EP3723907A1 - Systèmes et procédés d'essai et de manipulation de liquide automatisés - Google Patents

Systèmes et procédés d'essai et de manipulation de liquide automatisés

Info

Publication number
EP3723907A1
EP3723907A1 EP18888893.7A EP18888893A EP3723907A1 EP 3723907 A1 EP3723907 A1 EP 3723907A1 EP 18888893 A EP18888893 A EP 18888893A EP 3723907 A1 EP3723907 A1 EP 3723907A1
Authority
EP
European Patent Office
Prior art keywords
chamber
sample
pump
emulsion
measurement
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.)
Pending
Application number
EP18888893.7A
Other languages
German (de)
English (en)
Other versions
EP3723907A4 (fr
Inventor
Richard Nordman
Michael PONSTINGL
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Custom Sensors and Technology
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from US15/974,450 external-priority patent/US11154855B2/en
Application filed by Individual filed Critical Individual
Publication of EP3723907A1 publication Critical patent/EP3723907A1/fr
Publication of EP3723907A4 publication Critical patent/EP3723907A4/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/4105—Methods of emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/65—Mixers with shaking, oscillating, or vibrating mechanisms the materials to be mixed being directly submitted to a pulsating movement, e.g. by means of an oscillating piston or air column
    • B01F31/651—Mixing by successively aspirating a part of the mixture in a conduit, e.g. a piston, and reinjecting it through the same conduit into the receptacle
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/2131—Colour or luminescence

Definitions

  • This disclosure is related to the field of liquid extraction systems. More particularly to systems methods, and apparatus for performing liquid extraction and manipulation of a sample for testing and measurement.
  • an emulsion is a specific type of colloid, a multi-phase system of matter when two usually immiscible substances form a mixture. Unlike a solution, whose solute and solvent constitute a single phase, a colloid has a dispersed phase comprising suspended particles, and a continuous phase, comprising the medium of suspension.
  • An emulsion is a specific type of colloi d in which both substances are liquids, also known as a liquid-liquid mixture; that is, both the dispersed substance and the medium of dispersion are liquids.
  • the liquids may itself be a solution.
  • the oils (a liquid) are typically dispersed as small droplets throughout a water solution, such as water and acetic acid (also a liquid), which is the dispersion medium,
  • the dispersed substance is typically formed into small particles, which are distributed throughout the medium of dispersion, often with the aid of an emulsifier, which acts as a chemical mediator between the two immiscible substances, or through the application of force which breaks the dispersed substance into smaller“particles” and distributes them throughout the medium of dispersion.
  • an emulsifier which acts as a chemical mediator between the two immiscible substances, or through the application of force which breaks the dispersed substance into smaller“particles” and distributes them throughout the medium of dispersion.
  • M ixing (or remixing) of the dispersant into the medium may be performed through the application of a external force, such as mechanical agitation. Once this force is removed, however, the dispersed substance begins to separate from the medium of dispersion. This also can be seen with ordinary salad dressing, i which the oils will separate from the wafer over time, but are easily remixed via manual agitation by shaking the bottle,
  • Colloids an emulsions can present unique problems when present in chemical processes. Specifically, it is often desirable in the chemical and industrial arts to measure the respec tive dispersant to medium content, or other chemical property, of the emulsi on or a portion of the emulsion. It can be particularly valuable to do so in situ or near in situ and to do so with a sample from a moving environment such as fluid flowing through a pipeline or an industrial process.
  • a a simple example, crude oil and other materials present in an oil refinery or other processing facility for oils often comprise emulsifications of oil and water. As it is generally desired that the emulsifications he separated as part of the processing (or as pari of waste disposal) it can be valuable to determine the amount of water present in the emulsification to make sure this process is performe effectively and economically.
  • the process of separation can take time and for products such as crude oil the separation can result in residues being left in the measuring device or otherwise presenting a situation where the measuring instrument requires substantial cleaning between tests to avoid inaccurate calculations. This means that performing in situ measurements, or even
  • a device for handling a sample comprising: a pump; a pump chamber; and a valve arrangement wherein, the pump will provide a liquid sample from a sample source to the pump chamber, the liquid sample passing through the valve arrangement; wherein, while sa e sample is moving through the valve arrangement, a liquid additive is simultaneously pulled fro an additive source through the valve
  • the device further comprises : a mixing chamber, wherein the 1 mixture can be moved from the pump chamber to the mixing chamber through the valve arrangement by the pump, the mixfttre being agitated by the movement.
  • a mixing chamber wherein the 1 mixture can be moved from the pump chamber to the mixing chamber through the valve arrangement by the pump, the mixfttre being agitated by the movement.
  • an additional liquid additive is mixed into the mixture as it passes through the valve arrangement,
  • the ixture can be returned to the pump chamber .from the mixing chamber through the valve arrangement by the pump, the mixture being agitated by the movement.
