Classifications

• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
  • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
  • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
  • G01N2030/906—Plate chromatography, e.g. thin layer or paper chromatography pressurised fluid phase
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T436/00—Chemistry: analytical and immunological testing
  • Y10T436/25—Chemistry: analytical and immunological testing including sample preparation

Definitions

• the invention relates to the field of separation on a stationary phase of the constituents of a so-called “complex” sample, using a forced flow.
• Separation under forced flow is a technique used to separate the constituents of a sample, deposited in at least a first chosen location on a layer called " stationary phase ", using a carrier fluid, called" mobile phase ", undergoing external pressure. Trained by the mobile phase, the constituents migrate to the stationary phase in a known order depending on their retention.
• certain treatment devices include a separation chamber, into which at least one stationary phase is introduced and which comprises external pressurization means, making it possible to apply an external pressure of selected intensity on an upper face of the phase stationary, distribution means, making it possible to deliver at least one mobile phase at at least one second chosen location of the stationary phase, at least one input for supplying these distribution means and at least one output allowing the evacuation of the mobile phase .
• the mobile phase which is introduced into the separation chamber of this type of device, moves in the stationary phase according to a front called "alpha front".
• the alpha front expels the air which is trapped in the stationary phase, the latter being initially dry.
• part of the air remains trapped in an area known as the “alpha area” located immediately behind the alpha front and preceding a completely wet area known as the “total humidity area”.
• the total humidity front is not linear, which affects the efficiency of the separation, the reproducibility of the results and the accuracy of the analyzes carried out simultaneously or consecutively. No known solution allows sufficiently precise control of the linearity of the fronts, and in particular that of the total humidity front.
• the invention therefore aims to improve the situation.
• mobile phase will be understood to mean any fluid making it possible to move the constituents of a sample over the stationary phase. It may therefore be a liquid, such as an eluent, or a gas, such as air, making it possible to expel a solvent previously introduced into the separation chamber.
• These regulation means preferably comprise at least one valve placed downstream from the first mobile phase outlet and arranged to vary the flow rate of the mobile phase at the outlet of the chamber between a zero value and a maximum value.
• the regulating means further comprise means making it possible to measure the pressure of the mobile phase upstream of the first inlet and / or downstream of the first outlet, as well as a module arranged to control the valve in function a comparison between the measured pressure and the limit pressure linked to the chosen external pressure (or more briefly, limit pressure), the valve being open to let out the mobile phase when the measured pressure becomes greater than or equal to the limit pressure.
• This limit pressure is by definition lower than the external pressure.
• control module jointly controls the valve, the supply means and the external pressurization means so that the supply in mobile phase is carried out for the entire duration of the separation by keeping the valve closed, that is until the measured pressure of the mobile phase reaches the limit pressure (or threshold pressure). Then, the mobile phase supply is interrupted, then the valve is opened and the external pressure is released.
• the separate constituents on the stationary phase are identified and / or quantified using analyzers, on this stationary phase and / or online at the outlet of the bedroom. This will, for example, be analysis by ultraviolet or visible detection or else by mass spectrometry. In this case of online analysis, the separate constituents are eluted by the mobile phase which leaves the chamber.
• control module also jointly controls the valve, the supply means and the external pressurization means so that the mobile phase supply takes place throughout the duration of the separation and analysis by keeping the valve closed as long as the measured pressure of the mobile phase is lower than the limit pressure, then keeping it open.
• the sample can be placed on the stationary phase either before the mobile phase feed begins, or after the valve has been placed in the open position.
• the device according to the invention may include other additional characteristics, taken separately or in combination, and in particular: -
• the chamber can be arranged so as to receive an extractable cassette comprising the stationary phase;
• the external pressurization means may include a flexible film housed opposite the upper face of the stationary phase and application means suitable for pressing the film against the stationary phase to apply the external pressure of selected intensity;
• the application means may include a fluid reservoir intended to generate the external pressure (or more briefly “external pressurizing fluid”), coupled to a supply circuit; but, other means can be envisaged, such as pneumatic or mechanical means;
• the external pressurization fluid reservoir and the mobile phase supply means can be housed in the same fluid supply unit;
• the stationary phase may be provided with the sample to be treated before being introduced into the chamber, or else be provided with this sample once introduced into the chamber, via the same inlet or else via another inlet;
• the control module can be arranged so as to order, before the introduction of the sample, on the one hand, the valve to be placed in a state preventing the evacuation of the mobile phase and, on the other hand , to the supply means for supplying the stationary phase with a selected mobile phase volume, preferably, so that this volume corresponds to a measured mobile phase pressure substantially equal to the limit pressure.
