WO2016073672A1 - Compositions, appareil et procédés de détermination des ions chlorure dans une composition d'analyte - Google Patents

Compositions, appareil et procédés de détermination des ions chlorure dans une composition d'analyte Download PDF

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Publication number
WO2016073672A1
WO2016073672A1 PCT/US2015/059160 US2015059160W WO2016073672A1 WO 2016073672 A1 WO2016073672 A1 WO 2016073672A1 US 2015059160 W US2015059160 W US 2015059160W WO 2016073672 A1 WO2016073672 A1 WO 2016073672A1
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composition
microwells
titrant
chloride ion
iron
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PCT/US2015/059160
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English (en)
Inventor
Justin M. DRAGNA
Tyler WEST
Adam Garland
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Water Lens, LLC
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Publication of WO2016073672A1 publication Critical patent/WO2016073672A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/02—Adapting objects or devices to another
    • B01L2200/025—Align devices or objects to ensure defined positions relative to each other
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/14—Process control and prevention of errors
    • B01L2200/148—Specific details about calibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/16—Reagents, handling or storing thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/02—Identification, exchange or storage of information
    • B01L2300/025—Displaying results or values with integrated means
    • B01L2300/027—Digital display, e.g. LCD, LED
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • B01L3/5085—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates
    • B01L3/50855—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates using modular assemblies of strips or of individual wells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/251—Colorimeters; Construction thereof
    • G01N21/253—Colorimeters; Construction thereof for batch operation, i.e. multisample apparatus
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Definitions

  • kits and methods of the present invention are used to determine the chloride ion concentrate in an analyte composition by adding the analyte composition to a lyophilized titrant composition in each microwell of the plurality of microwells to form a solution in each microwell having a detectable absorbance in response to the chloride ion in the analyte composition
  • the solution resides in the use of lyophilized titrant samples in a microwell plate.
  • Analyte samples are added to the lyophilized samples and the absorbance of the resulting samples is measured and the chloride concentration of the analyte composition is determined based on the measured absorbance value.
  • the present invention eliminates the drawbacks of traditional manual titrations by eliminating the subjective naked- eye determination and provides a rapid analysis and accurate analysis of the analyte composition at the user site.
  • the present invention removes the subjective naked-eye determination of an endpoint by using a spectrophotometer to determine the endpoint.
  • a chloride ion assay kit includes a) a microwell plate and b) a lyophilized titrant composition comprising an acid compound, an iron (III) compound, and mercury (II) thiocyanate.
  • a plurality of microwells of the microwell plate contain the lyophilized titrant composition such that when an analyte composition is added to the lyophilized titrant composition in each microwell of the plurality of microwells a solution forms having an absorbance at a detectable wavelength in response to chloride ion comprised in the analyte composition.
  • the chloride ion in the analyte composition causes the mercury (II) thiocyanate to dissociate.
  • the free thiocyanate can then coordinate to iron (III) forming a colored complex.
  • the amount of the colored complex formed is proportional to the amount of chloride present in the sample. By developing calibration curves based on these proportions, the chloride concentration can be determined quantitatively.
  • the detectable wavelength can be between 440 nm and 460 nm, and preferably at 450 nm.
  • the microwell plate can include 6, 24, 96, 384, or 1536 microwells.
  • the microwell plate includes 6 microwells and each microwell contains the same amount of titrant composition or at least 2 microwells have the same amount of titrant and the rest of the microwells have a different amount of titrant composition.
  • the microwell plate has at least 24 or 96 microwells and at least 10 microwells contain the same amount of titrant solutions or at least 10 microwells contain the same amount of titrant composition, and some of the microwells have a different amount of titrant composition as other microwells.
  • the amounts of lyophilized titrant are used at a 1 :3 or a 1 :2 dilution with the analyte composition.
  • the plurality of microwells can be sealed to prevent the titrant composition from exiting the plurality of microwells.
  • the plurality of microwells is sealed with a plastic film or a foil.
  • the chloride ion assay kit can also include a spectrophotometer capable of measuring ultra violet and visible wavelengths.
