Programmable semi-automatic and full-automatic single-task or multi-task liquid extraction and purification system

Abstract

A user selectable and programmable multitasking system for a liquid extraction and purification system. The system has a multi-pump device for transferring solvent from a solvent source to an output line and a multi-tandem column array connected to the output line. The system includes a controller for selecting a solvent source and a plurality of associated pumps. Each pump may move solvent from a selected source to an associated output line. The multi-pump apparatus also includes control of each of the plurality of pumps. Each control may selectively activate an associated pump. A timer may operate each activated pump for a specified duration or dispense a specified amount of solvent. The system may also include a pressure monitor to monitor the pressure in the output line and trigger an alarm when the pressure exceeds a threshold. A flow rate selector may select a flow rate at which the activated pump is to operate.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority to U.S. Provisional Patent Application No. 63 / 334,379, filed on April 25, 2022, entitled “Vacuum Liquid Extraction and Purification System and Method,” which is incorporated herein by reference in its entirety. Technical Field

[0003] The present invention relates generally to liquid extraction and purification and, more particularly, to an automated single-task or multi-task system and method for liquid extraction and purification of trace amounts of unwanted substances from sample materials. Background Art

[0004] Various patents describe systems and methods for liquid extraction, purification, fractionation and / or concentration (also referred to herein as extraction and purification) of solvents and solid materials (including water, wastewater, serum, milk, food, environmental, bioagricultural and pharmaceutical samples) that contain trace substances that may be the subject of subsequent analysis or may be used as pharmaceutical ingredients. For example, see Shi rkhan et al., "Vacuum Liquid Extraction and Purification System and Method", U.S. Patent No. 10,955,392, issued on March 23, 2021, the disclosure of which is incorporated herein by reference in its entirety. Liquid extraction and purification systems can be used for the extraction, fractionation, purification and / or concentration of trace substances (e.g., pesticides, chlorinated pesticides, dioxins, bromine compounds, polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs)).

[0005] A problem with prior art liquid extraction and purification systems is that they do not employ automation and cannot be scaled up for automated and unattended high throughput sample analysis. Therefore, there is a need for an improved liquid extraction and purification system that is more automated and easily scaled up to perform a large number of analyses simultaneously.

[0006] This section is intended to provide background or context. The specification may include concepts that could be pursued but not necessarily previously conceived or pursued. Unless otherwise indicated, what is described in this section is not considered prior art to the specification and claims and is not admitted to be prior art by inclusion in this section. Summary of the invention

[0007] The following is representative only and is not intended to be limiting.

[0008] The above-described problems may be overcome and other advantages may be achieved by using the disclosed embodiments and their equivalents.

[0009] In a first aspect or embodiment, the present invention provides a programmable multitasking system for extracting and purifying target compounds in environmental, biological and food samples. The programmable multitasking system has a set of 6 (more or less can be considered) multi-pump devices for transferring solvents from multiple solvent sources to the relevant input pipelines of a set of 6 column assemblies for purifying and fractionating target compounds. It also includes a multi-series Snap-in quick connection column assembled in series. The multi-pump device includes a source selector for selecting one of the multiple solvent sources and multiple pumps. Each pump can move the solvent from the selected solvent source to the relevant output pipeline. The multi-pump device also includes a control switch for each of the multiple pumps. Each control switch can selectively start the relevant pump. The timer can operate each enabled pump for a specified time to deliver a precise volume at a specified flow rate. The multi-pump device also includes a pressure monitor for monitoring the pressure in the output pipeline and triggering an alarm when the pressure exceeds a threshold. The flow rate selector can select one of the multiple flow rates, and each enabled pump will run at this flow rate. For each of the multiple pumps, the indication signal responds to the pressure in the relevant output pipeline exceeding the threshold to remind the user. The indication signal may be an LED light, an LED or LCD display and / or an alarm sound. The multi-pump device may suspend the operation of all pumps in response to the pressure in any output line exceeding a threshold value.

[0010] In another aspect, a second embodiment of the present invention provides a column element for performing selective extraction and purification of a target compound. The column element includes a first end fitting disposed at a first end and a second end fitting disposed at a second end. The body of the column element defines an internal cavity of the column element extending between the first end fitting and the second end fitting. The column element may also include a plurality of layers; a first material layer and a second material layer, which are separated by an internal glass sintered filter disposed between the first material layer and the second material layer.

[0011] In another aspect, an embodiment provides a method of operating a multi-pump device for extracting and purifying a target compound. The method includes selecting a first solvent source from a plurality of solvent sources using a source selector, and selecting at least one pump to move the first solvent from the selected solvent source to an associated output line. A flow selector is provided to select one of a plurality of flow rates at which each enabled pump operates.

[0012] The volume measurement controller or timer is set to run for a specified duration of time so that the selected at least one pump runs for the specified duration of time. The output line is connected to the sample cartridge and the analytical column. The method also includes starting the multi-pump device so that the selected at least one pump performs a single extraction and / or purification process task using at least one sample and one column.

[0013] The present invention features a programmable, semi-automatic and automated single-task or multi-task liquid extraction and purification system including at least one solvent source. A programmable controller is fluidly coupled to the at least one solvent source, the programmable controller being configured to be pre-programmed or manually programmed to selectively control the selection of the at least one solvent source and to provide the selected at least one solvent source at one or more of a user programmable flow rate, duration and pressure. At least one column array is fluidly coupled to the controller. The at least one column array includes at least one sample holding cartridge fluidly coupled to at least one column element, the at least one column element comprising at least one material for processing a sample in the sample holding cartridge.