• the invention also relates to a process for treating the constituents of at least one sample by separation under forced flow.
• This process comprises the following steps: a) placing in a chamber at least one stationary phase suitable for receiving at least one first location chosen at least one sample to be treated, b) supplying in mobile phase at least one second location chosen from the phase stationary, while applying an external pressure of selected intensity to the upper face of this stationary phase and preventing the mobile phase from leaving the stationary phase, c) measure the pressure of the mobile phase upstream and / or downstream of the chamber, d) compare each pressure measured with a limit pressure, linked to the external pressure chosen, and, when the measured pressure becomes greater than or equal to the limit pressure, reduce the pressure of the mobile phase so that it remains less than or equal to this limit pressure.
• FIG. 1 schematically illustrates an example of a device according to the invention suitable for separation in infusion and / or infusion-transfusion mode
• FIG. 2 is a cross-sectional view of the separation chamber of FIG. 1,
• FIG. 3 is a variant of FIG. 1 in which the external pressurization means are not hydraulic but, for example, mechanical,
• FIGS. 4a and 4b are diagrams comparing the changes as a function of time of the alpha fronts and of total humidity and of the pressure measured for the modes of infusion (a) and infusion-transfusion (b), in the case of regulation on the pressure of the mobile phase measured upstream of the chamber,
• Figures 5a to 5d are variants of the devices of Figures 1 and 3.
• treatment of a sample is understood here to mean mainly the separation of the constituents which compose it, possibly coupled with one or more on-line and / or off-line analysis of these constituents.
• the device illustrated in Figures 1 and 2 firstly comprises a separation chamber 1 adapted to receive a layer 2 (in English "sorbent layer") forming a stationary phase.
• This layer 2 is for example made up of powder or particles of silicate gel, alumina, magnesium silicate, talc based on inorganic components, cellulose, synthetic resin, polyamides based on organic components, or else derivatives or mixtures of some of these components on a support plate comprising a layer 2 with one or two stationary separation phases.
• the material used and its surface condition depend on the type of sample to be treated.
• This layer 2 preferably rests on a rigid support 3 supported by the bottom of the lower part 4 of the chamber 1, and at a distance from it so that a cavity 12 is formed under the support 3. or the samples to be treated are placed in at least a first chosen location 6 on the upper face 5 of the layer 2, opposite the bottom 4. Furthermore, the mobile phase is introduced on this same upper face 5, in at least a second chosen location 7. As indicated above, the mobile phase is intended to cause the migration of the constituents of the sample.
• location means both a localized location and an extended location of the straight line, curvilinear or circular type, or of any other chosen shape.
• first 6 and second 7 places can be at least partially confused.
• a person skilled in the art knows how to choose the first and second places according to the type of treatment he wishes to perform.
• the separation can be unidirectional or bidirectional, or circular, or even anti-circular. But all of this is well known to those skilled in the art, and is not the subject of the present invention.
• a flexible waterproof film 8 for example of Teflon.
• this film 8 is intended to apply an external pressure, uniform or not, on the upper face 5 of the stationary phase 2.
• the film 8 comprises, opposite at least part of the second location 7, a first opening 9 for the sealed passage of the end of a tube 10 intended to distribute the mobile phase at the second location 7.
• layer 2 (or stationary phase) can be housed beforehand in a cassette arranged to be introduced into the chamber before treatment.
• the upper wall of this cassette can optionally include the flexible external pressurization film.
• it is preferable that the sample is implanted in the stationary phase 2, before introduction of the cassette into the chamber 1. But this is not compulsory, in particular when the cassette does not include a flexible film.
• the film 8 comprises, opposite at least part of the first location 6, a second opening for the sealed passage of the end of a tube intended for the introduction of the sample at the first location 6.
• a single opening may be sufficient for the introduction of the mobile phase and the sample.
• the upper part of the chamber 1 is closed by a wall 11 placed, in the example illustrated in FIGS. 1 and 2, slightly above the film 8.
