EP2678106A1 - Mikrofluidische extraktionsvorrichtung mit stabilisierter flüssig-flüssig-schnittstelle - Google Patents
Mikrofluidische extraktionsvorrichtung mit stabilisierter flüssig-flüssig-schnittstelleInfo
- Publication number
- EP2678106A1 EP2678106A1 EP12705683.6A EP12705683A EP2678106A1 EP 2678106 A1 EP2678106 A1 EP 2678106A1 EP 12705683 A EP12705683 A EP 12705683A EP 2678106 A1 EP2678106 A1 EP 2678106A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- liquid
- pillars
- carrier liquid
- micro
- extraction device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 175
- 238000000605 extraction Methods 0.000 title claims abstract description 51
- 238000009736 wetting Methods 0.000 claims abstract description 54
- 239000002904 solvent Substances 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims description 44
- 239000000758 substrate Substances 0.000 claims description 32
- 238000012546 transfer Methods 0.000 claims description 29
- 230000003068 static effect Effects 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- PXELHGDYRQLRQO-UHFFFAOYSA-N 1-butyl-1-methylpyrrolidin-1-ium Chemical compound CCCC[N+]1(C)CCCC1 PXELHGDYRQLRQO-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000000622 liquid--liquid extraction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000000638 solvent extraction Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000000708 deep reactive-ion etching Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000000138 intercalating agent Substances 0.000 description 2
- 230000009545 invasion Effects 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 210000003463 organelle Anatomy 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 1
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 1
- SCZKICLHKCRNNY-UHFFFAOYSA-N 1-butyl-1-methylpyrrolidin-1-ium trifluoromethanesulfonamide Chemical compound NS(=O)(=O)C(F)(F)F.NS(=O)(=O)C(F)(F)F.CCCC[N+]1(C)CCCC1 SCZKICLHKCRNNY-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000008365 aqueous carrier Substances 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- 238000000206 photolithography Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0496—Solvent extraction of solutions which are liquid by extraction in microfluidic devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502753—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by bulk separation arrangements on lab-on-a-chip devices, e.g. for filtration or centrifugation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502769—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by multiphase flow arrangements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B1/00—Devices without movable or flexible elements, e.g. microcapillary devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2300/00—Additional constructional details
- B01L2300/08—Geometry, shape and general structure
- B01L2300/0809—Geometry, shape and general structure rectangular shaped
- B01L2300/0816—Cards, e.g. flat sample carriers usually with flow in two horizontal directions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2300/00—Additional constructional details
- B01L2300/08—Geometry, shape and general structure
- B01L2300/0861—Configuration of multiple channels and/or chambers in a single devices
- B01L2300/0864—Configuration of multiple channels and/or chambers in a single devices comprising only one inlet and multiple receiving wells, e.g. for separation, splitting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/04—Moving fluids with specific forces or mechanical means
- B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
- B01L2400/0472—Diffusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2400/00—Moving or stopping fluids
- B01L2400/08—Regulating or influencing the flow resistance
- B01L2400/084—Passive control of flow resistance
- B01L2400/086—Passive control of flow resistance using baffles or other fixed flow obstructions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/381—Diluting, dispersing or mixing samples by membrane diffusion; Permeation tubes
Definitions
- the present invention relates to the general field of microfluidics and relates to a microfluidic device for liquid - liquid extraction of analytes of interest.
- the extraction of the analytes of interest is carried out in an extraction chamber of the micro-device in which the two liquids circulate, separated from each other by micro-pillars arranged parallel to the flows.
- the analytes of interest may be chemical and / or biological particles, such as macromolecules, cells, organelles, pathogens, or even intercalating agents.
- microfluidic extraction device finds application particularly in biotechnology, chemistry and environmental sciences.
- C f is the case for example the field of diagnosis, monitoring food or environmental monitoring.
- the analysis steps may require, prior to the detection of the analytes and the measurement of their concentration, to transfer said analytes of interest from a carrier liquid to a liquid solvent to obtain a high concentration of analytes in the liquid solvent. . This makes it possible to increase the efficiency and accuracy of the detection of said analytes by the current analysis means.