[0014] In one embodiment, the system includes a plurality of different solvent sources and may further include a nitrogen source and a bidirectional valve fluidly coupled to the nitrogen source and at least one solvent source and electronically coupled to a controller. The bidirectional valve is configured to be controlled by the controller to selectively allow one or the other of nitrogen from the nitrogen source or solvent from at least one solvent source to enter at least one sample holding cartridge constituting a portion of at least one column array.

[0015] In another embodiment, at least one column array includes at least one sample holding tube, the sample holding tube being fluidly coupled to a plurality of column elements, the plurality of column elements containing at least one material for processing a sample in the sample holding tube, each of the plurality of column elements including an input end and an output end. At least one column array may include a nitrogen source and a first two-way valve, the first two-way valve being fluidly coupled to the nitrogen source and at least one solvent source, and being electronically coupled to a controller. The two-way valve is configured to be controlled by the controller to selectively allow one or the other of nitrogen from the nitrogen source or solvent from at least one solvent source to enter at least one sample holding tube constituting a portion of the at least one column array. Additional embodiments may also include a first column element containing at least one material for processing a sample in the sample holding tube, the first column element including an input end and an output end, and a second two-way valve, which is fluidly connected between the output end of the sample holding tube and the input end of the first column element, and is fluidly connected to at least one nitrogen source or at least one solvent source, the second two-way valve being electronically coupled to the controller, and being configured to be controlled by the controller to provide at least one of the nitrogen source or at least one solvent source to the input end of the first column element.

[0016] A third two-way valve may be provided, the third two-way valve being fluidly connected between the output end of the first column element and one or more of the material collection container or the waste container, and being configured to be controlled by a controller to provide the output of the output end of the first column element to one or more of the material collection container or the waste container.

[0017] In a preferred embodiment, at least one column array includes at least one sample holding tube fluidly coupled to a first column element, the first column element containing at least one first material for processing a sample in the sample holding tube, wherein the first column element is fluidly coupled to at least one second column element, the second column element containing at least one second material for processing a sample in the sample holding tube, the second material being different from the first material in the first column element.

[0018] In another embodiment, at least one pillar element in at least one pillar array comprises first and second materials for processing a sample in a sample-containing cartridge. The first and second materials are separated by a separator that is permeable to a fluid material.

[0019] In a preferred embodiment, at least one column element comprises a first end and a second end, wherein one of the first and second ends is closed by one of the male connector or the female connector, and wherein the other of the first and second ends is closed by the other of the male connector or the female connector. At least one column element and the sample holding cartridge may be disposable.

[0020] In a preferred embodiment, the system includes a plurality of solvent sources, and wherein the programmable controller is fluidly coupled to the plurality of solvent sources and is configured to be pre-programmed using a stored program or manually programmed to selectively control selection of at least one solvent source from one of the plurality of solvent sources and to provide the selected at least one solvent source at one or more of a user programmable flow rate, volume, duration, and pressure.

[0021] In another embodiment, at least one column element includes a polytetrafluoroethylene (PTFE) tube body that defines an internal cavity of the column element that extends between a first end and a second end of the PTFE tube. A first joint is disposed at the first end of the PTFE tube, and a second joint is disposed at the second end of the PTFE tube. The column element may also include a first glass sintered filter disposed at the first end joint of the PTFE tube, a second glass sintered filter disposed at the second end joint of the PTFE tube, and at least a first material layer disposed in the internal cavity of the PTFE tube. The first joint is preferably one of a male Luer joint or a female Luer joint, wherein the second joint is one of a male Luer joint or a female Luer joint. The first and second joints can be permanently pressed into the body of the (PTFE) tube and formed integrally with the body of the PTFE tube.

[0022] In a preferred embodiment, the at least one first material in the pillar elements is selected from the group consisting of silica, carbon and alumina. In another embodiment, the PTFE tube comprises first and second materials inside, the first and second materials being separated by a material separator sintered filter.

[0023] The present invention also includes a method of operating a programmable, semi-automatic and automated single-task or multi-task liquid extraction and purification system. The method includes the acts of providing a programmable, semi-automatic and automated single-task or multi-task liquid extraction and purification system, the system including a plurality of solvent sources and a programmable controller, the programmable controller fluidly coupled to the at least one solvent source, the programmable controller configured to be pre-programmed or manually programmed to selectively control the selection of the at least one solvent source and provide the selected at least one solvent source at one or more of a user programmable flow rate, duration and pressure. At least one column array is provided and fluidly coupled to the controller, the at least one column array including at least one sample holding cartridge, the sample holding cartridge fluidly coupled to at least one column element, the at least one column element containing at least one material for processing a sample in the sample holding cartridge.

[0024] The method also includes selecting a first solvent source from a plurality of solvent sources using a programmable controller, the act of selecting the first solvent source from the plurality of solvent sources using the controller including the controller operating a valve coupled to the first solvent source. The programmable controller is configured to select at least one pump configured to move the selected first solvent from the selected first solvent source to an associated output line, and the programmable controller is also configured to select a flow rate of the first solvent for the at least one pump. The programmable controller is also configured to set at least one of a specified duration or a specified volume of solvent for the at least one pump to operate. The method also includes connecting the output line from the programmable controller to the analytical column array; and activating the at least one pump to perform a single purification process task using the programmable controller.

[0025] The purification processing tasks of the method may include one or more of the following steps, including adjusting one or more analytical column arrays, loading samples on one or more analytical column arrays, purifying and removing interferences in one or more adjusted and sample-loaded analytical column arrays, and collecting fractions from one or more analytical column arrays.

