Apparatus, system and process for computer-assisted in-process optimization of mineral extraction and purification processing

Abstract

In an embodiment, a system for controlling an extraction process comprising a plurality of stages is disclosed. The system includes a processor and memory. The processor is configured to obtain sensor data corresponding to a concentration of a target material of interest from a sensor device at least partially disposed in fluid communication with a fluid corresponding to a given stage of the plurality of stages of the extraction process. The process is further configured to determine, based on the sensor data, a concentration of the target material of interest, compare the determined concentration of the target material of interest to a predetermined threshold and control at least a portion of the extraction process based at least in part on a result of the comparison of the determined concentration of the target material of interest to the predetermined threshold.

Description

APPARATUS, SYSTEM AND PROCESS FOR COMPUTER-ASSISTED IN-PROCESS OPTIMIZATION OF MINERAL EXTRACTION AND PURIFICATION PROCESSINGCOPYRIGHT NOTICE

[0001] A portion of the disclosure of this patent document contains material which is subject to copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyright rights whatsoever.CROSS REFERENCE TO RELATED APPLICATION

[0002] This application claims the benefit of U.S. Provisional Patent application No. 63 / 580,370, filed on September 2, 2023, and entitled “AUTONOMOUS REACTOR UNIT AND SYSTEM FOR HYDROMETALLURGICAL EXTRACTION PROCESSING” the entirety of which is incorporated by reference herein.

[0003] This application is related to a PCT application filed with the U.S. Patent and Trademark Office as receiving office on even date herewith and entitled “ADAPTIVE HYDROMETALLURGICAL PROCESS CONTROL SYSTEM AND METHODS OF USING THE SAME” by Dean G Gouramams, the entirety of which is incorporated by reference herein.

[0004] This application is related to a PCT application filed with the U.S. Patent and Trademark Office as receiving office on even date herewith and entitled “SYSTEM FOR COMPUTER-ASSISTED IN-PROCESS OPTIMIZATION OF MINERAL SOLUTION EXTRACTION” by Dean G Gouramams, the entirety of which is incorporated by reference herein.BACKGROUND

[0005] This application relates to process controls in hydrometallurgical systems, and in particular, to systems and methods for performing process controls based on concentration measurements of target elements in fluids of a fluid system.

[0006] A fluid system often comprises more than just a particular fluid such as, e.g., water. Instead, depending on the particulars of the fluid system, various other elements or materials may either be suspended or dissolved in the fluid.

[0007] One example of a fluid system is an industrial process stream, such as those comprising fluids flowing within pipes and tanks in an industrial processing center. Such fluid systems may be pressurized, corrosive, hazardous, extremely hot, extremely cold, located in hard-to-reach areas or have other attributes that may make it difficult to obtain measurements directly from the fluids. Typically, a sample of the fluid in an industrial process stream must be manually extracted from the industrial process stream and taken to another location for measurement testing, e.g., in a local laboratory on-site or in a remote laboratory. Such a manual process for measurement testing of an industrial process stream may be dangerous to the individual taking the sample, e.g., due to the potentially hazardous nature of the industrial process stream. In addition, such a manual process may lose accuracy relative to the target element concentrations actually found in the industrial process stream due to the delay involved in taking the sample, the delay in relocating the sample to the laboratory, the delay in testing the sample at the laboratory, theopportunity for contamination of the sample and a change in environmental variables relative to those existing in- situ at the industrial process stream.

[0008] In chemical engineering the need for chemical analysis of a sample is fundamental. From lab-scale research to large-scale continuous manufacturing facilities, the knowledge of the exact chemical composition of a mixture at any given time may be of central importance to controlling the process and parameters of the facility. However, peering into the world of molecular interactions often requires sophisticated and expensive instrumentation.

[0009] State-of-the-art technologies for determining elemental concentrations in material samples are typically based on inductively -coupled plasma (ICP) instrumentation. ICP analyzers heat material samples to thousands of degrees centigrade in order to induce energy emission which is analyzed by a spectrometer in order to deduce elemental concentration. While ICP analysis provides accurate elemental concentration measurements, the technology presents inherent limitations. For example, liquid samples must first be filtered and dehydrated in order to produce solids for ICP analysis, and the sample preparation is a lengthy process, which generally requires manual labor, lab equipment and consumable supplies. Producing a measurement typically requires at least 1 hour before data is available and often takes days or even weeks depending on the availability of ICP analysis equipment.

[0010] Due to the delay in obtaining ICP analysis results, creating effective process controls may be challenging. Process controls for an industrial facility is instead or often predicated in old / stale data, modeling and other techniques that serve to estimate the ideal process. Such process controls, however, are inherently unable to handle changes in the fluid system including, e.g., fluid composition, feedstock composition, or other parameters of the process, in a timely manner due to the delay in obtaining the ICP analysis.SUMMARY

[0011] In an embodiment, a system for controlling an extraction process comprising a plurality of stages is disclosed. The system comprises a processor and memory. The processor is configured to obtain sensor data corresponding to a concentration of a target material of interest from a sensor device at least partially disposed in fluid communication with a fluid corresponding to a given stage of the plurality of stages of the extraction process. The process is further configured to determine, based on the sensor data, a concentration of the target material of interest, compare the determined concentration of the target material of interest to a predetermined threshold and control at least a portion of the extraction process based at least in part on a result of the comparison of the determined concentration of the target material of interest to the predetermined threshold.

[0012] In an embodiment, the sensor device is installed such that the sensor device is at least partially disposed within inflow piping supplying the fluid from a prior stage to the given stage.

[0013] In an embodiment, the sensor device is installed such that the sensor device is at least partially disposed within outflow piping providing fluid from the given stage to a subsequent stage.

[0014] In an embodiment, the sensor device is installed such that the sensor device is at least partially disposed within fluid of the given stage.

[0015] In an embodiment, the sensor device comprises a plurality of sensor devices and a first sensor device of the plurality of sensor devices is installed such that the first sensor device is at least partially disposed within an aqueous phase of the given stage. The first sensor device is configured to measure a concentration of the target material of interest within the aqueous phase. A second sensor device of the plurality of sensor devices is installed such that thesecond sensor device is at least partially disposed within an organic phase of the given stage. The second sensor device is configured to measure a concentration of the target material of interest within the organic phase.

[0016] In an embodiment, the processor is further configured to monitor the transfer of the target material of interest between the aqueous phase and the organic phase based on sensor data received from each of the first and second sensor devices that corresponds to the relative concentration of the target material of interest in each of the aqueous phase and organic phase and cause at least one of the aqueous phase and the organic phase to move to another stage of the extraction system based on the monitoring.

[0017] In an embodiment, a third sensor device of the plurality of sensor devices is installed such that the third sensor device is at least partially disposed within an aqueous phase of the given stage. The third sensor device is configured to measure a concentration of a target contaminant within the aqueous phase. A fourth sensor device of the plurality of sensor devices is installed such that the fourth sensor device is at least partially disposed within an organic phase of the given stage. The fourth sensor device is configured to measure a concentration of the target contaminant within the organic phase. The processor is further configured to monitor the transfer of the target contaminant between the aqueous phase and the organic phase based on sensor data received from each of the third and fourth sensor devices that corresponds to the relative concentration of the target contaminant in each of the aqueous phase and organic phase and cause at least one of the aqueous phase and the organic phase to move to another stage of the extraction system based on the monitoring.

[0018] In an embodiment, at least one of the first and third sensor devices comprise the same sensor device and the second and fourth sensor devices comprise the same sensor device.

[0019] In an embodiment, the predetermined threshold comprises a target material of interest concentration threshold for a subsequent stage to the given stage. The processor is further configured to control an actuation of a valve of the extraction process to transfer the fluid from the given stage to the subsequent stage based at least in part on a determination that the determined concentration of the target material of interest is greater than or equal to the predetermined threshold and control an actuation of a valve of the extraction process to transfer the fluid from the given stage to the prior stage based at least in part on a determination that the determined concentration of the target material of interest is less than the predetermined threshold.

[0020] In an embodiment, the processor is further configured to obtain second sensor data corresponding to a concentration of a target contaminant from a second sensor device and determine, based on the second sensor data, a concentration of the target contaminant. The processor is further configured to inhibit actuation of the valve of the extraction process to transfer the fluid from the given stage to the subsequent stage based at least in part on a determination that the determined concentration of the target contaminant is greater than or equal to the second predetermined threshold and control the actuation of the valve of the extraction process to transfer the fluid from the given stage to the prior stage based at least in part on a determination that the determined concentration of the target contaminant is greater than or equal to the second predetermined threshold.

[0021] In an embodiment, the sensor device and the second sensor device comprise the same sensor device.

[0022] In an embodiment, the processor is further configured to operate the extraction process for the given stage according to a first process workflow and controlling the at least a portion of the extraction process based at least in part on the result of the comparison of the determined concentration of the target material of interest to the predetermined threshold comprises the processor executing an interrupt event, the interrupt event comprising one of an adjustment to at least one operating parameter of the first process workflow based on the result and a replacement of the first process workflow with a second process workflow corresponding to the result.

[0023] In an embodiment, the processor is configured to execute the interrupt event for at least one of a predetermined amount of time, a predetermined number of cycles, and until a predetermined condition in the extraction process is met. The processor is configured to return the extraction process to the first process workflow based on a completion of the interrupt event.

[0024] In an embodiment, the processor is configured to provide the sensor data to a central dashboard, the central dashboard being configured for presentation to an operator of the extraction process.

[0025] In an embodiment, the target material of interest comprises a lanthanide.

[0026] The foregoing summary is illustrative only and is not intended to be in any way limiting. These and other illustrative embodiments include, without limitation, apparatus, systems, methods and computer-readable storage media. In addition to the illustrative aspects, embodiments, and features described above, further aspects, embodiments, and features will become apparent by reference to the drawings and the following detailed description.BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The invention is illustrated in the figures of the accompanying drawings which are meant to be exemplary and not limiting, in which like references are intended to refer to like or corresponding parts.

[0028] FIG. 1 is a block diagram of an example system according to an embodiment.

[0029] FIGS. 2 and 3 are perspective views of a sensor device and control station of the system of FIG 1 according to an embodiment.

[0030] FIG. 4 is a perspective view of the sensor device of FIG. 1 according to an embodiment.

[0031] FIG. 5 is a cut-away perspective view showing the sensor device of FIG. 4 installed in a pipe structure according to an embodiment.

[0032] FIG. 6 is an exploded perspective view of the sensor device of FIG. 4 according to an embodiment.

[0033] FIG. 7 is a cross-sectional view of a sampling and measurement unit of the sensor device of FIG. 4 according to an embodiment.

[0034] FIG. 8 is a cross-sectional view of a sampling and measurement unit utilizing a fiber optic cable according to another embodiment.

[0035] FIG. 9 is a perspective view of a control station of the system of FIG 1 that is configured for use with the sampling and measurement unit of FIG. 8 according to an embodiment.

[0036] FIGS. 10-13 are cross-sectional views of the sampling and measurement unit of FIG. 7 illustrating an example sampling process according to an embodiment.

[0037] FIG. 14 is a block diagram of an autonomous reactor unit (ARU) according to an embodiment.

[0038] FIG. 15 is a perspective view of an example analyzer ARU according to an embodiment.

[0039] FIG. 16 is a diagram of an example analyzer ARU and a primary stream ARU according to an embodiment.

[0040] FIG. 17 is a flow diagram of an example mineral digestion analysis process using the analyzer ARU of FIG. 16 according to an embodiment.

[0041] FIG. 18 is an example chart of the efficacy of different lixiviants on MOI concentration when used in the process of FIG. 17 according to an embodiment.

[0042] FIG. 19 is an example chart of the efficacy of different lixiviants on MOI and contaminants when used in the process of FIG. 17 according to an embodiment.

[0043] FIG. 20 is a block diagram of an example extraction system according to an embodiment.

[0044] FIG. 21 is a block diagram of an example section of the extraction system of FIG. 20 according to an embodiment.

[0045] FIG. 22 is a flow diagram of an example automated process performed by the extraction system of FIG. 20 according to an embodiment.

[0046] FIG. 23 is a flow diagram of another example automated process performed by the extraction system of FIG. 20 according to an embodiment.DETAILED DESCRIPTION OF THE INVENTION

[0047] Subject matter will now be described more fully hereinafter with reference to the accompanying drawings, which form a part hereof, and which show, by way of illustration, exemplary embodiments in which the invention may be practiced. Subject matter may, however, be embodied in a variety of different forms and, therefore, covered or claimed subject matter is intended to be construed as not being limited to any example embodiments set forth herein; example embodiments are provided merely to be illustrative. It is to be understood that other embodiments may be utilized, and structural changes may be made without departing from the scope of the illustrative embodiments. Likewise, a reasonably broad scope for claimed or covered subject matter is intended. Throughout the specification and claims, terms may have nuanced meanings suggested or implied in context beyond an explicitly stated meaning. Likewise, the phrase “in one embodiment” as used herein does not necessarily refer to the same embodiment and the phrase “in another embodiment” as used herein does not necessarily refer to a different embodiment. It is intended, for example, that claimed subject matter include combinations of exemplary embodiments in whole or in part. Among other things, for example, subject matter may be embodied as methods, devices, components, or systems. Accordingly, embodiments may, for example, take the form of hardware, software, firmware or any combination thereof (other than software per se). The following detailed description is, therefore, not intended to be taken in a limiting sense.

[0048] The disclosed embodiments describe systems, devices and processes for performing precision hydrometallurgical extractions in an automated manner to extract one or more materials of interest (MOIs) such as, e.g., metallic or other elements, from fluid system comprising a solid, semi-solid or liquid feedstock. A solid or semi-solid MOI may be digested by a chemical extraction process such as, e.g., leeching, using a lixiviant. As an example, a lixiviant may comprise water, acids, organic solvents, or any other type of lixiviant commonly used in chemical extraction processes. Example organic solvents that may be utilized as a lixiviant include petroleum- derived organic solvents, synthetic solvents, carbon dioxide, or any other organic solvents. The extraction process may be utilized to produce a pregnant leach solution (PLS) containing the MOL The PLS may be the intended endproduct of the extraction process, for example, as part of a large scale extraction process that is designed to efficiently extract soluble metals from rock ore. The PLS may also or alternatively facilitate an automatic measurement process as described in more detail herein.

[0049] Data obtained from the automatic measurement process may be communicated to a process control computer in order to facilitate event-driven process parameter adjustments, for example, adjustments that result in efficiency optimizations in the extraction process. The measurement process may be implemented as part of the extraction process or it may be conducted in parallel to the extraction process, e.g., during at least part of the extraction process or at a time prior to the start of the extraction process.

[0050] The PLS may comprise a liquid having dissolved or dispersed materials which enables sampling of the PLS through the use of fluid control systems such as pipes, pumps and valves of the fluid system. In some embodiments,the PLS may comprise a fully digested and ionized solution. In other embodiments, the PLS may comprise a slurry mixture of ionized materials and particulates. The content of the PLS may change during the extraction process, e.g., due to variations in a feedstock of the fluid system, variations in the amount of lixiviant being used to digest the feedstock or for any other reason.