  • the titrant can be a composition that includes an acid compound, an iron (III) compound, and mercury (II) thiocyanate, where the composition has an absorbance at a detectable wavelength in response to chloride ion comprised in the solution.
  • the acid compound can be camphor sulfonic acid, p-toluenesulfonic acid 1,4- piperazinediethanesulfonic acid, 2-(N-morpholino)ethanesulfonic acid, 3-(N- morpholino)propanesulfonic acid, or any combination thereof, with 2-(N- morpholino)ethanesulfonic acid and camphor sulfonic acid being preferred.
  • the iron (III) compound can be iron (III) nitrate, iron (III) sulfate, iron (III) chloride, iron (III) triflate, or any combination thereof, with iron (III) nitrate being preferred.
  • the titrant composition consists essentially of a 2-(N-morpholino)ethanesulfonic acid, iron nitrate, and mercury (II) thiocyanate.
  • the composition can be a powder.
  • the powder can be made by providing an aqueous solution of the titrant composition to one or more containers and subjecting at least one of the containers to lyophilizing conditions sufficient to remove the water from the aqueous solution to form the powder.
  • the one or more containers are microwells of a microwell plate.
  • the powder can be packaged (for example, a bag, vial, or encapsulated). The powder can be sold separately from the kit.
  • the chloride ion assay kit of the present invention can be used to determine the chloride concentration of an analyte composition or a plurality of analyte compositions.
  • the method can include a) obtaining any one of the chloride ion assay kits described throughout this Specification; b) obtaining an analyte composition; c) adding substantially the same volume of the analyte composition to each of the plurality of microwells of the microwell plate to form solutions from the analyte composition and the lyophilized titrate compositions in each of the plurality of microwells; and d) measuring the absorbance value for each solution in each of the plurality of microwells at a wavelength and determining the chloride ion concentration of the analyte composition based on the measured absorbance values in response to chloride ion comprised in the analyte composition.
  • the pH of the formed solution can be from 6 to 9.
  • the measured absorbance ranges from 0.1 to 1.1 and the concentration of chloride ions ranges from greater than 0.1 up to 250 mg/L at a wavelength of 450 nm. In some instances, the measured absorbance can be 0.1932 and the concentration of chloride ions is 1 mg/L and/or the measured absorbance can be 0.9903 and the concentration of chloride ions is 200 mg/L at a wavelength of 450 nm.
  • the analyte can be obtained from a variety of sources such as a subsurface well, a hydrocarbon subsurface, a water well in a subsurface hydrocarbon formation, or a wastewater reservoir or tank.
  • the analyte composition is obtained from a hydrocarbon drilling or fracking process. In some instances, a plurality of solutions having the same analyte is obtained, and each analyte composition is obtained from a different well of a plurality of subsurface wells or a plurality of different wastewater units.
  • the chloride ion assay kits described throughout the Specification can be made by a) obtaining a microwell plate; b) obtaining a lyophilized titrant composition comprising an acid compound, an iron (III) compound and mercury (II) thiocyanate; wherein a plurality of microwells of the microwell plate contain the lyophilized titrant composition such that when an analyte composition is added to the lyophilized titrant composition in each microwell of the plurality of microwells a solution forms having an absorbance at a known wavelength in response to chloride ion comprised in the analyte composition.
  • the lyophilized titrant composition can be obtained by providing an aqueous solution of the titrant composition to one or more microwells of the microwell plate and subjecting the microwell plate to lyophilizing conditions sufficient to remove the water from the aqueous solution and form a powder.
  • Embodiment 1 describes a composition for determining the chloride content of a solution.
  • the composition can include an acid compound, an iron (III) compound, and mercury (II) thiocyanate and the composition can have an absorbance at a detectable wavelength in response to chloride ion contained in the solution.
  • Embodiment 2 is the composition of embodiment 1, where the acid compound can include camphor sulfonic acid, p- toluenesulfonic acid 1 ,4-piperazinediethanesulfonic acid, 2-(N-morpholino)ethanesulfonic acid, 3-(N-morpholino)propanesulfonic acid, or any combination thereof, with 2-(N- morpholino)ethanesulfonic acid, or any combination thereof.