[0026] The conditioning, sample loading, purification, and fraction collection steps may be performed one task at a time using one or more analytical column arrays, and include the acts of assembling at least one sample cartridge, assembling at least one column array, the at least one column array including the assembled sample cartridge and further including a plurality of column array elements, each column array element comprising one or more of silica, alumina, and carbon. For each assembled column array, the method includes connecting an output line of an associated solvent pump to a first column element of the assembled column array, activating the associated solvent pump to move a selected solvent from a selected first solvent source to an associated output line, and conditioning the column array using the first solvent.

[0027] In another aspect of the invention, the sample loading action includes connecting an output line of a nitrogen or solvent pump to at least one sample holding cartridge and transferring the sample from the sample cartridge to the column array using one or both of the nitrogen or solvent pumps. The purification action may include connecting a pump output line to each of a plurality of analytical column elements containing silica and activating at least one pump device to pass solvent through the plurality of analytical column elements.

[0028] The present invention is also characterized in that the sample barrel container includes a barrel; an embedded male connector located at a first end of the barrel and a removable barrel cover located at a second end of the barrel. The removable barrel cover preferably includes an O-ring seal. The barrel includes a body that defines an internal cavity of the barrel element, the cavity extending between the first end and the second end, and a first sintered filter is disposed at the first end, near the embedded male connector. In one embodiment, the embedded male connector is a male Luer connector, and the removable barrel end cap connector is a female Luer connector.

[0029] In a preferred embodiment, a removable cartridge cap with an associated o-ring may seal the cartridge by placing the end cap over the second end of the cartridge and twisting the end cap approximately 90 degrees. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In the present invention, the following two configurations are described: semi-automatic extraction and purification, performing multiple steps in one task, where multiple steps can be manually programmed into a single task at the beginning of each run, and automatic multi-task extraction and purification methods and systems, which perform multiple tasks sequentially and automatically using a multi-task program stored in the system memory. These and other features and advantages of the present invention will be better understood by reading the following detailed description in conjunction with the accompanying drawings, in which:

[0031] Figure 1 is a block diagram of a programmable semi-automatic and automatic single-task or multi-task liquid extraction and purification system according to the present invention; Figure 2A and 2B are views of a system controller and a control panel, respectively, according to an aspect of the present invention;

[0032] Figure 2C is a view of a system controller, a control panel, and a sample handling portion of a system according to the present invention;

[0033] Figure 2D is a detailed diagram of a multi-channel automated sample cleanup for dioxin and PCB analysis, comprising a system controller, a control panel, and a sample handling portion of a system according to the present invention, including the plumbing connections required according to one embodiment of the present invention;

[0034] Figure 2E yes Figure 2D A simplified diagram of the piping connections required for an embodiment of the present invention shown in FIG.

[0035] Figure 2F is an illustration of a system diagram for multi-channel automated sample cleanup and EPH analysis according to a method of use of the present invention;

[0036] Figure 2G yes Figure 2F A simplified diagram of the piping connections required for an embodiment of the present invention shown in FIG.

[0037] Figure 3 are diagrams showing various column elements, element sizes, shapes, and end caps;

[0038] Figure 4A and 4B is a detailed view of one embodiment of a sample cartridge end cap according to one aspect of the present invention;

[0039] Figure 5A and 5B It is an exploded perspective view and a cross-sectional view of a column element loaded with a single material;

[0040] Fig. 6A and 6B are exploded perspective and cross-sectional views of column elements loaded with two materials separated by a sintered filter or other element;

[0041] Figures 7A-7C is a perspective view and a cross-sectional view of a male Luer connector according to one aspect of the present invention;

[0042] Figures 8A-8C are perspective and cross-sectional views of a female Luer connector according to one aspect of the present invention; and

[0043] Fig. 9A and 9B Figures showing unassembled and assembled column elements, respectively. DETAILED DESCRIPTION

[0044] Various embodiments of the present invention disclosed and described herein provide a programmable, semi-automatic or fully-automatic, single-task or multi-task liquid extraction and purification system.

[0045] According to the present invention, Figure 1The extraction and purification system 100 in the embodiment of the present invention includes one or more (preferably multiple) solvent sources 112 connected to a controller 120. The controller 120 is user programmable and can run a pre-programmed program or be manually individually programmed to selectively control the selection of one of a plurality of solvent sources (or nitrogen or other inert gases) and supply the solvent (or nitrogen) to, for example, a sample column array 130 containing one or more (preferably multiple) array columns through conduits 112 and 115 at a user programmable flow rate, time and pressure, as will be explained in more detail below. After processing the sample, any waste from the column array is directed to a waste container / receiver 140. The controller 120 also controls the supply of nitrogen or other similar inert gas from a nitrogen source 145 to the sample column array 130 through a hose or conduit 117. A plurality of two-way valves 119 are controlled by the programmable controller 120 for selectively and sometimes sequentially controlling the supply of solvent or nitrogen 145 or other inert gas from one or more solvent sources 112.

[0046] Programmable, semi-automatic and automatic single-task or multi-task extraction and purification system uses a multi-pump device in a controller 120 to transmit selected one or more solvents 112 from multiple solvent sources 112 through relevant output pipelines 113. Afterwards, the controller 120 delivers the selected solvent to one or more sample cylinders and column arrays 121 in the sample column array 130. A plurality of serial column elements (as explained in more detail below) are assembled together so as to be arranged in series with the sample cylinder (collectively referred to as column arrays herein) and used to process samples. The controller 120 allows a user to select and program one of the multiple solvent sources 112 to provide it to a specific column array through one or more solvent pumps. Each pump can move the solvent from the selected solvent source 112 to the relevant output pipelines 113, 115 and the selected column array 121. The controller 120 includes a control switch for each of the multiple pumps. Each control switch can be programmed to selectively start the relevant pump. A timer can run each enabled pump for a specified duration. System 100 also includes a pressure monitor that monitors the pressure in output lines 113, 115, and 117 and triggers an alarm when the pressure exceeds a threshold. The flow rate selector can be programmed to select one of the multiple flow rates at which each enabled pump is to be operated. By selecting which solvent 112 to use and how much to provide, the column array 121 can be adjusted and used for sample processing. Each processing step can include resetting the multi-pump device to select the solvent, flow rate, and duration or volume to be used. These columns can be assembled (and reassembled) to properly process the sample, for example, by removing unwanted compounds and sending them to a waste container 140 and / or moving the required extraction elements for collection. Using a programmable, semi-automatic, multi-tasking system 100, the system 100 can be operated without repeated cleaning or replacement of tubes. This can speed up the extraction and purification process and reduce the chance of error.