• This upper wall 11 comprises a first inlet 13 for the sealed passage of the end of the tube 10 for distributing the mobile phase.
• the lower wall 4 of the chamber comprises a second inlet 14 for the sealed passage of the end of a tube 15 for supplying external pressurization fluid.
• This external pressurization fluid (or pressure transfer fluid) can be a gas or, as in the example described below, a liquid such as oil.
• the external pressurization fluid preferably circulates in a closed circuit, the upstream supply part of which is formed by the tube 15 and the downstream part is formed by a tube 19 of which a first end 20 opens into the cavity 12 of the chamber 1 by a sealed opening 21 formed, for example, in its lower wall 4, while the opposite end 22 of this tube 19 opens into a reservoir of external pressurization fluid 27.
• This reservoir 27 is coupled to a first micro-pump which is controlled by the control module 25 of the device and, preferably, housed in a unit 23 for supplying fluid.
• the tube 15 for supplying external pressurization fluid is provided with a pressure sensor 32 which delivers its pressure measurement to the control module 25.
• control module 25 can act on the first micro- pump to fix, as required, the flow rate of supply of external pressurizing fluid, and consequently the external pressure applied to the layer 2. It is also possible to provide on the tube 20, between the opening 21 and the reservoir 27, a valve 34.
• the external pressurization fluid When the external pressurization fluid circulates, it exerts a substantially vertical external pressure on the underside of the support 3, which leads to lifting it and consequently pressing the film 8 and the stationary phase 2 against each other according to an external pressure of selected intensity.
• the chamber comprises, at at least a third chosen location 16, localized or extended, a zone for collecting the mobile phase having served for the separation of the constituents of the sample.
• This third location can be located on the stationary phase 2, as illustrated in FIG. 2, or else on the periphery thereof.
• the film 8 comprises a second opening 17 for the sealed passage of the end of a tube 24 for collecting the mobile phase
• the chamber 2 comprises a sealed outlet 18 allowing the passage of this end of the tube 24.
• the second opening is not useful, and therefore only the outlet 18 is required.
• the tube 10 which feeds layer 2 in mobile phase has one end
• the second micro-pump is also housed in unit 23.
• the fluid supply unit 23 is only used for mobile phase supply, and therefore it only has one micro-pump.
• a pressure sensor 29 is provided upstream from the mobile phase inlet 13 of the chamber 1, or a pressure sensor 30 downstream from the mobile phase outlet 18 from this chamber 1.
• first pressure sensor 29 upstream of the mobile phase inlet 13 of the chamber 1 and a second pressure sensor 30 downstream of the outlet of mobile phase 18 of this chamber 1.
• the first sensor 29 is arranged so as to carry out its pressure measurement on the mobile phase which circulates in the supply tube 10
• the second sensor 30 is arranged so as to carry out its pressure measurement on the mobile phase which circulates in the collection tube 24.
• the first sensor 29 therefore delivers an upstream pressure measurement PI to the control module 25, while the second sensor 30 delivers a downstream pressure measurement PO to said control module 25.
• the invention also provides a valve 31 arranged to control the flow of the mobile phase downstream of the mobile phase outlet 18.
• This valve is therefore installed on the collection tube 24, preferably downstream of the second sensor. pressure 30 (when this is planned).
• the operating state of the valve 31 is controlled by the control module 25 as a function of a first comparison between the first pressure PI measured by the first sensor 29 and a first pressure limit as PMI.U ⁇ I and a second comparison between the second pressure PO measured by the second sensor 30 and a second pressure limit that P o.um-
• the PMi.Lim and / or the P o.um are chosen smaller than the external pressure applied Pex t .
• the first PMI, L..T . and second PM O, L. _ T. limit pressures, as well as P ⁇ x t are stored in registers of a memory, preferably rewritable, so that the limit values can be adapted to the conditions of use for infusion or infusion-transfusion. The release of the external pressure comes after separation.
• the flow rate of the mobile phase which feeds the chamber 1 and the external pressure applied to the layer 2 are also controlled by the control module 25 at the level of the feed micro-pumps.
• the control module 25 therefore only has to carry out its comparison (s) to monitor whether the pressure or pressures measured are respectively higher or lower than the associated limit pressures.
