Method for measuring the pour point of a liquid body, and system for measuring the pour point of a liquid body
Patent Information
- Authority / Receiving Office
- EP · EP
- Patent Type
- Applications
- Current Assignee / Owner
- TOTALENERGIES ONETECH
- Filing Date
- 2023-08-02
- Publication Date
- 2026-06-10
AI Technical Summary
Current methods for measuring the flow point of liquids are manual, slow, unreliable, and not reproducible, and lack automation and precision, particularly at the micro-scale, where microfluidics could provide more accurate and efficient analysis.
A method using a microfluidic chip with microcanals to contact a liquid body with gas at a predetermined pressure and temperature, measuring the interface movement to determine the flow point, allowing for automated, precise, and reproducible measurements without the need for continuous operator intervention.
Enables rapid, reliable, and repeatable measurement of flow points on a micro-scale, reducing measurement time and volume usage while increasing statistical significance and adaptability to various fluid formulations.
Smart Images

Figure FR2023051233_06022025_PF_FP_ABST
Abstract
Description
Description TITLE: METHOD FOR MEASURING THE FLOW POINT OF A LIQUID, AND SYSTEM FOR MEASURING THE FLOW POINT OF A LIQUID technical field
[0001] The invention relates to the field of microfluidics. In particular, the invention relates to a method for measuring the flow point of a liquid body.
[0002] The invention further relates to a system for measuring the flow point of a liquid body. Previous technique
[0003] Below, we describe the known prior art from which the invention was developed.
[0004] To measure the pour point of a liquid body, the ASTM D97 standard is known, and in particular the ASTM D97-2022 standard.
[0005] In this standardized method, the sample is placed in a temperature-controlled (cold) bath and allowed to cool. Every 3 degrees Celsius, the sample is removed and the bottle is inverted a maximum of 90° (horizontally). The operator then observes whether the fluid flows under its own weight; the stress experienced by the liquid is therefore proportional to the liquid's density, the bottle's diameter, and gravity. The pour point is defined as the temperature at which the fluid no longer flows.
[0006] The main drawbacks of such a method, although standardized, lie particularly in its slowness and the need for a full-time operator. The operator manually checks whether the fluid is flowing or not at regular temperature intervals. Furthermore, such a manual, operator-centric method is therefore unreliable, inconsistent, and difficult to repeat.
[0007] Currently, there is no standardized method or measurement method for automated measurements of a fluid flow point.
[0008] Microfluidics allows the study of fluid behavior in microchannels. A fluid can be classified as simple or complex, single-phase or multiphase. Thus, it is possible to study fluids and, in particular, to perform fluid analysis. at the micrometric scale. In particular, at this scale, the study of fluids is facilitated.
[0009] To achieve micrometric dimensions, microfluidic chips have emerged. They consist of interconnected microchannels designed to perform a specific function. These microchannels are linked at the macroscopic level using input and output ports. The current diversity of these chips lies in the design of the microchannels and, in particular, in the materials used (glass, polymer, silicon). However, limitations exist regarding fluid manipulation capabilities and the design of complex chips, such as those integrated into systems or with variable geometry.
[0010] Documents have revealed the usefulness of microfluidics in the characterization of fluids.
[0011] For example, document EP3047101 proposes a system for detecting the wax-appearance temperature (WAT) of a hydrocarbon fluid sample. However, this document does not address the fluid's behavior, and in particular its pour point.
[0012] Similarly, document WO2022129400 proposes a temperature control system for a microfluidic chip incorporating a Peltier module. Temperature can be a key parameter in determining the pour point of a fluid. However, this document does not provide a means of measuring a fluid's pour point.
[0013] Document EP2954344 proposes a microfluidic device for parallelizing pressure-volume-temperature analysis, allowing for separate analysis of pressure, temperature, and volume. While this document enables parallel measurements, it does not allow for automated measurement of a flow point.
[0014] Finally, document EP2384429 proposes a microfluidic device for regulating fluid movement within channels. This movement is controlled by a valve, enabling the microfluidics to be linked to nucleic acid sequencing. However, this document makes no mention whatsoever of the flow point, let alone its measurement.
[0015] Thus, current methods only consider the macroscopic scale for measuring a flow point. Furthermore, these methods require an operator, involve numerous manipulations that can alter the results, offer limited precision, and involve relatively long measurement times. Moreover, current developments in microfluidics, while capable of achieving the precision of their respective scales, do not yet allow for the measurement of a fluid's flow point, nor do they enable the automation and parallelization of measurements. Indeed, microfluidics focuses on the analysis of fluids in various fields.
[0016] Thus, there is a need for new methods of measuring a flow point at the micrometric scale that are automated, parallelized, accurate and reproducible while avoiding the presence of an operator and particularly long measurement times, (compared to the ASTM D97 standard).