[0047] Figure 2C The automatic universal extraction and purification system 100 according to the preferred embodiment of the present invention is shown, which can process six (6) samples simultaneously using the controller 120 and the sample processing system 200 and according to its programming. Figure 2A and 2B ) allows multiple tasks to be programmed to control and establish the desired extraction, purification and clean-up processes. The sample cartridge 455, chromatography column 457, flow rate 407, volume 408 and pump start / stop switch 410 are programmed as tasks in the control panel 401 and using the control panel 401.

[0048] Programmable tasks also include selecting multiple column arrays 121 to control and select collection containers or waste bottles by selecting one or more valves 150. Column elements 714, 716 and 481 together form column arrays 121. During the operation of the programming and selected tasks, the control panel 401 displays the column array pressure 411, the solvent dispensed amount 405 and the elapsed time 409. The program can be temporarily stopped or paused using the pause button 404, and the program can be restarted by selecting the start button 402 so that the process or task restarts from the point where it was stopped. The program can be stopped by selecting button 403. Button 413 can be used to select nitrogen, while button 415 is used to save the selected program and parameters for future use, thereby eliminating the need to program the controller for repeated tasks each time. Edit button 420 allows editing of previously stored programs. The unique design of the system 100 of the present invention allows the system 100 to automate any and all extraction and purification processes using a pump and a simple two-way valve 150 network. The system 100 can be configured to perform simple extractions using one column per sample, or to perform multi-column applications. As examples, the following applications include single column purification and cleanup of EPH and multi-column array purification and cleanup of dioxins and PCBs.

[0049] Figure 2D A close up view of six (6) parallel sample clean-ups and fractionations of dioxins and PCBs from various different samples is shown. In the controller module 120 , the power switch 412 , the nitrogen pressure regulator 138 , the nitrogen pressure gauge 486 , and the control panel 401 are components of the controller module 120 .

[0050] In this application, control panel 401 is used to create and run the multi-task program required to perform a dioxin and PCB sample cleanup. Five tasks are required to perform this sample cleanup. Task 1 Column Conditioning; Task 2 Sample Injection; Task 3 Dilution of Target Analytes through the Silica Column; Task 4 Dioxin Fraction Collection; Task 5 PCB Fraction Collection.

[0051] Figure 2E Shows Figure 2D Single-line piping diagram for dioxin and PCB cleanup and fractionation.

[0052] Task 1 The regulation of the column elements (column elements 714, 716 and 481 together form column array 121) is accomplished by selecting the flow rate and volume of pump 527, drawing solvent hexane 512, through solvent valve 525, through pressure sensor 411, selecting the solvent port in solvent / nitrogen valve 125, bypassing sample cylinder 712 by selecting bypass valve 482, through silica column 114, through valve 128, through carbon column 716, through valve 129, through valve 416, through alumina column 148, through valve 130 to waste bottle 127. All of these selection and control processes are accomplished using programmable controller 120.

[0053] Each column element can include materials for processing the sample, for example, removing unwanted chemicals, filtering physical contaminants, and / or extracting desired substances. By assembling a column array with different column elements, the sample can be processed differently depending on the desired results. After assembling the columns, the bottom element can be placed on the manifold and the column secured with a column clamp. Depending on the process to be performed, the column can be connected at the top to a solvent connector or a nitrogen connector, or to a two-way valve connected to a solvent source and a nitrogen source, and can be selectively programmed to provide one or the other of solvent or nitrogen or other gases to the column array.

[0054] Controller 120 is a programmable controller including a dedicated microcontroller for controlling various components of system 100. The components of programmable controller 120 include a power supply; a microcontroller and an input / output (I / O) section. Such hardware is well known in the art. The input section of the programmable controller is located on control panel 401.

[0055] Task 2 sample injection, first by making the controller 120 select the nitrogen port and valve 482 on the two-way valve 125, use nitrogen 113 to pass through the sample cylinder 712, thereby pushing the sample in the sample cylinder through the silica column 114, through valve 128, through the carbon column 716, through valve 129 and valve 416, through the alumina column 148, and through valve 130 to the waste liquid bottle 127, all operations are performed under the program control of the controller 120.

[0056] Task 3 elutes the analyte of interest, pump 527 draws solvent hexane 512 through solvent valve 525, passes through pressure sensor 411, and then selects the solvent port in solvent / nitrogen valve 125, whereby the solvent flows through sample cylinder 712 through selection valve 482, through silica column 114, through valve 128, through carbon column 716, through valve 129, through valve 416, through alumina column 148, and through valve 130 to waste bottle 127.

[0057] Task 4 is to collect the purified dioxin fraction by using pump 527 and selecting solvent valve 525 to extract toluene solvent 514 through valve 129, pass through carbon column 716 in the opposite direction, pass through valve 128, and then collect in dioxin fraction container 415.