• the control module 25 acts on the valve 31, and possibly on at least one of the supply micro-pumps, so that the mobile phase can, or not, leave the chamber 1
• the valve 31 has a variable flow rate (as opposed to binary operation of the "all or nothing" type)
• the authorized collection (or evacuation) flow rate is determined as a function of the difference between the measured pressure and the pressure associated limit, during the period during which the partially wet zone leaves stationary phase 2 and chamber 1.
• valve 31 is switched from the "closed” state to the "open” state, or the reverse depending on the result of comparisons.
• the "closed” state corresponds to a flow of a zero value, while the "open” state corresponds to a flow of a maximum value.
• the first mode corresponds to an operation of the “offline” or “infusion” type device, in which the processing in the device consists only in the separation of the constituents of the sample.
• the analysis (determination and / or quantification) of these constituents is carried out in an external analyzer after separation of the constituents then extraction of the stationary phase 2. Any type of analysis known to those skilled in the art can be envisaged.
• the sample can be placed before or after introduction of the stationary phase 2 into the chamber 1, it is preferably started from a stationary "dry" phase, that is to say before the phase stationary is powered in mobile phase.
• the control module 25 orders the complete closure of the valve 31 and then the mobile phase supply.
• the valve 31 is kept closed throughout the duration of separation, that is to say as long as the measured pressure PI of the upstream mobile phase remains below PMI, L. _ TI OR, as will be explained below with reference to FIG. 4b, to P M i.umo-
• the valve 31 is open, which amounts to reducing the pressure of this mobile phase , for example at ambient pressure, and finally the external pressure is released.
• the valve 31 operates in all or nothing mode, it is switched from the closed state to the open state.
• the valve 31 is at variable flow, it is switched from the closed state to one of its open states at non-zero flow (strictly greater than zero and less than or equal to the maximum flow). This state is chosen by the control module according to a criterion depending on the separation conditions. It is based on the difference in viscosity between the air and the mobile phase.
• the second mode corresponds to an operation of the “online” or “infusion-transfusion” type device.
• the processing in the device consists in the separation of the constituents of the sample coupled to an online analysis of its constituents and / or to an external analysis.
• the separate constituents are therefore identified and / or quantified on the stationary phase 2 and / or outside of this chamber by analysis of the mobile phase leaving this chamber, which comprises the separate constituents.
• the constituents of the sample are separated under the joint action of a permanent supply in mobile phase and a management of the state of the valve 31.
• the command 25 first orders complete closure of the valve 31 and then the mobile phase supply.
• the valve 31 is kept closed as long as the measured pressure PI of the mobile phase upstream of the chamber remains below the limit pressure PMi.um or, as will be set out below with reference to FIG. 4b, at P i.umo-
• the valve 31 when the limit PMI.U ⁇ I (or P i.um o) is reached or exceeded, the increase in the mobile phase is maintained and the valve 31 is open, which amounts to reducing the pressure of this mobile phase.
• the valve 31 when the valve 31 operates in all or nothing mode, it is switched from the closed state to the open state authorizing a maximum discharge rate for the mobile phase (out of the chamber).
• the valve 31 when the valve 31 is of variable flow, it is switched from the closed state to one of its open states authorizing a non-zero flow (strictly greater than zero and less than or equal to the maximum flow) for discharging the mobile phase (outside the room).
• This state is chosen by the control module according to a criterion depending on the separation conditions.
• a current or voltage supply module 33 can be provided for supplying electrodes housed in the chamber 1 for separation by electro-chromatography or electrophoresis. These electrodes are placed parallel or perpendicular to the flow, the electrophoresis being carried out either simultaneously or sequentially, relative to the separation by the mobile phase.
• electro-chromatography can be carried out after a pre-wetting (or pre-wetting) infusion in the open state of the valve 31, using electrodes perpendicular to the flow.
• the electro-chromatography and the chromatography can be carried out simultaneously or sequentially.
• the chromatographic and electrophoretic separation can be carried out simultaneously or sequentially on the pre-wetted stationary phase, using electrodes parallel or perpendicular to the flow.
• the electrophoresis is of course carried out in the wet (or wet) phase.
• the stationary phase can also include several identical or different zones, each making it possible to carry out a particular treatment (separation and / or analysis).
• the external pressurization means used in the different zones may possibly be different, or else they may be identical but provide different pressures.
• rectangles designated by A, B, C and D illustrate, for four successive instants, the instantaneous profiles of the alpha (1) and total humidity (2) fronts.
