Patent Application
20220331795
Embodiments described herein relate to Luer fittings and Solid Phase Extraction systems including such Luer fittings.
Solid phase extraction (SPE) involves removing minor chemical constituents from a sample of water or other liquid. This is generally done for two purposes. The first of these two purposes is to capture the method analytes (the chemicals a given SPE procedure seeks to isolate) on an SPE disk for the purpose of identifying the specific chemicals present and determining their concentration in the original water or other liquid sample. The second of these two purposes is to remove or isolate the chemical constituents that are not analytes of the testing procedure being employed. These chemical constituents are removed because they can interfere with the accurate identification or quantification of the method analytes. The chemical identity and concentration of the chemical constituents removed as interferents by the solid phase extraction process are not determined. It is possible for a procedure to employ both processes described. An SPE procedure is usually followed by a determinative technique to identify the specific chemical identity and concentration of the method analytes. These determinative techniques include gas chromatography, liquid chromatography, mass spectrometry, and optical (or light absorption) techniques. There is a need for improved systems to improve solid phase extraction and reduce costs thereof.
In some embodiments, a Luer lock includes a tapered female member and a tapered male member defining a passage. A tubing is inserted through the passage. The tubing defines an outer cross-section corresponding to an inner cross-section of the passage. The tapered male member is configured to be inserted into the tapered female member such that the tube is in fluid communication with the tapered female member, and the tubing exerts a compressive force at a mating surface between the tapered male member and the tapered female member to increase friction therebetween and inhibit leakage.
In some embodiments, a Luer lock includes a tapered female member, and a tapered male member defining a central axis and passage along a central axis. A side port is defined through a sidewall of the tapered male member, the side port defining a lateral passage. A tubing is inserted through the passage along the central axis, the tubing defining an outer cross-section corresponding to an inner cross-section of the passage. The tapered male member is configured to be inserted into the tapered female member such that the tube is in fluid communication with the tapered female member.
In some embodiments, a disk holder for Solid Phase Extraction (SPE) includes a cylindrical cavity with a closed bottom including an angled section, a first recess having a first diameter and a first thickness, a second recess defining a second diameter and a second thickness and an opening. A SPE disk and a porous member is disposed in the cavity. A male Luer fitting is disposed on a Luer valve, the male Luer fitting installed in the opening. The porous member has a diameter equal to the second diameter and a thickness equal to the second thickness. The SPE disk has a thickness equal to the first diameter and a thickness equal to the first thickness.
It should be appreciated that all combinations of the foregoing concepts and additional concepts discussed in greater detail below (provided such concepts are not mutually inconsistent) are contemplated as being part of the inventive subject matter disclosed herein. In particular, all combinations of claimed subject matter appearing at the end of this disclosure are contemplated as being part of the inventive subject matter disclosed herein.
The foregoing and other features of the present disclosure will become more fully apparent from the following description and appended claims, taken in conjunction with the accompanying drawings. Understanding that these drawings depict only several implementations in accordance with the disclosure and are therefore, not to be considered limiting of its scope, the disclosure will be described with additional specificity and detail through use of the accompanying drawings.
An SPE procedure is usually followed by a determinative technique to identify the specific chemical identity and concentration of the method analytes. These determinative techniques include gas chromatography, liquid chromatography, mass spectrometry, and optical (or light absorption) techniques. SPE disks are often used to perform the SPE procedure. The SPE disks are filters used to remove chemicals from liquids as part of a SPE procedure. These SPE disks generally contain one or more sorbents embedded in a glass fiber matrix. This glass fiber matrix forms the structure of the SPE disk. Sorbents may consist of particles of silica with or without surface modifications, or particles of polymeric material that have hydrophobic, hydrophilic or ion exchange functionality. Both the sorbent particles and the glass fiber matrix adsorb chemical constituents (analytes and interferents) from liquid samples passed through the SPE disk. A filtration apparatus is employed to filter the sample through the SPE disk. The filtration device may consist of a bottom piece on which the SPE disk rests and a funnel, or reservoir, that attaches to the bottom piece while also securing the SPE disk in place. The bottom piece needs to incorporate a mesh, porous member or other type of permeable member to allow liquids to pass through the disk, generally aided by vacuum, in a uniform manner. A means to collect the liquids that pass through the disk is also necessary. A variety of filtration apparatuses are available, from simple manually operated systems to complex automated systems.
A SPE disk, after installation in a filtration device, may first be rinsed with a suitable solvent to remove impurities that may be present in the SPE disk with the solvent being removed from the SPE disk, under vacuum (or forced through the SPE disk under positive pressure). This solvent is collected and usually discarded.
Certain SPE disks need to be preconditioned in order to function properly. An example of an SPE procedure using an SPE disk requiring preconditioning would be a procedure employing an SPE disk containing a C-18 sorbent being used to test drinking water for chemical contaminants. C-18 sorbent consists of particles of silica or polymer with an octadecyl surface modification imparting hydrophobic properties. If using a C-18 disk, after any rinsing with solvent to remove impurities as previously described, the SPE disk is rinsed with methyl alcohol to precondition the C-18 sorbent. The methyl alcohol is partially pulled through the SPE disk displacing any prior rinse solvents but is not completely pulled through the disk exposing the C-18 sorbent to air. After this conditioning with methyl alcohol, the SPE disk must remain immersed in methyl alcohol or water until the sample filtration step is complete. Next, water is added to the reservoir diluting the methyl alcohol covering the top of the disk. The water is partially pulled through the disk, substantially displacing the methyl alcohol but again leaving a layer of water on top of the disk to avoid exposing the C-18 sorbent to air. Next, the water sample undergoing analysis is added to the reservoir and vacuum applied under the disk to facilitate filtering the water sample through the SPE disk. As the water sample passes through the SPE disk, chemicals such as pesticides or herbicides present in the water sample are retained by adsorption onto the C-18 sorbent or adsorption onto the glass fiber structural material of the SPE disk. After the filtration of the water sample is complete, air is generally passed through the disk, aided by the continued application of vacuum, for a short time to remove residual water.
If it is desired to first remove impurities that may have been retained by the SPE disk that could interfere with the identification and quantification of method analytes using the intended determinative technique, then the following procedures are employed. A suitable rinse solution such as an aqueous salt solution or a polar organic solvent may be added to the reservoir. An organic solvent, if used, would need to be a polar solvent as a strongly non-polar organic solvent would not mix with or displace the residual water left in the disk. The non-polar organic solvent may also fail to pass through the disk under vacuum due to the immiscibility of water and the strongly non-polar organic solvent. Care must be exercised in choosing a rinse solvent as the rinse solvent must remove the impurities without removing the analytes filtered out of the original water sample. This rinse solvent is normally discarded.
The next step is to transfer the analytes removed from the water sample by the SPE disk to a suitable solvent. This step is necessary prior to conducting a determinative analysis to identify the chemical composition and concentration of the analytes that were present in the original water sample. First, a small volume of a polar organic solvent, such as acetone or ethyl acetate, is added to the reservoir and soaks through the disk. This polar elution solvent serves two purposes: it helps remove any remaining water, and it begins the process of transferring the chemicals removed from the original water sample to organic solvent. This first solvent rinse, or elution solvent, is removed under vacuum and collected in a clean container. This may be followed by adding a small volume of a non-polar solvent to the reservoir as necessary to remove certain hydrophobic analytes that are more strongly retained by the SPE disk. This solvent is also removed under vacuum and collected, usually in the same container as the first polar elution solvent. This step may be repeated several times as necessary depending on the specific procedure being employed. When the necessary or proscribed elution procedure has been completed, it is often necessary to remove any water from this collected elution solvent (or extract) before proceeding. This can be done by passing the solvent extract through an anhydrous salt such as sodium sulfate.
This dried solvent extract can undergo a variety of determinative techniques to identify and determine the concentration of the analytes present in the solvent extract. These determinative techniques include gas chromatography, liquid chromatography, mass spectrometry, and optical (or light absorption) techniques. This information from the determinative technique on the concentration of analytes in the extract can be used to calculate the concentration of the analytes in the original water sample. These calculations would also require the volume of the original water sample and the final volume of the solvent extract, both of which should be determined. The extract may also be partially evaporated from a volume of, for example, 20 mL to a volume of 0.5 mL prior to analysis by the determinative technique, provided the extract solvents are sufficiently volatile. For example, a 40-fold reduction in volume would increase the concentration of analytes in the extract by up to 40 times. This increase in the concentration of analytes in the extract results in the determinative technique being able to detect the method analytes at a 40-fold lower concentration. Method analytes may be partially lost during the evaporation step if the boiling points of the extract solvents are not significantly lower than the boiling point of a given method analyte. Alternately, if the method analytes are sufficiently non-volatile, the extract may be evaporated to dryness and reconstituted in a solvent appropriate for the intended determinative technique. It is also possible to evaporate the solvent to dryness and determine the concentration of material extracted from the original water sample by weighing the residue left after the evaporation is complete. This weighing, or gravimetric technique, does not identify the specific chemicals that were present in the original water sample.