[0058] Task 5 is to collect the purified PCB fraction. Pump 527 is used. Solvent valve 525 draws toluene solvent 514 through pressure sensor 411, through valve 130, through alumina column 148 in the opposite direction, through valve 416, and the PCB fraction is collected in PCB fraction container 480.

[0059] Figure 2FAn overview view showing six (6) parallel column array sample cleanup for separation and fractionation of EPH. This application uses only one column array element (silica) for sample cleanup to purify and fractionate aliphatic and aromatic hydrocarbons and collect them in separate containers.

[0060] Figure 2G Shown Figure 2F Single-line piping diagram for EPH sample cleanup, purification, separation and fractionation of aliphatic and aromatic hydrocarbons and collection in separate vessels.

[0061] Performing sample cleanup, separation, and fractionation of aliphatic and aromatic hydrocarbons requires four tasks.

[0062] Task 1 adjusts the silica column 470, uses the pump 2420 to specify the flow rate and volume of the solvent, and then draws hexane 2412 by selecting the solvent valve 2410, through the pressure sensor 2422, through the solvent / nitrogen valve 471 selected as the solvent end, bypassing the sample cylinder 901, through the silica column 470, and through the valve 473 into the waste liquid bottle 127.

[0063] Task 2 injects the sample into the silica column using nitrogen 113 (instead of solvent) through nitrogen valve 471 and valve 482, pushing the sample into the silica column 470 through sample tube 901, and into the waste bottle 127 through valve 473.

[0064] Task 3 is to collect aliphatic hydrocarbons, wherein pump 2420 is selected to extract solvent hexane 2412 through solvent valve 2410 , through pressure sensor 2422 , through valve 471 and valve 482 , through silica column 470 , through valve 473 , to collect the aliphatic hydrocarbon fraction in collection container 472 .

[0065] Task 4 is to collect aromatic hydrocarbons, where pump 2420 is selected to extract solvent DCM (dichloromethane) 2414 through solvent valve 2410, through pressure sensor 2422, through valve 471 and valve 482, through silica column 470, through valve 473, to collect the aromatic hydrocarbon fraction in container 474.

[0066] Figure 3 Various column elements 2100 are shown. As shown, there are 4 column element styles - large column element 2110, narrow column element 2120, narrow column element 2130 and sample container or tube 2140. In alternative embodiments, the column elements can have other thicknesses, sizes, shapes and styles. Likewise, the cross-section of the column elements can be circular and / or can have other cross-sectional shapes, such as hexagonal.

[0067] The large column element 2110 generally includes a female Luer connector 2112 at the upper end. The female Luer 2112 is fixed within the column element body 2116, and the sintered filter 2114 is disposed adjacent to the female Luer 2112. At the bottom end, a female Luer connector 2118 and an adjacent sintered filter 2114 are disposed to cover the column element 2116.

[0068] The narrow column element 2120 is configured similarly to the large column element 2110, except that a male Luer 2122 can be located at the upper end and a sintered filter 2124 of appropriate size is located within the column element body 2126. In an alternative embodiment, the male / female Luers 2112 / 2122 can be interchanged with the opposite type. In this case, the female Luer connector 2118 can be replaced with a male end Luer. The narrow column element 2130 illustrates this concept, in which the female Luer 2132 replaces the male Luer 2122. In addition, the narrow column element 2130 includes a sintered filter 2134 and a gasket ring 2135, both of which are sized and designed to fit within the column element body 2136.

[0069] The sample containment cartridge 2140 may vary in size and have a removable end cap 2142 including a male or female Luer-style end formed to fit into the cartridge body 2144 .

[0070] In another embodiment of the sample holding cartridge unit 2160, Figure 4A and 4B , the sample barrel 2160 can be equipped with a removable end cap 2162 and an "O" ring seal 2163 that seals the barrel body 2236 by placing the cap 2162 on the barrel 2236 so that the protrusion 2165 on the cap 2162 slides over the flat area 2167 in the barrel 2236, and then subsequently twisting the cap 2162 90 degrees to lock the cap 2162 to the barrel 2236. The cap 2162 can have a male or female Luer end connection.

[0071] Figure 5A and 5B An exploded view and a cross-sectional view, respectively, of an exemplary single packed column element 2220 are shown. The column element 2220 has a column body 2236 having a male Luer end fitting 2232 including a sintered filter 2234 and a retaining washer 2235 disposed at one end, and a female Luer end fitting 2238 including a sintered filter 2234 and a retaining washer 2235 disposed at the other end.

[0072] Between the two sintered filters 2234 is a packing material 2242. The packing material 2242 may be selected to facilitate purification or extraction of compounds passing through the column unit 2220. The packing material 2242 may include, but is not limited to, silica, carbon, alumina, and the like.

[0073] The sintered filter 2234 can be made of various materials, such as polytetrafluoroethylene (PTFE, trade name ) and stainless steel. The sintered filter material can also be a filter material such as glass, cotton or wool.

[0074] Fig. 6A and 6B An exploded view and a cross-sectional view of an exemplary multi-packing column unit 2320 are shown. The multi-packing column unit 2320 includes a column body 2336 that houses a first packing 2342 and a second packing 2344 separated by a sintered filter 2334. At the ends are a male Luer connector 2332 and a female Luer connector 2338, each having an associated sintered filter 2334.

[0075] Figures 7A-7C A perspective view and a cross-sectional view of a female Luer end connector are shown, and Figures 8A-8C A perspective view and a cross-sectional view of a male luer end connector are shown.

[0076] Fig. 9A and 9B An unassembled column array 2300 is shown, Fig. 9A The sample cartridge 2440, column elements 2442, 2444 and 2446 are included. Fig. 9B Sample cartridge 2440 and column elements 2442, 2444, and 2446 are shown as an assembled column array 2440.