• M1 denotes the place of introduction of the mobile phase (or second place chosen 7), while MO denotes the place of collection of the mobile phase (or third place chosen 16).
• Reference (6) designates the location of the sample between Ml and MO.
• the reference (4) indicates the place and the instant when the alpha front (1) disappears.
• the reference (5) indicates the place and the instant when the total humidity front (2) disappears. Otherwise :
• - P IU ⁇ TI designates the limiting pressure of the mobile phase, linked to the external pressure, upstream of the inlet 13 of the chamber;
• - PO designates the pressure measured downstream of the outlet 18 of the chamber
• P ⁇ x t designates the external pressure applied to the stationary phase by the external pressurization means (P ⁇ x t is always strictly greater than P M i.um, typically PMi.um is chosen to be substantially equal to approximately 80% of Pgxt, for example; done, at the start of programming the external pressure is chosen and the control module automatically deduces the limit pressure);
• - PMi.um o designates in the infusion-transfusion mode a limit pressure of the mobile phase, also linked to the external pressure, but chosen lower than the limit pressure P ⁇ y ⁇ , um- It is in fact a pressure of security.
• this pressure is the actual limit pressure which is preferably used by the control module to make the comparison with the pressure PI measured upstream of the chamber. It therefore corresponds, at the moment when it is decided to open the valve 31, while maintaining the supply in mobile phase.
• the control module directly calculates P M i.umo from PB ⁇ .
• FIGS. 5a to 5d describe different variants of the devices illustrated in FIGS. 1 and 3.
• all the elements substantially identical to those of FIGS. 1 and 3 bear identical references.
• these variants are only a few examples of implementation among many others.
• FIG. 5a illustrates a first variant in which a unit 35 is provided which makes it possible to supply the stationary phase both in mobile phase and in sample.
• This unit 35 is therefore placed on the fluid supply tube 10, between the upstream pressure sensor 29 and the inlet 13 of the chamber 1, and it is connected to a tube 36 for injecting the sample which penetrates into the chamber by an inlet provided for this purpose and opens opposite the first location 6.
• a single tube 10 could be provided for injecting both the mobile phase and the sample.
• FIG. 5b illustrates a second variant in which a unit 37 is provided, making it possible to supply the stationary phase at two different and independent second locations for performing a bidirectional type separation, or else two separations of samples placed on two different stationary phases.
• a tube 38 supplies the unit 37 in mobile phase, while two tubes 39 and 40 leave the unit 37 to each supply one of the two second places, after having entered the chamber by two inlets 41 and 42 and passed through the film 8 at two sealed openings 9 and 17 provided facing the two second places.
• a substantially linear mobile phase line is produced between the two injection sites and the separation takes place substantially perpendicular to this line.
• This unit 37 also has the function of directing the (or the different) mobile phase (s) to appropriate zones of the stationary phase (s).
• This chamber therefore comprises two independent collection outlets 43 and 44 which supply two tubes 45 and 46 connected to the valve 31, which consequently has two inlets and one outlet.
• FIG. 5c illustrates a third variant in which a unit 37 is provided allowing a parallel supply of the stationary phase in three second different and independent locations, possibly formed on the same stationary phase or on three different stationary phases.
• a tube 38 feeds the unit 37 in mobile phase, while three tubes 47, 48 and 49 leave the unit 37 to feed each one of the three second places, after having entered the chamber by three inlets 50, 51 and 52 and passed through the film 8 at three sealed openings 9 provided opposite the three second locations.
• This chamber therefore comprises three independent collection outlets 53, 54 and 55 which supply three tubes 56, 57 and 58 connected to the valve 31, which in this variant is a triple valve making it possible to let out separately and independently each of the three mobile phases collected.
• FIG. 5d illustrates a fourth variant in which a unit 59 is provided making it possible to supply the stationary phase both in mobile phase and in sample.
• the mobile phase supply can be carried out in parallel on three channels, as in FIG. 5c, just like the sample implantation which can be carried out in parallel on three channels.
• This unit 59 is therefore connected, on the one hand, to three mobile phase supply tubes 60, 61 and 62 which enter the chamber by three fluid inlets 66, 67 and 68 and pass through the film 8 at three watertight openings 9 provided opposite three second places, and on the other hand, three sample injection tubes 63, 64 and 65 which enter the chamber through three sample inlets 69, 70 and 71 and pass through the film 8 at three watertight openings provided opposite three first places.