[0017] The invention aims to overcome the drawbacks of the prior art. In particular, the invention aims to provide a method for measuring a flow point, said method being automated, fast, reliable, reproducible, repeatable, and allowing measurement of a flow point at the micrometer scale while avoiding the continuous presence of an operator. Summary of the invention
[0018] The invention aims to overcome these drawbacks. The following presents a simplified summary of selected aspects, embodiments, and examples of the present invention in order to provide a basic understanding of the invention. However, this summary does not constitute an exhaustive overview of all aspects, embodiments, and examples of the invention. Its sole purpose is to present selected aspects, embodiments, and examples of the invention in a concise form as an introduction to the more detailed description of the aspects, embodiments, and examples of the invention that follows the summary.
[0019] The invention relates in particular to a method for measuring the flow point of a liquid body implementing at least one microfluidic chip comprising at least one microchannel, said measurement method comprising: - A step of bringing the liquid body into contact with a gas within at least one microchannel so as to form a liquid / gas interface; the gas being at a predetermined pressure and the liquid body being at an injection temperature, A step of measuring the movement of the interface, as a function of at least one predetermined temperature and at least one strain pressure; A step of determining the flow point of the liquid body as a function of at least one predetermined temperature and an evolution of the movement of the interface during the step of measuring the movement of the interface.
[0020] The applicant has developed a method for measuring the flow point of a liquid body by taking into consideration microfluidics.
[0021] Such a method makes it possible to determine the pour point of a liquid. Furthermore, such a measurement method is capable of meeting the needs of the field. In particular, a measurement method according to the invention is reliable, reproducible, and repeatable. It allows for parallel and automated measurements without operator intervention. Moreover, a method according to the invention is precise. Such a method eliminates the need for an operator. Furthermore, the method improves predictive accuracy by increasing the statistical power of the measurements. Such a method according to the invention therefore allows for obtaining statistically significant results. A method according to the invention is also faster because it allows for multiple measurements to be performed in a single operation.
[0022] Thus, a method according to the invention makes it possible to monitor the evolution of an interface. Furthermore, such a method reduces the volume of material used compared to the standardized method. The method ensures the relevance and robustness of the measurements while being adaptable to all formulations.
[0023] Advantageously, such a method can also be used to measure other parameters such as precipitation and / or crystallization.
[0024] Depending on other optional characteristics of the method, the latter may optionally include one or more of the following characteristics, alone or in combination: - the liquid substance is selected from a pure liquid, a mixture of liquids, a liquid solution, a dispersion and / or a mixture thereof, - the injection temperature is selected from ambient temperature, a temperature between the solidification temperature of the liquid substance and the boiling point of the liquid substance, - the contact stage includes a gas injection stage, - The gas injection stage is carried out in co-current, counter-current, or perpendicular flow to the liquid body flow. - the gas is selected from among rare gases, air, CO2, nitrogen, sulfur hexafluoride, and / or a mixture thereof, - The motion measurement step includes a gas injection shutdown step, - The motion measurement step includes a temperature modification step until a predetermined temperature is reached. - The temperature modification step includes cooling or heating the microfluidic chip and / or at least one microchannel to reach at least one predetermined temperature, - at least one predetermined temperature is lower or higher than the injection temperature, - at least one predetermined temperature is a temperature gradient, - at least one predetermined temperature is a constant temperature, - The interface motion measurement step includes a gas reinjection step, - the gas reinjection step is carried out at a strain pressure, preferably at constant pressure, - the interface motion measurement step includes at least one step of measuring the evolution of the interface; the interface evolution measurement step includes at least one comparison of the interface revolution as a function of at least one predetermined temperature. - The motion measurement step of the interface is selected from optical detection, electrical detection, thermal detection and / or acoustic detection, - The step of measuring interface movement is repeated until a comparison of interface evolution includes a measurement of the absence of interface evolution, - The pour point determination step includes measuring the absence of change at the liquid / gas interface, - the pour point determination step is selected from optical detection, electrical detection, thermal detection and / or acoustic detection.
[0025] According to a second object, the invention relates to a flow point measurement system comprising: At least one microfluidic chip comprising at least one microchannel configured to bring a liquid body and a gas into contact at a predetermined injection temperature and pressure, said at least one microchannel being further configured to convey a liquid / gas interface at at least a predetermined temperature and strain pressure, - At least one thermalization element configured to impose at least one predetermined temperature on said microfluidic chip or at least one microchannel, - At least one interface motion detection device configured to measure interface changes, - At least one pour point determination device configured to measure the pour point of the liquid body.
[0026] A system according to the invention makes it possible to measure a flow point.
[0027] A microfluidics-based flow point measurement system allows for the determination of a liquid's flow point with precise, reliable, reproducible, and repeatable measurements. Such a system enables parallel and automated measurements without operator intervention. Furthermore, the system according to the invention eliminates the need for an operator. The system also improves predictive accuracy by enhancing the statistical power of the measurements, thus yielding statistically significant results. The system according to the invention allows for faster measurement acquisition because it enables multiple measurements to be performed in a single operation.