- such a micro-extractor 1 comprises an extraction chamber 30 formed of two transfer zones 31A, 31B separated from one another in the longitudinal direction by a plurality of micro-pillars. 32.
- the longitudinal direction coincides with the direction of flow of the liquids in the extraction chamber. It corresponds to the direction in which the interface between the two liquids is extended.
- the extraction chamber 30 is delimited by lower, upper and lateral walls.
- the micropiliers 32 are aligned in the longitudinal direction and extend each between the lower and upper walls.
- Each transfer zone 31A, 31B communicates with a microchannel 40A, 40B which ensures the fluid circulation of two liquids in the extraction chamber. 30 along the longitudinal direction thereof.
- the carrier liquid P of analytes of interest circulates within the first transfer zone 31A, and the liquid solvent S flows into the second transfer zone 31B.
- the carrier liquid P is water or an aqueous solution
- the liquid solvent S is an organic solution. Both liquids are immiscible with each other.
- the analytes of interest may be chemical and / or biological particles, such as macromolecules, cells, organelles, pathogens, or even intercalating agents.
- the interface of the carrier liquid P with the liquid solvent S is located between each micropillar 32 and extends between the lower and upper walls. More specifically, the carrier liquid P forms a plurality of interfaces with the liquid solvent S, which are each in contact with two adjacent micro-pillars 32 and the lower and upper walls.
- the analytes of interest diffuse through the interfaces, from the carrier liquid to the liquid solvent, and bind, for example ligands so that they can not return to the carrier liquid, or, for example because of a better solubility in the solvent.
- the interfaces are in particular subjected to capillary wetting forces due to the contact of the fluids considered with the microbeams and said walls, during their circulation.
- a first liquid for example the carrier liquid
- a wetting angle that is too high in particular greater than 165 ° or even 170 °
- the second liquid for example the solvent
- 1 / invention aims to provide a microfluidic device for extracting analytes of interest of a carrier liquid in a solvent liquid, the interface f of the carrier liquid with the liquid solvent has improved stability compared to the realization of the prior art mentioned above.
- the subject of the invention is a microfluidic device for extracting analytes of interest from an aqueous carrier liquid in a liquid solvent immiscible with the carrier liquid, comprising an extraction chamber delimited by lower walls. , top and side, and formed of a first and of f a second transfer zones forming respectively a part of a first microchannel and a second microchannel and being separated one from each other in the longitudinal direction by a plurality of micro-pillars extending between said lower and upper walls, said device comprising means for ensuring a circulation in said microchannels of the carrier liquid with a non-zero flow Dl and liquid solvent with a non-zero flow D2, with D1 / D2> 1, said first transfer zone containing said carrier liquid and said second transfer zone containing said liquid solvent, said liquid solvent forming with the said carrier liquid a plurality of interfaces each of which extends between two adjacent micro-pillars and said lower and upper walls, said device being characterized in that the carrier liquid bathed in the liquid solvent and
- 9 min > 45 ° and 9 max ⁇ 135 ° which defines a first range in which the average of the wetting angles ⁇ and ⁇ 2 can change.
- a second narrower range is defined, between 9 min and 9 raax limit angles such as 9 min > 70 ° and 9 raax ⁇ 110 °.
- the inventors have found that more has approaches 0 °, (ie when the average ⁇ ⁇ wetting angles and 9 2 defined above approaches the limit angles 45 ° or 135 °) plus the change in pressure both sides of the interface must be controlled, and less than a critical pressure variation APmax, described later.
- the wetting angles ⁇ 1 and ⁇ 2 are greater than 10 ° or even 15 ° and less than 170 °, or even 165 ° in order to avoid the appearance of a film of wetting. contact with one of the materials constituting the device.
- a be between 25 ° and 45 °.
- the previously defined wetting angles are contained in a restricted angular range whose limit values 9 min and 9 max are such that 9 min > 70 ° and e max ⁇ 120 °.
- Such a restricted angular range allows, for example, good stability of the interface, being relatively insensitive to pressure fluctuations on either side of the interface.
- This range can, for example, be obtained using the following materials and liquids:
- second liquid ionic liquid, for example [BMP], [NTf] - (1-butyl-methylpyrrolidinium bis- (trifluoromethane sulfonamidide).