Luer Lock fittings are commonly used in SPE for fluid communication across various components and steps. Luer Lock fittings are commonplace not just in SPE but also in medical applications and many others. For example, Luer lock fittings may be utilized within intravascular or hypodermic applications of medical devices/instrumentation (such as needles, syringes, catheters, and infusion sets) to facilitate a leak-free or substantially leak-free administration of various fluids to a patient through a central line, eliminating the need for multiple needle insertions within a given patient. As used herein, the term “leak-free” or “substantially leak-free” implies that there is less than 0.01% of leakage of a fluid form a sealing interface of two surfaces that are in contact with one another.
Luer fittings are categorized as Luer slip and Luer lock connectors. A Luer slip fitting consists of a tapered male member that slips onto its mating tapered cavity of a female member and relies on compression forces and resulting friction between the mated surfaces to achieve a leak-free connection. Accidental separation can happen in Luer slip connections when the connection is inadvertently pulled. To mitigate accidental separation, Luer-lock fittings are used which have integrated locking threads in addition to the components of a Luer Slip fitting. In a Luer lock fitting, when the male and female parts are screwed together, the surfaces are compressed in the same manner as the Luer slip; however, due to the threaded coupling, the connection cannot be simply pulled apart. Owing to their simplicity, Luer slip fittings are typically used in low-pressure applications while threaded Luer lock fittings are use in applications where more robust and secure connections are needed. As described herein, there is an incentive to deploy Luer connections with better fluid communication under higher pressure and/or during the use of more aggressive solvents that may leak through conventional Luer fittings. In addition, there may be further benefits of a more secure connection in a Luer Slip design without the use of a threaded skirt as used in the Luer Lock fitting.
Embodiments of the various Luer lock fittings described herein and systems including such Luer lock fittings may provide one or more benefits, including, for example: 1) providing a tighter fit between a male Luer lock and a female Luer lock by providing a tube through an enlarged passageway of the male Luer lock so as to increase a compressive force on the corresponding female Luer lock and inhibiting leakage; 2) providing a side port in male and/or female Luer locks so as to enable application of a vacuum or pressure through the male and/or female Luer lock; 4) allowing modification of existing Luer locks to obtain a better fit; 4) providing simple shelving systems and manual operation thus, reducing capital and operational cost; 5) being equally applicable in various fields including analytical chemistry, water filtration, water sampling, etc.
In some embodiments, the tubing 46 that is inserted through the port 44 applies an outward compression force on the male Luer port 44 such that the male Luer port 44 has a tighter fit with an inner wall of a mating female Luer lock (e.g., the female Luer lock 54 shown in
Different from the male Luer fitting 32, the male Luer fitting 34 includes a side port 40 defined through a sidewall of the fitting 32. In some embodiments the side port 40 provides an additional fluid flow pathway from the male Luer fitting under the effect of an externally applied vacuum or a positive pressure of the fluid passing through the male Luer lock and the tubing 46. In some embodiments, the side port 40 may serve as a vent. In some embodiments, a portion of the fluid input at the male Luer lock passed through the tubing 46 out of the port 44 and another portion of the fluid flows through side port 40 providing an additional pathway for fluid pathway for additional purpose. In some embodiments the fluid flowing through the tubing 46 through the port 44 is utilized for a different purpose than the fluid flowing through the side port 40. In some embodiments the fluid flowing through the tubing 46 through the port 44 is utilized for a same purpose as the fluid flowing through the side port 40. In some embodiments, the side port 40 is used for purpose other than fluid flow.
As shown in
The lower end of tubing 46 extends beyond the end of tip 44 and extends into cavity 66 of fitting 58B. The tubing 46 inserted through the port 44 applies an outward compression force on the male Luer port 44 such that the male Luer port 44 has a tighter fit with the inner wall of the female Luer port resulting in a higher friction at the interface thus creating a leak free connection. In some embodiments, the tubing 46 is narrower than the upper opening of the port 44 and wider than the lower opening of the port 44 such that the tubing applies an external compressive force on at least a portion of the interface between male Luer port 44 and the female port 58B when they are mated. This compression force due to the insertion of tube 46 creates an additional friction at the interface between the male Luer port 44 and female Luer port 58B thereby providing a leak free connection.
Vial cap 88 (for example, having 24-414 thread) may be press fit or friction fit into recess 77 and PTFE washer 90 sits at the top of vial cap 88. Both vial cap 88 and washer 90 are secured by bushing 92 which is threaded into hole 78. Washer 90 fits tightly around bushing 92 creating a seal between the two pieces. Fitting 34 is threaded into bushing 92. The vial 94 can thread into vial cap 88 with vial 94 positioned against washer 90 establishing an airtight seal with vial 94. Note that vial cap 88 can accept a container of any volume in the range of 20-60 mL Female Luer 58B (for example ×¼-28 thread× 1/16″ barb fitting) has tubing 46B attached to barb 64 (for example with diameter 1/16″). The end of tubing 46B that is not attached to fitting 58B is attached to port 156 of vacuum manifold 154, both shown in
Vacuum manifold may also have a port which is connected to a container to collect waste liquids and a source of vacuum. The vial 94 (or other 24-414 thread container) is installed into vial cap 88 in one configuration. Fitting 58B can be attached to fitting 30. In this configuration vacuum can be applied to the interior of the vial 94. The vacuum passage may extend from fitting 30 through holes 74, 72 and 78, through bushing 92 and 1/16″ port 40 on fitting 34. In use fitting 110 on disk holder 104 would be installed into fitting 58A or, optionally, but preferentially, male×female 2 port Luer valve 114 may be installed onto fitting 58A of block 70 and fitting 110 of disk holder 104 installed on the second female Luer port of Luer valve 114 as shown in
Liquids pass through SPE disk 100, recess 108 with porous member 102, fitting 110, Luer valve 114, fitting 58A and tubing 46A directly into vial 94. Port 40 in fitting 34 is part of a separate passage for the application of vacuum. Tubing 46A passes through, but is separate from, the passage used to apply vacuum to vial 94. In an alternate configuration vial 94 is removed from vial cap 88 and fitting 58B is attached directly to fitting 34 with the tip of tubing 46A extending into cavity 66 of fitting 58B. This allows liquids introduced into disk holder 104 to pass through SPE disk 100 and tubing 46A and into tubing 46B which is attached to a container used to collect liquids and a source of vacuum. This configuration is used to filter the water sample through SPE disk 100 as part of a solid phase extraction procedure. Two port Luer valve 114, optionally, but preferentially, located in between fitting 58A on block 70 and fitting 110 on disk holder 104 can be used to control the flow of liquids in this configuration. Luer valve 114 can also be used to control the flow of air or another gas through SPE disk 100. Note that bushing 92 and fitting 34 could be replaced by a single ¼ NPT×male Luer lock fitting with the same modifications as fitting 34.
Recess 106 may be slightly larger than SPE disk 100. For example, the SPE disk 100 having a diameter of 47 mm may correspond to the recess 106 having a diameter of approximately 47.25 mm. The cylindrical edge of glass fiber SPE disk 100 is not perfectly uniform and smooth due to the fibrous nature of glass fiber. SPE disk 100 can be inserted into recess 106, aided by angled section 116 for securing SPE disk, with the lower portion or entire cylindrical edge of SPE disk 100, not being perfectly smooth and uniform, making intermittent contact with the cylindrical walls of recess 106. Angled section 116 at the bottom of cavity 112 and immediately above recess 106, aids in installing SPE disk 100 into recess 106. Angled section 116 also helps limit the amount of organic solvent necessary for the wash and elution steps of a solid phase extraction procedure by narrowing the bottom of cavity 112. In some embodiments, the thickness of the SPE disk may be less than, greater than, or equal to the thickness of the recess. In some embodiments, the diameter of the SPE disk may correspond to the diameter of the recess, for example the SPE disk may have a slightly smaller diameter than the recess diameter (for example, in a range of about 0.01 mm to about 0.25 mm, inclusive, less than the diameter of the recess). Porous member 102 may be slightly smaller than recess 108 or it may be approximately the same size as recess 108 and snap into place and be held securely. Fitting 110, a ¼-28 male thread×male Luer fitting (for example a ¼-28 male thread×male Luer fitting), is installed into hole 80 (for example with ¼-28 female threads). Fitting 110 serves to connect disk holder 104 to a solid phase extraction system and is used to apply vacuum to recess 108. Optionally, male×female 2 port Luer valve 114 may be installed onto fitting 58A of block 70 and fitting 110 of disk holder 104 to control the flow of liquids and gases through SPE disk 100. Vacuum applied to recess 108 is distributed under SPE disk 100 by the void space created by porous member 102. This vacuum aids in moving liquids or gases through SPE disk 100. In some embodiment the vacuum is applied to the recess 108. In some embodiments, the vacuum is applied to the cavity of the disk holder.