[0028] Thus, a system according to the invention makes it possible to monitor the evolution of an interface. Furthermore, it reduces the space required compared to existing systems. The system according to the invention ensures the relevance and robustness of the measurements while... being suitable for all formulations.
[0029] Advantageously, such a system can also allow the measurement of other parameters such as precipitation and / or crystallization.
[0030] Depending on other optional system features, the system may optionally include one or more of the following features, alone or in combination. - at least one input is configured to include a liquid injection device and / or a gas injection device, - the gas injection device is configured to be arranged in co-current, counter-current or perpendicular flow to the flow of the liquid injection device, - at least one microchannel is configured to be wider than it is narrow, - at least one microchannel is configured so that its width is strictly greater than its height, - at least one microchannel is configured so that its length is strictly greater than its width. Brief description of the drawings
[0031] Other features and advantages of the invention will be better understood from the description that follows and with reference to the attached drawings, given for illustrative purposes only and not for limitation.
[0032] [Fig. 1] Figure 1 represents a diagram of a method for measuring a flow point according to an embodiment of the invention.
[0033] [Fig. 2] Figure 2 represents a diagram of a contacting step according to one embodiment of the invention.
[0034] [Fig. 3] Figure 3 represents a diagram of a motion measurement step according to one embodiment of the invention.
[0035] [Fig. 4] Figure 4 represents a diagram of a point measurement system flow according to an embodiment of the invention.
[0036] [Fig. 5] Figure 5 represents a diagram of a flow point measurement system according to one embodiment of the invention.
[0037] [Fig. 6] Figure 6 represents a diagram of a flow point measurement system according to one embodiment of the invention.
[0038] [Fig. 7A] Figure 7A represents a movement of an interface at constant temperature.
[0039] [Fig. 7B] Figure 7B represents a movement of an interface along a temperature gradient.
[0040] [Fig. 8A] Figure 8A represents a graph of an implementation of a step-by-step temperature change, the predetermined temperature being a constant temperature.
[0041] [Fig. 8B] Figure 8B represents a graph of one embodiment of a constant temperature change, the predetermined temperature being a temperature gradient.
[0042] The figures do not necessarily respect scales, particularly in thickness, for illustrative purposes.
[0043] Aspects of the present invention are described with reference to flowcharts and / or functional diagrams of processes, devices (systems) according to embodiments of the invention.
[0044] In the figures, flowcharts and functional diagrams illustrate the architecture, functionality, and operation of possible implementations of systems and processes according to various embodiments of the present invention. In this regard, each block in the flowcharts or block diagrams can represent a system, device, or module for implementing the specified function(s). In some implementations, the functions associated with the blocks may appear in a different order than that shown in the figures. For example, two blocks shown successively may, in fact, be executed substantially simultaneously, or the blocks may sometimes be executed in reverse order, depending on the functionality involved. Description of the implementation methods
[0045] Below, we describe a summary of the invention and the associated vocabulary, before presenting the disadvantages of the prior art, and finally showing in more detail how the invention remedies them.
[0046] The expression "predetermined pressure" can correspond to a pressure equal to, greater than, or less than the strain pressure.
[0047] The expression "injection temperature" can refer to a temperature equal to, above, or below a predetermined temperature.
[0048] The term "fluid" in the context of the invention can refer to a gas and / or a liquid.
[0049] The term "liquid" in the context of the invention refers to any body capable of flowing under its own weight.
[0050] The invention proposes to address the drawbacks of current methods for measuring a flow point. In particular, the invention proposes a method for measuring the flow point of a liquid. To this end, the invention proposes the implementation of microfluidics.
[0051] Thus, the invention relates to a method for measuring the flow point of a liquid body using at least one microfluidic chip comprising at least one microchannel. The invention is not limited by the size of a microfluidic chip or by the number of microchannels. A method for measuring a flow point can be illustrated with reference to Figure 1.
[0052] A method for measuring 100 of a flow point of a liquid body 2 implementing a microfluidic chip 10 comprising at least one microchannel 1 may include a step of contacting a liquid body 2 with a gas 3, a motion measurement step 120 and a step of determining 130 of the flow point of the liquid body 2.
[0053] Furthermore, a method for measuring 100 of a flow point of a liquid body 2 may include a preparation step 105 of a liquid body 2, a temperature control step 140, a pressure control step 150, a time measurement step 160.
[0054] A method for measuring 100 the pour point of a liquid body 2 may include a preparation step 105 of a liquid body 2. A preparation step 105 of a liquid body 2 may be implemented using glassware and / or means commonly used in the field.
[0055] A preparation step 105 of a liquid body 2 may include any means of obtaining a liquid. Preferably a liquid body at ordinary pressure and temperature, that is to say, more preferably at atmospheric pressure and ambient temperature.