  • Embodiment 3 is the compositions of any one of embodiments 2 or 3 where the acid compound is camphor sulfonic acid, 2-(N-morpholino)ethanesulfonic acid, or both.
  • Embodiment 4 is the compositions of any one of embodiments 1 to 3 where the iron (III) compound can include iron (III) nitrate, iron (III) sulfate, iron (III) chloride, iron (III) triflate, or any combination thereof.
  • Embodiment 5 is the composition of embodiment 4, wherein the iron (III) compound is iron (III) nitrate.
  • Embodiment 6 is the composition of embodiment 1, wherein the composition consists essentially of 2-(N-morpholino)ethanesulfonic acid, iron (III) nitrate, and mercury (II) thiocyanate.
  • Embodiment 7 is the compositions of embodiments any one of 1 to 6, wherein the composition is a powder.
  • Embodiment 8 is the composition of embodiment 7, wherein the powder is made by providing an aqueous solution of the titrant composition to one or more containers and subjecting at least one of the containers to lyophilizing conditions sufficient to remove the water from the aqueous solution to form the powder.
  • Embodiment 9 is the composition of embodiment 8, wherein the one or more containers are microwells of a microwell plate.
  • Embodiment 10 is the compositions of any one of embodiments 8 or 9, wherein the container is a bag or a vial.
  • Embodiment 11 describes a chloride ion assay kit.
  • the chloride ion assay kit can include (a) a microwell plate; and (b) a lyophilized titrant composition that includes an acid compound, an iron (III) compound, and mercury (II) thiocyanate.
  • a plurality of microwells of the microwell plate contain the lyophilized titrant composition such that when an analyte composition is added to the lyophilized titrant composition in each microwell of the plurality of microwells a solution forms having an absorbance at a detectable wavelength in response to chloride ion comprised in the analyte composition.
  • Embodiment 12 is the chloride ion assay kit of embodiment 11, wherein the microwell plate comprises 6, 24, 96, 384, or 1536 microwells.
  • Embodiment 13 is the chloride ion assay kit of any one of embodiments 11 or 12, wherein the microwell plate comprises 6 microwells and each microwell contains the same amount of titrant composition.
  • Embodiment 14 is the chloride ion assay kit of any one of embodiments 11 to 12, wherein the microwell plate comprises 24 microwells or 96 microwells, and at least 10 microwells contain the same amount of titrant composition.
  • Embodiment 15 is the chloride ion assay kit of any one of embodiments 11 to 12, wherein the microwell plate comprises 6 microwells and at least 2 microwells have the same amount of titrant and the rest have of the microwells have a different amount of titrant composition.
  • Embodiment 16 is the chloride ion assay kit of any one of embodiments 11 to 15, wherein the amounts of lyophilized titrant are used at a 1 :3 or a 1 :2 dilution with the analyte composition.
  • Embodiment 17 is the chloride ion assay kit of any one of embodiments 11 to 16, wherein the micro well plate comprises 24 microwells or 96 microwells, and at least 10 microwells contain the same amount of titrant composition, and some of the remaining microwells have a different amount of titrant composition.
  • Embodiment 18 is the chloride ion assay kit of embodiment 17, wherein the acid compound camphor sulfonic acid, p-toluenesulfonic acid 1 ,4-piperazinediethanesulfonic acid, 2-(N-morpholino)ethanesulfonic acid, 3-(N- morpholino)propanesulfonic acid, or any combination thereof.
  • Embodiment 19 is the chloride ion assay kit of embodiment 18, wherein acid compound is 1,4- piperazinediethanesulfonic acid.
  • Embodiment 20 is the chloride ion assay kit of any one of embodiments 11 to 19, wherein the iron (III) compound is iron (III), nitrate, iron (III) sulfate, iron (III) chloride, iron (III) triflate, or any combination thereof.
  • Embodiment 21 is the chloride ion assay kit of embodiment 20, wherein the iron (III) compound is iron nitrate.
  • Embodiment 22 is the chloride ion assay kit of any one of embodiments 11 to 22, wherein the detectable wavelength is between 440 nm and 460 nm, and preferably at 450 nm.
