1. A degasser for at least partially degassing a gas-containing liquid, the degasser comprising: a liquid accommodation volume for accommodating the gas-containing liquid during degassing; a negative pressure chamber in which a negative pressure, compared to the liquid accommodation volume, is to be generated; a gas permeable membrane separating the liquid accommodation volume from the negative pressure chamber and arranged so that ultrasound forces at least part of gas of the gas-containing liquid to move through the membrane by a combination of the negative pressure and the ultrasound; and an ultrasound source comprising an electroactive material and being configured for generating ultrasound for actuating the gas-containing liquid and/or the gas permeable membrane.
2. The degasser according to claim 1, wherein the ultrasound source is integrally formed with the gas permeable membrane.
3. The degasser according to claim 2, wherein the ultrasound source and the gas permeable membrane are formed as a stack.
4. The degasser according to claim 3, wherein the stack comprises a porous spacer layer between the gas permeable membrane and the ultrasound source.
5. The degasser according to claim 2, wherein the ultrasound source and the gas permeable membrane are formed as a patterned ultrasonic source sheet having one or more through holes filled at least partially with one connected or multiple separate sections of gas permeable material.
6. The degasser according to claim 2, comprising a sealing structure sealing the ultrasound source with regard to the gas permeable membrane.
7. The degasser according to claim 1, wherein the ultrasound source and the gas permeable membrane are formed as separate members.
8. The degasser according to claim 7, wherein the ultrasound source is arranged in a wall which delimits at least part of the negative pressure chamber.
9. The degasser according to claim 1, comprising a negative pressure source configured for generating the negative pressure in the negative pressure chamber.
10. The degasser according to claim 9, wherein the negative pressure source is integrally formed with the ultrasound source in a wall which delimits at least part of the negative pressure chamber.
11. The degasser according to claim 1, comprising a pressure sensor for sensing a pressure in the negative pressure chamber.
12. The degasser according to claim 11, wherein the pressure sensor is integrally formed with at least one of the ultrasound source or the gas permeable membrane.
13. The degasser according to claim 1, wherein the ultrasound source comprises electrodes between which the electroactive material is arranged and to which an electric signal is applicable for exciting the electroactive material.
14. The degasser according to claim 1, wherein the liquid accommodation volume comprises at least one liquid channel through which the gas-containing liquid is drivable during degassing.
15. The degasser according to claim 1, comprising at least one of the following features: wherein at least one of the electroactive material or the gas permeable membrane comprises a silicone; wherein at least one of the electroactive material or the gas permeable membrane comprises a fluorosilicone; wherein the gas permeable membrane comprises a supporting grid; comprising a support structure on which the gas permeable membrane is mounted and being configured for maintaining at least a predefined minimum volume of the liquid accommodation volume; wherein the electroactive material is configured to act as a sensor and an actuator simultaneously.
16. A degasser for at least partially degassing a gas-containing liquid, the degasser comprising: a liquid accommodation volume for accommodating the gas-containing liquid during degassing; a negative pressure chamber in which a negative pressure, compared to the liquid accommodation volume, is to be generated; and a gas permeable membrane separating the liquid accommodation volume from the negative pressure chamber so that at least part of gas of the gas-containing liquid is to move through the membrane by the negative pressure, wherein the gas permeable membrane comprises a silicone.
17. The degasser according to claim 16, comprising at least one of the following features: wherein the gas permeable membrane comprises a fluorosilicone; wherein the gas permeable membrane has a thickness in a range from 1 μm to 1 mm; wherein the gas permeable membrane has a thickness in a range from 10 μm to 100 μm; configured so that the gas-containing liquid and/or the gas permeable membrane is or are to be actuated by ultrasound to force at least part of gas of the gas-containing liquid to move through the membrane by a combination of the negative pressure and the ultrasound, and wherein the degasser further comprises an ultrasound source configured for generating ultrasound for actuating the gas-containing liquid and/or the gas permeable membrane.