[0077] Various embodiments provide a semi-automatic, multi-tasking system for extraction and purification systems. The programmable semi-automatic, multi-tasking system has a multi-pump device for transferring solvents from multiple solvent sources to related output pipelines. Multiple series columns are assembled in a series arrangement. The multi-pump device includes a source selector (for selecting one of multiple solvent sources) and multiple pumps. Each pump can move solvent from the selected solvent source to the related output pipeline. The multi-pump device also includes a pump start switch for each of the multiple pumps. Each control switch can selectively start the related pump. A timer or volume controller can enable each enabled pump to run for a specified duration. The multi-pump device also includes a pressure monitor for monitoring the pressure in the output pipeline and triggering an alarm when the pressure exceeds a threshold. The flow selector can select one of multiple flow rates, and each enabled pump runs at the selected flow rate.

[0078] In another embodiment of any of the above programmable, semi-automatic, multi-tasking systems, the multi-pump device includes a flow rate selector for selecting one of a plurality of flow rates at which each enabled pump operates. The amount of solvent moved by the pump through the associated output line is determined by the selected flow rate and the specified duration.

[0079] In another embodiment of any of the above programmable, semi-automatic, multi-tasking systems, the multi-pump device includes an indicator signal for each of the plurality of pumps to alert a user in response to the pressure in the associated output line exceeding a threshold value. The indicator signal may be an LED light, an LED or LCD display, and / or an alarm sound. The multi-pump device may suspend operation of all pumps in response to the pressure in any output line exceeding the threshold value.

[0080] In another embodiment of any of the above programmable, semi-automatic, multi-tasking systems, the multi-pump assembly further comprises a nitrogen controller to monitor and regulate nitrogen flow into the one or more column arrays.

[0081] Additional embodiments provide a column element for a multi-series column assembly. The column element includes a first connector disposed at a first end and a second connector disposed at a second end. The body of the column element defines an internal cavity of the column element extending between the first end and the second end. A first sintered filter is disposed at the first end and a second sintered filter is disposed at the second end. The column element also includes a first material layer and a second material layer, which are separated by an internal sintered filter disposed between the first material layer and the second material layer. In a further embodiment of the above-mentioned column element, the first connector is a male Luer connector or a female Luer connector.

[0082] In another embodiment of any of the above column elements, the second connector is a male Luer connector. The second connector can be integral with the body.

[0083] In a further embodiment of any of the foregoing pillar elements, the first material may be selected from silicon dioxide, carbon, and aluminum oxide.

[0084] In another embodiment of any of the above column elements, the first sintered filter is a glass sintered filter and / or the second sintered filter is a glass sintered filter.

[0085] In a further embodiment of any of the above column elements, the column element further comprises a Teflon sintered filter disposed at the first end and / or a Teflon sintered filter disposed at the second end.

[0086] An additional embodiment provides a method for operating a multi-pump device for an extraction and purification system. The method includes using a controller as a source selector to select a first solvent source from a plurality of solvent sources, and selecting at least one pump to move the first solvent from the selected first solvent source to an associated output line. A flow rate selector is provided as part of the controller to select one of a plurality of flow rates at which each enabled pump is to operate. A first specified duration or volume of a timer is set in the controller to cause the selected at least one pump to operate for a specified duration. The output line is connected to an analytical column. The method also includes starting the multi-pump device so that the selected at least one pump performs a single purification process task. In another embodiment of the above method, the purification process tasks include adjusting a column array; sample loading; purification and interference removal; and fraction collection.

[0087] In another embodiment of any of the above methods, conditioning the column array includes assembling a tandem column array assembly having a plurality of tandem column arrays. Each column array is comprised of a plurality of column elements - one silica, one alumina, and one carbon. For each of the plurality of tandem column arrays, an output line of an associated pump is connected to a first column element of the associated tandem column array. The multi-pump assembly is activated to move solvent from a selected solvent source to an associated output line and condition the tandem column array assembly.

[0088] In another embodiment of any of the above methods, sample loading includes assembling a loaded column array by adding a sample holding cartridge to the top of the column array (e.g., to the first silica column of a series column assembly). A nitrogen output line is connected to the sample holding cartridge. The sample is transferred to the series column array assembly using nitrogen.

[0089] In a further embodiment of any of the above methods, purifying and removing interferents includes removing a sample cartridge container from each of the plurality of first silica analytical column elements. A pump output line is connected to each of the plurality of first silica analytical column elements. A multi-pump device is activated to move solvent through the plurality of first silica analytical column elements.

[0090] In another embodiment of any of the above methods, for each of the plurality of analytical column arrays, fraction collection includes: disconnecting an output line from the analytical column array; disassembling the serial column array assembly by removing the carbon and alumina column elements from the serial column assembly; placing the carbon and alumina column elements in the fraction collection assembly; and connecting the output line to the fraction collection assembly. A multi-pump device is activated to move the solvent so as to collect the dioxin fraction from the carbon element and collect the polychlorinated biphenyl (PCB) fraction from the alumina column element. The serial column array assembly may include at least one silica column element, at least one alumina column element, and at least one carbon column element.

[0091] In another embodiment of any of the above methods, column conditioning, sample loading, purification, and fraction collection steps may be performed sequentially to purify and collect dioxins and polychlorinated biphenyls (PCBs) from biological, environmental, and food samples.

[0092] In another embodiment of any of the above methods, solvent selection, flow rates, and duration can be manually set or modified using a controller prior to each processing step, or can be pre-programmed to enable automated processing and repeatable processing steps.

