WO2025030201A1 - Procédé standardisé de mesure de l'efficacité de sorption d'un sorbant - Google Patents

Procédé standardisé de mesure de l'efficacité de sorption d'un sorbant Download PDF

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WO2025030201A1
WO2025030201A1 PCT/AU2023/050738 AU2023050738W WO2025030201A1 WO 2025030201 A1 WO2025030201 A1 WO 2025030201A1 AU 2023050738 W AU2023050738 W AU 2023050738W WO 2025030201 A1 WO2025030201 A1 WO 2025030201A1
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contaminant
mixture
sorbent
formula
matrix
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Ross NEFODOV
Matthew ASKELAND
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Ade Consulting Group Pty Ltd
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Ade Consulting Group Pty Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24—Earth materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
    • B09B3/10—Destroying solid waste or transforming solid waste into something useful or harmless involving an adsorption step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09C—RECLAMATION OF CONTAMINATED SOIL
    • B09C1/00—Reclamation of contaminated soil
    • B09C1/002—Reclamation of contaminated soil involving in-situ ground water treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09C—RECLAMATION OF CONTAMINATED SOIL
    • B09C1/00—Reclamation of contaminated soil
    • B09C1/08—Reclamation of contaminated soil chemically
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8693—Models, e.g. prediction of retention times, method development and validation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B2101/00—Type of solid waste
    • B09B2101/40—Asphalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B2101/00—Type of solid waste
    • B09B2101/90—Soil, e.g. excavated soil from construction sites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09C—RECLAMATION OF CONTAMINATED SOIL
    • B09C2101/00—In situ
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/06—Contaminated groundwater or leachate
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/8872—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample impurities
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G01N33/1813—Specific cations in water, e.g. heavy metals
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G01N33/182—Specific anions in water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G01N33/1826—Organic contamination in water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24—Earth materials
    • G01N33/241—Earth materials for hydrocarbon content