Removing SPE disk 100 from disk holder 104 is accomplished by inverting disk holder 104 and tapping it on a lab bench or other suitable surface. If porous member 102 is retained in recess 108 during this process disk holder 104 is ready for reuse. If porous member 102 comes out of disk holder 104 along with SPE disk 100 porous member 102 must be reinstalled into recess 108 before the next use of disk holder 104. Care must be exercised not to dislodge porous member 102 from recess 108 when installing SPE disk 100 into recess 106. In some embodiments, SPE disk 100 shown in
The disk holder 104 provides unexpected benefits over known disk holders. For example, not all known SPE disks may be suitable for use with SPE disk holder 104. Known SPE disks that do not have sorbent 268 uniformly distributed across the entire diameter, and have sorbent 268 located in a central disk shaped section surrounded by a substantial ring containing only glass fiber, are not suitable for use with disk holder 104. This construction, if used with disk holder 104, can allow the water sample being filtered by the disk to pass through the outer ring containing only glass fiber without contacting the central disk section containing sorbent 268. Many prior art manual SPE systems employ a clamping mechanism to secure SPE disk 100 to a porous base below and a reservoir above to contain the sample. This leaves the edge of SPE disk 100 exposed. In such known disks it is necessary to maintain vacuum under SPE disk 100 when liquid is in the reservoir to avoid having liquid seep out of the exposed edge of SPE disk 100. This is easily accomplished during the water filtration step by applying vacuum immediately after adding water to the reservoir above SPE disk 100 and maintaining vacuum until the filtration of the water sample is complete. During the elution step after the completion of the filtration of the water sample through SPE disk 100 it is necessary to add organic solvent to the reservoir above SPE disk 100.
Most SPE procedures specify a “soak” time of 1 to 3 minutes to allow analytes retained by SPE disk 100 to be released from SPE disk 100 and transferred to the organic solvent. During this soak period the vacuum must not be applied, or the organic solvent will pass through SPE disk 100 prematurely before the specified soak time has elapsed. With vacuum not being applied, this organic solvent may seep out of the exposed edge of SPE disk 100 resulting in loss of the organic solvent containing the analytes of interest. Some prior art manual and automated SPE systems use a disk holder design that has a cavity, similar to cavity 112 on disk holder 104 and employ a clamping mechanism often consisting a cylindrical collar that is inserted into the cavity similar to cavity 112, and held in place by a mechanism employing a threaded member to secure the collar so it is firmly clamped on the outer perimeter of the upper circular surface of SPE disk 100. In a disk holder intended for use with 47 mm diameter SPE disk 100 this collar might have an internal diameter of 41 mm and a height of 25 mm to 75 mm. The periphery of 47 mm SPE disk 100 that is under the collar is effectively sequestered and not available to filter the water sample. This reduces the available surface area for filtration by approximately 25%. Any analytes that do migrate into the perimeter of SPE disk 100 that is located under this collar may be difficult to effectively remove during the subsequent wash or elution with organic solvent. Such known disk holder designs often have a male Luer to interface with the SPE system in a similar manner to the use of fitting 110 at the base of disk holder 104.
Some other known disk holder designs employ a press fit of SPE disk 100 into a recess similar to recess 106, leaving the entire top surface exposed and available for filtration. This disk holder design specifies that the recess into which SPE disk 100 is press fit is of a smaller diameter than SPE disk 100. The intent is that SPE disk 100 will compress and conform to the smaller recess and establish a seal between the cylindrical edge of SPE disk 100 and the cylindrical wall of the smaller recess. In practice, installing SPE disk 100 into a smaller recess, particularly without the aid of angled section 116 of this invention, results in damage to SPE disk 100. This prior art design provides for the entire upper circular surface of SPE 100 to be available to filter the water sample. The concern that the water sample could migrate around the edge of SPE disk 100 without passing through SPE disk 100 is addressed in this prior at design by use of a recess smaller than SPE disk 100 as described above.
In contrast, disk holder 104 does not rely on attempting to establish a seal between recess 106 and SPE disk 100. Instead, the disk holder 104 relies on physical forces and chemical processes to prevent the passage of any analytes of interest around the sorbent containing portion of SPE disk 100. SPE disk 100, having the properties making it suitable for use with disk holder 104, specifically as follows.
SPE disk 100, constructed of glass fiber and containing sorbent 268, uniformly distributed across the entire diameter, or SPE disk 100, constructed of glass fiber and containing sorbent 268, uniformly distributed across the entire diameter and having a layer of glass fiber containing no sorbent that is not thicker than 0.4 mm covering the bottom circular surface or SPE disk 100, constructed of glass fiber and containing sorbent 268, uniformly distributed across the entire diameter, excepting a layer of glass fiber containing no sorbent that is not thicker than 0.4 mm covering the bottom circular surface, and the portion of the cylindrical outside edge that is exterior to the disk shaped, sorbent containing, portion of SPE disk 100, is suitable for disk holder 104. The layer of glass fiber containing no sorbent covering the bottom circular surface, and the portion of the cylindrical outside edge that is exterior to the disk shaped, sorbent containing, portion of SPE disk 100 is best exemplified by a glass fiber filter paper such as WHATMAN™ GFA PN: 1820-047 (for 47 mm diameter), WHATMAN™ GFA PN:1820-060 (for 60 mm Diameter) having a thickness of 0.3 mm.
In use, disk holder 104 may have a column of water between 15 mm and 60 mm high above the top surface of SPE disk 100. This creates a positive pressure relative to the ambient atmosphere at the interface of the water column and the top circular surface of SPE disk 100 of approximately 0.15 kPa for a 15 mm column of water. A typical SPE extraction procedure will employ a vacuum of between 50 kPa and 85 kPa relative to the ambient atmosphere below SPE disk 100 in recess 108, containing porous member 102. The interior of SPE disk 100 experiences a pressure gradient between these two pressures. This pressure differential holds SPE disk 100 in place with the bottom circular surface of SPE disk 100 pressed down on the bottom circular surface of recess 106 and the upper surface of porous member 102. The movement of liquid under the influence of vacuum would serve to close any gap between the bottom circular surface of SPE disk 100 and the bottom circular surface of recess 106.
In use with disk holder 104 in certain examples, SPE disk 100 as described above, may include a 0.3 mm glass fiber layer on the bottom circular surface if using the Whatman™ GFA filter paper described above. Several factors would limit or eliminate any passage of analytes of interest in the water sample being filtered, around the sorbent 268 portion of SPE disk 100. The preferred material of construction for disk holder 104 is PTFE. PTFE is extremely hydrophobic. This hydrophobicity of PTFE makes the wall of recess 106 hydrophobic. Given that the gap between the cylindrical edge of SPE disk 100 and the cylindrical wall of recess 106, assuming a reasonably central placement of 47 mm SPE disk 100 into 47.25 mm recess 106, leaves a gap between the cylindrical edge of SPE disk 100 and the cylindrical wall of recess 106 of 0.1 mm to 0.15 mm. This hydrophobicity of the PTFE cylindrical wall of recess 106 will limit or stop the migration of the water sample being filtered down the gap between the cylindrical wall of recess 106 and SPE disk 100. Recess 106 on disk holder 104, intended for use with 47 mm SPE disk 100, may be approximately 1 mm to 2 mm deep. Any water sample migrating in between the cylindrical wall of recess 106 and the cylindrical edge of SPE disk 100 in spite of this hydrophobicity, would be minimal in quantity and be subject to passing through the 0.3 mm to 0.4 mm thick layer of glass fiber not containing sorbent 268 (if present) covering the cylindrical edge of SPE disk 100 before reaching the bottom of recess 106. The water sample would then pass through sorbent 268 portion of SPE disk 100 traveling both laterally and downward to the edge of recess 108 containing porous member 102.