[0051] The PLS may be considered a representative sample of the material from which it was produced, e.g., the fluids in the fluid system. The concentration of certain chemical constituents of the PLS may be proportional to or representative of the concentration of certain mineral species or chemical compounds within the feedstock or the fluid system as a whole.

[0052] The term “feedstock” as used herein describes a raw material that is the input to a hydrometallurgical extraction system. For example, feedstocks may comprise rock ore, coal, shredded mass from a recycling process such as, e.g., shredded battery material or other recycled components, industrial waste products, river sludge, clay, sand, mine tailings, acid mine drainage or any other bulk material containing at least one MOI and at least one contaminant.

[0053] The term “material of interest” (MOI), as used herein, describes an element, chemical compound or complex that is the target of an engineered extraction process. For example, MOIs may include ions, compounds or complexes containing a specific material such as, e.g., rare earth elements, lanthanides, cobalt, magnesium, copper, nickel, platinum, gold, silver, lithium or any other element. The extraction process may produce the MOI in ionized form, or it may produce an ionized chemical compound containing the desired material. For example, a feedstock comprising sand containing cobaltite minerals or any other mineral species may be reacted with a lixiviant such as, e.g., sulfuric acid, to produce ionized sulfide salts or any other ionized compound that are dissolved in a solution.

[0054] As used herein, MOI may refer to a single chemical or species, or it may refer to a mixture of substances that are collectively of interest for separation by the extraction system. In a multi-stage extraction process, the MOI from one stage of the extraction process may differ from the MOI in other stages of the extraction process. A raffinate from one stage may comprise a MOI that is further refined in subsequent stages. For example, cobalt and copper may be extracted together from a feedstock or raffinate in a single stage of the process where the resulting solution comprising both cobalt and copper may be considered a MOI for that stage. In another example, the digestion of cobalt ore using a strong acid lixiviant may result in a variety of cobalt-containing chemical products that may be referred to individually or collectively as an MOI or MOIs.

[0055] The term “contaminant” or “bulk contaminant” as used herein describes a material, chemical compound, or element that results from a chemical extraction process performed on feedstock or raffinate materials from a prior stage, or directly originates from the feedstock or raffinate materials, which is not a target of the extraction process. For example, the extraction process may be configured to prevent or inhibit the contaminant from being dissolved by the lixiviant when forming the PLS.

[0056] In some embodiments, an MOI from one stage may be considered a contaminant in a subsequent stage of the extraction process. For example, a PLS may be formed containing multiple MOIs in one stage, with further refinement in the extraction process removing one or more of those materials as a contaminant relative to one or more other MOIs in a later stage. For example, an extraction process that is designed to extract neodymium from a mine waste comprising mostly iron oxide and calcium carbonate may be accomplished by using a lixiviant that selectively forms a PLS containing the neodymium and one of the iron oxide and the calcium carbonate as MOIs but not the other of the iron oxide and the calcium carbonate, e.g., inhibiting or preventing the presence of the other of the iron oxide and calcium carbonate in the PLS in a first stage. In some embodiments, the selectivity of the lixiviant may simply ignore the other of the iron oxide and the calcium carbonate when forming the PLS.

[0057] In a second stage, a lixiviant may be utilized that selectively forms a PLS containing neodymium as a MOI relative to the remaining iron oxide or calcium carbonate contaminant, e.g., by inhibiting or preventing the presence of the remaining contaminant in the PLS. In some cases, the second stage may alternatively target the remaining iron oxide or calcium carbonate as the MOI for the PLS, leaving the neodymium for collection separate from the PLS.

[0058] The terms “measurement” or “quantify” as used herein may refer to a measurement of a concentration of a particular MOI, contaminant, element or other material of interest. For example, in some embodiments, the measurement or quantification may be in units of parts-per-million, milligrams per liter or another unit. In other embodiments the term “measurement” may refer to rough measurements or relative measurements such as high concentration, medium concentration or low concentration. In some embodiments, the term “measurement” may refer to a binary measurement such as, e.g., greater-than or less-than a particular threshold concentration, e.g., 100 parts per million or another concentration value, of any target MOI, contaminant, element or other material of interest. Measurements may be absolute or qualitative in some embodiments but still be sufficiently accurate to achieve an intended process-control outcome. Some system designs may trade-off accuracy in order to achieve faster measurements, or vice versa, in order to achieve in-process adjustment capability with adequate temporal responsiveness.

[0059] The term “measurement latency” as used herein refers to the minimum elapsed time between when a measurement is commanded and when corresponding data is available. For example, a laboratory assay may have a measurement latency of 36 hours, while a sensor device such as that disclosed herein may have a measurement latency of two minutes or less. While two minutes is provided as an example, in some embodiments the sensor devices disclosed herein may have an even smaller measurement latency.

[0060] As used herein, “real-time” measurements or controls take into account minor delays due to data storage, processing, networking or other similar minor delays, delays due to the time it takes for a chemical processes associated with a reagent to interact with a sample, delays due to the time it takes a component such as a valve or motor to activate in response to a command, or any other minor delay. The term “real-time” also comprises near real-time measurements and controls, e.g., within milliseconds, seconds or even minutes where the number of minutes is still substantially smaller than a period of time required for manually operated systems that rely on ICP-S or other similar laboratory -based techniques for measurement and control.

[0061] As used herein, the term “fluid system” comprises, for example, a fluid stream, an industrial process stream, wastewater stream, river, water supply, standing pool, leeching pond, remediation vessel, tank or pond, fluid drainage system, fluid container, processing vessel or any other fluid flow or fluid containing system, all of which are individually and collectively referred to herein as a fluid system for brevity. In some embodiments, a fluid system as described herein may also or alternatively refer to a flow of fluid from a fluid source to system 100, e.g., by piping that receives fluid from the fluid source for use by system 100 or for any another purpose.

[0062] With reference to FIGS. 1-22, an example system 100 and embodiments are disclosed that implement precision hydrometallurgical extraction, processing or purification in an automated manner to extract one or more (MOIs) through the use of automated process controls in conjunction with a platform for autonomously performing concentration measurements in-situ in fluids of a fluid system.

[0063] System 100 comprises integrated instrumentation that is packaged within a sensor device 110 that is deployable at least partially within the fluids of the fluid system or in fluid communication with the fluid system and is configured to autonomously perform measurements of concentrations in-situ on the fluids of the fluid system. In an embodiment, system 100 is configured to utilize a reagent that interacts with an element, chemical compound orcomplex of interest, also referred to individually or collectively herein as the target analyte, that is found in the fluid system in order to induce a detectable change, e.g., a fluorescence, a change in absorption, a chromatic change or any other detectable change, that may be utilized to quantify a concentration of the target analyte in the fluid system. In some embodiments, non-reagent based optical methods may be utilized to detect and quantify a concentration of the target analyte in the fluid system including, e.g., absorption, chromatography or any other non-reagent based optical method.

[0064] Sensor device 110 comprises functionality that facilitates automated collection of measurement data directly from the fluid system, enabling a more accurate, targeted and timely measurement of concentrations of the target analyte within the fluid system while also reducing the exposure of individuals, such as workers at a processing facility, to the fluid system during the manual sampling typically needed for a laboratory -based analysis. Sensor device 110 is configured to leverage reagent and non-reagent based optical analytical techniques in an automated package that is deployable at a variety of locations in-situ in fluids of the fluid system to perform autonomous concentration measurements of the target analyte in real-time with little or no human supervision. In some use cases, for example, sensor device 110 may be located in harsh or remote environments that may not be easily accessible by a human on a regular basis. Sensor device 110 may be configured to provide measurement data electronically, e.g., in a wired or wireless manner, to a computer network, server, or any other computing device. Sensor device 110 may also be configured to receive commands or operating parameter adjustments electronically, e.g., in a wired or wireless manner, from the computer network, server, or any other computing device.

[0065] Sensor device 110 is readily configurable to quantify the concentrations or presence of various analytes by selecting and configuring corresponding sub-systems including, e.g., reagents, light sources, optics, filters, parameter calibration files and other components of sensor device 110. Sensor device 110 may, for example, be selectively configured with the sub-systems necessary for the detection of specific analytes and their concentrations within a particular fluid system and environment. Sensor device 110 is configured to mix a controlled volume of a reagent, such as consumable liquid reagent, with a sample obtained automatically by sensor device 110 from the fluid system, and rapidly perform the measurement process, e.g., in real-time before significant degradation of the reagent occurs.

[0066] With reference to FIGS. 1 and 2, system 100 comprises a sensor device 110, a sensor control station 300, a main control computing device 400, a sensor data storage server 410, a fluid control mechanism 600, reagent tubing 112, fluid tubing 114, a data input / output connection 116 and a network 118. In some embodiments, each of reagent tubing 112, fluid flow tubing 114 and data input / output connection 116 may connect between sensor device 110 and control station 300 to provide a flow of fluids and data between control station 300 and sensor device 110. In other embodiments, one or more of tubing 112 and 114 and connection 116 may alternatively connect sensor device 110 to another location, device, or otherwise.

[0067] Reagent tubing 112 is configured for use by control station 300 to supply a reagent to sensor device 110. In some embodiments, for example, control station 300 may be configured to supply reagent to sensor device 110 at a predetermined rate, on-demand at a predetermined volume, or in another manner. As an example, in some embodiments, control station 300 comprises one or more metering pumps 302 that are actuatable to cause a predetermined or variable target amount of reagent to be supplied to sensor device 110 via reagent tubing 112 within a particular amount of time.

[0068] Fluid tubing 114 is configured for use by control station 300 or another device to supply a fluid to sensor device 110. In some embodiments, for example, control station 300 may be configured to supply fluids to sensor device 110 at a predetermined rate, on-demand at a predetermined volume, or in another manner. As an example, insome embodiments, control station 300 comprises one or more metering pumps 302 that are actuatable to cause a predetermined or variable target amount of fluid to be supplied via fluid tubing 114 to sensor device 110 within a particular amount of time. In some embodiments, for example, fluid tubing 114 may be utilized to supply water, a non-reactive liquid or any other liquid to sensor device 110, e.g., for flushing sensor device 110, diluting a sample being measured by sensor device 110, mixing the sample with the reagent or for any other reason. Other fluids may also or alternatively be supplied to sensor device 110 by fluid tubing 114 in other embodiments. As an example, in some embodiments, fluid tubing 114 may be utilized to supply a gas to sensor device 110, e.g., to facilitate mixing of a sample with the reagent supplied by reagent flow tubing 112, to facilitate a chemical reaction between the reagent and a target analyte or for any other reason.

[0069] Network 118 is configured to connect sensor device 110, control station 300, computing system 400 and sensor data storage 410 together comprises one or more wired, wireless or combined wired / wireless networks and corresponding hardware such as hubs, switches, access points, network interfaces or other hardware commonly found in a network. Example wired and wireless networks that may be utilized include the Internet, a wide area network (WAN), a local area network (LAN), satellite, telephone, cable, a fiber-optic, cellular, ethemet, WiFi, WiMAX, Bluetooth®, any other network or connection or any combination thereof.

[0070] Sensor Device

[0071] With reference again to FIGS. 4-13, sensor device 110 comprises a housing 120 and a sampling and measurement unit 160.

[0072] Housing 120 comprises a tubing and connection hub 122, a mounting mechanism 124, a circuit cavity 128, circuitry 130A-13D, and a cavity 129 for receiving sampling and measurement unit 160. Circuitry 130A-130D may also collectively and individually be referred to herein as circuitry 130.

[0073] Tubing and connection hub 122 is configured to fluidly couple reagent tubing 112 and fluid tubing 114 to sensor device 110 and to electrically couple data input / output connection 116 to sensor device 110.

[0074] Mounting mechanism 124 comprises, for example, a pipe fitting or other similar component that is configured for easy and standardized installation on portions of a fluid system such as, e.g., pipes, tanks, ducts or other components of a fluid system through which a fluid flows. For example, mounting mechanism 124 may comprise a screw, a snap-fit, friction fit, clamp, compression fitting, gasket fitting or any other mounting mechanism. Mounting mechanism 124 or any other component of housing 120 may be fabricated or injection molded from a sturdy and corrosion resistant material such as stainless steel, nylon, polytetrafluoroethylene (PTFE) plastic or other corrosion resistant materials. In some embodiments, mounting mechanism 124 may be configured in accordance with NPT Pipe Plug fittings, Sanitary Quick-Connect fittings or Tri-Clamp sanitary fittings standards in order to facilitate integration with widely used industrial equipment.

[0075] In some embodiments, sensor device 110 is configured for at least partial insertion into a mounting location 502 of a structure 500 of a target fluid system such as, e.g., a mine, a chemical processing facility, or any other environment having a cavity 504 in which a fluid of the fluid system resides or flows. For example, as shown in FIG. 5, structure 500 may comprise a pipe, tank wall, duct or other component having a cavity 504 in which the fluid of the fluid system resides or flows. Mounting mechanism 124 may be configured to mate with mounting location 502, such that mounting mechanism 124 and mounting location 502 together seal structure 500 against egress of fluid from the fluid system with at least a portion of sampling and measurement unit 160 being exposed in fluid communication with the fluid. In some embodiments, no mounting mechanism 124 may be needed and sensor device 110 may instead be partially or fully submerged in the fluid system, e.g., a pond, lake, river, tank, vessel or any other fluid system.

[0076] With reference to FIGS. 6-13, sampling and measurement unit 160 comprises a sensor body 170, a window 172, circuitry cavity 173, a sample mixing unit 190, a porous member 192 and a cap 210. Sampling and measurement unit 160 is configured to receive an assembly of circuitry 130A and 130B, light shroud 132 and filters 152 within circuitry cavity 173 such that the optical sensors 150 of circuitry 130A, filters 152 and the light source 146 of circuitry 130B are in optical communication with window 172. Sampling and measurement unit 160 is configured for insertion into cavity 129 of housing 120 such that sample mixing unit 190 and cap 210 extend out of housing 120, e.g., for insertion into the fluid system. In some embodiments, a material such as a liquid, gas, epoxy or other material may be disposed within circuitry cavity 173 between sensor body 170 and circuitry 130A and 130B to provide protection or other properties. In some embodiments, a length of sensor body 170 may be selected for a particular use case. For example, sensor bodies 170 having various lengths may be available for integration into sensor device 110 to ensure that when installed in a target environment, sample mixing unit 190 and cap 210 extend into a fluid of the fluid system.

[0077] With reference to FIG. 7, sensor body 170 comprises light pathway channels 174 each of which is aligned with a corresponding one of optical sensors 150 and a light pathway channel 176 which is aligned with light source 146. While only six light pathway channels 174 and optical sensors 150 are illustrated and described herein, in other embodiments, a larger or smaller number of light pathway channels may alternatively be utilized, e.g., depending on the particular use case, target analyte, and target environment. Similarly, while only one light pathway channel 176 and light source 146 is illustrated and described herein, any other number of light pathway channels 176 and light sources 146 may alternatively be utilized. As an example, multiple light sources 146 may be present that emit light in different wavelengths along one or more light pathway channels 176. In some embodiments, multiple light sources 146 may utilize the same light pathway channel 176 or even emit light in the same wavelength along multiple pathway channels.