18. A sample separation device for separating a fluidic sample, the sample separation device comprising: a pump for driving a mobile phase and the fluidic sample when injected in the mobile phase; a sample separation unit for separating the fluidic sample in the mobile phase; and a degasser according to claim 1 for at least partially degassing a gas-containing liquid, wherein the at least partially degassed gas-containing liquid is supplied for creation of the mobile phase.
19. The sample separation device according to claim 18, further comprising at least one of the following features: the sample separation device is configured as a chromatography sample separation device; the sample separation device comprises a detector configured to detect the separated fluidic sample; the sample separation device comprises a fractioner unit configured to collect separated fractions of the fluidic sample; the sample separation device comprises an injector configured to inject the fluidic sample in the mobile phase.
20. A method of at least partially degassing a gas-containing liquid, the method comprising: accommodating the gas-containing liquid in a liquid accommodation volume for degassing; generating a negative pressure, compared to the liquid accommodation volume, in a negative pressure chamber; and actuating the gas-containing liquid and/or a gas permeable membrane, which separates the liquid accommodation volume from the negative pressure chamber, by ultrasound generated by an ultrasound source comprising an electroactive material to thereby force at least part of gas of the gas-containing liquid to move through the membrane by a combination of the negative pressure and the ultrasound.
Description
BRIEF DESCRIPTION OF DRAWINGS
[0051] Other objects and many of the attendant advantages of embodiments of the present invention will be readily appreciated and become better understood by reference to the following more detailed description of embodiments in connection with the accompanying drawings. Features that are substantially or functionally equal or similar will be referred to by the same reference signs.
[0052]
[0053]
[0054]
[0055]
[0056]
[0057]
[0058]
[0059]
[0060] The illustration in the drawings are schematic.
DETAILED DESCRIPTION
[0061] Before describing the figures in further detail, some basic considerations of the present invention will be summarized based on which exemplary embodiments have been developed.
[0062] For degassing of solvent, thermal degassing is conventionally applied. For thermal degassing, solvent may be heated up to the boiling point which leads to a reduced solubility of gas. A disadvantage of such an approach is that it may be undesired to have boiling solvents, because this may be dangerous.
[0063] Another conventional alternative is chemical degassing. In this context, special chemicals are added to the solvent which is to be degassed. However, pure solvents may be strongly preferred in mobile phase-based sample separation technologies such as HPLC applications.
[0064] Still another option of degassing is ultrasonic degassing. Sound may be excited with an ultrasonic frequency which leads to degassing of the solvent.
[0065] Yet another way of degassing is vacuum degassing. By vacuum degassing, liquid may be separated from a vacuum chamber by a gas-permeable membrane. Gas permeates through the membrane from the solvent into the vacuum chamber.
[0066] According to an exemplary embodiment of a first aspect of the invention, a degasser for degassing a gas-containing liquid is provided which boosts the degassing function by combining vacuum degassing with ultrasound-enhanced degassing. Such a degasser may be implemented particularly advantageously in a sample separation device such as a liquid chromatography device, more particularly an HPLC (high performance liquid chromatography) device. Ultrasound generation may be accomplished in a simple, compact and efficient way by the use of an electroactive material for the construction of the ultrasound source.
[0067] In particular, an exemplary embodiment combines a vacuum-based degasser with an electroactive ultrasonic degassing promoter. In particular, an electroactive polymer-based ultrasonic source may be integrated in a gas permeable membrane for achieving a pronounced compactness. Hence, an ultrasonic transducer may generate ultrasound by an electroactive layer. Ultrasonic enhancing degassing may for instance be applied indirectly onto the liquid, for instance the ultrasonic waves may be applied to an evacuated chamber and may propagate from there to the membrane being functionally coupled with the gas-containing liquid to be degassed. Alternatively, ultrasonic waves may be applied directly onto the liquid by integrally forming the gas permeable membrane and the ultrasound source. An electroactive polymer layer may be implemented in the degasser for operating as a sensor, in particular as a pressure sensor. A dielectric elastomer may be used for a gas permeable membrane and/or in an ultrasound source of a degasser according to an exemplary embodiment.