- glass for example Pyre
- carrier liquid is meant a liquid containing analytes of interest.
- liquid solvent a liquid capable of receiving and keeping the analytes of interest initially contained in the carrier liquid.
- the longitudinal direction coincides with the direction in which f s extends the interface between the carrier liquid and the liquid solvent. When the carrier liquid and possibly the liquid solvent are flowing, the longitudinal direction coincides with the direction of flow of the liquid (s).
- the longitudinal direction is in a plane substantially orthogonal to the lower and upper walls.
- the respective widths w1, w2 of said transfer zones are chosen so as to verify the relationship:
- the dynamic pressure difference between the carrier liquid and the liquid solvent in the extraction chamber is constant along the longitudinal direction thereof.
- a threshold value APmax beyond which the interface is likely to break.
- This threshold value may be the capillary pressure jump 2 ⁇ / ⁇ , where y is the surface tension of the liquid solvent in contact with the carrier liquid, and ⁇ is the average spacing between two adjacent micropiliers.
- the microfluidic extraction device comprises means adapted to impose, upstream or downstream of the extraction chamber, the static pressure of each of said liquids, said imposed static pressures being substantially equal to one another.
- a pressure variation ⁇ on both sides of the interface, as close as possible to 0, and in all cases, lower than the critical value APmax.
- the dynamic pressure difference between the two liquids at any one of said interfaces is substantially zero, and therefore strictly less than the capillary threshold value 2 ⁇ / ⁇ .
- the microfluidic extraction device according to The invention can be made from two substrates. A lower substrate and an upper substrate, said micro-pillars and said bottom wall being made within said lower substrate while said top wall is formed by said upper substrate.
- said lower substrate is made of silicon oxide and said upper substrate is made of glass.
- FIG. 1, already described, is a diagrammatic view from above of a microfluidic extraction device according to an example of the prior art
- Figure 2 already described, is an enlarged perspective view of a portion of the microfluidic extraction device shown in Figure 1;
- Fig. 3 is a representation of the wetting angle ⁇ formed by a first liquid L1 wetting in a second liquid L2, in contact with the surface of a material M;
- FIG. 4 is a schematic perspective view of the extraction chamber of a microfluidic extraction device according to the method of preferred embodiment of the invention.
- Figure 5 illustrates a cross-section of the microfluidic device of FIG. 4 when the condition of stability is not respected.
- Figure 4 shows a microfluidic device for liquid - liquid extraction, or microextraorganisme, allowing the transfer of f analytes of interest of a carrier liquid to a liquid solvent according to the preferred embodiment of the invention.
- a direct orthonormal coordinate system in Cartesian coordinates (X, Y, Z) shown in FIG. 3 is used.
- the direction X is oriented in the longitudinal direction corresponding to the direction of circulation of the liquids.
- the direction Y is orthogonal to the direction X and the direction Z is oriented according to the height of the device.
- the device 1 comprises an extraction chamber 30 delimited by lateral walls, lower 11 and upper 12.
- the extraction chamber 30 is formed of first and second transfer zones 31A, 31B separated from each other longitudinally by a plurality of micro-pillars 32.
- micro-pillars 32 are aligned in the longitudinal direction and extend in the Z direction between said lower 11 and upper 21 walls.
- They are preferably cylindrical in the general sense of the term, and may have a circular, oblong or even polygonal section.
- the section is polygonal, for example triangular, square, rectangular, and has sharp angles.
- the extraction chamber 30 is formed by a lower substrate and an upper substrate.
- the transfer zones 31A, 31B and the micro-pillars 32 are formed in the lower substrate.
- the upper substrate, or cover, is assembled to the lower substrate.
- the micro-pillars 32 are made in the lower substrate, while the upper wall 21 is a face of the upper substrate.
- Each transfer zone 31A, 31B communicates with a microchannel 40A, 40B (not shown in FIG. 4) identical to that illustrated in FIG. 1.
- the microchannel 40A, 40B is formed of an inlet duct 41A, 41B and an outlet duct 42A, 42B disposed respectively upstream and downstream of the extraction chamber 30 ( Figure 1).