Disk holder 104 is mounted on Luer valve 114 which is installed on fitting 58A of block 70. Rear legs 150A support upper shelf 142, lower shelf 144 and vacuum manifold 154. Front legs 150C support lower shelf. In place of rear legs 150A and front legs 150C, support for upper shelf 142, lower shelf 144 and vacuum manifold 154 could also be accomplished with two pieces of plastic or wood with the same width as upper shelf 142 and lower shelf 144 and of suitable height. System rack 138 sits on work surface 146 which may be located in a fume hood due to the solvents typically employed in solid phase extraction procedures. Note that square holes 148 on upper shelf 142 are offset to the right relative to square holes 148 on lower shelf 144. This is due to the asymmetry of fluid management block 70 with hole 80, into which fitting 58A and Luer valve 114 is installed, and on which disk holder 104 is mounted, is offset to the right.
In some embodiments, upper shelf 142 can be removable and can be installed oriented with square holes 148 offset to the left if desired. This would be done if installing block 70 oriented with fitting 58A and disk holder 104 on the left also. Upper shelf 142 is also removable, as after the water sample in the sample bottle attached to bottle holder and valve assembly 120 has been filtered through SPE disk 100, removing upper shelf 142 makes accessing disk holder 104 easier, as may be desirable to complete the remaining steps in the solid phase extraction procedure. Vacuum manifold 154 is attached to rear legs 150A and located below lower shelf 144. Vacuum manifold 154 has vacuum port(s) 156, with one vacuum port 156 for each fluid management block 70 that can be accommodated on shelf 144. Vacuum port(s) 156 is attached to tubing 46B with a suitable fitting and supplies vacuum to fitting 30 and fitting 34 on fluid management block 70. Vacuum port(s) 156 may have a valve attached to provide individual control to each vacuum port 156 and this valve may be, but is not necessarily, a Luer valve. This valve may be located at any point in between port 156 and fitting 30 or fitting 34 on block 70 through tubing 46B and attached fitting 58B. Vacuum manifold 154 also has vacuum port 158 which is connected to a waste-water container and vacuum source. Vacuum manifold 154 may also be equipped with a vacuum gauge to monitor vacuum. Rack 138 as shown can accommodate components for one to three sample extractions, being able to hold up to three block 70 and up to three bottle holder and valve assembly 120. Rack 138 can be configured to accommodate components for any number of sample extractions.
Individual upper shelf segment 143A is shown in an upright position. This orientation improves access to disk holder 104 as may be desired to complete certain steps in a solid phase extraction procedure. Individual upper shelf segment 143A may be put into the upright orientation (143A) after the sample filtration step is complete and bottle holder and valve assembly 120, with attached sample bottle, has been removed from rack 140. Rear legs 150A support horizontal support 141, lower shelf 144 and vacuum manifold 154. Front legs 150C support lower shelf. In place of rear legs 150A and front legs 150C, support for horizontal support 141 and lower shelf 144 could also be accomplished with two pieces of plastic or wood with the same width as lower shelf 144 and of suitable height. System rack 140 sits on work surface 146 which may be located in a fume hood due to the solvents typically employed in solid phase extraction procedures. Note that individual upper shelf segment(s) 143/143B are offset to the right relative to square holes 148 on lower shelf 144. This is due to the asymmetry of fluid management block 70 with hole 80, into which fitting 58A and Luer valve 114 are installed and on which disk holder 104 rests are offset to the right. Individual upper shelf segment 143/143A could be installed oriented with an offset to the left if desired. This may be done if installing block 70 oriented with hole 80, fitting 58A, Luer valve 114 and disk holder 104 on the left also.
Individual upper shelf segment 143A is shown in an upright orientation and individual upper shelf segment 143B is shown folded down in the orientation necessary to support bottle holder and valve assembly 120 during filtering of the water sample. Individual upper shelf segment 143 can be securely attached to horizontal support 141 and is removable after the water sample in the sample bottle attached to bottle holder and valve assembly 120 has been filtered through SPE disk 100. Individual upper shelf segment 143 can be securely attached to horizontal support 141 and hold bottle holder and valve assembly 120 in a vertical orientation during the filtration of the water sample through SPE disk 100, as part of a SPE procedure. Removing individual upper shelf segment 143 makes accessing disk holder 104 easier and is an alternate configuration to an attached individual upper shelf segment 143 shown as being in the upright orientation (143A) and horizontal orientation (143B). Accessing disk holder 104 is necessary to complete the remaining steps in the solid phase extraction procedure after the water sample has been filtered through SPE disk 100 and bottle holder and valve assembly 120 has been removed. In some embodiments, individual upper shelf segment 143 and support block 130 may be combined as a single piece with block 130 part of, or securely attached to, individual upper shelf segment 143.
Vacuum manifold 154 is attached to rear legs 150A and located below lower shelf 144. Vacuum manifold has vacuum port(s) 156, with one vacuum port 156 for each fluid management block 70 that can be accommodated on rack 140. Vacuum port(s) 156 is attached to tubing 46B with a suitable fitting and supplies vacuum to fitting 30 and fitting 34 on fluid management block 70 through tubing 46B and attached fitting 58B. Vacuum port(s) 156 may have a valve attached to provide individual control to each vacuum port 156 and this valve may be, but is not necessarily, a Luer valve. This valve may be located at any point in between port 156 and fitting 30 or fitting 34 on block 70. Vacuum manifold 154 also has vacuum port 158 which is connected to a wastewater container and vacuum source. Vacuum manifold 154 may also be equipped with a vacuum gauge to monitor vacuum. Rack 140 as shown can accommodate components for one to three sample extractions, being able to hold up to three block 70 and up to three bottle holder and valve assembly 120. Rack 140 can be configured to accommodate components for any number of sample extractions.
Vial cap 88 (for example with 24-414 thread) is press fit into recess 77 and PTFE washer 90 sits at the top of vial cap 88 and establishes a seal with vial 94 or another container with 24-414 or 24-410 thread. Both vial cap 88 and washer 90 are secured by bushing 208 which is threaded into hole 78. Washer 90 fits snuggly around bushing 208 creating a seal between the two pieces. Fitting 32 is threaded into bushing 208. Bushing 208 has a hole or port 212 in the hex flats, which may be used to apply a vacuum. Fitting 32 when installed in fitting 208 does not extend into fitting 208 far enough to block hole or port 212. Vial 94 (for example with a 20 mL, 24-414 thread) can thread into vial cap 88 with vial 94 seated up against washer 90 establishing an airtight seal between washer 90 and vial 94. During system use, with vial 94 installed into hole cap 88 and a seal established by washer 90, the vacuum passage extends from the interior of vial 94, through port 212 on bushing 208, through the interior of bushing 208, through hole 78, hole 72 and hole 74, through fitting 30, fitting 214 and tubing 46B which is connected to port 156 on vacuum manifold 154. Note that vial cap 88 can accept a 24-414 or similar thread container of any volume with 20 mL, 30 mL, 40 mL, 60 mL and 125 mL containers being other examples of containers that can be accepted.
Female Luer with wing grips× 1/16″ barb fitting 214 (for example with × 1/16″ barb fitting) has tubing 46B attached to barb 64 (for example with 1/16″ barb). In some embodiments, barb fitting 214 is a Female Luer× 1/16″ barb fitting with winged grips on the end of cartridge connecting tubing that attaches to the modified male Luer fitting that is installed in the ¼ NPT×⅛ NPT fitting that secures the 24-414 thread hole cap. The end of tubing 46B not attached to fitting 212 is attached to port 156 on vacuum manifold 154, which are both shown in
Leaf 224A is shown in the raised position. Leaf 224B is shown in the lowered position and holds bottle holder and valve assembly 120 with support block 130 resting on two adjacent leaves 224B. Horizontal member 222 may be adjustable so that the distance between leaf 224B or leaf 225B and shelf 227 can be adjusted. This adjustment can facilitate the use of SPE media of different heights, such as SPE cartridges, or the use or non-use of Luer valve 114 in between fitting 58A and fitting 110 of disk holder 104. Shelf 227 has openings 228 into which fluid management block(s) 200 are installed and secured with threaded fasteners or by other means. The threaded fasteners pass through suitable holes in the interior walls of opening(s) 228 and into threaded mounting hole(s) 201 of Block 200.
In use, disk holder 104 is mounted on fitting 58A or Female Luer port 54 of valve 114. Bottle holder and valve assembly 120 is placed in between two adjacent leaves 224B with support block upper section 130A resting on the top surface of two adjacent leaf 224B and support block lower section 130B resting in between two adjacent leaf 224B. Sample delivery tube 136 of bottle holder and valve assembly 120 extends into cavity 112 of disk holder 104. Detachable support leaf 225 serves the same purpose as hinged leaf 224 but instead of being hinged they are detachable. Leaf 225A is shown as detached when not in use as to facilitate access to disk holder 104 as is necessary to complete certain steps in a solid phase extraction procedure. Leaf 225B is shown as installed on horizontal support 222 and functions the same as hinged leaf 224B.