[0078] In some embodiments, one or more of light pathway channels 174 and 176 may comprise fiber optics or other light transmission mediums. In other embodiments, light pathway channels 174 and 176 may also or alternatively be formed from or coated with a reflective or absorbative material. For example, in some embodiments, an absorbative material that is configured to absorb the type of light being measured as part of the measurement process may be utilized where, for example only light that travels directly down a particular light pathway channel 174 may be received by the corresponding optical sensor 150. Such a configuration may, for example, enhance the quality of the measurement signal and reduce noise in the measurement signal. In an embodiment where the amount of light that is being measured directly is insufficient to quantify effectively, a reflective coating or light transmissive medium may alternatively be utilized to enhance the quantity of light that is received at the corresponding optical sensor 150. Any other configuration or material for light pathway channels 174 or 176 may also or alternatively be utilized.

[0079] With continued reference to FIG. 7, sensor body 170 further comprises an inner cavity 182 and a window shelf 184. Window shelf 184 is configured to receive window 172 to seal inner cavity 182 and inhibit the inflow of fluids into inner cavity 182 via window shelf 184. In an embodiment, each light pathway channel 174 and 176 extends to inner cavity 182 such that a light path from light source 146 extends into inner cavity 182 via light pathway channel 176 and a light path from inner cavity 182 extends through each light pathway channel 174 to a corresponding optical sensor 150. While each light pathway channel 174 and 176 is shown as extending to inner cavity 182, in other embodiments, one or more of the light pathway channels may alternatively extend to window 172 separately from the other light pathway channels.

[0080] Window 172 may comprise an optically transparent window. As an example, window 172 may be formed of a material such as glass, quartz, sapphire, silicon or any other material that is transparent to the wavelength of light selected for emission by light source 146 toward sample measurement unit 190 and the wavelengths of light emitted / reflected from the fluid sample back toward light pathway channels 174 and the corresponding optical sensors 150. The material used for window 172 may also be selected based on the environment and composition of the fluid system where some fluid systems may be more corrosive or damaging to a particular material than others.

[0081] The interface between each light pathway channel 174 and 176 and inner cavity 182 may comprise lens components (not shown) to focus light traveling between the corresponding light pathway 174, 176 and inner cavity 182. In some embodiments, window 172 may also or alternatively comprise a lens. The lens components may comprise collimating lenses or any other type of lens.

[0082] Sensor body 170 is configured to optically expose light source 146 and optical sensors 150 to the fluid sample via light pathway channels 174 and 176, inner cavity 182 and window 172. Window 172 is configured to allow light emitted by light source 146 and traveling through light pathway channel 176 and inner cavity 182 to enter a portion of the fluid sample that is temporarily captured by sample measurement unit 190. Window 172 is also configured to allow light from sample measurement unit 190 to return through inner cavity 182 and light pathway channels 174 to corresponding optical sensors 150. As an example, fluorescence or reflections caused by the light emitted by light source 146 may be received from the sample. In some embodiments, a reduction in light due to absorption may also be measured, e.g., by performing two or more measurements, performing pre -reagent dispensing and post reagent dispensing measurements, periodic measurements or in any other manner.

[0083] With reference to FIGS. 6 and 7, light shroud 132 is disposed between circuitry 130A and circuitry 130B when assembled together and is configured to inhibit or shroud the direct exposure of optical sensors 150 to light generated by light source 146. For example, as shown in FIG. 7, when circuitry 130A, circuitry 130B and light shroud 132 are assembled together and inserted into circuitry cavity 173 of sensor body 170, a portion of light shroud 132 extends into light pathway channel 176 to inhibit light from bleeding back onto optical sensors 150.

[0084] Light source 146 is configured to illuminate a fluid sample to cause the fluid sample to fluoresce, reflect or absorb light in a manner that may be measured by sensor device 150. The brightness, wavelength, or both of light source 146 may be modulated by circuitry 130, for example, by DAC circuitry which is in communication with an MCU. In some embodiments, light source 146 comprises an electronically modulated precision light source, for example, one or more light emitting diodes (LEDs). As an example, light source 146 may comprise several LEDs which are multiplexed by a switching circuit of circuitry 130 to the DAC in some embodiments. Other types of light sources 146 may also or alternatively be utilized including, for example, lasers, xenon arc lamps, phosphor-based white light sources, incandescent lamps or any other type of light source. Light source 146 may be configured to emit in any electromagnetic wavelength including, e.g., visible light, radio, microwave, infrared, ultraviolet, deep ultraviolet, x-ray, gamma ray or any other wavelength of electromagnetic radiation. For example, in some embodiments, a type of light source 146 may be selected based on characteristics or parameters associated with a target analyte, reagent, environment, or any other characteristics or parameters.

[0085] In some embodiments, a brightness detector 148 is located on circuitry 130B such that when circuitry 130B is assembled with light shroud 132, brightness detector 148 is exposed to light from light source 146 and able to measure the light output by light source 146. Such measurements by brightness detector 148 may be utilized, for example, to quantify the amount of light being generated and provided to the sample by light source 146, for calibration or for any other purpose. As an example, components of circuitry 130 (e.g., a DAC and MCU), light source 146 and brightness detector 148 may be configured as a closed-loop constant-brightness light source systemthat is configured to reduce or inhibit errors caused by temperature fluctuations or service life degradation of the electronic and optical components. In some embodiments, brightness detector 148 is optically isolated from reflections or emissions of the fluid sample contained within sample measurement unit 190.

[0086] Optical sensors 150 are disposed on circuitry 130A and positioned such that they are exposed to light received via light pathway channels 174 from a fluid sample contained in sample measurement unit 190. Optical sensors 150 may comprise, for example, photodiodes or any other type of optical sensor. In some embodiments, optical sensors 150 may comprise six optical sensors, e.g., as shown in FIG. 6. In other embodiments, any other number of optical sensors 150 may be utilized, e.g., 1, 2, 4, 6, 8, 10, 12 or any other number. In some embodiments, optical sensors 150 may be arranged radially around light source 146. In other embodiments, optical sensors 150 may be arranged in any other manner relative to light source 146. Optical sensors may be configured to detect any electromagnetic wavelength including, e.g., visible light, radio, microwave, infrared, ultraviolet light, x-rays, gamma rays or any other wavelength of electromagnetic radiation. For example, in some embodiments, a type of each optical sensor 150 may be selected based on characteristics or parameters associated with a target analyte, reagent, environment, or any other characteristics or parameters. For example, the type of optical sensor 150 may be selected based on a wavelength of electromagnetic radiation to be detected.

[0087] Filters 152 may be assembled on optical sensors 150 as shown in FIG. 7 such that each filter 152 filters light received by a corresponding optical sensor 150 from a corresponding light pathway channel 174. As an example, filters 152 may be disposed on optical sensors 150, e.g., as a film or layer. In some embodiments, filters 152 may have the same shape as optical sensors 150. In some embodiments, filters 152 may comprise band-pass filters which correspond with emission or reflectance peaks of a variety of chemical compounds. The bandpass filters may, for example, be cylindrical with the bandpass filter coating on one of the circular surfaces, an anti- reflective coating on the opposite circular surface, and a light absorbing coating, e.g., a black coating, around the cylindrical diameter. In some embodiments, the combination of an optical sensor 150 with a corresponding filter 152 may form a non-dispersive optical sensor.

[0088] Sensor body 170 also comprises a reagent flow channel 178 and a fluid flow channel 180 that are disposed in fluid communication with reagent tubing 112 and fluid tubing 114, respectively, when sampling and measurement unit 160 is installed in housing 120.

[0089] With reference to FIGS. 7-13, sample measurement unit 190 comprises a reagent flow channel 194, a fluid flow channel 196, a sample flow channel 198, a sample mixing chamber 200 and a fluid distribution chamber 202. Each of reagent flow channel 194, fluid flow channel 196, sample flow channel 198, sample mixing chamber 200 and fluid distribution chamber 202 are disposed in fluid communication with each other. In some embodiments, fluid distribution chamber 202 is configured to receive a porous member 192 between an inlet from fluid flow channel 196 and sample mixing chamber 200.

[0090] Cap 210 comprises a cavity 212 that is configured to receive sample measurement unit 190. Cap 210 also comprises a reagent flow channel 214, a fluid flow channel 216 and a sample flow channel 218.

[0091] Sampling and measurement unit 160 is assembled by attaching sensor body 170, sample measurement unit 190 and cap 210 together, for example, as shown in FIGS. 7-13. As shown in FIG. 7, reagent flow channel 214 is disposed between reagent flow channel 178 of sensor body 170 and reagent flow channel 194 of sample measurement unit 190 to provide fluid communication between reagent flow channels 178 and 194 for dispensing reagent into sample mixing chamber 200. Fluid flow channel 216 is disposed between fluid flow channel 180 of sensor body 170 and fluid flow Reagent flow channel 196 of sample measurement unit 190 to provide fluidcommunication between fluid flow channels 180 and 196 for dispensing fluids into sample mixing chamber 200 via fluid distribution chamber 202 and porous member 192.

[0092] With reference to FIGS. 10-13, the use and function of sample mixing unit 190 is described in an embodiment. One function of sample mixing unit 190 is to react a predetermined volume of the fluid system with a predetermined volume of reagent and to optically interface the mixed sample with the optical sensors 150.

[0093] Cap 210 and sample mixing unit 190 are immersed within a fluid of the fluid system with fluid flowing past cap 210. Cap 210 is configured to cause turbulence in the fluid which creates a pressure differential between the upstream and downstream sides of the cap 210. Opposing orifices 220 (FIG. 5) of the cap 210 provide access to sample flow channel 218 and allow a portion of a fluid in the fluid system to enter cap 210 as a fluid sample. In an embodiment, sample flow channel 218 is a flat, pancake shaped void in cap 210, e.g., providing fluid flow between orifices 220 as a substantially flat sheet of fluid. In other embodiments, sample flow channel 218 may have other shapes or configurations. In some embodiments, powered doors or valves may be actuated to open and close off orifices 220 before, during and after measurement to isolate any fluid sample contained within measurement and sensing unit 160.

[0094] Sample flow channel 198 fluid couples sample flow channel 218 to sample mixing chamber 200. Sample mixing chamber 200 is fluidly coupled to sample flow channel 218 by sample flow channel 198. Sample flow channel 198 is configured to provide a sufficient amount of separation distance and a sufficiently small cross- sectional area between sample mixing chamber 200 and sample flow channel 218 in order to inhibit significant amounts of diffusion or washing of fluid materials into the sample mixing chamber 200 during measurement which may corrupt the accuracy of measurements.

[0095] Sampling and measurement unit 160 is configured to rapidly disperse a fixed volume of reagent into an isolated portion of the fluid sample. The geometry of sample mixing chamber 200 may be structured to create crosscurrents or eddy currents in the presence of an alternating displacement pressure wave produced by control station 300. In an embodiment, the sample mixing chamber 200 comprises a conical shape with sample flow channel 198 being located at the tip of the cone. Other configurations may alternatively be utilized.

[0096] At the opposite end of the sample mixing chamber 200 is an opening to a fluid distribution chamber 202, e.g., a circular opening in some embodiments. In some embodiments, a porous member 192 such as, e.g., a sintered fluoropolymer disk, plastic screen, a membrane or another porous member, is positioned within fluid distribution chamber 202 across the opening and sealed around the circumference to the fluid distribution chamber 202 such that fluid flowing between fluid distribution chamber 202 and sample mixing chamber 200 is forced through the porous material. When fluid flows through the porous member 192, a backpressure may be exerted evenly across the surface which causes an equalization of the flow rate across the surface and through porous member 192. Porous member 192 may comprise or be formed of porous matrix materials such as, e.g., plastic, organic polymer, elastomer, cellulose, stainless steel, graphite, ceramic or other porous matrix materials.

[0097] As mentioned above, fluid mixing chamber 200 is fluidly coupled to fluid, reagent and sample channels. Fluids such as water, Dimethylformamide (DMF), or other fluids are delivered from fluid flow channel 196 to fluid mixing chamber 200 via fluid distribution chamber 202 and porous member 192. Reagents are delivered to fluid mixing chamber 200 from reagent flow channel 194 and samples of the fluid are delivered to fluid mixing chamber 200 via sample flow channels 218 and 198.

[0098] When a fluid such as water or DMF is pumped via fluid distribution chamber 202 through the large end of fluid mixing chamber 200 toward the small end, flow is mostly laminar, with flow velocity increasing as fluid mixing chamber 200 tapers. In this manner, it is possible to completely purge fluid mixing chamber 200 bypumping in one direction, with water or another purging fluid entering through porous member 192 and exiting through sample flow channel 198 the small orifice into the fluid of the fluid system via sample flow channel 218 and orifices 220.

[0099] When fluid is pumped through fluid flow channel 196 in reverse, sample fluid from the fluid system is drawn into the sample mixing chamber 200 from sample flow channel 218 via sample flow channel 198. In some embodiments, pump control module 312 of control station 300 may be configured to intelligently modulate flow patterns within the sample mixing chamber 200 by modulating the flow rate and flow direction. For example, when pumped slowly, fluid entering sample mixing chamber 200 through sample flow channel 198 is able to expand radially into the widening conical void of sample mixing chamber 200. The conical shape results in decreasing flow velocity of the sample, causing a slight pressure gradient from the entry point of the sample near sample flow channel 198 to the porous member 192. In this manner, it is possible to fill sample mixing chamber 200 with mostly fluid of the fluid system by pumping slowly in reverse.

[0100] If a reverse flow is rapidly pulsed, fluid from the fluid system may be jetted through sample flow channel 198 into sample mixing chamber 200. The inertia of the high-velocity liquid carries it past the tapered middle region of sample mixing chamber 200 towards the large end and porous member 192, forming eddy currents within the conical void, which may be toroidal in shape.

[0101] In some embodiments, the volume and cross-sectional area of sample flow channel 198 may be designed based on a target flow rate during such pulsing. For example, in some embodiments, the length or diameter of sample flow channel 198 may be selected so that it has a volume that is greater than the displacement volume of the pulses. Likewise, the pulses may be tuned so that the displaced volume is less than the channel volume of sample flow channel 198. In this manner, oscillating flow pulses may be utilized without ejecting fluid from sample mixing chamber 200 into the fluid system. In some embodiments, the magnitude and frequency of altemating / oscillating flow pulses may also be tuned based on the viscosity of the fluids being utilized in order to achieve specific eddy current patterns and maximize mixing action.

[0102] As seen in FIG. 7, light from light pathway channel 176 is directed at sample flow channels 198 and 218 and light is received from sample flow channels 198 and 218 by light pathway channels 174. In some embodiments, a focal region of light pathway channels 174 and 176 may be within sample flow channel 198, within sample mixing chamber 200 or within sample flow channel 218 when sampling and measurement unit 160 is assembled. In other embodiments, the focal region may alternatively be any other portion of sample measurement unit 190 or cap 212.

[0103] With reference again to FIGS. 1 and 7, circuitry 130 of sensor device 110 comprises one or more processing devices 250, an IO interface 252 and memory 254.