  • a further additional liquid additi ve is mixed into the mixture as it passes through the valve arrangement from the mixing chamber to the pump chamber.
  • the liquid sample is an emulsion.
  • the measurement is performed on the liquid sample while the sample is an emulsion.
  • the liquid additive is a solvent separating a first immiscible from the emulsion.
  • the measurement is performed on the first immiscible.
  • the measurement is performed on what remains of the emulsion after the first Immiscible has been separated
  • the device further comprises: a mixing chamber, wherein first immiscible is moved from the sample chamber to the mixing chamber through the valve arrangement by the pump and what remains of the emulsion after the first immiscible Is left In the pump chamber.
  • the first immiscible is then exhausted from the system and the remains of the emulsion after the first immiscible is separated is moved to the mixing chamber by the pump.
  • the remains of the emulsion after the first immiscible is separated is mixed with an additional additive from the valve arrangement as it is moved to the mixing chamber by the pump.
  • the remains of the emulsion after the first immiscible Is separated is then exhausted from the system and the first immiscible is moved to the pump chamber by the pump.
  • the first immiscible is mixed with an additional additive from the valve arrangement as It is moved to the pump chamber by the pump,
  • the emulsion is an oil and water emulsion.
  • the additive is toluene
  • the measurement is a fluorescence measurement [033] In an embodiment of the device, the measurement is a light absorption measurement
  • FIG. .1 depicts a front perspective view of a first embodiment of a liquid handling system.
  • FIG. 2 depicts a front; plan view of the embodiment of FIG. 1.
  • FIG. 3 depicts a detail view of the stream switch ing valve system of the embodiment of FIG 1.
  • FIGS. 4A and 4B depict side elevation views of the embodiment of FIG. 1.
  • FIG. 4.4 shows connection panels in place while FIG. 4B has them removed.
  • FIG. 5 depicts a schematic diagram of an embodiment of a fluid valve suc h as can be used in the stream switching valve system of FIG. 3,
  • F IG. 6 depicts a schematic diagram of an embodiment of a regulator and syringe pump system.
  • FIG, 7 depicts a schematic diagram of an embodiment of a switching module according to the present disclosure for illustrating fluid flow
  • FIG, 8 depicts a chart of valve and piston positions of the device of FIGS. 1 through 4B according to an embodiment of a etho of handling liquid.
  • FIG. 9 depicts a chart of valve and piston positions of the device of FIGS. 1 through 4B according to an alternative embodiment of a method of handling liquid
  • FIG, 1:0 depicts a chart of valve and piston positions of the device of FIGS, I through 4B according to a embodiment of a method of cleaning the device.
  • FIG. 11 depicts a front perspective vie of a second embodiment of a liquid handling system which utilizes only a single pump, but two sample chambers.
  • FIG. 12 depicts a front perspective view of a second embodiment of a liqui handling system which utilize only a single pump an single sample chamber.
  • AES automated extraction systems
  • AES are generally configured to perform a fully automated liquid-liquid extraction, and to deliver the extract to an analysis cell either in a original mixed form or a separated form, generally having been mixed with an additive to assist in the analysis, although that is not required.
  • the AES will then also include traditional measurement or analysis tools attached thereto to perform an analysis on the extract such as, but not limited to, measuring the amount of a dispersant or other material in the mixture. Finally, an AES will generally be able to return the tested sample to the process stream, or dispose of it, an provide the results of the measurements performed to a computer or human for analysis,
  • Measurement on the extracted sample may be performed by, among other things, using an absorbance or fluorescence measurement to determine the concentration of the extracted solute within the sample. These type of measurements ma he performed by any type of testing or measurement instrument known now or later discovered and these
  • the AES may he used to allow the analysis on the extracted sample to occur prior to separation of components of an emulsion or similar composition, on an emulsion which has been allowed to separate naturally, or on an emulsion to which specific solvent or other additi ves have been added to induce stronger or faster separation.
  • the latter will generally be the preferred method of operation, however, the AES described herein allow for any and all of such actions to be performed on any sample and can be operated to provide different measurements on a sample in multiple different states based on the test to be performed
  • Embodiments of AES described herein will generally perform the: mechanical functions of extracting a sample fro a process en vironment and then manipulating that sample for testing. Often the sample will be withdrawn from a continuous flow (such as through a pipeline) hut that is not required an in alternative embodiments sample c an be taken from more static sources (such as, for example, settling tanks). As such, the AES will generally be mounted near a process line at which measurement will be performed.
  • the AES generally contains components required to operate the handling system and manipulate the sample and will commonly have mounted thereto a selection of apparatus to perform any absorbance, fluorescence, or other measurement oh the sample.
  • the system is designed to be mounted remotely in a non- hazardous location, or to be contained within a purged enclosure or other clean room suitable for the particular installation area.