Hinged leaf(s) 224B may be rotated to the upright position and detachable leaf(s) 225B may be detached after completion of the sample filtration step for the sample(s) using the bottle holder and valve assemblies 120 they are supporting. System rack 220 sits on work surface 146 which may be located in a fume hood due to the solvents typically employed in solid phase extraction procedures. Note that leaf 224B and Leaf 225B are offset to the right relative to square openings 228 on shelf 227. This is due to the asymmetry of fluid management block 200 with hole 78, into which bushing 202 (e.g., stainless steel reducing bushing with a tapered ¼-18 NPT male thread and ¼-28 female thread), fitting 58A and Luer valve 114 are installed, and on which disk holder 104 rests, are offset to the right. System components could be manufactured and/or installed with an offset to the left if desired or with no offset if block 200 were manufactured with hole 78 centered in block 200. Vacuum manifold 154 is attached to rear legs 150A and located below shelf 227. Vacuum manifold has vacuum port(s) 156, with one vacuum port 156 for each block 200 that can be accommodated on rack 220. Vacuum port(s) 156 is attached to tubing 46B with a suitable fitting and supplies vacuum to fitting 30 and fitting 32 on fluid management block 200 through tubing 46B and attached fitting 214.
Vacuum port(s) 156 may have a valve attached to provide individual control to each vacuum port 156 and this valve may be, but is not necessarily, a Luer valve. This valve may be located at any point in between port 156 and fitting 30 or fitting 32 on block 200. Vacuum manifold 154 also has vacuum port 158 which is connected to a waste-water container and vacuum source. Vacuum manifold 154 may also be equipped with a vacuum gauge to monitor vacuum. Rack 220 as shown can accommodate components for one to five sample extractions, being able to hold up to five block(s) 200 and up to five bottle holder and valve assembly 120. Rack 220 can be configured to accommodate components for any number of sample extractions.
Leaf 224 may be constructed with a variety of materials or techniques. Leaf 224, as shown in
Leveling leaf 224 allows leaf 224 to hold support 130 of bottle holder and valve assembly 120 in a horizontal orientation during the sample filtration step of an SPE procedure. Set screw 238 has hexagonal recess 239 which, for example, accepts an Allen wrench to facilitate installation and adjustment of set screw 238. In some instances, leaf 224 has pins 230, which may have ¼-28 thread socket cap screws. Lower section 130B of support block 130 sits in between pins 230 with pins 230 positioning support block 130 of bottle holder and valve assembly 120 so that sample delivery tube 136 rests approximately in the center of cavity 112 of disk holder 104. Leaf 224, if not located at either end of horizontal member 222 will have pins 230 located on both sides of leaf 224 to facilitate the use of bottle holder and valve assembly 120 on either side of leaf 224. Leaf 224, if located at either end of horizontal member 222, need only have pins 230 on the side of leaf 224 that will be used to support bottle holder and valve assembly 120. Pins 230, as shown in
Leveling leaf 225 allows leaf 225 to hold support 130 of bottle holder and valve assembly 120 in a horizontal orientation during the sample filtration step of an SPE procedure. Set screw 238 has hexagonal recess 239 which accepts an Allen wrench to facilitate installation and adjustment of set screw 238. Leaf 225 has pins 230, which may be, but are not necessarily, socket cap screws (for example with ¼-28 thread). In use, support block 130 sits in between two adjacent leaf 225. Lower section 130B of support block 130 sits in between pins 230 with pins 230 positioning support block 130 of bottle holder and valve assembly 120 so that sample delivery tube 136 rests approximately in the center of cavity 112 of disk holder 104. Leaf 225, if not located at either end of horizontal member 222 will have pins 230 located on both sides of leaf 225 to facilitate the use of bottle holder and valve assembly 120 on either side of leaf 225. In practice, as leaf 225 is detachable, it may be desirable to have all leaves 225 have pins 230 on both sides as this would allow all leaves 225 to be used on any mounting point 226. Pins 230, as shown in
Bottle holder and valve assembly 120 is placed in between two adjacent leaf 244B with support block upper section 130A resting on the top surface of two adjacent leaf 244B and support block lower section 130B resting in between two adjacent leaf 244B. Sample delivery tube 136 of bottle holder and valve assembly 120 extends into cavity 112 of disk holder 104. Detachable support leaf 245 serves the same purpose as hinged leaf 244 but instead of being hinged are detachable. Leaf 245A is shown as detached when not in use as to facilitate access to disk holder 104 as is necessary to complete certain steps in a solid phase extraction procedure. Leaf 245B is shown as installed on horizontal support 242 and functions the same as hinged leaf 244B. Hinged leaf(s) 244B may be rotated to the upright position and detachable leaf(s) 245B may be detached after completion of the sample filtration step for the sample(s) using the bottle holder and valve assemblies 120 they are supporting.
Horizontal member 242 has peg 242A onto which leaf 245A may be placed for storage while detached and not in use. Rear legs 150A and middle legs 150B support horizontal member 242 and shelf 227. Front legs 150C support shelf 227. Horizontal member 242 is oriented in a plane at a right angle to the plane that passes through both rear legs 150A. System rack 240 sits on work surface 146 which may be located in a fume hood due to the solvents typically employed in solid phase extraction procedures. Note that leaf 244B and Leaf 245B are offset to the right relative to square openings 228 on shelf 227. This is due to the asymmetry of fluid management block 200 with hole 78, into which bushing 202, fitting 58A and Luer valve 114 are installed, and on which disk holder 104 rests, are offset to the right. System components could be manufactured and/or installed with an offset to the left if desired or with no offset if block 200 were manufactured with hole 78 centered in block 200.
Vacuum manifold 154 is attached to rear legs 150A and located below shelf 227. Vacuum manifold has vacuum port(s) 156, with one vacuum port 156 for each block 200 that can be accommodated on rack 240. Vacuum port(s) 156 is attached to tubing 46B with a suitable fitting and supplies vacuum to fitting 30 and fitting 32 on fluid management block 200 through tubing 46B and attached fitting 214. Vacuum port(s) 156 may have a valve attached to provide individual control to each vacuum port 156 and this valve may be, but is not necessarily, a Luer valve. This valve may be located at any point in between port 156 and fitting 30 or fitting 32 on block 200. Vacuum manifold 154 also has vacuum port 158 which is connected to a wastewater container and vacuum source. Vacuum manifold 154 may also be equipped with a vacuum gauge to monitor vacuum. Rack 240 as shown can accommodate components for one to five sample extractions, being able to hold up to five block(s) 200 and up to five bottle holder and valve assembly 120. Rack 240 can be configured to accommodate components for any number of sample extractions.
Leaf 244 has end piece 235 located at one end of leaf 244 to provide a surface on which to mount hinge 234. End piece 235 also has hole 237 (for example, with ¼-28 threads) to accept set screw 238 (for example, ¼-28 thread). Hole 237 lines up with hole 237A in leaf 234A of hinge 234. Hole 237A is separate from the holes used to mount leaf 234A to end piece 235. Hole 237A, may be, but is not necessarily, also threaded (for example, with ¼-28 thread). Set screw 238, when installed in hole 237, and passing through hole 237A, is in contact with leaf 234B of hinge 234. Leaf 234B is attached to horizontal member 242 with the screws (not shown) used to attach leaf 234B to horizontal member 242 passing through standoff 236. Set screw 238 can be adjusted to make leaf 244 level when in the lowered position. Leveling leaf 244 allows leaf 244 to hold support 130 of bottle holder and valve assembly 120 in a horizontal orientation during the sample filtration step of an SPE procedure. Set screw 238 has hexagonal recess 239 which accepts an Allen wrench to facilitate installation and adjustment of set screw 238. Leaf 244 has pin 230, which may be, but is not necessarily, a socket cap screw (for example with ¼-28 thread). Lower section 130B of support block 130 sits in between pin 230 and horizontal member 242 with pins 230 and horizontal member 242 positioning support block 130 of bottle holder and valve assembly 120 so that sample delivery tube 136 rests approximately in the center of cavity 112 of disk holder 104. Leaf 244, if not located at either end of horizontal member 242 will have pins 230 located on both sides of leaf 244 to facilitate the use of bottle holder and valve assembly 120 on either side of leaf 244. Leaf 244, if located at either end of horizontal member 242, need only have pin 230 on the side of leaf 244 that will be used to support bottle holder and valve assembly 120. Pin 230, as shown in
Leveling leaf 225 allows leaf 225 to hold support 130 of bottle holder and valve assembly 120 in a horizontal orientation during the sample filtration step of an SPE procedure. Set screw 238 has hexagonal recess 239 which accepts an Allen wrench to facilitate installation and adjustment of set screw 238. Leaf 225 has pins 230, which may be, but are not necessarily, socket cap screws (for example with ¼-28 thread). In use, support block 130 sits in between two adjacent leaves 225. Lower section 130B of support block 130 sits in between pins 230 with pins 230 positioning support block 130 of bottle holder and valve assembly 120 so that sample delivery tube 136 rests approximately in the center of cavity 112 of disk holder 104. Leaf 225, if not located at either end of horizontal member 242 will have pins 230 located on both sides of leaf 225 to facilitate the use of bottle holder and valve assembly 120 on either side of leaf 225. In practice, as leaf 225 is detachable, it may be desirable to have all leaves 225 have pins 230 on both sides as this would allow all leaves 225 to be used on any mounting point 226. Pins 230, as shown in
The presence of mounting point 226 at more than one height allows the distance between leaf 225A and shelf 227 to change depending on whether lower mounting point 226A or upper mounting point 226B is chosen to mount leaf 225A. The differing mounting heights can facilitate the use of SPE media of different heights, such as SPE cartridges, or the use or non-use of Luer valve 114 in between fitting 58A and fitting 110 of disk holder 104. Shelf 227 has openings 228 into which fluid management block(s) 200 are installed and secured with threaded fasteners or by other means. The threaded fasteners pass through suitable holes in the interior walls of opening(s) 228 and into threaded mounting hole(s) 201 of Block 200.