[0104] Processing device(s) 250 may comprise, for example, a processor, a microprocessor, a microcontroller (MCU), an application-specific integrated circuit (ASIC), a field-programmable gate array (FPGA), a graphics processing unit (GPU), a printed circuit board (PCB), or any other processing device.

[0105] Circuitry 130 may also comprise any of an analog-to-digital converter (ADC), a digital-to-analog converter (DAC), sensor interfaces, photomultipliers, motor controllers, a power supply, or any other type of circuitry, as well as portions or combinations of such circuitry elements. Circuitry 130 may comprise electrical fault protection circuitry in order to ensure resilience to electrical noise commonly found in industrial facilities. One or more of light source 146, optical sensors 150 and brightness detector 148 may be physically coupled to circuitry 130 or may be attached to housing 120 in another manner.

[0106] Memory 254 may comprise, e.g., random access memory (RAM), read-only memory (ROM), flash memory or other types of memory, in any combination. The memory and other memories disclosed herein shouldbe viewed as illustrative examples of what are more generally referred to as “processor-readable storage media” that may store executable program code of one or more software programs. In some embodiments, memory 254 may store one or more software files that are executable to implement a calibration framework and perform one or more computational algorithms that control the operation and processing of sensor device 110 and one or more calibration profiles that may be used when processing sensor data 260 obtained by optical sensors 150. Sensor data 260 generated by optical sensors 150 may also be stored in memory 254. In some embodiments, memory 254 may also or alternatively comprise removable storage media such as, e.g., a flash drive, USB drive, external hard drive or other removable storage media for storing sensor data 260. In some embodiments, for example, a technician may periodically remove the removable storage media, download sensor data 260 and reattach the removable storage media.

[0107] IO interface 252 may comprise a wired or wireless communication interface. In some embodiments, IO interface 252 may comprise a serial communication interface such as, e.g., a serial communication interface in accordance with RS-485 standards. Other wired interfaces may alternatively be utilized. In some embodiments, sensor device 110 may communicate with control station 300, main control computing system 400, sensor data storage 410, control mechanism 600 or any other industrial process control equipment using a standardized protocol such as, e.g., MODBUS or another standardized protocol. In other embodiments, any other communication protocol may also or alternatively be utilized.

[0108] In some embodiments, electrical connections may be vulnerable to corrosion from an acidic environment. Sensor device 110 may be configured for non-electrical communication with the host computer, such as RF telemetry or fiber optic communication. For example, sensor device 110 may be configured to receive power without electrical communication, e.g., through a fiber optic cable or an on-board energy harvesting system.

[0109] While four circuit boards are illustrated for circuitry 130, other configurations including fewer circuit boards or a larger number of circuit boards with the same or alternative functionality may also or alternatively be utilized. As an example, in some embodiments, the functionality and components of circuitry 130A and 130B may be implemented on a first circuit board and the functionality of circuitry 130C and 130D may be implemented on a second circuit board. Any other combination of circuit boards and functionality may alternatively be utilized.

[0110] With reference to FIGS. 8 and 9, in some embodiments, some or all of circuitry 130 may also or alternatively be located in control station 300 instead of in sensor device 110, e.g., as part of an industrial computer, as separate circuitry or in any other manner. For example, in some embodiments, sensor body 170 may comprise a fiber optic or other light transfer mechanism 186 that may be utilized to optically connect circuitry 130 disposed in control station 300 to window 172, e.g., optically connect one or more light sources and optical sensors disposed in control station 300 to window 172 via one or more fiberoptic cables or other light transfer mechanisms. In some embodiments, control station 300 may be optical connected to sensor body 170 via a fiber optic cable 188. A lens component 189 may be disposed in cavity 182 between window 172 and light transfer mechanism 186 and configured to focus light traveling between light transfer mechanism 186 and window 172 in either direction.

[0111] The environment occupied by sensor device 110 may contain corrosive or biological substances that act to degrade the components of sensor device 110 over time. Sensor device 110 may be designed to anticipate interface surfaces that may be subject to destructive substances. For example, exterior surfaces of sensor device 110 or those components being exposed to the fluid system or other hazardous or corrosive environments may be formed of materials that may be resistant to these environments such as, e.g., fluoropolymers, e.g., Polytetrafluoroethylene, PVDF, etc., plastic materials, metal or glass-coated graphite, ceramics or other materials as needed to facilitate the deployment of sensor device 110 within those environments, to extend the life of sensor device 110 within thoseenvironments or for any other purpose. In some embodiments, inner cavities or components of sensor device 110 may be filled with corrosion-inhibiting substances such as oil or epoxy where feasible in order to reduce the occurrence of degradation in the components.

[0112] Additional embodiments of sensor devices are also described in U.S. Patent Application Serial No. 18 / 340,967, filed June 26, 2023, entitled “AUTONOMOUS MEASUREMENT SYSTEM FOR PERFORMING CHEMICAL CONCENTRATION MEASUREMENTS IN AN INDUSTRIAL PROCESS STREAM,” and International Patent Application No. PCT / US23 / 74423, filed September 17, 2023, entitled “AUTONOMOUS MEASUREMENT SYSTEM FOR PERFORMING CONCENTRATION MEASUREMENTS IN A FLUID STREAM,” the entirety of each of which is incorporated herein by reference.

[0113] Control Station

[0114] With reference again to FIGS. 1-3, control station 300 comprises one or more metering pumps 302, processing device(s) 304, memory 306, an IO interface 308, a network interface 310, valves, transducers or any other components that may be utilized to support and control fluid and data connections with sensor device 110. Processing device 304, memory 306 and IO interface 308 may function in a similar manner to those components described above for sensor device 110. One or more of the electrical components of control station 300 may also or alternatively be mounted or integrated into one or more circuit boards 320, e.g., forming an industrial computer. In some embodiments, a single control station 300 may service several sensor devices 110.

[0115] Control station 300 may comprise several precise metering pumps 302, such as peristaltic pumps or piston pumps, and may comprise one or more refillable reservoirs 322 for storing reagents or other fluids. Reservoirs 322 may be located internal or external to the case of control station 300 depending on factors such as, e.g., operating environment, reagent characteristics, etc. For example, a reagent that may break down when exposed to light, heat or another environmental variable may be stored in an appropriate manner, e.g., in a blackout reservoir, in a climate- controlled reservoir or in any other manner. Control station 300 may also or alternatively be connected with piping to sources of reagents or other fluids that are located at a central reservoir, larger storage tanks or other sources of reagents or fluids. For example, a central reservoir may be located at any distance from the metering site such as, e.g., in a laboratory, and may be utilized to supply reagents or other fluids to one or more sensor devices 110.

[0116] Processing device 304 is configured to collect and store sensor data 318 from one or more sensor devices 110, e.g., via IO interface 308, and send commands to one or more sensor devices 110 during reagent metering according to pump control module 312 stored in memory 306. Sensor data 318 may comprise raw sensor data, e.g., digital or analog signals output by optical sensors 150 or other components of circuitry 130A, sensor data that is pre- processed by circuitry 130 such as removal of noise, selection of peak values, etc., or any other form of sensor data received from sensor devices 110. In some embodiments, processing device 304 may be configured to perform computation module 316 on sensor data 318 received from a sensor device 110 to determine a concentration of a particular analyte. The output of computation module 316 may be stored as part of the corresponding sensor data 318. In some embodiments, the sensor data 318 may be received from the sensor device 110 after the sensor device 110 has performed concentration processing logic where, for example, sensor data 318 may comprise one or more of raw sensor data, processed sensor data, and concentration values for the target analyte.

[0117] Memory 306 comprises on-board memory and also, in some embodiments, removable storage media such as, e.g., a flash drive, USB drive, removable hard-drive or SSD, or any other removable storage media. In some embodiments, for example, sensor data 318 may be stored in the on-board memory of control station 300, in the removable storage media or both. For example, if the target environment where measurements are being taken is located in a remote area without network connectivity, sensor data 318 stored in the removable storage media maybe obtained by a technician for later processing, e.g., using a portable computing device. The technician may then provide the sensor data 318 to computer system 400 once the technician returns to a network connected location.

[0118] Network interface 310 may comprise a wired or wireless communication interface that is configured to communicate with sensor device 110, computing system 400 and sensor data storage 410, e.g., via network 118.

[0119] In some embodiments, processing device 304 may also be configured to push updated calibration profiles to sensor device 110 for storage on sensor device 110 and for use by sensor device 110 in future measurements.

[0120] One fluid that may be utilized by the sensor device 110 is water. For example, pure water may be used to purge the sample mixing unit 190 of mixed fluid in between individual measurement cycles. High-purity water such as distilled water or reverse-osmosis water may be used in order to ensure that contaminants in the purging water do not cause false signals. In other embodiments, the purge liquid may be any other pure liquid, such as an organic solvent. In some embodiments, pumps may circulate fluids from the fluid system for purging.

[0121] Water, being an incompressible fluid, may also provide hydraulic energy transfer functionality in system 100. Metering pumps 302 contained in control station 300 are able to produce precise fluid displacements. Displacements that are generated in the control station 300 are conserved through the tubing leading to sensor device 110 and are transferred as alternating flow pulses to the sample mixing unit 190. Metering pumps 302 may be under computer control by processing device 304 to produce alternating flow at high frequency, for example, at sonic frequency or ultrasonic frequency. Alternating flow pulses transduced by computerized metering pumps may be used to induce eddy currents and mixing within the sample mixing unit 190 of each sensor device 110.

[0122] An example reagent circuit of control station 300 may comprise an intake tube of a metering pump 302, such as a piston syringe pump, valve-less metering pump, peristaltic pump, diaphragm pump or another pump, connected to a reservoir 322 storing a reagent. Metering pump 302 may be driven by an actuator under control of pump control module 312, such as a servo motor. Reservoir 322 may comprise, for example, a Pyrex bottle, a sealed container such as a canister that is pressurized with inert gas, a sealed stainless-steel tube that contains pressurized reagent being supplied from a nearby laboratory or any other type of reservoir 322 which may be selected based on the environment surrounding the fluid system. Metering pump 302 acts to dose a specific volume of fluid into tubing 112 for delivery to sensor device 110.

[0123] In some embodiments, a pressure wave transducer 324 (FIG. 3) may be connected in parallel with fluid tubing 114. Pressure wave transducer 324 may comprise a linearly actuated pressure surface, such as a piston or diaphragm which acts to displace a specific volume of fluid in fluid tubing 114 as the pressure surface travels from its minimum stroke position to an extended position. The pressure surface may be driven by a computer-controlled actuator such as a solenoid, voice coil, piezoelectric actuator, ultrasonic transducer, or a rotary motor that is connected to a cam shaft. Pressure wave transducer 324 comprises a sealed chamber with at least one surface that is actuated in order to produce volumetric displacement and pressure waves. The pressure waves may have a symmetrical alternating displacement waveform such as, e.g., a sine wave.

[0124] Fluid tubing 114, being connected to pressure wave transducer 324, has a flow rate that is equal to the displacement generated by metering pump 302 in addition to displacement generated by pressure wave transducer 324. By utilizing both metering pump 302 and pressure wave transducer 324, it is possible for control station 300 to produce fluid flow patterns that comprise alternating sine waves that are superimposed on precise computer- controlled positive displacement flows.

[0125] Similar functionality may also be utilized to control the flow of reagent through reagent tubing 112.

[0126] Main Control Computing System

[0127] Main control computing system 400 may comprise one or more processing device(s) 402, memory 404, a network interface 406 or any other components commonly used by a computing system. Processing device 402, memory 404 and network interface 406 may function in a similar manner to those components described above for sensor device 110 and control station 300. In some embodiments, computing system 400 may store calibration profiles that are utilized to calibrate sensor device 110. For example, the calibration profiles may be generated based on lab-based analytical testing to configure and calibrate the parameters of sensor device 110. Calibration profiles may be pushed down to control station 300 for storage or transfer to sensor device 110 or directly to sensor device 110.

[0128] Sensor data storage 410 comprises data storage devices or data storage systems that are configured for storage of large volumes of sensor data that may be utilized by computing system 400. Example data storage devices that may be utilized by sensor data storage 410 include hard disk drives (HDD), solid state drives (SSDs) or other storage technologies. In some embodiments, the data storage devices may be implemented using non-volatile memory (NVM) devices such as flash memory.

[0129] Control Mechanism

[0130] Control mechanism 600 may comprise any control mechanism that may be commanded by main control computing system 400 to adjust an operational parameter of system 100, e.g., based on sensor data 260 obtained from sensor device 110 or sensor data 318 obtained from control station 300. For example, main control computing system 400 may be configured to command control mechanism 600 to actuate a valve to redirect a flow of fluid, the feedstock, the PLS or any other liquid in the fluid system. In some embodiments, control mechanism 600 may be configured to actuate a motor or other device to activate or deactivate the dispensation of a lixiviant or other chemical agent, to increase or decrease a dispensation of the lixiviant or other chemical agent, or to otherwise adjust another parameter of the extraction process. In some embodiments, main control computing system 400 may be configured to command control mechanism 600 to activate or deactivate a valve, motor or other mechanism to start, stop or otherwise inhibit the flow of feedstock into system 100 or to redirect the flow of feedstock or fluids in portions of the fluid system to another location.

[0131] Autonomous Reactor Unit

[0132] With reference to FIG. 14, an embodiment of an Autonomous Reactor Unit (ARU) 1000 is disclosed that is configured to implement nominal execution of a particular chemical process in the presence of fluctuating environmental parameters. Some example environmental parameters that may fluctuate include pH fluctuations, temperature fluctuations, barometric pressure fluctuations, bacterial colonization of the vessel, fluctuations in feedstock composition or any other environmental parameter associated with or relevant to the particular chemical process.

[0133] The term “Autonomous Reactor Unit” or “ARU” as used here in describes a repeating unit that may be part of a larger chemical processing system. In an embodiment, an ARU comprises a portion of the fluid system such as, e.g., at least one fluid vessel, at least one sensor device, e.g., a sensor device 110, and at least process control unit (PCU), however more sophisticated embodiments of ARUs are also described herein. The PCU may be implemented as part of control station 300, main control computing system 400, or both as an example. In some embodiment, the materials and processes within a given ARU may be under intelligent control and may be independent from the processes occurring in any other ARU. In some embodiments, multiple ARUs may interact with each other or interact with a central PCU in order to accomplish intended system outputs. For example, multiple ARUs may utilize the same control station 300, main control computing system 400 or both in some embodiments.

[0134] ARU 1000 comprises a Process Control Unit (PCU) 1200 and one or more sensor devices 1300. In some embodiments, PCU 1200 may be implemented as part of control station 300 (FIG. 1), e.g., utilizing processing device(s) 304, memory 306 and any other components of control station 300, part of main control computing system 400 (FIG. 1), e.g., utilizing processing device(s) 402, memory 404 and any other components of main control computing system 400, or as part of a combination of control station 300 and main control computing system 400. In some embodiments, PCU 1200 may be implemented by a combination of both control station 300 and main control computing system 400. An example sensor device 1300 may comprise, e.g., sensor device 110 such as described above.