  • the automatic extraction systems an methods described herein may be used to extract one or .more variable volume(s) of liquid samples from a process stream which Will generally have within it an emulsion, often of a petroleum or other oil and water such as can be the case with crude oil or similar materials.
  • the systems and methods ma also be used to add to this mixture one or more reagents or indicators. These ma be added both as the sample is withdrawn and later as the sample is manipulated depending on embodiment and foe testing to be performed. These reagents or indicators may provide a measurable reading of the component(s) of the process stream and/or to help separate or identify the components of the process stream.
  • toluene may be added to an oil and water mixture to help foe oil and water separate quickly and cleanly.
  • the systems and methods may also be used to dynamicall dilute one or more samples with a solvent, extract one or more components from a liquid sample, maintain or recreate a colloidal mixture, react one or more reagents with a sample (such as to form a color or a fluorescing tagged molecule), aeid/base titration, filter solids from a liquid sample, and other functions each with the ability to control various parameters in the process.
  • the systems and methods may he used with a
  • UV-ViS ultraviolet-visible spectroscopy or spectrophotometry
  • MR near-infrared optical spectrometer
  • pH electrode pH electrode
  • oxidatixm/reduction potential electrode conductivity electrode
  • temperature measuring device any number of other measuring devices or methods known in the art.
  • FIGS. 1 through 4B depict a first embodiment of an AES 101 in accordance with the present disclosure.
  • the depicted system 101 of FIGS. 1 through 4B utilizes two pumps and two sample chambers and is shown from a front perspective view in FIG. 1, a front- perspective view in FIG. 2, and in two different side views in FIGS 4A and 4B.
  • FIG. 3 provides a detail view of the stream switching valve system.
  • the depicted handling system 101 of FIGS, 1 through 4B comprises lour major component systems.
  • the depicted handling system 101 comprises a stream switching valve system 103, which is configured to direct and control fluid movement through various configurable .fluid paths through the system 101.
  • the depicted system 101 comprises a variable displacement yringe pump system 105 configured to meter fluid volumes and provide Hold propulsion within the system 101.
  • the depicted system 101 comprises two dif!erent sample chambers which are referred to as mixing chamber 10? and syringe pump chamber 108 which are used to perform liquid-liquid extraction (or emulsification) as well as mixing of the sample with various other chemicals.
  • the depicte system 101 comprises an analysis system 109 configured to perform measurement, such as using absorbance or fluorescence. Also shown in FIGS. 1 through 4R are connections for parts 111 for external instrumentation or other connections,
  • the stream switching valve system 103 comprises a modular component system 03 having one or more stream-select modules 113.
  • One or more of these stream-select modules 113 may comprise built-in pneumatic actuat.or(s) configured to introduce any one of a plurality of different fluids to the syringe pump System 105.
  • the stream switching val ve system 103 comprises a compact assembly of one or more stream-select modules 113.
  • the number of stream-select modules 113 is determined or selected based on the number of incoming fluid streams.
  • Each of the stream-select modules 113 will generally be connected to a source of liquid and/or to an exha ust port. At least one of the stream-select modules 113 will be connected to the process stream or other source from which the sample is to be drawn. Other stream-select modules 113 will be connected to sources of solvents, reactants, markers, or other materials which are to be / mixed with the sample or a portion of the sample.
  • the system 1111 can be modified to accept any number of solvents, samples, or other materials simply by including additional stream-select modules 13 to the stream switching valve system 103 and introducing additional fluid inlet and/or outlet paths.
  • the stream switching valve system 103 is constructed of stainless steel and may include Kalrez seals. The method and manner of producing such an assembly Is well within the knowledge of one of ordinary skill In the art.
  • variable displacement syringe pump system 105 configured to meter both solvent and sample volumes, and to propel fluids throughout the system 101.
  • sol vent and samp le ratios may be dynamically calibrated to sui t the needs of each particular installation.
  • the pum syste 105 comprises a pneumatic cy linder 114 sealedly connecte to a syringe pump chamber 108, which is feorosiKcate glass tube in the depicted embodiment but that is by no means required and the pump chamber 108 may be constructed of stainless steel or other materials depending o the needs of the particular material to be handled and the tests to be performed. Steel tubes will often be preferred for while they provide for less ability to perform direct optical
  • a steel chamber 108 can often be more readily connected to other components without risk of leakage through the use of
  • An internal syringe piston 115 in the pump chamber 108 comprises a piston hea 117 sealedly disposed in the syringe pump chamber 108
  • the syringe pisto head 117 is connected to an opposing cap en U S in the pneumatic cylinder 114 by a rod 120 extending therebetween.
  • the pump system 105 volume is approximately one hundred fifty milliliters (150 raL), hut the volume in any particular embodiment may vary according to the needs of the installation
  • a second syringe piston .115 will generally be similarly positioned in the mixing chamber 107 with the second syringe piston 115 operating In tandem with the first 115.