  • Embodiment 23 is the chloride ion assay kit of any one of embodiments 11 to 22, wherein the plurality of microwells are sealed to prevent the titrant composition from exiting the plurality of microwells.
  • Embodiment 24 is the chloride ion assay kit of embodiment 23, wherein the plurality of microwells are sealed with a plastic film or a foil.
  • Embodiment 25 is the chloride ion assay kit of any one of embodiments 11 to 24, further comprising a spectrophotometer capable of measuring ultra violet and visible wavelengths.
  • Embodiment 26 is a method of determining the chloride ion concentration of an analyte composition.
  • the method can include (a) obtaining any one of the compositions as of any one of embodiments 1 to 10 or an one of the chloride assay kits of embodiments 11 to 25; (b) obtaining an analyte composition; (c) adding substantially the same volume of the analyte composition to each of the plurality of microwells of the microwell plate to form solutions from the analyte composition and the lyophilized titrate compositions in each of the plurality of microwells; and (d) measuring the absorbance value for each solution in each of the plurality of microwells at a wavelength and determining the chloride ion concentration of the analyte composition based on the measured absorbance values in response to chloride ion contained in the analyte composition.
  • Embodiment 27 is the method of embodiment 26, wherein a ratio of the amount of titrant to sample is from 1 :2 to 1 :3.
  • Embodiment 28 is the method of any one of embodiments 26 to 27, wherein the wavelength is 450 nm and the measured absorbance ranges from 0.1 to 1.1 and the concentration of chloride ions ranges from greater than 0.1 up to 250 mg/L.
  • Embodiment 29 is the method of embodiment 28, wherein the wavelength is 450 nm and the measured absorbance is 0.1932 and the concentration of chloride ions is 1 mg/L.
  • Embodiment 30 is the method of embodiment 28, wherein wavelength is 450 nm and the measured absorbance is 0.9903 and the concentration of chloride ions is 200 mg/L.
  • Embodiment 31 is the method of any one of embodiments 26 to 30, wherein the acid compound is 1 ,4-piperazinediethanesulfonic acid.
  • Embodiment 32 is he method of embodiment 26, wherein the titrant composition consists essentially of a 1,4- piperazinediethanesulfonic acid, iron nitrate, and mercury (II) thiocyanate.
  • Embodiment 33 is the method of any one of embodiments 26 to 32, wherein the analyte in is an aqueous composition obtained from a subsurface well.
  • Embodiment 34 is the method of any one of embodiments 26 to 33, wherein the analyte composition comprises a plurality of solutions having the same analyte, and each analyte composition is obtained from a different well of a plurality of subsurface wells.
  • Embodiment 35 is the method of embodiments 33 or 34, wherein the well is a hydrocarbon well or a water well in a subsurface hydrocarbon formation.
  • Embodiment 36 is the method of any one of embodiments 26 to 35, wherein the analyte composition is obtained from a drilling process or fracking process.
  • Embodiment 37 is the method of any one of embodiments 26 to 36, wherein the analyte composition is obtained from a wastewater tank or reservoir.
  • Embodiment 38 is a method of making any one of the chloride assay kits of embodiments 12 to 25.
  • the method can include (a) obtaining a microwell plate; and (b) obtaining a lyophilized titrant composition that includes an acid compound, an iron (III) compound and mercury (II) thiocyanate, wherein a plurality of microwells of the microwell plate contain the lyophilized titrant composition such that when an analyte composition is added to the lyophilized titrant composition in each microwell of the plurality of microwells a solution forms having an absorbance at a known wavelength in response to chloride ion contained in the analyte composition.
  • Embodiment 39 is the method of embodiment 38, wherein obtaining a lyophilized titrant composition can include providing an aqueous solution of the titrant composition to one or more microwells of the microwell plate and subjecting the microwell plate to lyophilizing conditions sufficient to remove the water from the aqueous solution and form a powder.
  • Embodiment 40 is the method of any one of embodiments 38 or 39, wherein the plurality of microwells are sealed to prevent the titrant composition from exiting the plurality of microwells.
  • Embodiment 41 is the method of embodiment 40, wherein the plurality of microwells are sealed with a plastic film or a foil.