[0135] ARU 1000 may also comprise one or more additional components depending on the type of hydrometallurgical process being monitored and controlled. Such additional components may comprise, e.g., a fluid vessel 1102, one or more auxiliary sensors such as, e.g., a pH sensor 1104, a temperature sensor 1106, any other sensors or any combination thereof, valves / pumps 1108, heaters / chillers 1110, motorized mixers 1112, motorized conveyor belts, motorized skimmers 1116, ultrasonic transduction agitators 1118, light sources 1120, sump 1122, baffle 1124, metering pump 1126 or any combination thereof. Any of the above components may be autonomously controlled by PCU 1200. PCU 1200 may communicate with any of the additional components, e.g., via one or both of network interfaces 310 and 406.

[0136] PCU 1200 comprises ARU control logic 1208 (FIG. 1) that may be stored in memory, e.g., memory 306, memory 404, or both, and executable by one or more processing devices, e.g., processing device(s) 304, processing device(s) 402, or both. ARU control logic 1208 comprises algorithms and functionality as described herein for controlling the operation of one or more ARUs 1000, e.g., activating and deactivating pumps or other components, opening and closing valves, and performing other actions based on data inputs from sensor devices 1300, pH sensors, temperature sensors or any other sources. For example, such other components may comprise control mechanism 600. In some embodiments, external data sources may also be utilized such as, e.g., weather data or other data that may impact the performance of a hydrometallurgical process.

[0137] ARU 1000, PCU 1200 and sensor device 1300 may facilitate technology transition from research to large- scale commercial operations. For example, research and process flowsheets are typically developed in a laboratory setting and often only consider a limited number of failure modes and nominal idealistic outcomes of a chemical process specification. Process specifications developed by users based on such research or based on any other data are migratable to PCU 1200 using computer software which adjusts ARU control logic 1208 for controlling ARU 1000, e.g., based on data obtained from sensor device 1300 or any other environmental data. PCU 1200 may maintain process variables for one or more of the above-mentioned environmental parameters in order to perform the prescribed process.

[0138] In some embodiments, sensor device 1300 comprises an Active-Sensitization Fluorometer (ASF). The ASF is configured for positioning at least partially within a fluid of the fluid system, e.g., within a fluid vessel of the ARU, to react a liquid sample with a fluorescent sensitizer reagent such as, e.g., a Zinc Adeninate Metal Organic Framework dispersed in dimethyl formaldehyde and water such as that described in “Influence of the Anionic Zinc- Adeninate Metal-Organic Framework Structure on the Luminescent Detection of Rare Earth Ions in Aqueous Streams” by Scott E. Crawford et al., ACS Applied Materials & Interfaces 2021 13 (6), 7268-7277. In some embodiments, sensor device 1300 is configured to emit ultraviolet light which is absorbed by the reagent. The reagent acts to transfer electrons to element ions, causing the ions to emit light. The emitted light possesses a unique spectral signature that is identifiable by the sensor device 1300. Sensor device 1300 is also referred to herein as an Integrated Active-Sensitization Fluorometer (IASF). While sensor device 1300 is described as using ZincAdeninate Metal Organic Framework, any other fluorescent sensitizer reagent may alternatively be utilized, e.g., depending on the properties of an element targeted for separation. Similarly, while sensor device 1300 is described as emitting ultraviolet light, sensor device 1300 may be configured to also or alternatively emit any other type of light. In some embodiments, sensor device 1300 may also or alternatively be configured to detect reflectance or absorption of a target element where, in such an embodiment, a fluorescent sensitizer reagent may not need to be dispensed or otherwise utilized.

[0139] ARU 1000 is configured to implement high-fidelity measurement and control in real-time through the use of PCU 1200 and one or more sensor device 1300 located in-situ at the hydrometallurgical process itself, as compared to manually operated systems or systems that are maintained using traditional ICP-S sampling and assaying techniques. ARU 1000 may be utilized for various types of separation techniques and hydrometallurgical processes by leveraging the flexible hardware and software configurations of sensor devices 1300 or by modifying other software parameters.

[0140] Lixiviant Leaching

[0141] When ore or another raw material is immersed in a lixiviant, the concentration of lanthanides and aluminum MOI increases as a function of time as part of a leaching process. Historically this increase in concentration has been demonstrated using ICP-S assays. As an example, small fluid samples are typically collected at regular time intervals throughout the leaching process and then all of the samples are sent to a laboratory as a batch where the concentration measurements of each sample are performed using an ICP-S assay. The data resulting from the assay is compiled in a 2D plot, also referred to as a profile. This method of concentration measurement is limited in its ability to make real-time adjustments to the leaching process due to the long lead time between when the sample is obtained, and the results of the assay are generated. In order to mitigate this concern, the chemical engineering discipline typically focuses on the development of well-understood process flowsheets. However, even where systems execute these rigid procedures, the outcomes may still fluctuate with each batch over time due to the lack of actionable real-time data.

[0142] Control algorithms of PCU 1200 may be configured to accept manual data entry of configuration data that is generated based on external instrumentation or external laboratory assays in order to improve the precision of the process. For example, high-accuracy ICP-based data may be entered once per month, allowing PCU 1200 to recalibrate the rough measurements obtained from the in-process sensor devices 1300.

[0143] In one example, coal, also sometimes referred to as carbon ore, comprises components such as, e.g., carbon, clay, lanthanides and aluminum. The majority of coal is carbon and clay. In some cases, one or more of the lanthanides may be MOIs while aluminum may be considered a contaminant. Lanthanides are typically released rapidly during the leaching of coal, e.g., within 120 seconds for example, while aluminum is released at a significantly slower rate. One challenge in operating a selective leaching process at scale is that the exact leaching rate and time for each component varies with each batch of feedstock, e.g., ore, AMD or other solid, liquid or mixed material feedstock, and may also vary with temperature. The use of static process designs and flowsheets such as those mentioned above are typically unable to effectively address these concerns due to a lack of actionable realtime data. For example, if a fluid vessel is drained too early, valuable MOI materials will be left in the feedstock and will be wasted. Instead, static process designs and flowsheets are designed to always drain the fluid vessel after ample time has been allowed for the lanthanides or other MOIs to be released. This conservative strategy results in a leachate solution that has a higher level of contamination, e.g., aluminum in this case, as compared to a process that is capable of draining the fluid vessel based on actionable real-time data that be used to verify that a threshold concentration of the MOI has been released or a threshold rate of release has been achieved, e.g., a target leach ratebelow a minimum threshold. The use of ARU 1000 enables process controls that mitigate contamination during leaching, inhibit costly lixiviants from being overconsumed, and decrease the cost of subsequent refinement operations which would be needed to remove the additional contamination that typically results from a static process.

[0144] One or more sensor devices 1300 of ARU 1000 may be configured to measure both the concentration of various MOIs, e.g., lanthanides or other elements, and also the concentration of various contaminants, e.g., aluminum, iron, or other contaminants. Such real-time measurements of both MOIs and contaminants enable PCU 1200 to calculate a ratio of MOIs to contaminants directly during the chemical process. By using this information, PCU 1200 may execute processes controls that maximize the total extracted MOI in the output, maximize the separation ratio of MOI to contaminants in the output, minimize the contaminants in the output or maximize, minimize or adjust any other parameter of the process to reach a desired output. For example, the extraction rate, e.g., in units of ppm-per-minute, of an MOI such as neodymium may be greater than the extraction rate of a contaminant such as iron. A material’s extraction rate may also be non-linear. For example, the extraction rate for a particular MOI or contaminant may have a first rate initially and may increase, decrease, or both over time. In some cases, the extraction rate for a particular MOI or contaminant over time may be defined by a curve or other rate plot, e.g., increasing and then decreasing or vice versa. By using real-time concentration measurements of MOIs, contaminants, or both, the relative purity of a leachate may be controlled or maximized, e.g., by terminating the process when the separation ratio peaks. As an example, when the separation ratio peaks or another threshold in concentration or extraction rate is met for one or more MOIs or contaminants, PCU 1200 may cause the vessel to be drained.

[0145] Analyzer ARU

[0146] With reference to FIG. 15, an example analyzer ARU 1800 will be described according to another embodiment. Analyzer ARU 1800 is configured for pre-processing or optimizing the sample fluid prior to measurement. For example, analyzer ARU may be utilized to further digest the sample fluid, e.g., by adding additional acids or other chemicals to a small sample, optimizing the separation-factor in refinement processing systems, such as, e.g., centrifuge separators, mixer-settler circuit systems or other refinement processing systems, or performing any other process on a sample obtained from a fluid system prior to measurement by a sensor device 110. In some embodiments, for example, salts and carbonates may be digested by analyzer ARU 1800 into a form that is measurable by the sensor device 110.

[0147] Analyzer ARU 1800 comprises a vessel 1802 and a vessel 1804 that are fluidly connected by a valve or orifice 1806.

[0148] Vessel 1802 comprises a cavity 1808 that is fluidly connected to a sample inlet 1810, e.g., a tube or other type of inlet, by a valve 1812 and fluidly connected to a reagent inlet 1814, e.g., a tube or other type of inlet, by a valve 1816. Valves 1812 and 1816 may comprise one-way values such as, e.g., check valves, which are configured to inhibit the flow of fluids from cavity 1808 into sample inlet 1810 and reagent inlet 1814. Similarly, valve or orifice 1806 may also comprise a one-way valve that is configured to inhibit the flow of fluids from vessel 804 into vessel 1802. An agitator 1818 is disposed at least partially within cavity 1808 or disposed against a side of vessel 802 and is activatable to agitate the contents of vessel 1802, e.g., physically, ultrasonically or in another manner.

[0149] A valve or orifice 1806 is configured to maintain a pressure differential between cavities 1808 and 1820 while sample materials are flowing through cavity 1808, then through valve or orifice 1806 into cavity 1820. In some embodiments, the pressure differential between cavity 1808 and cavity 1820 inhibits a backflow of materials from 1802 into 1808, for example, in the event of an exothermal reaction or gasification of the mixture in 1820.

[0150] Cavity 1820 of vessel 1804 is fluidly connected to an outlet 1822, e.g., a tube or other type of outlet, by a valve 1824. Valve 1824 may comprise a one-way valve that is configured to inhibit the flow of fluids from outlet 1822 into vessel 1804. A sensor device 1826 such as, e.g., a sensor device 110 (FIG. 1), is disposed at least partially in cavity 1820 and comprises a data communication interface 1828, e.g., a wired data input / output connection 116 as shown in FIG. 1, a wireless interface or both, and a fluid reagent inlet 1830.

[0151] Analyzer ARU 1800 is configured to digest fluidized samples that contain non-ionized particulate mineral matter such as, e.g., salt crystals, sand, clay, coal fly ash or other matter, which are dispersed throughout a fluid, allowing for mechanical manipulation of the sample by pumping or pressurization through connected tubing. In some embodiments, for example, analyzer ARU 1800 may be utilized to digest one cubic inch of a sample or any other volume of a sample. Analyzer ARU 1800 may be configured to digest and analyze the sample in a continuous fashion where, for example, the sample and a reagent such as, e.g., a lixiviant, are pumped into fluid vessel 1802 at one end of analyzer ARU 1800 via inlets 1810 and 1814, and digested fluid exits analyzer ARU 1800 from the other end via outlet 1822. The analyzed sample may be returned to the process stream where lixiviants such as strong acid are neutralized by abundant minerals or otherwise discarded. In some embodiments, analyzer ARU 1800 may also or alternatively be configured to digest and analyze the sample in batches.

[0152] Vessel 1802 of analyzer ARU 1800 may be constructed of a chemical-resistant material with high heat tolerance, such as, e.g., polytetrafluoroethylene, stainless steel, carbon or another material that may be selected depending on the use case, and is configured to function as a pressure vessel where chemical reactions may occur. For example, a sample may enter cavity 1808 of vessel 1802 from sample inlet 1810, e.g., by pressure generated by an external pump, centrifuge or another source pressure source. A reagent such as an acidic lixiviant may also enter cavity 1808 of vessel 1802 from reagent inlet 1814 at a rate that is proportional to the sample flow rate, at a constant rate or at any other rate. In some embodiments, for example, the flow rate of the reagent may be metered by a dosing pump such as a peristaltic pump. Other types of pumps may alternatively be utilized. The pumping of the sample, reagent, or both into cavity 1808 of vessel 1802 may be configured to generate high pressure within cavity 1808 such that cavity 1808 functions as a pressure vessel. Heating caused by the pressure increase may also assist in rapid digestion of mineral matrices, clays, silica, salt crystals or other materials that are suspended within the sample. A heat source such as, e.g., an electric resistance heating element or another heat source, may be utilized to add further thermal energy to the fluid contained within cavity 1808.

[0153] The heat source in cavity 1808 may be transduced by RF or microwave radiation or heat may be generated by high-frequency alternating current being passed through the material in cavity 1820.

[0154] Agitator 1818, e.g., an ultrasonic transducer, may be mounted in the wall of the vessel 1802. In some embodiments, an end portion of agitator 1818 may be exposed to cavity 1808 where the end portion may be made from a corrosion and abrasion resistant material such as, e.g., tungsten carbide or other materials. The remainder of agitator 1818 may be located external to cavity 1808 of vessel 1802 and configured for receiving electrical energy in the form of high voltage alternating current, e.g., via a wire 1832. Electrical excitation of agitator 1818 is configured to cause a high-frequency and high-energy resonance of the immersed surfaces of cavity 1808, for example, a resonance at 30 KHz. Other resonances may also or alternatively be utilized such as sonic pressure waves, for example, with a frequency of 500 Hz. This resonance may cause a high-pressure standing wave to form within cavity 1808 of vessel 1802. In some embodiments, cavity 1808 may be geometrically shaped to evenly distribute the standing wave. In some embodiments, cavity 1808 may be shaped or otherwise configured to distribute the standing wave in a manner that causes a mixing of the solution contained within vessel 1808. Thecombination of ultrasonic agitation, heat, lixiviant and pressure is configured to result in rapid digestion of minerals contained in the sample.

[0155] Valve 1806 is configured to maintain a predetermined pressure differential within cavity 1808 of vessel 1802. In some embodiments, for example, valve 1806 may comprise an orifice that is formed of an abrasion, heat and chemical-resistant material such as, e.g., tungsten carbide. In some embodiments, valve 1806 may be connected to cavity 1820 of vessel 1804 by high-pressure tubing such as, e.g., stainless-steel tubing. In a case where the digestion described above causes gasification, heating and expansion of the fluid, fluid exiting vessel 1802 may be configured to interface with a chilled surface, such as a heat exchanger j acket disposed around the tubing or orifice, in order to condense the digested sample into liquid form before the digested sample enters vessel 1804.

[0156] A digested sample enters cavity 1820 of vessel 1804 from valve 1806. In some embodiments, cavity 1820 of vessel 1804 may be sized larger than cavity 1808 of vessel 1802, resulting in a decreased flow velocity and dwell time for analysis. Sensor device 1826 is mounted in the wall of vessel 1804 and is configured to performing continuous monitoring of target element ion concentrations within cavity 1820. The continuous flow of liquids in and out of cavity 1820 of vessel 1804, e.g., due to pressure from vessel 1802, maintains a continuous representation of the sample liquid stream. Sensor device 1826 may transmit measurements, e.g., via data communication interface 1828, in units such as parts-per-million, parts-per-billion or other units to a PCU 1200. In some embodiments, sensor device 1826 may dispense a sensitizing reagent into cavity 1820 of vessel 1804 via reagent inlet 1830 that is configured to support or enhance measurements performed by sensor device 1826.