  • any number of control systems or means may be used to activate and control the syringe pistons 115.
  • positional control of the syringe piston 115 is achieved by the use of one or more proportional pressure regulators 119 which are, in turn, controlled by a computer running appropriate software or a hardware control system in the form of wired electronics.
  • the proportional pressure regulator(s) 119 are configured to control the position of the syringe piston head 117 in the syringe pump chamber 108.
  • such regulators 119 facilitate variable displacement of fluids within the system 101 by moving the syringe piston 115 to push fluid out of the chamber 108 or 107 or create a vacuum to draw fluid into the chamber 108 or 107
  • a first regulator 119A maintains a constant pressure on the rod side 122A of the pneumatic cylinder 114
  • a second regulator P9B controls pressure on the cap side 122B.
  • one or more of the proportiona l pressure regulators 119 A and J19B may be of the type manufactured by
  • the regulators 119A and 119B are generally controlled by a controller 121, which is configured to send pressure command signals to the proportional pressure regulators 119A and 119B.
  • the controller 121 may be an analog device, digital device, or an external computer system running appropriate software.
  • the controller 1 .1 is an electro-pneumatic positioning controller 121.
  • the controller 121 may be configured to compare the pressure ratio of one side 122 A of the pneumatic cylinder 114 to the other 122B.
  • the controller 121 is a proportional-integral -derivative (FID) loop controller 121 configured to deliver an analog output to one or both of die proportional pressure regulators 119 A and 119B to adjust pressure as needed to move and place the piston 115. Pressure differentials on either side of the piston cap 118 cause or facilitate mo vement of the syringe piston 115.
  • the regulators 119 A and 119B may co tinually operate to control the pressure within the pneumatic cylinder P4. In an embodiment, the regulators 119 A and 119B control pressure to within 0.10 pounds per square inch (psi), with the positioning accuracy of the piston 115 of approximately plus or minus one millimeter.
  • FIG. I While the embodiment of FIG . I provides for two samp le chambers 107 and 108 each of which includes a piston pump 115, one of ordinary skill in the art will understand that if the chambers 107 and 108 are sealed, the movement between them may be accomplished by a single pump 115 in a single of the chambers 107 or 108. Specifically, the single pump 115 may utilize a push to move fluid from the chamber .107 or .108 in which ills mounted into the other chamber 107 or 108, or a pull (to create a vacuum) to move fluid not in the chamber into i
  • the mixing chamber 107 is a clear tube generally located in a position parallel to the syringe pump system 105.
  • chamber 108 a steel or similar material chamber maybe preferred for sealing reasons.
  • fluids will commonly alternate between the mixing chamber 108 and syringe pump chamber 108 to provide mixing or extraction action as appropriate.
  • the fluids exchanged between the syringe pump chamber 108 and the mixing chamber 107 pass through the stream switching valve arrangement 103. This facilitates that fluids within the system 101 being incorporated during an extractio or mixing process and accurate dispersion of solvents, additives, indicators, or other materials to be added to the emulsion provided
  • movement of the syringe piston 1.15 causes fluid flow through the system 101.
  • the pressure of fluid being added to or removed from die mixing chamber 107 may also result in movement of the mixing chamber piston 115 (if present).
  • the mixing chamber 1 7 is thus in fluid communication with the syringe pump chamber 108, it is preferable that the mixing chamber 107 be disposed in a v rtical alignment with respect to gravity such that the point of egress from the mixing chamber 107 is located at the bottom of the mixing chamber 107 with respect to gravity.
  • the piston 115 moves and creates a vacuum in the fluid path of the system 101, fluid in the mixing chamber 107 will more easily ⁇ egress from the mixing chamber 107 at the bottom, aided by gravity.
  • mixing chamber 107 and pump chamber 108 are preferably elongate in a vertical dimension.
  • gravity can also be used to more clearly and understandabl segregate non-mixing materials into layers. For example, it is well understood that if an oil and water emulsion is separated, the oil will be vertically (with respect to gravity) on top of the water. Thus, with vertical elongation of the chambers 107 and 108 tests performed from the top or bottom of the chamber will be clearly directed into a specific material first.
  • fluid is exchanged between the mixing chamber 107 and the syringe pump chamber 108 until the extraction process and all measurements are complete.
  • Operation, of the system 101 will generally operate loosely as follows, but various specific operations are discussed in conjunction with FIG, 8-10.
  • the valve arrangement 103 is set so tha a withdrawal action of one of the pistons P 5 will serve to pull fluid through the valve arrangement 103 fro the sample source.