  • acidic solution or “acid compound” refers to a solution that has a concentration of hydrogen ions greater than the concentration of hydroxide ion ([H+] > [OH ]).
  • basic solution or "alkaline solution” refers to a solution that has a concentration of hydrogen ions less than the concentration of hydroxide ion ([H+] ⁇ [OH ]).
  • the chloride ion assay kits and the methods of using and making the chloride ion assay kits of the present invention can "comprise,” “consist essentially of,” or “consist of particular ingredients, components, compositions, etc. disclosed throughout the specification. With respect to the transitional phase “consisting essentially of,” in one non-limiting aspect, a basic and novel characteristic of the kits of the present invention is the ability to determine the chloride concentration of an aqueous solution using spectrometric analysis.
  • FIGS. 1A-1C are schematics of chloride ion assay kits of the present invention.
  • FIG. 2 is a flow chart depicting a method of determining chloride concentration of a water body.
  • FIG. 3 is a graph of chloride concentration (mg/L) versus absorbance.
  • the titrant sample can include an acid compound, an iron (III) compound and mercury (II) thiocyanate.
  • Each microwell of the microwell of the microwell plates has at least two microwells having the same amount of titrant composition.
  • the analyte composition is added to the titrant to form a solution and the chloride concentration of the solution is determined by measuring the absorbance value for each solution in each of the plurality of wells at determining the chloride concentration of the analyte composition based on the measured absorbance values on a calibration curve.
  • the titrant composition can be made by preparing an aqueous solution of titrant solution and then subjecting the solution to lyophilizing conditions to remove the water and produce a powder.
  • a saturated solution of mercuric thiocyanate saturated in water can be prepared by adding mercuric thiocyanate.
  • the saturated solution can be filtered.
  • To the filtered solution the acid composition and iron (III) compound and diluted to a known volume to produce the titrant solution.
  • the amounts of acid, iron compound and mercuric thiocyanate can be determined using known stoichiometric calculations.
  • the titrant solution can have a pH from 3.3 to 3.7, preferable 3.5 and a concentration of 250 to 350 mM of acid, 25 to 35 mM iron (III) and saturated Hg(SCN) 2 .
  • the titrant solution can be lyophilized and then specific amounts of the resulting powder can be added to each microwell of a microwell plate. In some embodiments, the titrant solution is not lyophilized.
  • a known volume of titrant solution is added to the microwells of the microwell plate and the microwell plate subjected to lyophilizing conditions. Lyophilizing conditions include -60 °C and 100 mtorr.
  • the microwells of a 96-microwell plate can be filled with 100 microliters of aqueous titrant composition. If a 1 :2 dilution the analyte composition was to be used, the microwells of a 96-microwell plate can be filled with 150 microliters of aqueous titrant composition.
  • FIGS. 1A-1C depict schematics of embodiments of chloride ion assay system 100.
  • the chloride ion assay system or kit includes microwell plate 102 having a plurality of microwells 104.
  • the plurality of microwells 104 can be assembled in the removable holders 106.
  • Holders 106 may include members 108 that position on top of the side wall 110. Holders 106 may rest on, or be suspended above, bottom wall 112 of the microwell plate 102.
  • holder 106 includes eight (8) microwells 104, however, it should be understood that the number of microwells can be adjusted to the size of the microwell plate 102.
  • the number of the microwells 104 can be 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, etc.
  • the microwell plate 102 does not include any titrant composition.
  • FIG. IB depicts all of the microwells having titrant composition 114 and
  • FIG. 1C depicts some of the microwells having titrant composition 114.
  • the microwells 104 can hold a volume of 20, 50, 300, 500 microliters, preferably 300 microliters or 400 microliters.
  • the microwell plate 102, microwells 104, holders 106 can be made of any chemical resistant material.
  • Non-limiting examples of materials include polymers, copolymers of polymers, polystyrene, polypropylene, cyclo-olefms and the like.
  • the holders 106 may be polymeric or plastic tape with the microwells 104 embossed on the tape. Microwell plates are commercially available from Thermo Fisher Scientific (Waltham, MA, USA). [0031] As shown in FIG. IB, the microwells 104 can be filled with the same amount of lyophilized titrant composition. In other embodiments, the microwells 104 in each holder 106 can have the same amount of titrant composition, but a total amount of titrant composition in the holders 106 can be different.