[0157] In some embodiments, sensor device 1826 may utilize a fluorescent sensitizer reagent as part of the measurement process, e.g., as dispensed by reagent inlet 1830. Each fluorescent sensitizer reagent may have different parameters that define the accurate range of measurements by sensor device 1826. For example, sensor device 1826, when using a particular fluorescent sensitizer reagent, may have an accuracy in a range of 2-10 parts- per-million. In other cases, the system for producing concentrates may be configured to operate with target ion concentrations having higher parts-per-million than the accurate range, e.g., 200-1000 parts-per-million. In some embodiments, analyzer ARU 1800 may be configured to dilute the sample in order to produce a continuous stream of diluted sample which is representative of the input sample stream but falls within the measurable range of sensor device 1826 using the particular fluorescent sensitizer reagent. In other embodiments, sample materials of cavity 1820 may be directly excited without sensitizer using high-energy transduction.

[0158] In some embodiments, vessel 1802 or vessel 1804 may comprise a dilution injection inlet 1834 through which a diluting agent may be dispensed into the sample or digested sample. As an example, water or another agent may be utilized as a diluting agent and may be precisely injected into vessel 1802 or 1804 in known quantities at a known rate to ensure consistency in the dilution and the measurement by sensor device 1826. The dilution injection inlet 1834 may comprise a check valve 1836 that is configured to inhibit backflow of digested sample into the dilution injection inlet 1834. The accuracy of diluted measurement may be proportional to the accuracy of mix ratio between the digested sample fluid and dilution fluid. In some embodiments, an ultrasonic mixer 838, similar to agitator 1818, may be mounted in the wall of vessel 804 in order to rapidly mix the diluted solution, ensuring that sensor device 1826 receives thoroughly diluted samples.

[0159] Lixiviant Efficacy Analyzer ARU

[0160] With reference to FIGS. 16-18, in another embodiment, a small-scale analyzer ARU 1900 may be configured as a lixiviant efficacy analyzer under control of corresponding ARU control logic 1208 (FIG. 1). Analyzer ARU 1900 may comprise similar components to ARU 1000 including a fluid vessel 1901 and a sensor device 1300, but may be smaller is size than a full-size commercial process ARU 1000, allowing for faster analysis,less lixiviant waste and less feedstock waste. In some embodiments, analyzer ARU 1900 may alternatively comprise an analyzer ARU 1800 (FIG. 15). In some embodiments, the analysis may also or alternatively be performed directly in the primary stream ARU 1000. Analyzer ARU 1900 is in communication with PCU 1200 (FIG. 14).

[0161] Analyzer ARU 1900 may be utilized to rapidly repeat the leaching process several times using an array of lixiviants having various properties, referred to as lixiviants A-E in FIGS. 16 and 18, to identify and characterize which acid or strength of acid is needed to leach out the target purity of a particular MOI. For example, the lixiviants A-E may be categorized by acidity, acid strength, leaching strength or in any other manner. As an example, lixiviants A-E may comprise a variety of acids that may be utilized as lixiviants for hydrometallurgical digestion including, e.g., Acetic Acid (CHaCOOH), Citric Acid (CeHsO?), Sulfurous Acid (H2SO3), Phosphoric Acid (H3PO4), Hydrochloric Acid (HC1), Nitric Acid (HNOa), Sulfuric Acid (H2SO4), Perchloric Acid (HCIO4), Fluorosulfonic Acid (HSOaF), Triflic Acid (CF3SO3H) or any other acid or other lixiviant that may be used for leaching or digestion of a sample. While the system and process of FIGS. 16-18 is described with respect to the use of lixiviants, any other chemical or agent that may be utilized to perform hydrometallurgical processing may also or alternatively be utilized such as, e.g., sorbents. Similarly, while analyzer ARU 1900 is described for use in analyzing a leaching process, in other embodiments, analyzer ARU 1900 may be utilized in a remediation process where acidity is reduced, e.g., by acid-neutralizing materials such as sodium carbonate or other materials, the effectiveness of which may also be tested by analyzer ARU 1900 in a similar manner to that described below.

[0162] Using analyzer ARU 1900, it is possible for system 100 to auto-adjust or select which lixiviant to utilize for a particular feedstock while in-process to accommodate a wide range of feedstock characteristics or operate reliably while environmental parameters such as temperature or feedstock flowrate fluctuates.

[0163] A primary stream ARU 1000 may operate in tandem with analyzer ARU 1900 for adaptive optimization, for example, as shown in FIG. 16. With reference also to FIG. 17, an example process for operating analyzer ARU 1900 in conjunction with ARU 1000 is also described. The example process of FIG. 17 comprises steps 1950 through 1968 although additional or fewer steps may alternatively be implemented. The process of FIG. 17 may be performed before, after or in conjunction with the filling of mainstream ARU 1000 with feedstock, the activation of heating and agitation of the mainstream ARU 1000 or at any other time.

[0164] At step 1950, a pump 1902 transfers a small fluid sample of feedstock to fluid vessel 1901 of analyzer ARU 1900, e.g., directly from the feedstock fill line 1940 or from fluid vessel 1102 of ARU 1000. In some embodiments, the feedstock of ARU 1000 may be provided with surfactants or acids to cause the feedstock particles to be dispersed in the fluid which may then be pumped into fluid vessel 1901 of analyzer ARU 1900 for efficacy analysis.

[0165] At step 1952, a PSU 1200 of analyzer ARU 1900 activates heating and agitation of the feedstock.

[0166] At step 1954, ARU control logic 1208 of analyzer ARU 1900 activates a sensor device 1300 in analyzer ARU 1900 to obtain sensor data from the filled feedstock in fluid vessel 1901 of analyzer ARU 1900 and characterize the feedstock.

[0167] At step 1956, ARU control logic 1208 of analyzer ARU 1900 computes process parameters related to the feedstock based on the characterization of the feedstock, e.g., pH, temperature or other parameters.

[0168] At step 1958, ARU control logic 1208 of analyzer ARU 1900 activates a metering pump 1904 to dispense a reagent, e.g., a lixiviant in this example, based on the process parameters. For example, lixiviant storage vessels 1906A-1906E, collectively referred to herein as lixiviant storage vessel(s) 1906, may each contain a corresponding lixiviant, e.g., lixiviants A-E. Each lixiviant storage vessel 1906 may also comprise a corresponding valve that maybe actuated to open or close fluid communication between lixiviant storage vessel 1906 and metering pump 1904. In an embodiment where ARU 1000 may also be supplied with lixiviants by the same lixiviant storage vessels 1906, an additional valve 1908 may also be utilized to open or close fluid communication between lixiviant storage vessels 1906 and a metering pump 1942 of ARU 1000, between lixiviant storage vessels 1906 and metering pump 1904, or both.

[0169] In some embodiments, for example, ARU control logic 1208 may dispense lixiviant A into the feedstock in analyzer ARU 1900 to evaluate the efficacy of lixiviant A on the feedstock solution. For example, ARU control logic 1208 may activate the valve on lixiviant storage vessel 1906A and valve 1908, if present, to establish fluid communication between metering pump 1904 and lixiviant storage vessel 1906A, which contains lixiviant A. ARU control logic 1208 may then activate metering pump 1904 to dispense lixiviant A into the feedstock in fluid vessel 1901 of analyzer ARU 1900. In other embodiments, a lixiviant having stronger acidity or other parameter, e.g., lixiviant B, lixiviant C, etc., may be selected as the first test lixiviant based on the computed process parameters. The effectiveness of a lixiviant or extraction process may also be defined by the selectivity of the variant for the MOI over contaminants. For example, the strongest acid may dissolve both MOI and contaminant, while another acid may be preferential for dissolving only the MOI while leaving the contaminant intact, or vice versa. ARU control logic 1208 may also progressively dispense increasing quantities of the selected lixiviant, sweep the temperature range using heaters or chillers or agitate using various frequencies of the ultrasonic transducer as part of step 1958 in order to fully characterize the effectiveness of the selected lixiviant on the feedstock batch.

[0170] At step 1960, sensor devices 1300 are activated to monitor ions in the solution in analyzer ARU 1900 and provide sensor data to PCU 1200. In some embodiments, several combinations of parameters may be evaluated while sensor devices 1300 record data for ion concentration profiles of various elements.

[0171] At step 1962, ARU control logic 1208 determines based on the sensor data obtained from sensor device 1300, whether or not the ion concentration for a target element is rising, has plateaued / decreased, the rate of concentration change or any other parameter of the process. For example, when a lixiviant is added to the feedstock, which may be a mud or sludge, target element ions are released into the liquid. If the concentration is still rising or rising at a rate above a predetermined threshold rate, the process returns to step 1960 and additional ion monitoring is performed. If the concentration is no longer rising or has fallen below the predetermined threshold rate, e.g., the lixiviant is no longer releasing new ions from the feedstock or not releasing ions faster than the predetermined threshold rate, the process proceeds to step 1964.

[0172] At step 1964, ARU control logic 1208 determines whether or not there is an additional reagent available for testing, e.g., whether or not there is a stronger lixiviant left to test in this example. For example, if lixiviants A-C have been tested, ARU control logic 1208 may determine that lixiviant D is still available for testing. If there is a stronger lixiviant that still needs to be evaluated the process returns to step 1958 and the next lixiviant is dispensed. If all stronger lixiviants have already been tested, the process proceeds to steps 1966 and 1968. While reference to stronger lixiviants is utilized, in other embodiments, the order of lixiviant texting may be based on other properties of the lixiviants such as, e.g., selectivity to certain MOIs or contaminants, or any other parameters.

[0173] An example graph of the lixiviant testing is shown in FIG. 18. As shown in FIG. 18, for example, lixiviants A and C each show a substantial increase in ion concentration while lixiviants B, D and E each only show a minor increase in ion concentration. In another example, with reference to FIG. 19, the concentration of an MOI is shown to increase rapidly at the beginning and then plateau, while the concentration of a contaminant slowly increases at a constant rate. Analyzer ARU 1900 may be utilized to pinpoint the ideal time in the process to drain the fluid vessel, shut off lixiviant dispensation or take any other action.

[0174] At step 1966, ARU control logic 1208 computes improved process parameters based on the results of the lixiviant efficacy testing and provides the computed process parameters to PCU 1200 for use in the processing of feedstock in ARU 1000. As an example, based on efficacy data such as that found in FIGS. 18 and 19, ARU control logic 1208 of analyzer ARU 1900 may determine that lixiviants A and C provide the best MOI concentration increases, MOI to contaminant ratio, or other desired outcome and may update the computed process parameters accordingly. ARU control logic 1208 may provide these updated process parameters to ARU 1000 for use in controlling the processing of this batch of feedstock, e.g., to only use lixiviants A and C in ARU 1000 as an example.

[0175] At step 1968, ARU control logic 1208 drains the fluid vessel 1901 of analyzer ARU 1900 to prepare analyzer ARU 1900 for evaluating the next batch of feedstock and the process may return to step 1950. If no more batches need to be processed, the process may alternatively end. While the above steps are described as subsequently testing lixiviant A-E in an order on the same batch of feedstock, in other embodiments, each lixiviant may be evaluated on a separate batch of feedstock to determine the most effective lixiviant or combination of lixiviants on a sample that has not been pre-processed by the other lixiviants A-E.

[0176] Implementing a lixiviant efficacy analyzer in a small-scale analyzer ARU 1900 that may accompany a primary stream ARU 1000 enables autonomous real-time, in-process, efficacy testing of the effect of lixiviants on the particular feedstock in the primary stream ARU 1000 to identify the most efficient combination of lixiviants to be used during the primary stream hydrometallurgical process. This efficient and low-cost efficacy testing in realtime allows the primary stream ARU 1000 to be configured for processing the specific properties of the feedstock using improved and validated process parameters. The use of ARU 1900 does not rely on process control procedures that are based theoretical models, and instead validates the optimal parameters on a batch-by -batch basis or continuously. During the analysis process, the lixiviant analyzer may generate and record datasets per unit time including, for example, ultrasonic frequency, mixer speed, temperature, pH, lixiviant concentration and ion concentration. This data may be communicated to PCU 1200, where the most effective process parameter combination may be selected. Optimized process parameters are then communicated and implemented by PCU 1200 in the mainstream ARU for improved and more efficient bulk processing.

[0177] Systems which operate one or more analyzer ARUs 1900 in tandem with one or more production process ARUs 1000 produce datasets that are of statistical significance. For example, a system that operates year-round in various temperatures and processes feedstocks with varying characteristics will result in datasets that when analyzed statistically represent the most effective process parameters for general use based on empirical data. The data may be used to invent new processing procedures that are validated.

[0178] In some embodiments, multiple analyzer ARUs 1900 may be utilized to evaluate different combinations of lixiviants or other reagents, to evaluate the use of lixiviants or other reagents in different orders or in any other manner as desired to quantify and characterize the effectiveness of each lixiviant for updating the process parameter combination.

[0179] The particular processing operations and other system functionality described in conjunction with the flow diagram of FIG. 17 are presented by way of illustrative example only and should not be construed as limiting the scope of the disclosure in any way. Alternative embodiments can use other types of processing operations. For example, the ordering of the process steps may be varied in other embodiments, or certain steps may be performed at least in part concurrently with one another rather than serially. Also, one or more of the process steps may be repeated periodically, or multiple instances of the process can be performed in parallel with one another in order to implement the disclosed embodiments.

[0180] Solvent Extraction Automated Process Control

[0181] With reference to FIGS. 20-22, an example extraction control system 2000 is described according to an embodiment. Extraction control System 2000 is configured to utilize solvent extraction techniques under automated control to improve efficiency and reduce waste in the extraction and purification of target MOIs.

[0182] Solvent extraction functions through a mass transfer between two immiscible phases. For example, an aqueous solution phase that contains a target MOI is thoroughly mixed into an emulsion with an immiscible organic solvent phase. While these two phases mix, the target MOI is selectively transferred to the organic phase from the aqueous phase. The two phases are then separated based on their density differences and the target MOI may be recovered by further processing. The mixing and separation are together called a contact stage and may be implemented, e.g., by a mixer-settler unit or any other type of contact stage. The system typically involves multiple contact stages between the aqueous and organic phases because the target MOI is usually not completely recovered in a single stage. Several stages are commonly used in a continuous, counter-current cascade to efficiently achieve high degrees of separation and purification. Counter-current operation maximizes the concentration gradient driving force for mass transfer while still allowing continuous high process throughputs.

[0183] System 2000 comprises one or more extraction circuits 2100-1, 2100-2, . . . , 2100-N, individually and collectively referred to herein as extraction circuit(s) 2100. Extraction circuits may be configured in series or parallel or in any other manner to achieve a target purity of one or more target MOIs. For example, each extraction circuit 2100 may be configured with one or more sections according to an extraction flowsheet for the extraction of a particular target MOI or group of target MOIs, e.g., REE MOIs in some embodiments.