  • the valve 113 connected to the sample source is opened and piston 115 is moved to pull the sample in,
  • Tlie sample will generally, however, not be pulled in alone. Specifically, any numbe of additional valves 113 may be opened simultaneously so that the action of the piston 115 will actually pull fluid from multiple sources at the same time. A should be apparent, ho open each valve 113 is (as well as its size and configuration) relative to all the other valves 113 will determine a specific ratio of all the fit id to be pulled in with the single pump stroke.
  • the action of pulling the fluids from multiple sources will generally result in a strong mechanical agitation (mixing) of the liquids and, thus, the added chemicals will generally be strongly mechanically agitated with the sample as they are withdrawn.
  • This can provide for mixing of solvent or other additive to the sample a the sample is withdrawn into the system 101.
  • the sample will comprise a emulsion and at least one of the added liquids will comprise some form of emulsifier or sol vent depending on if measurements arc to be taken on the emulsion or on its separated components.
  • a solvent to separate the emulsion is added for ease of discussion.
  • the emulsion will neneraOv enter a first sample chamber (we are going to utilize pump chamber 108 asthis initial chamber simply for ease of discussion but either chamber 1.07 or 108 can be initially used) already combined with a solvent. Once the sample and solvent; combination is in the chamber 108, the sample will he allowed to settle and the emulsion will generally separate into its components. At this time, measurements may be performed oft either or both of the separated components and what measurement is performed on what; will generally be determined by the position of the various measuring instruments with regards to chamber 108.
  • the pumps 115 will sen to move the liquid item chamber 108 to chamber 107. As should be apparent, this will be performed by activating the pumps 115 and the liquid flowing through the valves 103. It should also be apparent that as the liquid goes through the val ves 103 additional valves 1 3 may be opened simultaneously or sequentially to mix additional chemicals with the liquids as they transfer between the two chambers. Further, the emulsion will also generally be reformed from the separated state due to the shear imparted on the liquid by passing through the valves 103.
  • the emulsion may again be allowed to separate and now measurements base on the instruments located in chamber 107 (as opposed to those in chamber 108) may be performed).
  • the liquid may be sent back through the valve assembl 103 to chamber 108 to perform additional measurement there if the addition of another chemical allows for a different measurement to be performed.
  • the valve arrangement 103 may be positioned to an exhaust position where the sample is disposed of or returned to the process stream as desired.
  • the system 101 provides for a large amount of different tests to be performed on the sample and allows for a near limitless number of additional chemicals to be added t the sample in the performance of those tests.
  • any test may be performed on the same sample i the emulsion state, in a separated state, and on each of the consti tuen ts of the separated state individually simply by how the sample is positioned within the system 101
  • the analysis system 109 is positioned in the fluid flow path and comprises the interface for the concentration measurenient
  • the interface may be secured to the chamber with high-performance liquid chromatography (HFLC) fittings.
  • HFLC high-performance liquid chromatography
  • Such fittings may provide a high-pressure seal, with low dead volume within the chamber.
  • the depicted analysis system 109 comprises an nalysis chamber and/or cell and/or may be configured for a fluorescence measurement interface* and/or one or more absorbance interfaces. Additionally* the optical path length is adjustable in absorbance applications. This maybe done, for example, by fastening the optical interface couplers in the proper position with the HPLC fittings.
  • the depicted system 101 is configured for use with a number of optional accessories.
  • the system may comprise additional ports for calibration, samples, or solvents, These maybe added for example, by incorporating additional stream select modules 113 to the stream switching valve system 103 Additionally; if waste is to be expelled to the sample stream, the waste port may be removed.
  • the system 101 may also be configured for one or more different measurement methods, and is configurable to perform automatic self-cleaning and instrument zero cycles, as described elsewhere herein.
  • a fluorescence instrument may be positioned to measure downward into chamber 108 (measure the“top” component of a separated emulsion)
  • an absorbance instrument may he positioned to measure upward into the same chamber 108 (measure the“bottom” components of a separated emulsion).
  • Chamber 187 may also have multiple instruments. It should he noted that instruments herein are generally mounted to measure the“botom” of the liquid or the“top” of the liquid.
  • While positioning the measurement instrument above or below the sample chamber 107 or 108 provides an eas method to determine which portion of the separated emulsion is being measured, it is not required, and an instrument may be presen ted at the side of the chamber * at any height, to provide for additional measurement options. The only key is that the portion of the sample of interest be able to reach the height of the instrument to allow the measurement to be performed on that portion
  • the water will be separated to chamber w ith the oil remaining in another.
  • the chamber of the oil will then be moved to exhaust and the oil exhausted to waste. If this is insufficient water for a measurement to be performed, the water may be moved to the other chamber while being mixed with additional sample material taken from the process flow (and additional sol vent to separate if appropriate), 1 ' his will increase the total amount of water in the device 101.
  • the ater may then again be separated and the oi l exhausted. This process can he repeated until one of the chamber is substantially full of water This will generally be sufficient for any measurement.