  • microwells 104-1 to 104-8 can have a different amount of titrant composition than microwells 104-9 to 104-16.
  • configuration of the amount titrant in the microwells can be any chosen configuration that correlates to a calibration curve.
  • the microwells 104 are filled with a known amount of an aqueous solution of titrant composition and then microwell plate is positioned in a lyophilizing unit and lyophilized under conditions sufficient to remove the water from the solution.
  • the microwells 104, microwell holders 106, and/or the microwell plate can be sealed with a known sealing agent (for example, plastic film or foil) to allow the microwell plate 102 or the microwell holders 106 to stored or transported.
  • a known sealing agent for example, plastic film or foil
  • the chloride assay system includes a spectrophotometer that is capable of measuring the absorbance of the chosen colorimetric dye and/or a calibration curve.
  • the calibration curve depicts the amount of chloride ion versus absorbance value.
  • a calibration curve is provided for each holder 106.
  • the chloride ion assay system and kit described throughout the specification can be used to determine the chloride concentration of a solution.
  • the solution can be a sample from a water body such as a subsurface water well in a hydrocarbon formation, a wastewater storage unit, a wastewater reservoir, a lake, a river, a canal or the like.
  • a flow chart for determining chloride concentration is depicted.
  • the microwell plate 102 containing the lyophilized titrant composition 114 is obtained in step 202.
  • step 204 a known amount of analyte composition (for example 300 microliters) is added to the lyophilized titrant composition 114 reagents in the microwells 104 using a delivery apparatus (for example, multichannel pipette).
  • a delivery apparatus for example, multichannel pipette.
  • step 206 after solids in the plate have fully dissolved, the microwell plate 102 is placed in a spectrophotometer (for example, a plate reader) and the absorbance at the known wavelength (for example 450 nm) for each microwell is measured. The chloride concentration is determined by referring to a calibration curve and selecting the chloride concentration that correlates to the absorbance value.
  • the system 100 can be automated to acquire data.
  • the acquired data can be transmitted to one or more computer systems.
  • the computer systems can include components such as CPUs or applications with an associated machine readable medium or article which may store an instruction or a set of instructions that, if executed by a machine, may cause the machine to perform a method and/or operations in accordance with the methods of the present invention.
  • the microwell plate 102 can be put in a plate reader and the spectrophotometer can automatically measure the absorbance of each sample.
  • the measured absorbance can be stored in a computer system in the spectrophotometer and/or transmitted to another computer system.
  • Either computer may be capable of processing the absorbance and displaying or printing a chloride ion value for a series of analytes.
  • Such a machine may include, for example, any suitable processing platform, computing platform, computing device, processing device, computing system, processing system, computer, processor, or the like, and may be implemented using any suitable combination of hardware and/or software.
  • the machine-readable medium or article may include, for example, any suitable type of memory unit, memory device, memory article, memory medium, storage device, storage article, storage medium and/or storage unit, for example, memory, removable or non-removable media, erasable or non-erasable media, writeable or re-writeable media, digital or analog media, hard disk, floppy disk, Compact Disk Read Only Memory (CD-ROM), Compact Disk Recordable (CD-R), Compact Disk Rewriteable (CD-RW), optical disk, magnetic media, magneto-optical media, removable memory cards or disks, various types of Digital Versatile Disk (DVD), a tape, a cassette, or the like.
  • CD-ROM Compact Disk Read Only Memory
  • CD-R Compact Disk Recordable
  • CD-RW Compact Dis
  • the instructions may include any suitable type of code, such as source code, compiled code, interpreted code, executable code, static code, dynamic code, and the like.
  • the instructions may be implemented using any suitable high-level, low-level, object- oriented, visual, compiled and/or interpreted programming language, such as C, C++, Java, BASIC, Perl, Matlab, Pascal, Visual BASIC, assembly language, machine code, and so forth.
  • the computer system may further include a display device such as monitor, an alphanumeric input device such as keyboard, and a directional input device such as mouse.