[0184] System 2000 or some or all of the extraction circuits 2100 may comprise components of system 100, e.g., sensor devices 110, control stations 300, main control computing system 400, sensor data storage 410 and control mechanisms 600, ARUs 1000, PCUs 1200, analyzer ARUs 1800, analyzer ARUs 1900 or any other component described above that is configured to enable real-time measurement of MOI concentrations and the execution of corresponding process controls based on those measurements for real-time monitoring and optimization of system 2000 as will be described in more detail below.

[0185] In an embodiment, an example extraction circuit 2100 may comprise one or more of a pre -treatment section 2200, an extraction section 2300, a scrub section 2400, and a strip section 2500, each comprising one or more stages, e.g., stages 1, 2, . . . , M-l, M, or other components common to solvent extraction processes. While each extraction circuit 2100 is illustrated as comprising a pre -treatment section 2200, an extraction section 2300, a scrub section 2400, and a strip section 2500, any other sections, duplicate sections or fewer sections may be included in a given extraction circuit 2100 depending on the particular target MOI being extracted and the process for the extraction of that particular MOI. For example, some extraction circuits 2100 may not require a pre-treatment section, a scrub section or both or may include duplicate sections or other sections commonly included in commercial extraction facilities.

[0186] Each extraction circuit 2100 may be configured to increase a purification of its target MOI or otherwise separate the target MOI from one or more other MOIs or contaminants where, for example, an output of a particular section from one extraction circuit 2100 may be fed into a section of another extraction circuit 2100 to further purify the same target MOI or separate and purify another target MOI. As an example, an aqueous phase solution comprising a first target MOI from strip section 2500 of extraction circuit 2100-1 may be provided as an aqueous phase input for the pre-treatment section or extraction section of extraction circuit 2100-2 which is configured to further purify the same first target MOI. In another example, an aqueous phase solution output from scrub section 2400 of extraction circuit 2100-1 may be provided as an aqueous phase input for the pre-treatment section orextraction section of extraction circuit 2100-N which is configured to target second MOI for separation and purification. Any output of any other section of an extraction circuit 2100 may also or alternatively be utilized as an input for any section of another extraction circuit 2100 in other embodiments. Further extraction circuits 2100 may be utilized in series, in parallel, as branches and leaves of a process tree or in any other manner to separate and purify one or more target MOIs within solvent extraction system 2000, e.g., a solvent extraction facility.

[0187] Prior to pre -treatment, the aqueous phase input may be generated utilizing leaching as described above or in any other manner. For example, the aqueous phase input may comprise the PLS leeched from a feedstock material as described above or may comprise an aqueous phase from another extraction circuit 2100 that is ready for further processing or being recirculated for additional processing.

[0188] Pre -treatment steps for pH control may be implemented to treat the aqueous phase or the organic phase solution in each stage. Pre-treatment techniques may involve dispensing chemical agents such as acid, soap, water, kerosene, engineered sorbents or any other chemical agent. Pre-treatment techniques may also include heating or cooling of the solution. Measurements from sensor device 110 may be utilized by PCU 1200 to determine the appropriate quantity of reagents to add for pre-treatment. The pre-treatment process may be automatic, for example PCU 1200 may automatically dispense chemical reagents.

[0189] For example, pre-treatment section 2200 may utilize saponification or other pre-treatment techniques react an organic acid (often present in the organic solvent) with a base, typically sodium hydroxide (NaOH) or potassium hydroxide (KOH), to form a soap-like compound. Saponification or other pre-treatment techniques may be utilized to significantly improve the selectivity and efficiency of the later extraction process. Pre-treatment section 2200 may comprise any pre-treatment component or functionality commonly utilized in a commercial solvent extraction process. PCU 1200 may utilize concentration measurements from sensor devices 110 in combination with pH, temperature or other measurements during pre-treatment section 2200 to further refine the pre-treatment process and achieve higher levels of efficiency and reduced waste.

[0190] Extraction section 2300 provides bulk separation of the target MOI from the aqueous phase into an organic phase, also referred to as loading the organic phase. The extraction stages may be performed by mixer-settler units, extraction columns or any other component that mixes the aqueous phase and the organic phase together into a dispersion before allowing them to settle and separate. Extraction section 2300 may also or alternatively utilize any extraction technology or process that is commonly utilized in commercial solvent extraction processes to load the organic phase with the MOI from the aqueous phase. The stripped aqueous phase may exit extraction section 2300 as raffinate or be recirculated for further processing.

[0191] The loaded organic solvent enters scrub section 2400, where non-target MOIs or other contaminants that were co-extracted into the loaded organic solvent in the extraction section are scrubbed from the loaded organic phase. Scrubbing may be accomplished by contacting the loaded organic phase with an aqueous solution that alters the acid or MOI equilibrium conditions to selectively scrub out the non-target MOIs or other non-target contaminants. Non-target MOI species or other contaminants are transferred to the aqueous phase, which may be recombined with the extraction aqueous phase input or otherwise recirculated to another part of system 2000 for further processing, e.g., to another extraction circuit 2100 for recovery of any target MOIs that were unintentionally scrubbed out of the loaded organic phase or to perform further processing for other MOIs that were not a target of extraction this extraction circuit 2100.

[0192] Finally, the scrubbed loaded organic phase enters strip section 2500, where the target MOI is recovered from the scrubbed loaded organic phase as a rich liquor (RL) product. For example, strip section 2500 may utilize a fresh aqueous solution that is configured to selectively strip the target MOI out of the scrubbed loaded organic phaseto generate a RL for the target MOI having a higher purity than the aqueous phase used as an input to pre-treatment section 2200 of the same extraction circuit 2100. The organic phase, now stripped of the target MOI, may be recycled for reuse in this extraction circuit 2100 or in another extraction circuit 2100.

[0193] As shown in FIG. 20, each extraction circuit 2100 and each section 2200, 2300, 2400, and 2500 may be connected to and under control of PCU 1200 where, for example, PCU 1200 may be configured to control and command any valves or other control mechanisms 600 to adjust one or more parameters of the extraction process, direct or redirect outflows from one or more sections of the extraction circuit 2100 or in any other manner.

[0194] With reference to FIG. 21, an example section 2600 of extraction circuit 2100 is illustrated. Section 2600 may correspond to any of pre-treatment section 2200, extraction section 2300, scrub section 2400 or strip section 2500 and comprises contact stages 1, 2, . . ., M-l and M, also individually and collectively referred to herein as contact stage(s), which together are configured to perform the process for section 2600. As an example, section 2600 may correspond to extraction section 2300 which is configured to extract a target MOI from the aqueous phase prepared by pre-treatment section 2200 into the organic solvent phase in the manner described above. As seen in FIG. 21, the organic solvent phase travels through the contact stages in a first direction, e.g., 1->M, while the aqueous phase travels through the contact stages in a second direction, e.g., M->1. In some embodiments, each contact stage may comprise for example, e.g., a mixer-settler unit, an extraction column or any other contact unit that is configured to mix the aqueous and organic solvent phases and transfer the MOI or contaminants from one of the phases to the other.

[0195] As further shown in FIG. 21, in an embodiment, each contact stage 1, 2, ... , M-l, M, may comprise one or more sensor devices 110 in communication with a control unit 300, main control computing system 400 or both that are configured to measure a concentration of a one or more MOIs or contaminants in the fluids of that contact stage, e.g., in the manner described above. While system 2000 is described utilizing as sensor devices 110, in other embodiments, sensor devices 1300 (FIG. 14), analyzer ARUs 1800 (FIG. 15) or analyzer ARUs 1900 (FIG. 16) may also or alternatively be utilized. For example, in a case where the fluids being measured require further preprocessing before measurement, an analyzer ARU 1800 or 1900 may be utilized instead of sensor devices 110 alone. Each stage may include one sensor device 110, two sensor devices 110 or any other number of sensor devices 110. For example, in some embodiments, a sensor device 110 may be installed on a tank or vessel of a contact stage to monitor and measure a concentration of one or more MOIs or contaminants in the aqueous phase while another sensor device 110 may be installed on the tank or vessel of the contact stage to monitor and measure a concentration of the one or more MOIs or contaminants in the organic solvent phase. An example of such a configuration is shown in ARU 1000 (FIG. 14) with sensor devices 1300 being installed on fluid vessel 1102 in both the aqueous and organic solvent phases.

[0196] In other embodiments, a single sensor device 110 may be installed on a particular stage based on which of the aqueous phase and organic solvent phase the MOI concentration needs to be monitored and measured in. For example, in extraction section 2300, a sensor device 110 may be used to measure MOI concentration in the organic solvent phase which is being loaded from the aqueous phase while in strip section 2300, a sensor device 110 may be used to measure the MOI concentration in the aqueous phase into which the MOI is being stripped from the organic solvent phase.

[0197] The piping between one or more of contact stages 1, 2, ... , M-l, M of section 2600 may also comprise one or more sensor devices 110 in communication with PCU 1200 in some embodiments. For example, the organic solvent phase inflow (which may be recirculated from a prior process of system 2000 or run through section 2600), the aqueous phase inflow, the organic solvent phase outflow, the aqueous phase outflow and any flows of both theorganic solvent phase and aqueous phase between the stages may also be monitored by sensor devices 110 and PCU 1200 to obtain data on the entirety of the system operation and movement and changes in MOI concentrations both between the contact stages and when exiting each section 2600. The data may be presented to system operators who can view large amounts of data in a dashboard. The data may also or alternatively be utilized directly by PCU 1200 to respond to events, for example by dispensing reagent, opening or closing valves, activating pumps or in any other manner.

[0198] Over the course of long-term operation of a solvent extraction system, unforeseen failure modes may cause the system to become chemically unstable. In situations where certain portions of the system have diverged from the acceptable operating range, the flow between stages, sections or circuits may need to be diverted to another stage, section or circuit for re -processing or a different type or processing. For example, if section or stage that is intended to contain over 99% neodymium has been contaminated by ytterbium, the contents of that section or stage may need to be reprocessed by another stage, section or circuit to remove the ytterbium. Due to the ytterbium contamination, the purity of neodymium may be reduced. In addition, reprocessing may result in the high purity neodymium being fed into a lower purity batch of neodymium at a different stage in the extraction system, further decreasing the purity and requiring a significant number of stages, sections or circuits to return the neodymium to the 99% purity for that stage.

[0199] System 2000 mitigates this contamination and reprocessing issue by utilizing sensor devices 110 to monitor the concentrations of target MOIs, contaminants or both for each stage, between stages, for each section, between sections, for each circuit, between circuits or any other level of system 2000 and provide actionable sensor data to PCU 1200 for taking actions to inhibit such contaminations, redirect flows, dispense additional chemicals, reduce chemical dispensation or in any other manner. For example, based on fluid sample measurements taken by sensor devices 110 within, after or between any stage, section or circuit, PCU 1200 may determine based on MOI concentration sensor data received from the corresponding sensor devices 110 that a purity of the target MOI is not sufficient to drain a stage or move to the next stage, section or circuit, or that a concentration of a contaminant is too high in the stage and either cause further processing within that stage or recirculation of that stage without contaminating stages further down the line. Sensor devices 110 may also be configured to detect changes in optical transmissivity of the corresponding aqueous phases and organic phases that may indicate microbial contamination or chemical degradation.

[0200] Concentration profile data can be analyzed by the ARU control logic 1208 (FIG. 1) of PCU 1200 to compute derivatives which may be utilized to obtain an indication of whether the stage, section or circuit is in stable or unstable operation. This actionable real-time data can be used to proactively predict failure modes such as, e.g., bacterial contamination. For example, during normal operation, the shape, derivatives and integral of each concentration should be substantially similar. 2D plots of these values may be analyzed by ARU control logic 1208 of PCU 1200 to detect abnormalities. Another benefit of an extraction control system 2000 is the capability for big data capture. Sensor devices 110 record sensor data at a high rate, for example, multiple samples per second, per minute, per hour, per day, or any other period of time. Each sensor device 110 may record continuously, for example 24 hours per day and 365 days per year. In a case where an extraction facility comprises a large number of stages, e.g., 900 or more stages, a significant amount of sensor data corresponding to concentration changes in system 2000 may be continuously collected by sensor devices 110 installed at each stage or even a portion of the stages and stored in sensor data storage 410 for further processing. Access to these large data sets by artificial intelligence or machine learning algorithms may facilitate predictive analytics that may be used to identify early indicators of an imbalance in the extraction system such as, e.g., batch contamination, component corrosion ordegradation, leaks, reagent degradation or depletion, fires or explosions. In contrast, the latency associated with traditional ICP-S assaying techniques has been a barrier to such comprehensive operational analysis.

[0201] Extraction control system 2000 may be configured to provide high-level indicators from the results of the data analytics performed by ARU control logic 1208 of PCU 1200 to a user, e.g., via a user interface or dashboard that may be presented to the user via a user computing device. For example, in addition to the automated process controls, users may be alerted or receive alert messages such as, “whenever rainy weather occurs, acid consumption increases,” or “data indicates that there is a high likelihood of bacterial contamination of stage C726B located in the west wing.” The computer-assisted data analytics performed by PCU 1200 is able to monitor huge datasets that are otherwise impossible for humans to process within relevant time constraints.

[0202] In some embodiments, PCU 1200 may be configured to control one or more metering pumps such as, e.g., metering pumps 1 126 (FIG. 14) for adding various chemicals or reagents to the fluid vessel 1 102 (FIG. 14) of a particular stage in precise quantities under control of ARU control logic 1208 based on sensor data received from sensor devices 1300 (FIG. 14). For example, fluid vessels 1 102 (FIG. 14) may be configured to precipitate high purity ions into oxide products, such as pure terbium oxide, for example. Precise quantities of reagents or chemicals such, e.g., ozone or terbium hydroxide, may be added to the mixing tank in controlled quantities based on the concentration feedback from sensor devices 1300. In some embodiments, a light source 1120 such as, e.g., an ultraviolet light source, may be utilized to accelerate oxidation. Auxiliary sensors, such as pH sensors 1 104 may monitor the acidity of the mixture and communicate measurements with PCU 1200, allowing PCU 1200 to precisely modulate reagent or chemical dispensing from metering pumps 1 126 for tightly controlled precipitation crystallization reactions. The sensor devices 1300 may monitor the decreasing levels of dissolved-ions as elements precipitate, allowing PCU 1200 to determine the exact time when valuable element products have been deposited in the sump at desired purity levels where in many cases, high-purity products should be removed from processing as soon as possible to avoid risk of contamination. PCU 1200 may activate pumps 1108, valves or conveyor belts to gently remove precipitates from sump 1122 of fluid vessel 1 102 continuously via pipe 1136. PCU 1200 may also or alternatively notify a human operator that the process for this stage is complete.

[0203] With reference also to FIG. 22, an example process for operating extraction system 2000 is also described. The example process of FIG. 22 comprises steps 3000 through 3014 although additional or fewer steps may alternatively be implemented. The process of FIG. 22 may be performed by PCU 1200 for controlling the process or fluid flow within or between any stage, section or circuit of extraction system 2000. While the process of FIG. 22 is described with respect process controls based on concentrations of MOIs, in other embodiments, the process of FIG. 22 may also or alternatively be utilized for process controls based on concentrations of contaminants.