[0056] Furthermore, a preparation step 105 of a liquid body 2 may include a mixing step of at least two liquids, at least one liquid and a gas, at least one liquid and a solid, at least one gas and a solid, at least two gases, or at least two solids. Thus, a liquid body 2 may be simple, i.e., comprising a single element (a gas, a solid, or a liquid), or complex, i.e., comprising at least two elements (identical or different). The invention is not limited by the number of elements present in the liquid body 2; however, and preferably, a liquid body 2 comprises at most 100 elements.
[0057] Thus, a preparation step 105 of a liquid substance 2 may include melting, liquefaction, or sublimation followed by liquefaction and / or condensation followed by melting, or any other reaction that yields a liquid. Obviously, if the liquid substance 2 is already in a liquid state, it is not necessary to implement a step to obtain a liquid. Furthermore, a preparation step 105 of a liquid substance may include a mixing step, preferably when the liquid substance 2 is complex. Thus, preferably, a liquid substance may be selected from a pure liquid, a mixture of liquids, a liquid solution, a dispersion (suspension, emulsion, foam), and / or a mixture thereof.
[0058] Furthermore, the invention is not limited by the type of substance as long as it is liquid. For example, a substance can be selected from a material, water, hydrocarbon, biological matter, gas (preferably CO2), bacterial suspension, food product, cosmetic product, and / or construction product.
[0059] A preparation step 105 of a liquid body 2 allows obtaining a body in its liquid form.
[0060] A method for measuring 100 of a flow point of a liquid body 2 can understand a step of bringing the liquid body 2 into contact with at least one gas 3, preferably with a gas 3. A step of bringing into contact 110 can be illustrated in relation to figure 2.
[0061] A contacting step 110 allows a liquid-gas or gas-liquid interface 4 to be formed preferably between the liquid body 2 and the gas 3. It should be noted that the expressions liquid / gas interface or gas / liquid interface in the sense of the present invention can be used similarly.
[0062] A contacting step 110 may include an injection step 111 of the liquid body 2 at an injection temperature, preferably into the microfluidic chip 10 and more preferably at at least one inlet 5 configured to receive a liquid body 2. The injection step 111 of the liquid body 2 allows the introduction of a liquid body 2 into the microfluidic chip 10, preferably into at least one microchannel 1. Advantageously, an injection temperature may be ambient temperature or a temperature between the solidification temperature of the liquid body and its boiling point. Preferably, the injection temperature is a constant temperature.
[0063] A contacting step 110 may include a homogeneity check step 112 of the liquid body, preferably in the case of a complex liquid body 2. Such a check may be selected from optical detection, electrical detection, thermal detection and / or acoustic detection.
[0064] A contacting step may include an injection step 113 of at least one gas 3, preferably at a predetermined pressure and preferably into the microfluidic chip 10, preferably into at least one microchannel 1 and more preferably at at least one inlet 5 configured to receive at least one gas 3. Advantageously, a predetermined pressure may correspond to a pressure enabling the injection of the gas 3. For example, a predetermined pressure may be at least 5 mbar, preferably at least 50 mbar. Alternatively, a predetermined pressure may be at most 10 bar, preferably at most 5 bar. A predetermined pressure may, for example, be selected from values ranging from 5 mbar to 10 bar, preferably ranging from 50 mbar to 5 bar.Preferably, the gas 3 injection step 113 is carried out at controlled pressure, preferably at constant pressure and even more preferably at atmospheric pressure (for example close to 1 bar at atmospheric pressure + / - 15% i.e. about 2 bar absolute pressure). However, those skilled in the art will know that such a predetermined pressure can be adjusted according to the viscosity of the liquid, the length of at least one microchannel 1, the material(s) constituting the chip 10, the geometry of at least one microchannel 1, etc. The gas injection step 113 introduces a gas 3 into the microfluidic chip 10, preferably into at least one microchannel 1. This gas injection step 113 can be carried out co-currently, counter-currently, or perpendicularly to the flow of the liquid 2.
[0065] Furthermore, a gas 3 can be selected from among a non-reactive (i.e. inert) gas with the liquid body 2. Preferably, a gas 3 that is little or not at all miscible with the liquid body 2. For example, a gas 3 can be selected from among noble gases (Helium, Neon, Argon, Krypton, Xenon, Radon), air, CO2, nitrogen, sulfur hexafluoride, and / or their mixture.
[0066] A contacting step 110 may also include a liquid / gas interface formation verification step 114. A liquid / gas interface formation verification step 114 may be selected from: electrical detection, optical detection, thermal detection and / or acoustic detection.
[0067] A method for measuring 100 the flow point of a liquid body 2 may include a step for measuring the motion 120 of the interface 4, preferably as a function of at least one predetermined temperature and at least one strain pressure. A step for measuring the motion 120 of the interface 4 may be illustrated in relation to Figure 3.