• This chamber therefore comprises three independent collection outlets 72, 73 and 74 which supply three tubes 75, 76 and 77 connected to the valve 31, which in this variant is a triple valve allowing to let out separately and independently each of the three mobile phases collected.
• the invention also relates to a method for processing a sample by forced flux separation (OPLC). This process includes the following steps.
• OPLC forced flux separation
• At least one stationary phase suitable for receiving is placed in a chamber, at least in a first chosen location, at least one sample to be treated.
• the chamber can be arranged to receive several stationary phases in parallel or in series, or else stacked on top of each other, as is well known to those skilled in the art.
• This stationary phase which is preferably a layer of the type presented in the description of the device according to the invention, is either directly placed in the chamber on a support provided for this purpose, or previously placed in a cassette which is then introduced in the bedroom.
• the sample can be placed on the stationary phase intended to separate its constituents before the stationary phase is introduced into the chamber, or else implanted (or injected) once the stationary phase is introduced into the chamber.
• At least one second selected location of the stationary phase is supplied with the mobile phase, while applying an external pressure of selected intensity to an upper face of the stationary phase and by preventing the mobile phase from leaving the phase. stationary.
• This external pressure is not necessarily uniform.
• the pressure of the mobile phase is measured upstream and / or downstream of the chamber.
• the upstream and / or downstream pressures are compared which has just been measured at an upstream and / or downstream limit pressure (s). Then, when the pressure (s) measured is (are) greater than or equal (s) to the associated limit pressure (s) and the pressure mobile phase limit, linked to the external pressure (P ⁇ x t ), which is greater than the limit pressure (s), the pressure of the mobile phase is reduced so that it remains lower or equal to the limit pressure. In an all or nothing type of operating mode, this pressure reduction is not adaptable (in fact the mobile phase is placed at ambient pressure). On the other hand, in a “variable” type operating mode, the value of the pressure can be chosen as a function of the result of the comparison.
• the method can be applied to the infusion mode (or “offline”) or to the infusion-transfusion mode (or “online”).
• the supply of the stationary phase in the mobile phase is definitively interrupted when the measured upstream pressure becomes greater than or equal to the pressure P i.Lim- En fact, as illustrated in figure 4b, it is possible to decide to use PMi.Lim o as limit pressure being used for comparison, which is strictly lower than PMi.um.
• the mobile phase is placed at ambient pressure, preferably, which amounts to reducing the pressure of this mobile phase, and finally the external pressure is released.
• the mobile phase is prohibited from leaving the room, then the mobile phase is supplied.
• the ban is maintained as long as the measured pressure of the mobile phase upstream of the chamber remains below the limit pressure.
• the limit pressure PMI.UITI or PMi.um o (depending on the choice made at the start) is reached or exceeded, the mobile phase supply is maintained and the mobile phase is allowed to leave the chamber, which amounts to reducing the pressure of this mobile phase.
• a flow regulation is carried out leaving the mobile phase so that the measured pressure (s) of this mobile phase remains (are) substantially between the associated limit pressure (s) ( s) and a minimum pressure, throughout the duration of the treatment.
• the external pressure is applied to the stationary phase by a fluid means, preferably hydraulic. But of course, other modes of application can be envisaged, in particular by mechanical or pneumatic means.
• the stationary phase with a mobile phase, before implanting the sample.
• This supply consists of filling the stationary phase with a selected volume. Evacuation of the mobile phase from the chamber is therefore prohibited during this feeding phase.
• the volume of mobile phase which is admitted into the chamber corresponds approximately to the total volume of the stationary phase when the pressure measured is substantially equal to the limit pressure.
• the flow regulation means advantageously comprise a control module coupled to a valve as well as to means for measuring the pressure of the mobile phase upstream and / or downstream of the chamber.
• the invention also relates to devices in which the flow regulation means only comprise a valve for regulating the flow rate of the mobile phase in the chamber, this valve being controlled either manually or by a programmable control module.
• the chamber treated only one or more stationary phases placed next to each other on a same support.
• the chamber can be adapted to receive several stationary phases stacked one on the other, with or without support, and used in series or in parallel, with or without interlayer.

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