  • the same type of action may a! so be perfumed to get a single- chamber substantially lull of oil
  • process measurements that require addition of a chemical reagent or solvent to form a color or extract an analyte can be performed within different industrial environments continuously and automatically thereby eliminating the time and expense of laboratory involvement by simply selecting appropriate additives and having them be mixed into the process fluid a part of the extraction step.
  • the process fluid can be pulled into a first chamber while being mixed with a first additive, a lest can be performed, and then the resultant fluid can be mixed with another additi ve and sent to the second chamber. This process can be repeated any number of times for different tests.
  • tests involving this problematic constituent can be performed first, the material can then be separated with that constituent being completely exhausted, and then the additive can be added to the remaining and positioned as needed.
  • This can provide a method of extracting a broad range of anions, cations or chemical species tha t are not soluble in broad range of chemical streams found in chemical, petrochemical, food/beverage, bioprocessing and pharmaceutical plants around the world,
  • hydrophilic or hydrophobic solvents can be used to separate components from analytes fioro either polar or non-po!ar matrices. Examples include, but are not limited to, detecting the presence and amount of corrosion inhibitors, scale inhibitors from produced water streams that contain both the cations and oil, calcium, magnesium ions in produced water streams that also contain interferences suc as aromatic or aliphatic hydrocarbons when measuring the spectroscopic characteristics of the sample
  • FIG, 7 depicts a schematic diagram of a piping and instrumentation layout for an embodiment of system 101
  • the depicted embodiment of FIG. 7 comprises a syringe pump system 105 in fluid communication with a mixing chamber 107 through a stream switching valve system 103
  • the syringe pum system 105 comprises a pneumatic cylinder 114 having a syringe piston 115
  • the analysis system 109 is disposed in the fluid path at the egress end of the syringe pump chamber 108.
  • a pair of regulators 119 A and 1.1.9B are attached at the ro end 122 A and ca end 122B of the cylinder 14,
  • FIG. S provides some detail on a valve arrangement within a valve 113 to indicate how material may be selected or not for that particular attache source
  • FIGS 8 through .10 provide for some specifics of operation of an arrangement as shown in FIG. 7 to perform a mixing and measurement operation.
  • the depicted method of FIG 8 comprises six steps; initialization 801, sample collection 803, solvent addition 805, mixing 807, measurement 809, and waste evacuation 811 Additionally, a solvent wash step 813 may he included.
  • initialization 801 valve 125 of each module 1131s closed, valve 123 of each module 113 is closed, and valve 1.2? of each module 113 Is open.
  • pistons 117 and 116 are both m“empty position. 5 '
  • the term“empty position’ means that die piston head is disposed at the egress side of the mixing chamber 107 or the syringe pump chamber 108, respectively in an embodiment, the pressure caused by fluid flow into the syringe pump chamber 108 can move the piston 115 out of empty position, Alternatively, the piston 115 may be pneumatically operated to create a vacuum in the fluid path and thereby pull fluid into the system.
  • valve system 103 comprises a plurali ty of stream-select modules 113.
  • Each stream-select module 113 is a stream-select module 113.
  • valve 125 for at least one module 113 is opened.
  • valve 125 for module C is opened. This is because the sample inlet line 128 and sample outlet line 129 are in fluid communication with valve 125 in module € By opening valve 125 in module C. sample may he received by module C on the sample inlet line 128 Additionally, valve 123 in module € is also opened.
  • valve 123 of each mo ule 113 in the valve syste 103 is in iiu id communication with the syringe pump system 105 via a syringe pump fluid line 131.
  • Each module 113 is in fluid communication with this line 131 via valve 123.
  • valve 123 is closed and all modules except module C, when sample is received on sample inlet line 128 by module C it flows through valve 125 and valve 123 to line 131, an from there to the syringe pump chamber 1118.
  • valves 123 are closed in. modules A, B and D, the sample cannot flow through those modules.
  • the path through the system is configured so that sample received oh line 128 flows only to chamber 108.
  • valves 125 and 123 in module C are closed, but valves 125 and 123 in module I ) are opened.
  • valve 1 5 of module D is in fluid communication with a solvent reservoir 133 via a solvent reservoir fluid line 135.
  • the fluid flow path is configured so that only solvent flows from the solvent reservoir 133 through the solvent fluid line 135 through valve 125 and 123 of module I> to the syringe pump fluid line 131 and from there into the syringe chamber 108,
  • the addition of the solvent moves th Syringe piston 115 to solvent position, meaning that the presence of both the sample and solvent in chamber 108 ha pushed the piston 115 into the pneumatic cylinder 114.
  • This arrangement is schematically represented in FIG. 8. [085]
  • mixing 807, valves 123 and 125 in module D are closed, valve 127 in module D is opened.
  • Valves 123 an 125 in module A are opened and valve 127 of module A is closed.