[0093] In another embodiment of any of the above methods, the method further comprises assembling four analytical column arrays in series; connecting an output line to each of the plurality of first analytical column array elements; and activating a pump associated with the output line connected to the first analytical column element.

[0094] In a further embodiment of any of the above methods, the method includes: for each of a plurality of analytical column arrays: removing an output line from the analytical column array; removing the collection (one or more) column elements from the analytical column array; assembling a second analytical column having a collection of column elements; and attaching the output line to the second analytical column array. The method also includes selecting a second solvent from a plurality of solvent sources using a source selector; selecting at least one pump configured to move the second solvent from the selected second solvent source to the associated output line; setting a second specified duration for a timer to run the selected at least one pump; and starting the multi-pump device so that the selected at least one pump runs for the second specified duration. The first solvent can condition the first analytical column array. The second solvent can perform elution and purification of the analytical column array. The third solvent can perform fraction collection of the analytical column array.

[0095] In another embodiment, a method for using a solvent delivery system is provided to set up multiple sequences to extract and purify persistent organic compounds (POPs) prior to analysis, such as by using gas chromatography, liquid chromatography, and mass spectrometry. Each sequence can use a solvent delivery system to distribute a given solvent through a selected series column array assembly. The solvent delivery system typically includes a pump, a pressure monitor, an overpressure detector, a solvent valve selector, a flow rate selector, and a volume selector (by setting the duration of the delivery). Nitrogen can be selected to deliver the sample from the sample element to the series column assembly. A pump can be selected to deliver a precise volume of a specified solvent to the series column assembly at a specified flow rate. Overpressure of the solvent delivery pressure can be monitored and controlled so that a pressure controller can stop the pump if an overpressure is detected.

[0096] A combination of multiple processes can be performed using a specific set of column chromatography to create different POP extraction and purification methods. For example, the method can be used to extract and purify dioxins, polychlorinated biphenyls (PCBs), pesticides, and polycyclic aromatic hydrocarbons (PAH) analytes. The extraction and purification of dioxins and PCBs can be used with three serial column array assemblies. The serial column assembly can include a silica column element, an alumina column element, and a carbon column element.

[0097] The method can perform four steps: column conditioning, sample loading, purification, and fraction collection. Sample loading is performed by pushing the sample through the serial column array assembly using nitrogen. Thereafter, column conditioning and purification sequences are performed by selecting the relevant solvent, flow rate, and volume (duration) for each sequence to pass the solvent through the serial column array assembly in order to condition and / or purify the dioxins. Fraction collection is accomplished by placing the carbon and alumina columns on a fraction collection manifold and selecting a second solvent, flow rate, and volume (duration) to collect the dioxins and PCBs in separate collection containers.

[0098] The foregoing description is directed to a specific embodiment. However, other changes and modifications may be made to the described embodiment to achieve some or all of its advantages. The above-described system and method may be modified without departing from the concepts disclosed herein. Therefore, the present invention should not be considered to be limited by the disclosed embodiments. In addition, the various features of the described embodiments may be used without the corresponding use of other features. Therefore, this description should be understood as merely illustrating various principles, rather than limiting the present invention.

Claims

1. A programmable, semi-automatic and automatic single-task or multi-task liquid extraction and purification system comprising: at least one solvent source; a programmable controller fluidly coupled to the at least one solvent source, the programmable controller configured to be pre-programmed or manually programmed to selectively control selection of the at least one solvent source and to provide the selected at least one solvent source at one or more of a user programmable flow rate, duration, and pressure; and at least one column array fluidly coupled to the controller, the at least one column array comprising at least one sample containing cartridge fluidly coupled to at least one column element, the at least one column element containing at least one material for processing the sample in the sample containing cartridge.

2. The system of claim 1, wherein the system comprises a plurality of different solvent sources.

3. The system according to claim 1, further comprising: Nitrogen source; as well as A two-way valve fluidly coupled to the nitrogen source and the at least one solvent source and electronically coupled to the controller, the two-way valve being configured to be controlled by the controller to selectively allow one or the other of the nitrogen from the nitrogen source or the solvent from the at least one solvent source to the at least one sample holding cartridge forming a portion of the at least one column array.

4. A system according to claim 1, wherein the at least one column array includes the at least one sample holding tube, the sample holding tube is fluidly coupled to a plurality of column elements, the plurality of column elements contain at least one material for processing the sample in the sample holding tube, each of the plurality of column elements includes an input end and an output end.

5. The system of claim 4, wherein the at least one pillar array comprises: Nitrogen source; a first two-way valve fluidly coupled to the nitrogen source and the at least one solvent source and electronically coupled to the controller, the two-way valve configured to be controlled by the controller to selectively allow one or the other of the nitrogen from the nitrogen source or the solvent from the at least one solvent source to the at least one sample containing cartridge forming a portion of the at least one column array; a first column element comprising at least one material for processing the sample in the sample-containing cartridge, the first column element comprising an input end and an output end; a second two-way valve fluidly connected between the output end of the sample containment cartridge and the input end of the first column element and connected to at least one of the nitrogen source or the at least one solvent source, the second two-way valve electronically coupled to the controller and configured to be controlled by the controller to provide at least one of the nitrogen source or the at least one solvent source to the input end of the first column element; as well as A third two-way valve is fluidly connected between the output end of the first column element and one or more material collection containers or waste containers, and is configured to be controlled by the controller to provide an output from the output end of the first column element to one of the material collection container or the waste container.

6. A system according to claim 1, wherein the at least one column array includes the at least one sample holding tube, the sample holding tube is fluidly coupled to a first column element, the first column element contains at least one first material for processing the sample in the sample holding tube, and wherein the first column element is fluidly coupled to at least a second column element, the second column element contains at least one second material for processing the sample in the sample holding tube, the second material is different from the first material in the first column element.