[0068] More specifically, an exemplary embodiment of the invention provides a vacuum degasser in which a core of an ultrasonic source is built of fluorosilicone. As said material is an dielectric elastomer, it can function as an ultrasonic source itself. Furthermore, also a gas permeable membrane may comprise fluorosilicone. Fluorosilicone can also be used for a direct pressure measurement in a degasser, in particular in a negative pressure chamber thereof. Preferably, an exemplary embodiment may combine an ultrasonic degasser and a vacuum degasser. Optionally, a pressure sensor may be implemented as well, in particular in a gas permeable membrane and/or in an ultrasound source, wherein sensor data may be supplied to a control unit via a control loop for controlling the degasser. An integrated ultrasonic actor and pressure sensor may be integrated directly into the degasser, which may lead to a greater performance and a reduced manufacturing effort.
[0069] According to an exemplary embodiment of a second aspect of the invention, a vacuum degasser for degassing a gas-containing liquid by selective gas diffusion through a gas permeable membrane into a vacuum chamber is provided which uses a silicone material for constructing the membrane. Such a silicone material, in particular fluorosilicone, may be manufactured with sufficiently small thickness promoting gas permeability while simultaneously ensuring a sufficient robustness of the membrane even in the presence of a high pressure difference between the opposing membrane sides. Moreover, a silicone membrane may be both deformable and durable. Advantageously but not necessarily, the high deformation capability of a silicone membrane enables to synergistically combine vacuum degassing with an additional ultrasound trigger rendering vacuum degassing much more efficient.
[0070] Referring now in greater detail to the drawings,
[0071] While the mobile phase can be comprised of one solvent only, it may also be mixed from plural solvents. Such mixing might be a low pressure mixing and provided upstream of the pump 20, so that the pump 20 already receives and pumps the mixed solvents as the mobile phase. Alternatively, the pump 20 may comprise plural individual pumping units, with plural of the pumping units each receiving and pumping a different solvent or mixture, so that the mixing of the mobile phase (as received by the separation unit 30) occurs at high pressure and downstream of the pump 20 (or as part thereof). The composition of the mobile phase may be kept constant over time, the so called isocratic mode, or varied over time, the so called gradient mode.
[0072] A data processing unit or control unit 70, which can be a PC or workstation, may be coupled (as indicated by the dotted arrows) to one or more of the devices in the sample separation device 10 in order to receive information and/or control operation. For example, the control unit 70 may control operation of the pump 20 (for example setting control parameters) and receive therefrom information regarding the actual working conditions (such as output pressure, etc. at an outlet of the pump 20). The control unit 70 may also control operation of the solvent supply 25 (for example setting the solvent/s or solvent mixture to be supplied), and in particular of the degasser 100 (for example setting control parameters and/or transmitting control commands to any of the components shown in
[0073]
[0074]
[0075]
[0076] The degasser 100 according to
[0077] As shown in
[0078] Moreover,
[0079] A deformable gas permeable membrane 106 separates the liquid accommodation volume 102 from the negative pressure chamber 104, i.e. is arranged in between. Since the gas permeable membrane 106 is permeable for gas but impermeable for liquid, the gas-containing liquid 121 in the liquid accommodation volume 102 contacting the membrane 106 from a bottom side will be separated into a gas-enriched portion propagating through the gas permeable membrane 106 and a gas-depleted portion consisting primarily of liquid and being incapable of traversing membrane 106. This separation is promoted by the vacuum in the negative pressure chamber 104 resulting in vacuum degassing.
[0080] In addition and as described below in further detail, the gas-containing liquid 121 can be actuated (i.e. to separate gas bubbles from liquid) and/or the gas permeable membrane 106 can be actuated (i.e. can be forced to move or oscillate), by ultrasound to additionally stimulate or force gas of the gas-containing liquid 121 to move through the membrane 106 by a combinatory effect of the negative pressure and the ultrasound. Without wishing to be bound to a specific theory, it is presently believed that separation of gas particles from liquid in gas-containing liquid 121 can be promoted by subjecting the gas-containing liquid 121 and/or the gas permeable membrane 106 to ultrasound.