  • valve 125 of module A is in fluid communication with the mixing chamber 107.
  • This configuration creates a fluid flow path from chamber 108 through fluid line 131 into valve 123 of module A, through valve 125 of module A to fluid line 137, and into mixing chamber 107.
  • the controller 121 activates regulator T19.4 to advance the syringe piston 115 into chamber 108, forcing the contents of the chamber 108 through this fluid path into the mixing chamber 107.
  • This step 807 can be reversed by actuating regulator 11SB via the controller 1 1 to withdraw the syringe piston 1.15, which creates a vacuum in the syringe chamber 108, which causes the mixture in the mixing chamber 107 to reverse through the fluid flow path back into the syringe pump chamber 108.
  • Thi process of alternately actuating regulators 119A and 11913 to insert an withdraw the syringe piston 115, and to thereby force the mixture back and forth through the fluid path to and from chambers 107 and 108, altematmg!y, may be repeated one or more times. It should be apparent that the process only requires the use of a single piston 115 as the operation ei ther to push fluid from the syringe chamber 108 or to create a vacuu which serves to pull fluid into the syringe chamber 108.
  • the next step, measurement 809 uses the same fluid path -configuration of the valve System 103, except that the syringe piston 115 is withdrawn into the pneumatic cylinder 114, pulling the mixture into chamber 108. Because the analysis system 109 is disposed in the fluid path between tire chamber 108 an fluid line 131, an amount of mixture is present in the analysis system 103 for measurement, Speetrographie, chromatographic, or other measurement may then be performed using the analysis system 109 according to techniques known in the art.
  • valves 123 and 125 in module A are closed, valve 127 is open, and valves 123 and 125 of module B are opened and valve 127 of module B is closed.
  • valve 125 of module B is in fluid communication with a waste fluid line 137.
  • the regulators 119 ⁇ and 119B may then activate the syringe piston 115 to force fluid into chamber 108 to evacuate the fluid line 131.
  • FIG, 9 depicts an embodiment of an extraction process in which a liquid-liquid extraction is performed with a single solvent and all fluids are expelled to the sample stream, instead of waste as in FIG. 8,
  • the same basic steps are followed, with some modifications.
  • six steps are described, along with the optional solvent wash process 813 at the end.
  • These depicted tops are initialisation 901, sample collectio 903, solvent addition 90S, mixing 907, measurement 909, and waste evacuation 911
  • the first five steps 901, 903, 905, 907 and 909 are all performed in essentially the same manner as i the depleted embodiment of FIG.
  • valves of the modules 113 in the same open and closed positions, and the regulators 119.4 and 119B used to move the piston 115 In the same manner.
  • waste evacuation 911, valves 123 and 125 of module B are closed and valves 123 and 125 of module C are open , with valve 127 of module C closed.
  • valve 125 of module C is in fluid communication with both a sample inlet 128 and sample outlet 129 fluid line.
  • a solvent wash/zeroing process 813 is shown to indicate how the system can utilize the attached material sources to perform actions which do not specifically relate to a sample measurement, hut utilize the same basic process of the device 101 to perform system maintenance and testing.
  • the depicted process of FIG. 10 cleans the system 101 with solvent to remove sample that may have coated the optical interfaces over time or where a particularly poor sample is present in the device 1 1 and needs to be effectively destroyed.
  • the cleaning and/or zeroing process 813 may be user-initiated or set or scheduled to occur at. a specific time interval.
  • the depicted eteniing/zeroing process of FIG 10 comprises four primary steps. They are: solvent addition 1001, deep cleaning 1003, solvent evacuation 1005 and solvent addition/zeroing 1007.
  • sol vent addition 1001 valve 125 on module 0 is ope to allow fluid flow from solvent reservoir 133 via line 135
  • valve 123 in module O is open to allow sol vent to flow from the reservoir 113 through fluid line .135 into module 0 and out of module 0 to fluid line 131 Because all other valves 123 to the other modules 113 are closed, the only available fluid path for the solvent is to chamber 108 through the analysis cell 109. This moves the syringe piston 115 into solvent position.
  • valves 123 and 125 of module A are closed and valve 127 of module A is: open.
  • Valves 123 and 125 of module B are opened and valve 127 is closed.
  • the syringe piston 115 can three the cleaning solvent through module B to the waste line 137,
  • valves 123 and 125 of module D are opened, and valve 127 is closed.
  • Fresh solvent may be placed in the solvent reservoir 133, and the piston 115 is withdrawn into the cylinder 114 to create a vacuum and pull the fresh solvent from the reservoir 133 through flui Hue 135 and module I> into the analysis system 109.
  • the zeroing process may then be carried out according to techniques known in the art,
  • the water would be first to be ejected, followed by the solvent/rag layer, and then the oil.
  • the layers can be physically separated by placing the target constituent alone in a chamber.