[0068] A motion measurement step 120 may include a gas injection stop step 121 3. This allows a location of the interface 4 to be defined.
[0069] A motion measurement step 120 may include a temperature modification step 122, preferably of the injection temperature, until a predetermined temperature is reached. A predetermined temperature may be greater than, less than, or equal to the injection temperature, preferably less than or greater than the injection temperature. Thus, a temperature modification step 122 may allow cooling, heating, or holding at temperature of at least one microchannel 1 and / or the microfluidic chip 10 so as to reach a predetermined temperature. A constant temperature may correspond to a precise temperature value as opposed to a temperature gradient, which may correspond to a temperature range (i.e., set of values). Furthermore, a temperature modification step 122 may be a constant or gradient modification of The temperature. Thus, a predetermined temperature can be a temperature gradient or a constant temperature. Advantageously, a predetermined temperature can be determined by successive trials up to the determination step 130 of the pour point of the liquid body 2. Furthermore, in a particular but non-limiting embodiment of the invention, the aging of liquid bodies 2 whose structure changes over time can also be studied (i.e., freezing at the same injection temperature). An example of a temperature modification step 122 until a predetermined temperature is reached can be illustrated with reference to Figure 8A or 8B. In Figure 8A, the temperature is modified in steps; the predetermined temperature then corresponds to a constant temperature. In Figure 8B, the temperature is modified constantly; the predetermined temperature then corresponds to a temperature gradient.
[0070] Advantageously, a motion measurement step 120 can include a latency step 123 until stabilization of the modified temperature (at least one predetermined temperature is reached).
[0071] A motion measurement step 120 of interface 4 may include a gas reinjection step 124 of gas 3, preferably after the latency step 123. This allows motion to be created or not in at least one microchannel 1 of interface 4, preferably depending on the temperature change. Advantageously, the motion measurement step 120 and, preferably, the gas reinjection step 124 of gas 3 may be operated at a strain pressure. A strain pressure may be a constant pressure. A strain pressure may be greater than, less than, or equal to a predetermined pressure. Advantageously, the strain pressure may be close to (i.e., less than 15% variation, preferably less than 10% variation) a pressure standardized according to ASTM D97, and preferably ASTM D97-2022. Preferably, the strain pressure is a function of the stress at interface 4, for example ranging from 10 to 1000 Pa
[0072] The motion measurement step 120 may include at least one step 125 of at least one measurement of the evolution of interface 4. For the purposes of this invention, evolution means movement, i.e., displacement or the absence of displacement. Preferably, step 125 of at least one measurement of the evolution of interface 4 may include at least one comparison 126 of the evolution of interface 4 as a function of the modified temperature and strain pressure, preferably as a function of the modified temperature and, more preferably, as a function of the modified temperature until the predetermined temperature is reached. The comparison may be performed by relationship to the displacement of interface 4 between each gas injection step 3 and as a function of the modified and / or predetermined temperature.
[0073] For example, at the start of the measurement method, interface 4 is formed during the contact step 110. Then, during the measurement step, the gas injection is stopped and the temperature is adjusted until a predetermined temperature is reached. The movement or lack of movement of interface 4 is then determined. The movement measurement step 120 of interface 4 can be selected from optical, electrical, thermal, and / or acoustic detection.
[0074] Furthermore, the motion measurement step 120 of interface 4 can be repeated OK until the comparison step 126 of the evolution of interface 4 includes a measurement of the absence NOK of evolution of interface 4. The comparison can be carried out by optical detection, electrical detection, thermal detection and / or acoustic detection.
[0075] Thus, the motion measurement step 120 of interface 4 may include, as disclosed above, a gas injection stop step 121 and a gas injection reinjection step 124 at each new motion measurement 120 of interface 4. Also, the motion measurement step 120 of interface 4 may include a temperature change step, or a predetermined temperature change step, at each new motion measurement of interface 4. Therefore, the motion measurement step 120 of interface 4 may include a temperature change, preferably from a predetermined temperature, until a new predetermined temperature is reached at each new motion measurement of interface 4. Advantageously, the latency step 123 is also repeated for each new motion measurement of interface 4.
[0076] An example can be illustrated in relation to Figure 7A or Figure 7B.
[0077] A method for measuring 100 of a flow point of a liquid body 2 may include a step of determining 130 the flow point of the liquid body 2, preferably as a function of at least a predetermined temperature and the evolution of the movement of the interface 4 during the step of measuring the movement 120 of the interface 4.
[0078] The determination step 130 can also be a function of the strain pressure. A determination step 130 of the flow point of the liquid body 2 can also be illustrated in relation to Figure 3.
[0079] A determination step 130 of the flow point of the liquid body 2 may include a measurement step of the absence of movement and preferably, of the absence of evolution 131, of the interface 4. Advantageously, the determination step 130 of the flow point of the liquid body 2 may be selected from optical detection, electrical detection, thermal detection and / or acoustic detection.