- the first microchannel 40A is connected to means 50A for circulating a liquid ⁇
- The. second microchannel 40B is connected to means 50B for circulating a liquid solvent S in the second transfer zone 31B with a flow D2, which can be zero ( Figure 1).
- liquids P, S can circulate in co-current or against the current.
- the first transfer zone 31A contains the carrier liquid P and the second transfer zone 31B contains the liquid solvent S.
- the liquid solvent S is ionic.
- the carrier liquid P forms with the liquid solvent S, in the extraction chamber 30, a plurality of interfaces 2 each of which extends between two adjacent micro-pillars 32 and between the lower and upper walls 11 and 21.
- each liquid in question in 1 case the carrier liquid 1 and the solvent liquid, wetting angles ⁇ and ⁇ 2 of the materials constituting the pillars, and the lower or upper surfaces can be defined.
- FIG. 3 particularly illustrates the definition of a wetting angle according to the invention.
- the wetting angle ⁇ can be defined, as corresponding to the contact angle, that a drop of a first liquid LI at rest, bathed in a second liquid L2 at rest, forms when it is placed. in contact with a material M.
- Anchorage angles are then characteristic of the materials constituting the device (the upper wall, the lower wall or the pillars) and not flows.
- a first wetting angle ⁇ can be defined, corresponding to the contact angle that a drop of this first liquid, bathed in the second liquid (the liquid solvent in this example), form when placed in contact with the material constituting the micro-pillars.
- the wetting angle at the bottom wall 11 is substantially equal to that measured at the micro-pillars 32. This angle will also be noted ⁇ .
- the bottom wall and the micro-pillars are made of the same material, since they are made in the lower substrate
- a second wetting angle ⁇ 2 is defined at the upper wall 21; it then corresponds to the contact angle that a drop of the first liquid, immersed in the second liquid (the solvent liquid in this example), forms when it is placed in contact with the material constituting the upper wall.
- the surfaces are said to be hydrophilic when the wetting angle ⁇ as represented in FIG. 3 is less than 90 ° and said hydrophobic for an angle ⁇ greater than 90 °.
- the wetting angle ⁇ may represent the angle ⁇ in the case where the material M is the material of the lower substrate, where ⁇ 2 in the case where M is the material of the upper substrate.
- the liquid considered is said to be wetting and in the second case, non-wetting. It should be noted that we are here in the situation of partial wetting and not in the case of total wetting.
- the carrier liquid P, the liquid solvent S and the materials of the micro-pillars and the upper or lower wall are chosen so that the wetting angles ⁇ 1 and ⁇ 2 satisfy the relationship:
- the wetting angles ⁇ ⁇ and ⁇ 2 are greater than 10 ° or even 15 ° and less than 170 °, or even 165 ° in order to avoid the appearance of a contact film with one of the materials constituting the device (the upper wall, the lower wall or the pillars).
- the interfaces 2 between two micro-pillars 32 are stable and remain in contact with the micro-pillars 32 and the lower walls 11 and upper 21.
- the average of the first and second wetting angles must be between two limit angles 9min and 9max, with 9min> 45 ° and 9max ⁇ 135 °.
- the interface 2 moves according to the bold arrows shown in FIG. 5, which can lead to an interface break.
- the first liquid LI invades the half-channel intended for L2. More specifically, it is shown in FIG. A cross-section of the microfluidic device of FIG. 4.
- the interface 2 has here moved beyond the micro-pillar 32 and has entered the part of the microchannel reserved for L2.
- the contact angles si and ⁇ 2 which have been shown, result from the flow conditions of the liquids Ln and L 2 in the device. These are not wetting angles ( ⁇ ⁇ or ⁇ 2 ) within the meaning of the invention.
- a wetting angle ⁇ is defined as 1 1 angle formed by a drop of a first liquid wetting material M, this drop bathing, at rest, in a second liquid.
- the interface 2 may be unstable when the average of the angles ⁇ 1 and ⁇ 2 is close to these limit angles. Indeed, under such conditions, the stability can be obtained only when the pressure variation AP on either side of 1 1 interface is lower than the threshold APmax previously defined. The slightest fluctuation of this pressure variation is liable to cause instability of the interface, which may lead to invasion of the channel occupied by the least wetting liquid by the most wetting liquid.