In use, disk holder 104 is mounted on fitting 58A or Female Luer port 54 of valve 114. Bottle holder and valve assembly 120 is placed in between two adjacent leaves 225B which are mounted at the same level above shelf 227. Support block upper section 130A rests on the top surface of two adjacent leaf 225B and support block lower section 130B rests in between two adjacent leaves 225B. Sample delivery tube 136 of bottle holder and valve assembly 120 extends into cavity 112 of disk holder 104. Detachable support leaf 225 serves the same purpose as hinged leaf 224 but instead of being hinged they are detachable. Leaf 225A is shown as detached when not in use as to facilitate access to disk holder 104 as is necessary to complete certain steps in a solid phase extraction procedure. Detachable leaf(s) 225B may be detached after completion of the sample filtration step for the sample(s) using the bottle holder and valve assemblies 120 they are supporting. System rack 250 sits on work surface 146 which may be located in a fume hood due to the solvents typically employed in solid phase extraction procedures. Note that leaf 225B is offset to the right relative to square openings 228 on shelf 227. This is due to the asymmetry of fluid management block 200 with hole 78, into which bushing 202, fitting 58A and Luer valve 114 are installed, and on which disk holder 104 rests, are offset to the right.
System components could be manufactured and/or installed with an offset to the left if desired or with no offset if block 200 were manufactured with hole 78 centered in block 200. Vacuum manifold 154 is attached to rear legs 150A and located below shelf 227. Vacuum manifold has vacuum port(s) 156, with one vacuum port 156 for each block 200 that can be accommodated on rack 250. Vacuum port(s) 156 is attached to tubing 46B with a suitable fitting and supplies vacuum to fitting 30 and fitting 32 on fluid management block 200 through tubing 46B and attached fitting 214. Vacuum port(s) 156 may have a valve attached to provide individual control to each vacuum port 156 and this valve may be, but is not necessarily, a Luer valve. This valve may be located at any point in between port 156 and fitting 30 or fitting 32 on block 200. Vacuum manifold 154 also has vacuum port 158 which is connected to a waste-water container and vacuum source. Vacuum manifold 154 may also be equipped with a vacuum gauge to monitor vacuum. Rack 250 as shown can accommodate components for one to five sample extractions, being able to hold up to five block(s) 200 and up to five bottle holder and valve assembly 120. Rack 250 can be configured to accommodate components for any number of sample extractions.
Leveling leaf 225 allows leaf 225 to hold support 130 of bottle holder and valve assembly 120 in a horizontal orientation during the sample filtration step of an SPE procedure. Set screw 238 has hexagonal recess 239 which accepts an Allen wrench to facilitate installation and adjustment of set screw 238. Leaf 225 has pins 230, which may be, but are not necessarily, socket cap screws (for example with ¼-28 thread). In use, support block 130 sits in between two adjacent leaves 225 which must be installed on mounting points 226 located at the same level. Lower section 130B of support block 130 sits in between pins 230 with pins 230 positioning support block 130 of bottle holder and valve assembly 120 so that sample delivery tube 136 rests approximately in the center of cavity 112 of disk holder 104. Leaf 225, if not located at either end of horizontal member 252 will have pins 230 located on both sides of leaf 225 to facilitate the use of bottle holder and valve assembly 120 on either side of leaf 225.
In practice, as leaf 225 is detachable, it may be desirable to have all leaves 225 have pins 230 on both sides as this would allow all leaves 225 to be used on any mounting point 226. Pins 230, as shown in
Sample delivery tube 136 of bottle holder and valve assembly 120 extends into cavity 112 of disk holder 104. Detachable fork(s) 274 may be detached after completion of the sample filtration step for the sample(s) using the bottle holder and valve assemblies 120 they are supporting. System rack 270 sits on work surface 146 which may be located in a fume hood due to the solvents typically employed in solid phase extraction procedures. Note that fork(s) 274 are offset to the right relative to square openings 228 on shelf 227. This is due to the asymmetry of fluid management block 200 with hole 78, into which bushing 202, fitting 58A and Luer valve 114 are installed, and on which disk holder 104 rests, are offset to the right.
System components could be manufactured and/or installed with an offset to the left if desired or with no offset if block 200 were manufactured with hole 78 centered in block 200. Vacuum manifold 154 is attached to rear legs 150A and located below shelf 227. Vacuum manifold has vacuum port(s) 156, with one vacuum port 156 for each block 200 that can be accommodated on rack 270. Vacuum port(s) 156 is attached to tubing 46B with a suitable fitting and supplies vacuum to fitting 30 and fitting 32 on fluid management block 200 through tubing 46B and attached fitting 214. Vacuum port(s) 156 may have a valve attached to provide individual control to each vacuum port 156 and this valve may be, but is not necessarily, a Luer valve. This valve may be located at any point in between port 156 and fitting 30 or fitting 32 on block 200. Vacuum manifold 154 also has vacuum port 158 which is connected to a wastewater container and vacuum source. Vacuum manifold 154 may also be equipped with a vacuum gauge to monitor vacuum. Rack 270 as shown can accommodate components for one to five sample extractions, being able to hold up to five block(s) 200 and up to five bottle holder and valve assembly 120. Rack 270 can be configured to accommodate components for any number of sample extractions. Rack 270 as shown in
Leveling fork 274 allows fork 274 to hold support 130 of bottle holder and valve assembly 120 in a horizontal orientation during the sample filtration step of an SPE procedure. Set screw 238 has hexagonal recess 239 which accepts an Allen wrench to facilitate installation and adjustment of set screw 238. Fork 274 has pins 230, which may be, but are not necessarily, socket cap screws (for example with ¼-28 thread). In use, support block 130 sits in between two arms 275 located on the same fork 274. Lower section 130B of support block 130 sits in between arms 275 with pins 230 positioning support block 130 of bottle holder and valve assembly 120 so that sample delivery tube 136 rests approximately in the center of cavity 112 of disk holder 104. Pins 230, as shown in
In operation, the solid phase extraction system described may be used to extract liquid samples, for example, water samples, by an SPE procedure. The objective may be to obtain an extract of organic solvent containing selected trace chemicals that were originally present in the water sample. This extract is typically, but not necessarily, an organic solvent and may have a volume, after concentration procedures, of 1/50th to 1/2,000th the volume of the original water sample. The extract is then tested using a determinative technique to determine the concentration of various trace chemicals in the extract. This data can be used to calculate the concentration of these trace chemicals in the original water sample.