[0080] Again, an example can be illustrated in relation to Figure 7A or Figure 7B.
[0081] Optical detection can be selected from: refraction, reflection or diffraction of a light source (e.g., diiodine, laser, monochromatic or polychromatic light), video analysis, image analysis (by difference or correlation), or colorimetry.
[0082] Electrical detection can be selected from: measurement of resistance, capacitance, impedance or conductivity at zero frequency or at a finite frequency.
[0083] Thermal detection can be selected from: infrared absorption or emission, thermocouple, thermal conductivity, specific heat, thermal resistance.
[0084] Acoustic detection can be selected from: ultrasound, attenuation, re-election, selection or diffraction of a sound or ultrasonic signal, reverberation, sound resonance.
[0085] In addition, optical, thermal, electrical and / or acoustic detection can be continuous and / or local (point).
[0086] Returning to Figure 1, a method for measuring the flow point of a liquid 2 may include a temperature control step. This temperature control step can be implemented by any means that allows for temperature control, for example, a Peltier assembly, a Peltier element, a temperature probe, and / or a thermostatic bath. Furthermore, the temperature may correspond to the injection temperature, the modified temperature, and / or the predetermined temperature.
[0087] A method for measuring the flow point of a liquid body may also include a pressure control step. A pressure control step can be implemented by any means that allows the pressure to be controlled. For example, a pressure controller linked to a pressure sensor. Furthermore, the pressure can correspond to the predetermined pressure and / or the strain pressure.
[0088] A method 100 for measuring the flow point of a liquid body 2 may also include a time measurement step 160. This time measurement step 160 is preferably carried out between the motion measurement step 120 of the interface 4 and the flow point determination step 130 of the liquid body 2. This allows for a more precise method 100. It also allows for a more precise determination of the pressure and / or temperature application times. Furthermore, such a step 160 can be implemented using any means for measuring time, for example, a stopwatch, a clock, or preferably an electronic clock.
[0089] Furthermore, and quite advantageously, the measurement method 100 for the flow point of a liquid 2 can preferably be repeated for the same liquid 2. This ensures the accuracy, reproducibility, and repeatability of the method. For example, the method 100 can be repeated 1 to 3 times, preferably 1 to 5 times, and most preferably 1 to 10 times. Advantageously, the method can be accurate, reproducible, and repeatable even without repeated repetition. This is because the method allows for multiple measurements at different temperatures to be performed in a single operation. Similarly, the measurement method allows for multiple measurements at different temperatures to be performed and each of these measurements to be replicated in a single operation.
[0090] Advantageously, a method for measuring the flow point of a liquid can be automated. This also saves time and eliminates the need for an operator.
[0091] Advantageously, a method for measuring 100 of a flow point of a liquid body can be a parallelized method.
[0092] A measurement method according to the invention allows for increasing the statistical accuracy of measurements and consequently their predictive power. A method according to the invention also allows for performing several tests at different temperatures in a single operation. A method according to the invention allows for performing several measurements at different temperatures and replicating each of these measurements in a single operation.
[0093] According to another aspect, the invention relates to a system for measuring the flow point of a liquid body.
[0094] A system for measuring the flow point of a liquid body can be illustrated in relation to Figure 4, 5 or 6.
[0095] A 200 system for measuring the flow point of a liquid body may include a 10 microfluidic chip.
[0096] A microfluidic chip 10 can be configured to include at least one microchannel 1 configured to bring a liquid body 2 and a gas 3 into contact. A microchannel 1 can be configured to carry a liquid / gas interface 4 according to at least one modified and / or predetermined temperature and / or according to at least one predetermined pressure and / or a strain pressure.
[0097] A microfluidic chip 10 can be configured to include at least one inlet 5. An inlet 5 can be configured to introduce a liquid 2 and / or a gas 3 into said microfluidic chip 10, preferably into at least one microchannel 1. Advantageously, an inlet 5 can be configured to include a liquid 2 injection device 51. Advantageously, an inlet 5 can be configured to include a gas 3 injection device 52. A gas 3 injection device 52 can be configured to be arranged co-current, counter-current, or perpendicular to the flow of the liquid 2 injection device 51.
[0098] A microfluidic chip 10 can be configured to include at least one output 6. An output 6 can be configured to discharge a liquid 2 and / or a gas 3 from the microfluidic chip 10.
[0099] A microfluidic chip 10 can be configured to include at least one microchannel 1, preferably at least two microchannels 1, preferably at least five microchannels 1, and even more preferably at least ten microchannels 1. A microfluidic chip 10 can be configured to include at most 1000 microchannels 1, preferably at most 800 microchannels 1, and preferably at most 500 microchannels 1. A microfluidic chip 10 can be configured to include between 1 and 1000 microchannels 1, preferably between 2 and 800 microchannels 1, preferably between 5 and 500 microchannels 1, and even more preferably between 10 and 500 microchannels 1.