  • Titrant Composition A saturated solution of mercuric thiocyanate saturated in water was prepared by adding mercuric thiocyanate (2 grams, ACS grade, Alfa) to distilled water (1L) and let stir overnight. The remaining slurry was filtered through a 0.22 micron filter and used to prepare all further reagents. 2-(N-morpholino)ethanesulfonic acid (14.8 g, (MES), ACS grade, Alfa) and iron (III) nitrate nonahydrate (3.1 g, ACS, grade, Alfa) were dissolved in the aqueous saturated Hg(SCN) 2 solution and diluted up to 250 mL volumetrically. The resultant solution was filtered through a 0.22 micron filter and constitutes the aqueous titrant composition: 300 mM MES, 30 mM iron (III), sat. Hg(SCN) 2 , pH 3.5.
  • the microwells of a 96-microwell plate were filled with 100 microliters of aqueous titrant composition. If a 1 :2 dilution the analyte composition was to be used, the microwells of a 96-microwell plate were filled with 150 microliters of aqueous titrant composition. The aqueous titrant composition was lyophilizing to remove water to obtain the lyophilized sample in the microwell plate at - 60 °C and lOO mtorr. [0037] Calibration Curve.
  • a calibration curve was produced by diluting a chloride standard (1000 mg/L, Hach) to the concentrations in Table 1, then filling a freeze-dried plate of a 100 microliter fill of the titrant composition with 300 microliters of sample. The data was then fit with a four-parameter Marquadt non- linear function as shown in FIG. 3.
  • the lyophilized titrant sample, the microwell plate, and, optionally, the calibration curve, constitute the chlorine assay kit.

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Abstract

L'invention concerne des compositions, des kits et des procédés d'utilisation des kits et des compositions pour déterminer la concentration de chlorure dans une solution. Le kit peut comprendre une solution titrée lyophilisée.
PCT/US2015/059160 2014-11-07 2015-11-05 Compositions, appareil et procédés de détermination des ions chlorure dans une composition d'analyte WO2016073672A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114018909A (zh) * 2021-11-08 2022-02-08 河海大学 快速检测污水中氯离子的试棒及其制备方法和应用
USD975312S1 (en) 2020-02-14 2023-01-10 Beckman Coulter, Inc. Reagent cartridge

Citations (4)

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Publication number Priority date Publication date Assignee Title
US4393142A (en) * 1982-02-01 1983-07-12 American Monitor Corporation Assay method and reagent for the determination of chloride
US4800168A (en) * 1985-10-17 1989-01-24 Hoffmann-La Roche Inc. Two reagent system for the colorimetric determination of chloride ions in body fluids
JP4012169B2 (ja) * 2003-05-09 2007-11-21 独立行政法人科学技術振興機構 複数種のイオン測定用器具
CN102621135A (zh) * 2012-02-17 2012-08-01 中国人民解放军海军工程大学 锅炉用水微量氯离子的测试方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4393142A (en) * 1982-02-01 1983-07-12 American Monitor Corporation Assay method and reagent for the determination of chloride
US4800168A (en) * 1985-10-17 1989-01-24 Hoffmann-La Roche Inc. Two reagent system for the colorimetric determination of chloride ions in body fluids
JP4012169B2 (ja) * 2003-05-09 2007-11-21 独立行政法人科学技術振興機構 複数種のイオン測定用器具
CN102621135A (zh) * 2012-02-17 2012-08-01 中国人民解放军海军工程大学 锅炉用水微量氯离子的测试方法

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FLORENCE, T. M. ET AL.: "Spectrophotometric determination of chloride at the parts-per-billion level by the Mercury (II) thiocyanate method", ANALYTICA CHIMICA ACTA, vol. 54, no. 2, April 1971 (1971-04-01), pages 373 - 377 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
USD975312S1 (en) 2020-02-14 2023-01-10 Beckman Coulter, Inc. Reagent cartridge
USD1012310S1 (en) 2020-02-14 2024-01-23 Beckman Coulter, Inc. Reagent cartridge
CN114018909A (zh) * 2021-11-08 2022-02-08 河海大学 快速检测污水中氯离子的试棒及其制备方法和应用

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