[0204] At step 3000, a sensor device 110 obtains a real-time fluid sample from the stage, section or circuit on which it is installed, e.g., installed in the contact stages, on piping between contact stages or in any other manner.

[0205] At step 3002, the sensor device 110 measures the concentration of a target MOI in the obtained fluid sample, while still installed in-situ in the stream.

[0206] At step 3004, PCU 1200 obtains sensor data from the sensor device corresponding to the measured concentration of the target MOI.

[0207] At step 3006, PCU 1200 calculates the target MOI concentration based on the obtained sensor data.

[0208] At step 3008, PCU 1200 determines a target MOI concentration, e.g., for the current stage, section or circuit, for the next stage, section or circuit, etc. PCU 1200 may determine the target MOI concentration, for example, by referencing a process flowsheet that indicates the target MOI concentration, a database comprising target MOI concentrations for each stage or in any other manner.

[0209] At step 3010, ARU control logic 1208 of PCU 1200 compares the determined MOI concentration to the target MOI concentration. If the determined MOI concentration is less than the target MOI concentration, the process proceeds to step 3012. Otherwise, if the determined MOI concentration is greater than or equal to the target MOI concentration the process proceeds to step 3014. While described with reference to determined and target MOI concentrations, in other embodiments determined and target contaminant concentrations may also or alternatively be measured and acted on. For example, determining whether the determined contaminant concentration is greater than, equal to or less than a target contaminant concentration.

[0210] At step 3012, if the determined MOI concentration is less than the target MOI concentration, ARU control logic 1208 causes extraction system to reprocess the stage, section or circuit, e.g., by opening valves corresponding to the appropriate stage, circuit or tank into which the aqueous or organic phase will be reprocessed. In some embodiments, step 3012 may alternatively trigger a process interrupt event which may interrupt an ongoing process due to the presence of a contaminant or due to an under purity event in the target MOI. The interrupt event may result in an adjustment to a process parameter in a current process flow or the activation of an alternative process flow without actually stopping the extraction processing, e.g., adding additional chemical agents, performing longer mixing or settling processes or in any other manner.

[0211] At step 3014, if the determined MOI concentration is greater than or equal to the target MOI concentration, ARU control logic 1208 causes extraction system to proceed with the next stage, section or circuit, e.g., by opening valves corresponding to the next stage, circuit or tank into which the aqueous or organic phase will next be processed according to the extraction flowsheet for the particular MOI being measured.

[0212] With reference also to FIG. 23, an example process for operating extraction system 2000 is also described. The example process of FIG. 23 comprises steps 4000 through 4006 although additional or fewer steps may alternatively be implemented. The process of FIG. 23 may be performed by PCU 1200 for controlling the process or fluid flow within or between any stage, section or circuit of extraction system 2000. While the process of FIG. 23 is described with respect process controls based on concentrations of MOIs, in other embodiments, the process of FIG. 23 may also or alternatively be utilized for process controls based on concentrations of contaminants.

[0213] At step 4000, a PCU 1200 delays processing and measurement by sensor device 110 for a pre-determined amount of time.

[0214] At step 4002, the PCU 1200 and sensor device 110 perform the measurement process to measure one or more characteristics of system 2000 for the current stage, section or circuit such as, e.g., MOI concentration, pH, temperature, contaminant concentration or any other characteristic.

[0215] At step 3010, PCU 1200 determines whether or not each measured characteristic is within a programmed threshold, e.g., MOI purity range, pH range, temperature range or any other programmed threshold. If the measured characteristic is within the programmed threshold, the process returns to step 4000. Otherwise, if the measured characteristic is not within the programmed threshold, the process proceeds to step 4006.

[0216] At step 4006, PCU 1200 triggers an interrupt event based on the determination that one or more of the measured characteristics are not within the programmed threshold. The interrupt event may terminate the process or, in some embodiments, modify the process in a predetermined manner, e.g., by selecting a new process flowsheet or adjusting the existing process flowsheet based on the measured data, which programmed thresholds are not being met or in any other manner. For example, under nominal operating conditions, a first process flowsheet may be utilizing having a variety of input and output parameters, concentration targets, chemical reagent dispensation amounts or any other operating parameter. When PCU 1200 triggers the interrupt event, the process may switch to a second process flowsheet having adjusted parameters.

[0217] For example, PCU 1200 may have access to a library of process flowsheets that may be utilized depending on the particular measurement values for each characteristic of system 2000. In the event that a suitable process flowsheet is not available, PCU 1200 may generate a new process flowsheet that is configured to move the process back toward the nominal operating conditions, e.g., utilizing Al or another analytical system to generate the new process flow.

[0218] In some embodiments, PCU 1200 may message or ping a human operator or otherwise provide data on the measured characteristic that does not meet the programmed threshold. PCU 1200 may, e.g., present the data via a system dashboard including color coding or other features to draw the user’s attention to the potential system issue. In some embodiments, PCU 1200 may request that the human operator provide an updated process flowsheet in a case where no existing process flow sheet corresponding to the interrupt event is available.

[0219] In some embodiments, PCU 1200 may execute the second process flowsheet having the adjusted parameters for a predetermined amount of time, number of cycles or under any other metric. For example, PCU 1200 may execute the second process flowsheet, e.g., dispense new reagent then mix for 20 minutes, then wait for 10 minutes, etc., and then after the parameters of the second process flowsheet are complete, or based on another trigger, return to the first process flowsheet.

[0220] In some embodiments, PCU 1200 may maintain the existing process flowsheet while adjusting one or more parameters temporarily based on the interrupt event, e.g., for a predetermined period of time, a predetermined number of cycles, etc. in an attempt to return the system 2000 to the nominal operating condition. For example, PCU 1200 may change the set-point on a thermostat from 20°C to 15°C temporarily or until the process is corrected.

[0221] The particular processing operations and other system functionality described in conjunction with the flow diagrams of FIGS. 22 and 23 are presented by way of illustrative example only and should not be construed as limiting the scope of the disclosure in any way. Alternative embodiments can use other types of processing operations. For example, the ordering of the process steps may be varied in other embodiments, or certain steps may be performed at least in part concurrently with one another rather than serially. Also, one or more of the process steps may be repeated periodically, or multiple instances of the process can be performed in parallel with one another in order to implement the disclosed embodiments.

[0222] In a large extraction system employing multiple sensor devices 110 to measure the various stages, sections or circuits and their connecting pipes at various points, the sensor data obtained from each sensor device 110 may be communicated to a data storage and processing computer system, either directly or after processing by a corresponding PCU 1200. For example, the data storage and processing computer system may comprise, e.g., servers, databases, cloud computing systems, local desktop computers, laptops, tables, mobile devices or any other components that may be utilized to store, process or present data. In some embodiments, for example, one or more components of the data storage and processing computer system may be located at the separation facility, at a remote location, in the cloud or in any other location. In one embodiment, a desktop computer that is located in an office at the processing facility may be utilized by a user to view, parse or otherwise manipulate the measurement data output by the sensor devices 110 and PCUs 1200 to obtain valuable insights into the operation of the separator system.

[0223] In some embodiments, the data storage and processing computer system may comprise materials informatics analysis software and algorithms that may be executed on the large datasets of measurement data produced by the analyzer ARUs and PCUs. Such material informatics analysis may comprise correlating recirculation-time with electric power consumption. Such material informatics analysis may also or alternatively comprise correlating recirculation-time and raffinate concentration with one or more of the age or wear time ofparticular equipment or components, the time of year, the weather, staff present on site, reagent vendors, reagent lot numbers, time, date and the geographic location from which particular lots of feedstock are obtained. Any other information relevant to the separation facility, feedstock, inventory or other parameters may also or alternatively be correlated by the material informatics analysis software and algorithms.

[0224] FIGS. 1 through 22 are conceptual illustrations allowing for an explanation of the disclosed embodiments of the invention. Notably, the figures and examples above are not meant to limit the scope of the invention to a single embodiment, as other embodiments are possible by way of interchange of some or all of the described or illustrated elements. Moreover, where certain elements of the disclosed embodiments can be partially or fully implemented using known components, only those portions of such known components that are necessary for an understanding of the disclosed embodiments are described, and detailed descriptions of other portions of such known components are omitted so as not to obscure the disclosed embodiments. In the present specification, an embodiment showing a singular component should not necessarily be limited to other embodiments including a plurality of the same component, and vice-versa, unless explicitly stated otherwise herein. Moreover, terms in the specification or claims are not intended to be ascribed an uncommon or special meaning unless explicitly set forth as such. Further, the disclosed embodiments encompass present and future known equivalents to the known components referred to herein by way of illustration.

[0225] It should be understood that the various aspects of the embodiments could be implemented in hardware, firmware, software, or combinations thereof. In such embodiments, the various components and / or steps would be implemented in hardware, firmware, and / or software to perform the functions of the disclosed embodiments. That is, the same piece or different pieces of hardware, firmware, or module of software could perform one or more of the illustrated blocks (e.g., components or steps). In software implementations, computer software (e.g., programs or other instructions) and / or data is stored on a machine -readable medium as part of a computer program product and is loaded into a computer system or other device or machine via a removable storage drive, hard drive, or communications interface. Computer programs (also called computer control logic or computer-readable program code) are stored in a main and / or secondary memory, and executed by one or more processors (controllers, or the like) to cause the one or more processors to perform the functions of the invention as described herein. In this document, the terms “machine readable medium,” “computer-readable medium,” “computer program medium,” and “computer usable medium” are used to generally refer to media such as a random access memory (RAM); a read only memory (ROM); a removable storage unit (e.g., a magnetic or optical disc, flash memory device, or the like); a hard disk; or the like.

[0226] The foregoing description will so fully reveal the general nature of the disclosed embodiments that others can, by applying knowledge within the skill of the relevant art(s) (including the contents of the documents cited and incorporated by reference herein), readily modify and / or adapt for various applications such specific embodiments, without undue experimentation, without departing from the general concept of the disclosed embodiments. Such adaptations and modifications are therefore intended to be within the meaning and range of equivalents of the disclosed embodiments, based on the teaching and guidance presented herein. It is to be understood that the phraseology or terminology herein is for the purpose of description and not of limitation, such that the terminology or phraseology of the present specification is to be interpreted by the skilled artisan in light of the teachings and guidance presented herein, in combination with the knowledge of one skilled in the relevant art(s).

Claims

CLAIMSWhat is claimed is:

1. A system for controlling an extraction process comprising a plurality of stages, the system comprising: a processor and memory, the processor being configured to: obtain sensor data corresponding to a concentration of a target material of interest from a sensor device at least partially disposed in fluid communication with a fluid corresponding to a given stage of the plurality of stages of the extraction process; determine, based on the sensor data, a concentration of the target material of interest; compare the determined concentration of the target material of interest to a predetermined threshold; and control at least a portion of the extraction process based at least in part on a result of the comparison of the determined concentration of the target material of interest to the predetermined threshold.

2. The system of claim 1 wherein the sensor device is installed such that the sensor device is at least partially disposed within inflow piping supplying the fluid from a prior stage to the given stage.

3. The system of claim 1 wherein the sensor device is installed such that the sensor device is at least partially disposed within outflow piping providing fluid from the given stage to a subsequent stage.

4. The system of claim 1 wherein the sensor device is installed such that the sensor device is at least partially disposed within fluid of the given stage.

5. The system of claim 4 wherein: the sensor device comprises a plurality of sensor devices; a first sensor device of the plurality of sensor devices is installed such that the first sensor device is at least partially disposed within an aqueous phase of the given stage, the first sensor device being configured to measure a concentration of the target material of interest within the aqueous phase; and a second sensor device of the plurality of sensor devices is installed such that the second sensor device is at least partially disposed within an organic phase of the given stage, the second sensor device being configured to measure a concentration of the target material of interest within the organic phase.

6. The system of claim 5 wherein the processor is further configured to: monitor the transfer of the target material of interest between the aqueous phase and the organic phase based on sensor data received from each of the first and second sensor devices that corresponds to the relative concentration of the target material of interest in each of the aqueous phase and organic phase; and cause at least one of the aqueous phase and the organic phase to move to another stage of the extraction system based on the monitoring.

7. The system of claim 4 wherein:a third sensor device of the plurality of sensor devices is installed such that the third sensor device is at least partially disposed within an aqueous phase of the given stage, the third sensor device being configured to measure a concentration of a target contaminant within the aqueous phase; a fourth sensor device of the plurality of sensor devices is installed such that the fourth sensor device is at least partially disposed within an organic phase of the given stage, the fourth sensor device being configured to measure a concentration of the target contaminant within the organic phase; the processor is further configured to: monitor the transfer of the target contaminant between the aqueous phase and the organic phase based on sensor data received from each of the third and fourth sensor devices that corresponds to the relative concentration of the target contaminant in each of the aqueous phase and organic phase; and cause at least one of the aqueous phase and the organic phase to move to another stage of the extraction system based on the monitoring.

8. The system of claim 8 wherein at least one of: the first and third sensor devices comprise the same sensor device; and the second and fourth sensor devices comprise the same sensor device.

9. The system of claim 1 wherein: the predetermined threshold comprises a target material of interest concentration threshold for a subsequent stage to the given stage; the processor is further configured to: control an actuation of a valve of the extraction process to transfer the fluid from the given stage to the subsequent stage based at least in part on a determination that the determined concentration of the target material of interest is greater than or equal to the predetermined threshold; and control an actuation of a valve of the extraction process to transfer the fluid from the given stage to the prior stage based at least in part on a determination that the determined concentration of the target material of interest is less than the predetermined threshold.

10. The system of claim 9 wherein the processor is configured to: obtain second sensor data corresponding to a concentration of a target contaminant from a second sensor device; determine, based on the second sensor data, a concentration of the target contaminant; inhibit actuation of the valve of the extraction process to transfer the fluid from the given stage to the subsequent stage based at least in part on a determination that the determined concentration of the target contaminant is greater than or equal to the second predetermined threshold; and control the actuation of the valve of the extraction process to transfer the fluid from the given stage to the prior stage based at least in part on a determination that the determined concentration of the target contaminant is greater than or equal to the second predetermined threshold.

11. The system of claim 1 wherein the sensor device and the second sensor device comprise the same sensor device.

12. The system of claim 1 wherein: the processor is configured to operate the extraction process for the given stage according to a first process workflow; controlling the at least a portion of the extraction process based at least in part on the result of the comparison of the determined concentration of the target material of interest to the predetermined threshold comprises the processor executing an interrupt event, the interrupt event comprising one of: an adjustment to at least one operating parameter of the first process workflow based on the result; and a replacement of the first process workflow with a second process workflow corresponding to the result.

13. The system of claim 12 wherein the processor is configured to execute the interrupt event for at least one of a predetermined amount of time, a predetermined number of cycles, and until a predetermined condition in the extraction process is met, the processor being configured to return the extraction process to the first process workflow based on a completion of the interrupt event.

14. The system of claim 1 wherein the processor is configured to provide the sensor data to a central dashboard, the central dashboard being configured for presentation to an operator of the extraction process.

15. The system of claim 1 wherein the target material of interest comprises a lanthanide.

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