[0100] Furthermore, at least one microchannel 1 can be configured to be wider than it is thin (i.e., wider than it is thick, with a thickness less than its width). Preferably, the width-to-height ratio can be greater than or equal to 0.1. The width-to-height ratio can be less than or equal to 20, preferably less than or equal to 10. In addition, at least one Microchannel 1 can be configured so that its width is strictly greater than its height. At least one microchannel 1 can be configured so that its length is strictly greater than its width.
[0101] At least one microchannel 1 can be configured to include at least one injection hole 53 (Figure 6), preferably at least one injection hole 53 is configured to be arranged perpendicular to the flow of the liquid body 2.
[0102] In a particular but non-limiting embodiment of the invention, at least one microchannel 1 can be configured to be arranged in a straight line between at least one input 5 and at least one output 6.
[0103] In a particular but non-limiting embodiment of the invention, a microfluidic chip 10 can be configured to include n microchannels 1, said microchannels 1 being able to be configured to be arranged in a straight line between at least one inlet 5 and at least one output 6 and in parallel with each other and / or equidistant from each other or two by two.
[0104] Furthermore, a microfluidic chip 10 is not limited within the meaning of the invention by its dimensions.
[0105] A microfluidic chip 10 can be disposable or reusable.
[0106] A flow point measurement system of a liquid body 2 may include at least one thermalization element 7. A flow point measurement system of a liquid body may include at most 4 thermalization elements 7. A flow point measurement system of a liquid body may include between at least one thermalization element and at most 4 thermalization elements 7, preferably between at least one thermalization element 7 and at most 3 thermalization elements 7, and more preferably between at least one thermalization element 7 and at most 2 thermalization elements 7. At least one thermalization element 7 may be configured to impose at least one predetermined temperature on the microfluidic chip 10 and / or on at least one microchannel 1 and / or to modify at least one temperature, preferably at least one predetermined temperature.A thermalization element 7 can be selected from: a Peltier element, a Peltier assembly, liquid nitrogen and / or a thermostatically controlled bath.
[0107] A 200-unit system for measuring the flow point of a liquid body may include at least one 11-unit motion detection device for the interface 4. A The motion detection device 11 for interface 4 can be configured to measure the evolution of interface 4. A motion detection device 11 for interface 4 can be selected from an optical detector, an electrical detector, a thermal detector and / or an acoustic detector.
[0108] A system 200 for measuring the flow point of a liquid body may include at least one device 14 for determining the flow point of a liquid body. At least one device 14 for determining the flow point of a liquid body may be configured to measure the flow point of a liquid body. A device 14 for determining the flow point of a liquid body may be selected from an optical detector, an electrical detector, a thermal detector, and / or an acoustic detector.
[0109] In a non-limiting embodiment of the invention, the motion detection device 11 of the interface 4 and the flow point determination device 14 of a liquid body 2 are configured to be common or separate.
[0110] A system 200 for measuring the flow point of a liquid body may include a control device 13 for the homogeneity of the liquid body 2. A control device 13 for the homogeneity of a liquid body 2 may be configured to check the homogeneity of a liquid body 2, preferably when a liquid body 2 is said to be complex within the meaning of the invention.
[0111] A 200 system for measuring the flow point of a liquid body may include a control device 12 of the interface 4. A control device 12 of the interface 4 may be configured to check the formation of a gas / liquid interface 4.
[0112] A system 200 for measuring the flow point of a liquid body may include a temperature control device 8. A temperature control device 8 may be configured to check and / or measure at least one injection temperature and / or at least one modified temperature and / or at least one predetermined temperature.
[0113] A system 200 for measuring the flow point of a liquid body may include a pressure control device 9. A pressure control device 9 may be configured to check and / or measure at least a predetermined pressure and / or a strain pressure.
[0114] The invention can be adapted into numerous variations and applications other than those described above. In particular, unless otherwise indicated, the various structural and functional characteristics of each of the implementations described above should not be considered as combined and / or closely and / or inextricably linked to one another, but rather as mere juxtapositions. Furthermore, the structural and / or functional characteristics of the various embodiments described above may be juxtaposed or combined, in whole or in part, in any different manner.
Claims
Claims 1. Method for measuring (100) a flow point of a liquid body (2) using at least one microfluidic chip (10) comprising at least one microchannel (1), said measuring method (100) comprising: A step of bringing (1 10) the liquid body (2) into contact with a gas (3) within the at least one microchannel (1) so as to form a liquid / gas interface (4); the gas (3) being at a predetermined pressure and the liquid body (2) being at an injection temperature, A step of measuring movement (120) of the interface (4), as a function of at least one predetermined temperature and at least one constraint pressure; A step of determining (130) the flow point of the liquid body (2) as a function of at least one predetermined temperature and a change in movement of the interface (4) during the step of measuring movement (120) of the interface (4).