[0081] In order to enable the synergistic combination of the vacuum-based and ultrasound-enhanced degassing, an ultrasound source 112 may be provided in the degasser 100. Advantageously, the ultrasound source 112 may comprise an electroactive material 124, preferably an electroactive polymer. Hence, the ultrasound source 112 may be configured for generating ultrasound for actuating the gas containing liquid 121 and/or the gas permeable membrane 106 by exciting the electroactive material 124 electrically to force it to deform for generating ultrasound. Preferably, the electroactive material 124 may be an electroactive polymer, such as an electroactive silicone, like fluorosilicone. Advantageously, also the membrane 106 may be made of a silicone such as fluorosilicone, since such a material combines a proper gas permeability with a liquid impermeability, is durable and properly deformable as well as manufacturable with sufficiently small thicknesses, d, of for instance 20 μm (please note that
[0082] According to the embodiment of
[0083] Advantageously, the degasser 100 may further comprise a pressure sensor 118 for sensing a pressure in the negative pressure chamber 104. The sensed pressure data may be supplied from the pressure sensor 118 to a control unit 70 (for instance a processor) controlling operation of the degasser 100. In particular, operation of the negative pressure source 110 and/or of the excitation unit 154 may be adjusted by the control unit 70 based on the detected pressure value.
[0084] Highly advantageously, the pressure sensor 118 can be integrally formed with the ultrasound source 112. Depending on the pressure value in the negative pressure chamber 104, the dielectric elastic layer of electroactive material 124 of the ultrasound source 112 will be deformed in a characteristic way. Together with the above-mentioned electrodes, the electroactive material 124 forms a capacitor with a value of the capacitance being characteristically influenced by the deformation of the electroactive material 124, and thereby depending on the pressure value in the negative pressure chamber 104. Hence, electrically measuring the capacitance allows to derive the pressure value in the negative pressure chamber 104 by simultaneously using the ultrasound source 112 as a pressure sensor 118.
[0085] As can be taken from
[0086] Advantageously, the dielectric elastomer according to reference sign 124 synergistically functions both as a pressure sensor 118 and for inducing ultrasonic waves in the negative pressure chamber 104, and hence in the membrane 106 and the liquid accommodation volume 102. This leads to an additional ultrasonic degassing of solvents with an integrated feedback sensor 118 within the actuator. This saves space and improves the performance of the degasser 100.
[0087]
[0088] The embodiment of
[0089] Now referring to
[0090] More specifically, stack 136 comprises the protective permeable sealing membrane 106, for example made of fluorosilicone. Electroactive material 124 may be a silicone insulation, for example made of fluorosilicone as well. Spacer layer 128 keeps the membrane 106 at a proper distance to the lower electrode 122 so that the lower electrode 122 does not block space for the diffusion process of degassing. For example, the spacer layer 128 can be a flat structure with holes, a grid-like pattern or a porous structure. The composition of stack 136 according to
[0091] According to
[0092] Furthermore and as shown in
[0093]
[0094] According to
[0095]
[0096] According to
[0097] Moreover, the stack 136 according to
[0098]
[0099] According to
[0100] Advantageously, also the gas permeable membrane 106 may be made of a silicone, preferably fluorosilicone. A thickness, d, of the gas permeable membrane 106 may be in a range from 10 μm to 100 μm. Such a configuration allows to obtain a mechanically robust and nevertheless properly deformable and elastic membrane 106 showing an excellent permeability for gas and a reliable impermeability for liquids. At the same time, said material is durable and compatible even with aggressive chemicals which may occur in liquid chromatography applications.
[0101] By configuring the gas permeable membrane 106 and the electroactive material 124 of the same material, preferably fluorosilicone, the number of implemented materials may be low which avoids material incompatibilities and reduces the manufacturing effort of the degasser 100.
[0102]
[0103] According to
[0104] It should be noted that the term “comprising” does not exclude other elements or features and the term “a” or “an” does not exclude a plurality. Also elements described in association with different embodiments may be combined. It should also be noted that reference signs in the claims shall not be construed as limiting the scope of the claims.