7. A system according to claim 1, wherein the at least one column element in the at least one column array comprises a first and a second material for processing the sample in the sample holding tube, wherein the first and the second materials are separated by a partition that is permeable to a fluid material.

8. The system of claim 1, wherein the at least one column element comprises a first end and a second end, wherein one of the first end and the second end is closed by one of a male connector or a female connector, and wherein the other of the first end and the second end is closed by the other of the male connector or the female connector.

9. The system of claim 1, wherein the at least one column element and the sample holding cartridge are disposable.

10. The system of claim 1, wherein the system includes a plurality of solvent sources, and wherein the programmable controller is fluidly coupled to the plurality of solvent sources and is configured to be pre-programmed using a stored program or manually programmed to selectively control selection of the at least one solvent source from one of the plurality of solvent sources and to provide the selected at least one solvent source at one or more of a user programmable flow rate, volume, duration, and pressure.

11. The system of claim 1 , wherein the at least one column element comprises: a polytetrafluoroethylene (PTFE) tubing body defining an interior cavity of the column element extending between a first end and a second end of the PTFE tubing; a first joint disposed at the first end of the PTFE tube; as well as A second joint is disposed at the second end of the PTFE tube.

12. The system according to claim 11, further comprising: A first glass sintered filter disposed at a first end joint of the PTFE tube; A second glass sintered filter disposed at the second end joint of the PTFE tube; as well as At least a first layer of material is disposed within the interior cavity of the PTFE tube.

13. The system of claim 12, wherein the first connector is one of a male Luer connector or a female Luer connector, and wherein the second connector is one of a male Luer connector or a female Luer connector.

14. The system of claim 11, wherein the first and second fittings are permanently pressed into and integral with the body of the PTFE tube.

15. The system of claim 12, wherein the at least first material is selected from the group of materials consisting of silicon dioxide, carbon, and aluminum oxide.

16. The system of claim 12, wherein the PTFE tube interior includes first and second materials separated by a material separation sintered filter.

17. A method of operating a programmable semi-automatic and automatic single-task or multi-task liquid extraction and purification system, the method comprising the steps of: A programmable semi-automatic and automated single-task or multi-task liquid extraction and purification system is provided, the system comprising: a plurality of solvent sources; a programmable controller fluidly coupled to the at least one solvent source, the programmable controller configured to be pre-programmed or manually programmed to selectively control selection of the at least one solvent source and to provide the selected at least one solvent source at one or more of a user programmable flow rate, duration, and pressure; and at least one column array fluidly coupled to the controller, the at least one column array comprising at least one sample holding cartridge fluidly coupled to at least one column element containing at least one material for processing the sample in the sample holding cartridge; The method further comprises: selecting a first solvent source from the plurality of solvent sources using the programmable controller, the step of selecting a first solvent source from the plurality of solvent sources using the controller comprising the controller operating a valve coupled to the first solvent source; selecting, using the programmable controller, at least one pump configured to move the selected first solvent from the selected first solvent source to an associated output line; selecting, using the programmable controller, a flow rate of the first solvent for at least one pump; using the programmable controller to set at least one of a specified length of time or a specified volume of solvent that the at least one pump is to operate; and Connecting an output line from the programmable controller to an analytical column array; and using the programmable controller, actuating the at least one pump to perform a single purification process task.

18. The method according to claim 17, wherein: The purification process task includes one or more of the following steps: conditioning one or more analytical column arrays; loading samples onto one or more analytical column arrays; purifying and removing interferents from the one or more conditioned and sample-loaded analytical column arrays; and collecting fractions from the one or more analytical column arrays.

19. The method according to claim 18, wherein: The conditioning, sample loading, purification, and fraction collection steps use one or more analytical column arrays to perform one task at a time and include the following steps: assembling at least one sample cartridge, assembling at least one column array comprising said assembled sample cartridge and further comprising a plurality of column array elements, each column array element comprising one or more of silica, alumina, and carbon; and For each assembled column array, connecting the output line of the associated solvent pump to the first column element of the assembled column array; activating the associated solvent pump to move the selected solvent from the selected first solvent source to the associated output line; and The column array is conditioned using the first solvent.

20. The method of claim 18, wherein the sample loading step comprises: connecting an output line of a nitrogen or solvent pump to at least one sample holding cartridge; and The sample is transferred from the sample cartridge to the column array using one or both of the nitrogen or solvent pumps.

21. The method of claim 18, wherein the purification step comprises: connecting a pump output line to each of a plurality of analytical column elements containing silica; and activating at least one pumping device to move solvent through the plurality of analytical column elements.

22. The method of claim 19, wherein the column array elements include silica column elements, carbon column elements, and alumina column elements, and wherein the method includes conditioning the column elements, loading a sample into a sample cartridge, purifying and collecting dioxins from the carbon column elements, and collecting a polychlorinated biphenyl (PCB) fraction from the alumina column elements.

23. A sample cartridge container, comprising: Bobbin; a recessed male connector at a first end of the barrel; a removable barrel cover at the second end of the barrel, the removable barrel cover including an O-ring seal; a body defining an interior cavity of the cartridge member extending between a first end and a second end; as well as A first sintered filter is disposed at the first end near the embedded male connector.

24. The sample cartridge container of claim 23, wherein the embedded male connector is a male Luer connector.

25. The sample cartridge container of claim 23, wherein the removable cartridge end cap connector is a female Luer connector.

26. The sample cartridge container according to claim 25, wherein: A removable cartridge cap with associated o-ring is used to seal the cartridge by placing the end cap over the second end of the cartridge and twisting the end cap approximately 90 degrees.

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