  • the additive would be added while the materiai is slowl ejected from the chamber to the material as it eaters the other chamber. As this is the water initially » the additi ve is only mixing with water. U on detection that the solvent/rag layer is approaching the bottom, the pump action may cease so none of the mg layer or oil layer ever leaves the initial chamber, At this time, there is only water and additive in the other chamber, and the appropriate test may he performed.
  • FIGS. 1 through 4B While the above focuses on the operation of the device shown in FIGS. 1 through 4B it should be apparent that it would operate similarly in less complex arrangements of chambers and pumps. These latter types of dev ices can be useful where the types of measurements are similar, but fewer measurements are: needed, less mixing is needed, or simply where less options lor foe mixing need to be available.
  • the device 191 of FIG. 1 1 provides For two sample chambers 107 and 108 and only a single pomp 115.
  • the device 191 of FIG, 11 generally is actually designe to only have measurement performed on chamber 107 with chamber 108 used purely for extraction, mixing, or separation steps.
  • the operation of device 191 while being simplified and having less options, is generall similar to the operation of device 101.
  • FIG 12 provides for a still farther simplification of the options by using device 193.
  • device 193 only a single chamber 108 and pump 115 is used.
  • the val ve arrangement 113 is also simplified and a valve selector 1213 is used.
  • the valve selector 1213 wi ll act to sequentially select torn the variety of input valves 113 as the pump 115 Is withdrawn. Amounts of each constituent (including die sample) wi ll be selected as the pump 115 withdraws with each being added sequentially to the sample.
  • valve selector 1213 may initially select a first input and the pump 115 withdraws to pull a first amount, the valve selector 1213 then changes the input to a second input after which the pump 115 withdraws more to add a second amount. This process may be repeated until all constituents are selected and pulled into chamber 108, Generally, the pumping action will provide sufficient shear to mix and to provide good mixing of the various inputs, but larger constituent amounts ma be added later in the process to further assist with this.
  • the device 193 may have a plurality of measurement devices 109 attached thereto which may be used to measure the result in emulsion, or the emulsion may be allowed to settle so measurements may be performed on different continuants, Qttee the
  • the pump selector 1213 will generally select a valve path 313 which is exhaust and the sample will be exhausted b the pump US reversing direction and pushing all the contents from the chamber 108.
  • this device 193 allows for many of the benefits of the devices 101 and 191, but doe not allow for movement of the sample between two chambers and therefore cannot; allow for later mixing of additional chemicals with the sample, or of complete physical separation of the two constituents on the emulsion,
  • F IG , 12 does still al low for a single of the continuants to be tested alone, so long as it is the last to he exhausted based on. tlie valve positions 113,

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

La présente invention concerne un système de mélange qui utilise une pompe avec un moyen hautement sensible pour ajouter et commander des volumes d'un ou plusieurs réactifs dans un volume contrôlable d'un échantillon, pour mélanger lesdits échantillons et réactifs, pour fournir le(s) moyen(s) d'utilisation d'un outil de mesure spécifique sur une partie de l'échantillon mélangé, et enfin pour rapporter les résultats à un élément de commande final automatiquement dans des conditions industrielles et souvent essentiellement in situ pour des écoulements de fluide tels qu'un fluide se déplaçant dans à un pipeline ou un processus industriel.
EP18888893.7A 2017-12-15 2018-12-14 Systèmes et procédés d'essai et de manipulation de liquide automatisés Pending EP3723907A4 (fr)

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US201762599645P 2017-12-15 2017-12-15
US15/974,450 US11154855B2 (en) 2017-05-08 2018-05-08 Automated liquid handling and testing systems and methods
PCT/US2018/065787 WO2019118896A1 (fr) 2017-12-15 2018-12-14 Systèmes et procédés d'essai et de manipulation de liquide automatisés

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EP0259259A3 (fr) * 1986-08-28 1989-05-17 Ciba-Geigy Ag Dispositif de préparation d'échantillons pour analyse
AU2001240104A1 (en) * 2000-03-07 2001-09-17 Symyx Technologies, Inc. Parallel flow process optimization reactor
US7101515B2 (en) * 2003-04-14 2006-09-05 Cellular Process Chemistry, Inc. System and method for determining optimal reaction parameters using continuously running process
DE10333384B4 (de) * 2003-07-23 2008-03-06 Sigrid Heide Mischanordnung zum Herstellen flüssiger oder halbfester Produkte
US8146655B2 (en) * 2009-10-13 2012-04-03 Schlumberger Technology Corporation Methods and apparatus for downhole characterization of emulsion stability
JP7071119B2 (ja) * 2014-10-13 2022-05-18 アドミニストレイターズ オブ ザ テューレイン エデュケイショナル ファンド 直列流れの中の溶液条件を変化させる装置および方法

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