- the carrier liquid P being an aqueous solution
- the solvent S being an organic solvent such as cyclohexane
- This threshold value corresponds substantially to the capillary pressure jump 2 ⁇ / ⁇ , where ⁇ is the surface tension of the carrier liquid P in contact with the liquid solvent S, and ⁇ is the average spacing between two adjacent micro-pillars 32.
- This critical length therefore limits the useful length of transfer in the extraction chamber.
- the respective widths w1, w2 of said transfer zones 31A, 31B are chosen so as to verify the relation: where ⁇ ⁇ is the dynamic viscosity of the liquid considered, and ⁇ ( ⁇ ) is a coefficient expressing the friction to which the liquid passing through the channel i is subjected. The smaller the channel, the higher the coefficient. For the targeted applications, this factor is generally between 1 and 5. In the case of a channel of rectangular section, we have:
- the width of the channel z " and H is the height of the channels, D, and D 2 are respectively the flow rates of the carrier liquid and the liquid solvent.
- the dynamic pressure difference between the carrier liquid P and the liquid solvent S in the extraction chamber 30 is constant along the longitudinal direction thereof.
- An extraction chamber 30 is thus obtained in which the interfaces 2 are stable in every respect.
- the extraction chamber 30 can therefore be of great length, which makes it possible to obtain a particularly important transfer surface area.
- each of the liquids P, S is fixed upstream or downstream of the extraction chamber 30, so that the imposed static pressures are substantially equal.
- the variation of the pressure being zero on both sides of the interface, the latter is very stable, and even more particularly when 70 ° ⁇ ( ⁇ 1 + ⁇ 2) / 2 ⁇ 110 °.
- the dynamic pressure difference between the two liquids P, S at any of said interfaces 2 is therefore substantially zero and always strictly less than the capillary threshold value 2 ⁇ / ⁇ .
- the upstream or downstream static pressures can be set by the means 50A, 50B adapted to circulate the liquids in the microchannels, for example microfluidic flow pumps (FIG. 1).
- the micro-extractor 1 according to the preferred embodiment of the invention can be made of as follows, as is partially described in the article by Tran et al. entitled “Micro-extractor for liquid-liquid extraction, concentration and in-situ detection of lead” I RET-10: 10th International Conference on Microneaction, AIchE 2008 pring National Meeting, 6-10 April 2008, New La, USA.
- the lower substrate is monolithic and may be silicon (Si0 2 ).
- the upper substrate may be silicon or glass.
- 31A, 31B forming the extraction chamber 30 and the micro-pillars 32 may be produced by conventional microtechnology techniques (for example photolithography followed by etching), for example by selective etching of the DRIE ("Deep Reactive Ion Etching") type. " in English) .
- DRIE Deep Reactive Ion Etching
- the surfaces of the lower and upper substrates may be treated by silanization, so as to possibly modify the wetting angles ⁇ 1 and ⁇ 2 of the carrier liquid.
- the assembly of the two substrates can be achieved by conventional molecular sealing techniques in the silicon / silicon case or anodic sealing in the silicon / glass case. It can also be done by screen printing glue.
- the height H of the chamber f extraction 30 may be between ⁇ and 1mm, preferably between 50 / um and 500 ⁇ .
- the length can be of some millimeters to a few centimeters, for example between 5mm and 10cm.
- the width w1, w2 of the transfer zones 31A, 31B may be between 0.5 and 10 times the height H.
- the micro-pillars 32 are substantially identical to each other. Their height is equal to the height H of the extraction chamber 30. Their side or the diagonal is between 0.02 and 1 times the height H.
- the micro-pillars 32 may have a diameter or a side of 30 / xm and a height of ⁇ .
- the micro-pillars 32 are spaced apart from one another by a distance preferably greater than ⁇ , for example a few microns to a few tens of microns, preferably of the order of 5 to ⁇ .
- the interface surface 2 is the transfer surface area, which can be from a few square millimeters to a few tens of square millimeters.
- the liquids P, S are immiscible with each other.
- the carrier liquid P is preferably aqueous, for example water.
- the liquid solvent S is advantageously ionic, for example [BMP] [NTf2] (1-butyl-1-methylpyrrolidinium bis (trifluoromethane sulfonamide)).