To perform an SPE extraction the following steps are taken. These steps are typically done with both block 70, block 200 and if using system rack 138, 140, 220, 240, 250, 270 or a system rack of similar design. The water sample to be extracted by SPE is typically collected in a glass bottle. Bottle holder and valve assembly 120 is attached directly to this sample bottle by means of the appropriate hole cap such as hole cap 122 (for example, for 33-430 thread bottles). Bottle holder and valve assembly 120 as depicted in
The actual volume of the water sample undergoing the SPE procedure is also normally determined. This is often done by marking the meniscus on the bottle for later determination by refilling the bottle to the meniscus mark with reagent water after the SPE extraction is complete. The volume of reagent water needed to refill the sample bottle to the meniscus mark is then determined. The sample to be extracted by the SPE procedure may require pH adjustment or the addition of preservatives, dichlorinating agents or other chemicals depending on the specific SPE procedure being conducted. After performing any steps necessary to prepare the water sample for extraction by the SPE procedure, bottle holder and valve assembly 120 are attached to the sample bottle by means of the appropriate hole cap.
Next, porous member 102 is placed in recess 108 and SPE disk 100 is installed in recess 106 of disk holder 104. Other known disk holders can also be used provided they have an outlet with male Luer tip 44 to interface with Luer valve 114 or fitting 58A, and a sufficient reservoir above disk 100 to contain the water sample delivered by sample delivery tube 136. SPE cartridge 260 could also be used in place of disk holder 104 and SPE disk 100 if a suitable reservoir were attached to flange 262.
If using system rack 138 or 140 the following steps are taken after completing the assembly of disk holder 104 and attaching bottle holder and valve assembly 120 to the sample bottle.
Block 70, with all the fittings and parts shown in
Next, a vial or bottle with 24-414 or 24-410 thread may be installed in recess 76 or hole cap 88 of block 70. Then fitting 58B with attached tubing 46B may be attached to fitting 30 as shown in
Next, ball valve 132 may be moved in the closed position and bottle holder and valve assembly 120 may be inverted with attached sample bottle. Then bottle holder and valve assembly 120 are placed, with attached sample bottle, in square hole 148 of upper shelf 142 of system rack 138 or in square hole 148 of individual upper shelf segment 143 of system rack 140. Cutout 152 as shown in
It is often desirable to wash SPE disk 100 with solvent prior to use to remove interfering compounds which may be present such as phthalate plasticizers. Some types of SPE disk 100 also require conditioning with a polar solvent such as methyl alcohol before use. If SPE disk 100 washing or conditioning is required, the appropriate wash or conditioning solvents are introduced into disk holder 104. Luer valve 114 is operated to transfer, under vacuum, the solvents from disk holder 104 to the vial or bottle, such as vial 94 (for example having 40 mL volume and 24-414 thread), installed in recess 76 or hole cap 88 of block 70. If conditioning is required SPE disk 100 should remain immersed and not be exposed to air until filtration of the water sample is complete. Note that 30 mL and 60 mL vials with 24-414 thread and 125 mL bottles with 24-410 thread are also available. The vacuum may be controlled by Luer valve 114 installed under disk holder 104 or by other means. The volume of the vial or bottle used is based on the anticipated volume of the wash solvents or conditioning solvents. The specific wash or conditioning solvents, the volume of solvent used and the order the solvents (which may include water) are introduced is typically specified in the SPE extraction procedure.
After any wash or conditioning steps are complete close Luer valve 114 under disk holder 104. Optionally, the vacuum may be turned off. A second valve installed on port(s) 156 or port 158 of vacuum manifold 154 is a convenient means for controlling vacuum but is not required.
Next, the vial installed in recess 76 or hole cap 88 of block 70 may be removed. Rinse and conditioning solvents contained in the vial are generally disposed. The vial may be rinsed with solvent for later use in collecting the extract. As a next step, fitting 58B with attached tubing 46B may be detached from fitting 30, and fitting 58B installed on fitting 34 as shown in
After filtration of the water sample is complete air or an inert gas may be passed through SPE disk 100 to remove residual water from SPE disk 100. Next, Luer valve 114 under disk holder 104 is closed and fitting 58B is removed from fitting 34. Install fitting 58B on fitting 30 and install a vial in recess 76 or hole cap 88 of block 70. The objective of the next step is to elute the trace chemicals captured by SPE disk 100 from the water sample off of SPE disk 100, transferring these trace chemicals from SPE disk 100 into a small volume of organic solvent.
These solvents are termed elution solvents. A polar elution solvent should be used first as a non-polar solvent, being immiscible with water, may fail to pass through water saturated SPE disk 100, even when vacuum or positive pressure is applied. Some SPE procedures require that the sample bottle first be rinsed with the elution solvent(s) before the solvent is transferred to disk holder 104. This polar organic elution solvent is added to disk holder 104 in a quantity sufficient to cover and saturate SPE disk 100. A typical 47 mm SPE disk using disk holder 104 might require 7 mL of solvent. Additional solvent may be required if the water sample contained sediment or debris. After allowing the elution solvent to soak SPE disk 100 for a specified time, open Luer valve 114 under disk holder 104, or otherwise apply vacuum, and collect the polar elution solvent in the vial installed in recess 76 or hole cap 88 of block 70. This step is usually repeated with a non-polar solvent with the specific SPE procedure being employed determining the solvents chosen and the number of elution steps performed.
If using system rack 220, the steps of the SPE procedure detailed above for system rack 138 and system rack 140 apply. The mounting of fluid management block 200 in system rack 200 differs from the mounting of fluid management block 70 in system rack 138 and system rack 140. The specifics for mounting bottle holder and valve assembly 120 on system rack 220 also differ from the specifics for mounting bottle holder and valve assembly 120 on system rack 138 and system rack 140. System rack 220 has horizontal member 222 oriented in the same plane as the plane that passes through rear legs 150A. Horizontal member 222 may be permanently mounted to legs 150A or may be adjustable in height above shelf 227. Adjusting the height of horizontal member 222 can allow for the use of different SPE consumables, such as SPE cartridge 260 or other disposable SPE consumables, or prior art SPE disk holders that have different heights while maintaining the correct clearance between the lower end of sample delivery tube 136 and the upper surface of SPE disk 100. The clearance between the lower end of sample delivery tube 136 and the upper surface of SPE disk 100 (or other SPE consumable) can also be adjusted by moving support block 130 up or down connecting tube 128.
If using system rack 240, the steps of the SPE procedure detailed above for system rack 138 and system rack 140 apply. The use and construction of system rack 240 is similar to that of system rack 220. The primary difference being horizontal member 242 is oriented in a plane at a right angle to the plane that passes through rear legs 150A and extends forward to middle legs 150B. As a consequence of this the rear part of larger width upper section 130A of block 130 rests directly on horizontal member 242 with hinged support leaf 244A or detachable support leaf 245A supporting the middle and front part of larger width upper section 130A of block 130. Leaves 244 and 245 also differ from leaves 224 and 225 in that leaves 244 and 245 have a single pin 230 which sits in front of narrower width lower section 130B of block 130.
Leaves 224 and 225 have two pins 230 with narrower width lower section 130B of block 130 sitting in between the two pins 230. Peg 242A is shown in
If using system rack 250, the steps of the SPE procedure detailed above for system rack 138 and system rack 140 apply. The use and construction of system rack 250 is similar to that of system rack 220. The primary difference being horizontal member 252 has attachment points 226 at two (or more) different levels. This serves to allow detachable leaf 225 to be installed at different heights above shelf 227. This allows bottle holder and valve assembly 120 to have differing heights above shelf 227 and block 200. This facilitates the maintenance of the proper clearance between the lower end of sample delivery tube 136 and the upper surface of SPE disk 100 as described above. This can allow for the use of different SPE consumables, such as SPE cartridge 260 or prior art SPE disk holders that have different heights or the use of SPE disk(s) 100 of differing thicknesses. Horizontal member 252 could be at a fixed height above shelf 227 or be adjustable in height.
If using system rack 270, the steps of the SPE procedure detailed above for system rack 138 and system rack 140 apply. The use and construction of system rack 270 is similar to that of system rack 250. The primary difference being support fork(s) 274 is used in place of support leaves 225. Two adjacent leaves 225 are required to hold block 130 of bottle holder and valve assembly 120 in system rack 220 and system rack 250. In system rack 270 the two arms of a single support fork 274 hold block 130 of bottle holder and valve assembly 120. Horizontal member 272 could be at a fixed height above shelf 227 or be adjustable in height above shelf 227. Rack 270 is shown with mounting points 276 at two heights above shelf 227. System rack 270 could have mounting point(s) 276 at a single height above shelf 227 or at two or more heights above shelf 227.