2. Measuring method (100) according to claim 1 characterized in that the liquid body (2) is selected from a pure liquid, a mixture of liquids, a liquid solution, a dispersion and / or their mixture.
3. Measuring method (100) according to claim 1 or 2 characterized in that the injection temperature is selected from an ambient temperature, a temperature between a solidification temperature of the liquid body (2) and a boiling temperature of the liquid body (2).
4. Measuring method (100) according to one of the preceding claims, characterized in that the contacting step (110) comprises a step of injecting (113) a gas (3).
5. Measuring method (100) according to claim 4 characterized in that the gas injection step (113) is carried out co-currently, counter-currently, or with a current perpendicular to the flow of the liquid body (2).
6. Measuring method (100) according to one of the preceding claims, characterized in that the gas (3) is selected from rare gas, air, CO2, nitrogen, sulfur hexafluoride, and / or their mixture.
7. Measuring method (100) according to one of the preceding claims, characterized in that the movement measuring step (120) comprises a step of stopping (121) the injection of gas (3).
8. Measuring method (100) according to one of the preceding claims, characterized in that the movement measuring step (120) comprises a step of modifying (122) the temperature until reaching at least one predetermined temperature.
9. Measuring method (100) according to claim 8 characterized in that the step of modifying (122) the temperature comprises cooling or heating the microfluidic chip (10) and / or the at least one microchannel (1) so as to reach the at least one predetermined temperature.
10. Measuring method (100) according to one of the preceding claims, characterized in that the at least one predetermined temperature is lower or higher than the injection temperature.
11. Measuring method (100) according to one of the preceding claims, characterized in that the at least one predetermined temperature is a temperature gradient.
12. Measuring method (100) according to one of the preceding claims, characterized in that the at least one predetermined temperature is a constant temperature.
13. Measuring method (100) according to one of the preceding claims, characterized in that the step of measuring (120) the movement of the interface (4) comprises a step of re-injecting (124) gas (3).
14. Measuring method (100) according to claim 13 characterized in that the step of reinjection (124) of gas (3) is carried out at a constraint pressure, preferably at constant pressure.
15. Measuring method (100) according to one of the preceding claims, characterized in that the step of measuring (120) the movement of the interface (4) comprises at least one step (125) of at least one measurement of the evolution of the interface (4).
16. Measuring method (100) according to claim 15 characterized in that the step of measuring the evolution (125) of the interface (4) comprises at least one comparison (126) of the evolution of the interface (4) as a function of at least one predetermined temperature.
17. Measuring method (100) according to one of the preceding claims, characterized in that the step of measuring movement (120) of the interface (4) is selected from optical detection, electrical detection, thermal detection and / or acoustic detection.
18. Measuring method (100) according to one of the preceding claims, characterized in that the step of measuring movement (120) of the interface (4) is repeated (OK) until a comparison (126) of the evolution of the interface (4) includes a measurement of the absence (NOK) of evolution of the interface (4).
19. Measuring method (100) according to one of the preceding claims, characterized in that the step of determining (130) the pour point comprises a measurement of the absence of evolution (131) of the liquid / gas interface (4).
20. Measuring method (100) according to one of the preceding claims, characterized in that the step of determining (130) the pour point is selected from optical detection, electrical detection, thermal detection and / or acoustic detection.
21. System (200) for measuring a pour point comprising: At least one microfluidic chip (10) comprising at least one microchannel (1) configured to bring a liquid body (2) and a gas (3) into contact according to a predetermined injection temperature and pressure, said microchannel (1) being further configured to convey a liquid / gas interface (4) according to at least one predetermined temperature and a constraint pressure, At least one thermalization element (7) configured to impose at least one predetermined temperature on said microfluidic chip (10) or on the at least one microchannel (1), At least one device (11) for detecting movement of the interface (4) configured to measure the evolution of the interface (4), - At least one pour point determination device (14) configured to measure the pour point of the liquid body (2).
22. System (200) for measuring a pour point according to claim 21 characterized in that the at least one microfluidic chip (10) comprises at least one inlet (5) configured to comprise a device (51) for injecting a liquid body (2) and / or a device (52) for injecting a gas (3).
23. System (200) for measuring a pour point according to claim 22 characterized in that the gas (3) injection device (52) is configured to be arranged in co-current, counter-current or perpendicular to the flow of the injection device (51) of a liquid body (2).
24. System (200) for measuring a pour point according to one of claims 21 to 23, characterized in that the at least one microchannel (1) is configured to be wider than thin.
25. System (200) for measuring a pour point according to one of claims 21 to 24, characterized in that the at least one microchannel (1) is configured so that its width is strictly greater than its height.
26. System (200) for measuring a pour point according to one of claims 21 to 25, characterized in that the at least one microchannel (1) is configured so that its length is strictly greater than its width.