- the two liquids P, S have a flow Dl and
- the carrier liquid P can have a flow rate of 1 to ⁇ / min and the liquid solvent S a flow rate of 0.01 to 5/1 / min.
- the two liquids P, S are preferably chosen so that the average of the angles of wetting ⁇ 1 and ⁇ 2 previously defined satisfies the relation 70 ° ⁇ ( ⁇ 1 + ⁇ 2) / 2 ⁇ 110 °.
- the flow of liquids P, S is obtained by syringe pumps and / or electronic nanopumps such as the Dionex Ultimate 3000.
- the description describes in detail only the embodiment in which the side walls, the bottom wall 11 and the micro-pillars 32 are made of the same material constituting the lower substrate, while the upper wall 21 is a face of the upper substrate made of another material.
- the first wetting angle ⁇ has been described as the angle formed by a first liquid bathed in a second liquid, in contact with the material constituting the pillars and the lower wall and the second wetting angle ⁇ 2 as 1 '. angle that forms said first liquid bathed in said second liquid, in contact with the material constituting the upper wall.
- the side walls, the upper wall 11, as well as the micro-pillars may according to a first variant of the embodiment described, be made of the same material constituting the lower substrate, while the lower wall is a face of the upper substrate made of another material.
- the first wetting angle ⁇ is the angle that forms a first liquid bathed in a second liquid, in contact with the material constituting the pillars and the upper wall; and the second wetting angle ⁇ 2 is the angle formed by said first liquid immersed in said second liquid, in contact with the material constituting the bottom wall.
- the bottom wall and the upper wall may be made of the same material, and the pillars in another material.
- the first wetting angle Q is the angle formed by a first liquid immersed in a second liquid, in contact with the material constituting the pillars; and the second wetting angle ⁇ 2 is the angle formed by said first liquid immersed in said second liquid, in contact with the material constituting the bottom wall and the upper wall.
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- Biochemistry (AREA)
- Molecular Biology (AREA)
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- Computer Hardware Design (AREA)
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Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1151571A FR2971953B1 (fr) | 2011-02-25 | 2011-02-25 | Dispositif microfluidique d'extraction a interface liquide-liquide stabilisee |
| PCT/EP2012/053159 WO2012113905A1 (fr) | 2011-02-25 | 2012-02-24 | Dispositif microfluidique d'extraction a interface liquide-liquide stabilisee |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP2678106A1 true EP2678106A1 (de) | 2014-01-01 |
Family
ID=45757011
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP12705683.6A Withdrawn EP2678106A1 (de) | 2011-02-25 | 2012-02-24 | Mikrofluidische extraktionsvorrichtung mit stabilisierter flüssig-flüssig-schnittstelle |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20140001116A1 (de) |
| EP (1) | EP2678106A1 (de) |
| FR (1) | FR2971953B1 (de) |
| WO (1) | WO2012113905A1 (de) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2945097B1 (fr) * | 2009-04-30 | 2011-06-03 | Commissariat Energie Atomique | Vanne microfluidique a usage unique. |
| FR3003033B1 (fr) | 2013-03-07 | 2015-04-17 | Commissariat Energie Atomique | Dispositif de prelevement d'un echantillon de liquide par capillarite et procede d'analyse associe |
| GB201710091D0 (en) | 2017-06-23 | 2017-08-09 | Univ Oxford Innovation Ltd | Solvo-dynamic printing |
-
2011
- 2011-02-25 FR FR1151571A patent/FR2971953B1/fr not_active Expired - Fee Related
-
2012
- 2012-02-24 EP EP12705683.6A patent/EP2678106A1/de not_active Withdrawn
- 2012-02-24 US US14/001,425 patent/US20140001116A1/en not_active Abandoned
- 2012-02-24 WO PCT/EP2012/053159 patent/WO2012113905A1/fr not_active Ceased
Non-Patent Citations (1)
| Title |
|---|
| See references of WO2012113905A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| US20140001116A1 (en) | 2014-01-02 |
| FR2971953A1 (fr) | 2012-08-31 |
| WO2012113905A1 (fr) | 2012-08-30 |
| FR2971953B1 (fr) | 2014-10-10 |
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