System rack 270 is also shown in
In use, the water sample undergoing extraction by an SPE procedure that specifies filtering the water sample through two SPE cartridges 260 in series or through SPE disk 100 followed by SPE cartridge 260 also in series would pass from the sample bottle, through bottle holder and valve assembly 120, into cavity 112 of disk holder 104 and through SPE disk 100. The water sample would then pass through tubing 46A (and associated fittings) of block 200 and into cartridge connecting tubing 279. Next, the water sample would then enter male Luer tip 44 at the bottom of SPE cartridge 260 as shown in
Some prior art SPE disk holder designs feature a mechanism to clamp down on the edge of SPE disk 100 to secure it in place. This prevents the water sample from flowing through the outside edge of the SPE disk held under this clamping mechanism and can effectively reduce the usable surface area of SPE disk 100 by 25%. Some of these prior art disk holders are compatible with the SPE extraction system described in this provisional patent application. If 25% of a 47 mm SPE disk's surface is covered by this prior art disk holder clamping mechanism 5 mL of solvent should be sufficient for an elution step. There are also disposable consumables that have a plastic housing holding sorbent material that functions as an SPE disk. These disposable consumables may also be compatible with this SPE extraction system provided they have male Luer tip 44 as an outlet and a sufficient reservoir that can function in the same way as cavity 122 of disk holder 104. Support block 130 on bottle holder and valve assembly 120 can be adjusted up or down connecting tube 128 to allow for consumables or prior art disk holders that have differing heights, maintaining a clearance (e.g., an approximate 7 mm clearance) below the lower end of sample delivery tube 136 and the upper surface of SPE disk 100.
A solvent extract obtained from this SPE extraction system normally undergoes a procedure to remove residual water in the extract. This water is the water that remained in SPE disk 100 when the polar elution solvent was added to disk holder 104. The extract may be dried by passing it through an anhydrous salt such as sodium sulfate or through a phase separation membrane. Fluid management block 70 or block 200 may be used to facilitate extract drying. A syringe barrel of suitable volume with a frit in the bottom can be used to hold sodium sulfate. The male Luer tip of the syringe barrel being installed directly on female Luer port 54 of Luer valve 114, located on fitting 58A. The solvent extract to be dried is poured into the syringe barrel with sodium sulfate, Luer valve 114 is opened, and the dried extract collected in a 24-414 vial installed in recess 76 or hole cap 88 of block 70 or block 200. Any phase separation membrane drying system with a male Luer outlet can be similarly used.
Male Luer fittings such as fitting 30, modified to allow ⅛″ outside diameter tubing 46 to pass through enlarged passageway 33 of male Luer tip 44 may or may not have tubing 46 fit with a friction fit through passageway 33. Examples of such modified male Luer fitting include, but are not limited to, fitting 32 and fitting 34. Male Luer fittings such as fitting 48, modified to allow ⅛″ outside diameter tubing 46 to pass through enlarged passageway 51 of male Luer tip 44 may or may not have tubing 46 fit with a friction fit through passageway 51. Examples of such modified male Luer fitting include, but are not limited to, fitting 50. ⅛″ outside diameter tubing 46 could be replaced with 3 mm outside diameter tubing or another diameter that would fit through male Luer port 44 with or without the described modifications to male Luer tip 44 shown in
Various concepts may be embodied as one or more methods, of which at least one example has been provided. The acts performed as part of the method may be ordered in any suitable way. Accordingly, embodiments may be constructed in which acts are performed in an order different than illustrated, which may include performing some acts simultaneously, even though shown as sequential acts in illustrative embodiments. Put differently, it is to be understood that such features may not necessarily be limited to a particular order of execution, but rather, any number of threads, processes, services, servers, and/or the like that may execute serially, asynchronously, concurrently, in parallel, simultaneously, synchronously, and/or the like in a manner consistent with the disclosure. As such, some of these features may be mutually contradictory, in that they cannot be simultaneously present in a single embodiment. Similarly, some features are applicable to one aspect of the innovations, and inapplicable to others.
In addition, the disclosure may include other innovations not presently described. Applicant reserves all rights in such innovations, including the right to embodiment such innovations, file additional applications, continuations, continuations-in-part, divisional s, and/or the like thereof. As such, it should be understood that advantages, embodiments, examples, functional, features, logical, operational, organizational, structural, topological, and/or other aspects of the disclosure are not to be considered limitations on the disclosure as defined by the embodiments or limitations on equivalents to the embodiments. Depending on the particular desires and/or characteristics of an individual and/or enterprise user, database configuration and/or relational model, data type, data transmission and/or network framework, syntax structure, and/or the like, various embodiments of the technology disclosed herein may be implemented in a manner that enables a great deal of flexibility and customization as described herein.
All definitions, as defined and used herein, should be understood to control over dictionary definitions, definitions in documents incorporated by reference, and/or ordinary meanings of the defined terms.
As used herein, the term “about” and “approximately” generally mean plus or minus 10% of the value stated, e.g., about 250 μm would include 225 μm to 275 μm, about 1,000 μm would include 900 μm to 1,100 μm.
The phrase “and/or,” as used herein in the specification and in the embodiments, should be understood to mean “either or both” of the elements so conjoined, i.e., elements that are conjunctively present in some cases and disjunctively present in other cases. Multiple elements listed with “and/or” should be construed in the same fashion, i.e., “one or more” of the elements so conjoined. Other elements may optionally be present other than the elements specifically identified by the “and/or” clause, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, a reference to “A and/or B”, when used in conjunction with open-ended language such as “comprising” can refer, in one embodiment, to A only (optionally including elements other than B); in another embodiment, to B only (optionally including elements other than A); in yet another embodiment, to both A and B (optionally including other elements); etc.
As used herein in the specification and in the embodiments, “or” should be understood to have the same meaning as “and/or” as defined above. For example, when separating items in a list, “or” or “and/or” shall be interpreted as being inclusive, i.e., the inclusion of at least one, but also including more than one, of a number or list of elements, and, optionally, additional unlisted items. Only terms clearly indicated to the contrary, such as “only one of” or “exactly one of,” or, when used in the embodiments, “consisting of,” will refer to the inclusion of exactly one element of a number or list of elements. In general, the term “or” as used herein shall only be interpreted as indicating exclusive alternatives (i.e., “one or the other but not both”) when preceded by terms of exclusivity, such as “either,” “one of” “only one of” or “exactly one of.” “Consisting essentially of,” when used in the embodiments, shall have its ordinary meaning as used in the field of patent law.
As used herein in the specification and in the embodiments, the phrase “at least one,” in reference to a list of one or more elements, should be understood to mean at least one element selected from any one or more of the elements in the list of elements, but not necessarily including at least one of each and every element specifically listed within the list of elements and not excluding any combinations of elements in the list of elements. This definition also allows that elements may optionally be present other than the elements specifically identified within the list of elements to which the phrase “at least one” refers, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, “at least one of A and B” (or, equivalently, “at least one of A or B,” or, equivalently “at least one of A and/or B”) can refer, in one embodiment, to at least one, optionally including more than one, A, with no B present (and optionally including elements other than B); in another embodiment, to at least one, optionally including more than one, B, with no A present (and optionally including elements other than A); in yet another embodiment, to at least one, optionally including more than one, A, and at least one, optionally including more than one, B (and optionally including other elements); etc.
In the embodiments, as well as in the specification above, all transitional phrases such as “comprising,” “including,” “carrying,” “having,” “containing,” “involving,” “holding,” “composed of,” and the like are to be understood to be open-ended, i.e., to mean including but not limited to. Only the transitional phrases “consisting of” and “consisting essentially of” shall be closed or semi-closed transitional phrases, respectively, as set forth in the United States Patent Office Manual of Patent Examining Procedures, Section 2111.03.
While specific embodiments of the present disclosure have been outlined above, many alternatives, modifications, and variations will be apparent to those skilled in the art. Accordingly, the embodiments set forth herein are intended to be illustrative, not limiting. Various changes may be made without departing from the spirit and scope of the disclosure. Where methods and steps described above indicate certain events occurring in a certain order, those of ordinary skill in the art having the benefit of this disclosure would recognize that the ordering of certain steps may be modified, and such modification are in accordance with the variations of the invention. Additionally, certain of the steps may be performed concurrently in a parallel process when possible, as well as performed sequentially as described above. The embodiments have been particularly shown and described, but it will be understood that various changes in form and details may be made.
This application claims priority to and the benefit of U.S. Provisional Patent Application No. 63/175,328, filed Apr. 15, 2021 and titled “Modified Luer Fittings and Solid Phase Extraction System,” and U.S. Provisional Patent Application No. 63/243,202, filed Sep. 13, 2021 and titled “Modified Luer Fittings and Improved Solid Phase Extraction System,” the disclosures of which are hereby incorporated by reference in its entirety.
| Number | Date | Country | |
|---|---|---|---|
| 63175328 | Apr 2021 | US | |
| 63243202 | Sep 2021 | US |