Definitions

  • the present disclosure relates to the remediation of contaminated materials.
  • the present disclosure relates to a method that supports remediation processes which involve the use of sorbents.
  • Soil and other materials at former industrial sites are often contaminated with a number of different organic and inorganic substances, including per- and polyfluoroalkyl substances (PFASs), which are of concern from a health and environmental perspective.
  • PFASs per- and polyfluoroalkyl substances
  • the materials must be remediated to remove or minimise the risk that such contaminants may otherwise pose.
  • the remediation can be done on-site, or, in some cases, such as in infrastructure projects where contaminated material is excavated and transported to other sites for reuse or disposal, materials that have been removed from a site may also need to be treated to minimise the risk of contaminants leaching off-site.
  • a common method of remediating such materials involves the use of sorbents which absorb or adsorb the contaminants.
  • the sorbents are applied to, for example, the soil and blended with the soil, resulting in the conversion of one or more contaminants to a less soluble, mobile and/or toxic form, and leading to a reduction in the hazard potential of the material.
  • this stabilisation results in a less soluble or mobile contaminant, this leads to a reduced level of leachability of that contaminant from the material. In turn, this results in a reduced risk that the material could cause groundwater contamination and/or toxicity to humans or animals contacting the material.
  • sorbents are blended into contaminated materials at a known percentage (% w/w) to immobilize contaminants.
  • contaminants are a structurally diverse group of compounds, and they therefore bind to sorbents by various binding mechanisms.
  • Current approaches to assessing sorbent performance include:
  • SSA specific surface area
  • Sorption/desorption kinetics modelling e.g., European Council of Chemical Manufacturers’ Federation, Test Methods for Activated Carbon 1986.
  • Leaching procedure testing e.g., Australian Standard Leaching Procedure (ASLP) tests, Australian Standard AS4439.
  • ASLP Australian Standard Leaching Procedure
  • Sorption/desorption kinetic modelling does offer a direct way to determine the sorption and desorption kinetics of a sorbent product for contaminants that is then comparable to other products.
  • the disadvantage of this method is that kinetics studies require multiple samples to be analysed over multiple time points. Therefore, it is not cost or time efficient to complete kinetics studies for standardizing the characterization of contaminant sorbent product efficacy. Further, for the results to be comparable, studies need to be completed in the same concentration range and experimental conditions, which is often not possible, particularly for on-site testing. Regarding the ASLP procedure, this measures contaminant leachability over a set period to simulate 100 years in a landfill.
  • the method is only applied to soil or treated soil samples with no easily calculable kinetics information once testing is complete, and it only calculates the leachable fraction but does not account for sorption as a single measure. It also does not allow for the easy comparison of different sorbents.
  • a method of determining the efficacy of a sorbent at sorbing a contaminant thereto comprising the following steps: 1) Testing a first mixture comprising a solution and a contaminant to determine an initial contaminant concentration (“IC”);
  • Step 4 [(PQ + NR)/200] x 100 (Formula V), wherein an SSQM score closer to 1 indicates that the sorbent has low efficacy at sorbing the contaminant thereto, and an SSQM score closer to 100 indicates that the sorbent has high efficacy at sorbing the contaminant thereto, and wherein Step 4) can be carried out after Step 5).
  • the method may include an additional step of adding a sample of a soil or other matrix to determine the efficacy of a sorbent for sorbing a contaminant thereto in the presence of the matrix. Therefore, in a second aspect, there is also provided a method of determining the efficacy of a sorbent at sorbing a contaminant thereto, the method comprising the following steps:
  • MSQM [(PQ + NR)/200] x 100 (Formula V), wherein an MSQM score closer to 1 indicates that the sorbent has low efficacy at sorbing the contaminant thereto in the presence of the matrix, and an MSQM score closer to 100 indicates that the sorbent has high efficacy at sorbing the contaminant thereto in the presence of the matrix, and wherein Step 4) can be carried out after Step 5).
  • the solution of the first mixture may be an aqueous solution.
  • the aqueous solution may be water.
  • the water may be purified water.
  • the contaminant may be added to the first mixture from a stock solution of the contaminant.
  • the contaminant may be added to the first mixture to achieve a contaminant concentration of about 1 mg/L in the second mixture.
  • the stock solution may be an alcohol solution.
  • the alcohol may be methanol or ethanol.
  • the weight ratio of solution to matrix may be about 1:20.
  • the weight ratio of solution to sorbent when no matrix is present (i.e., in the first aspect), the weight ratio of solution to sorbent may be about 2500:1. In the embodiment where matrix is present in the second mixture (i.e., in the second aspect), the weight ratio of solution to sorbent may be about 25:1.
  • the aqueous solution devoid of contaminant may be pure water.
  • the pure water may be ultrapure water.
  • the contaminant may be an organic contaminant.
  • the organic contaminant may be a per- and poly-fluorinated substance (PFAS).
  • the sorbent may be an alum-based sorbent, a carbon-based sorbent, a mineral-based sorbent, a resin-based sorbent, or a combination thereof.
  • the matrix may be soil, mining tailings and by-products, sludge waste, industrial waste, tunnelling and excavation spoils, rock, asphalt, compost, biosolids, or mixtures thereof.
  • Figure 1 is a flow chart depicting the application of one embodiment of the method of the present invention - in sorbent application optioning;
  • Figure 2 is a flow chart depicting a summary of an embodiment of the method of the present invention.
  • Figure 3 is a graph showing the SSQM score of various sorbents in respect of the PFAS perfluorohexanesulfonic acid (PFHxS);
  • Figure 4 is a graph showing the SSQM score of various sorbents in respect of the PFAS perfluorooctane sulfonate (PFOS);
  • Figure 5 is a graph showing the SSQM score of various sorbents in respect of the PFAS perfluorobutanesulfonic acid (PFBS);
  • Figure 6 is a graph showing the SSQM score of various sorbents in respect of the PFAS perfluorobutanoic acid (PFBA);
  • Figure 7 is a graph showing the SSQM score of various sorbents in respect of the PFAS perfluorohexanoic acid (PFHxA).
  • Figure 8 is a graph showing the SSQM score of various sorbents in respect of the PFAS perfluorooctanoic acid (PFOA).
  • PFOA perfluorooctanoic acid
  • the present inventors have surprisingly found that the efficacy with which a sorbent absorbs or adsorbs a contaminant from, for example, a site or material requiring remediation, can be assessed using well-understood experimental procedures, analytical methods, and simple calculations, in a way that also allows a variety of sorbent types to be compared with each other.
  • Step 4 [(PQ + NR)/200] x 100 (Formula V), wherein an SSQM score closer to 1 indicates that the sorbent has low efficacy at sorbing the contaminant thereto, and an SSQM score closer to 100 indicates that the sorbent has high efficacy at sorbing the contaminant thereto, and wherein Step 4) can be carried out after Step 5).
  • the present inventors have also surprisingly found that the method is amenable to the assessment of sorbent efficacy in the presence of a matrix, such as a soil. Therefore, the method may include an additional step of adding a sample of a soil or other matrix to determine the efficacy of a sorbent for sorbing a contaminant thereto in the presence of the matrix. Therefore, there is also provided a method of determining the efficacy of a sorbent at sorbing a contaminant thereto, the method comprising the following steps:
  • MSQM [(PQ + NR)/200] x 100 (Formula V), wherein an MSQM score closer to 1 indicates that the sorbent has low efficacy at sorbing the contaminant thereto in the presence of the matrix, and an MSQM score closer to 100 indicates that the sorbent has high efficacy at sorbing the contaminant thereto in the presence of the matrix, and wherein Step 4) may be carried out after Step 5).
  • the methods defined above are designed to be quick, simple, cheap and effective. They can directly measure the contaminant sorption/desorption in an economical and effective way. A set of values is produced that allows one to compare sorbent product efficacy for use in contamination treatment in a standardized way. The methods provide a way to benchmark sorbent products of any composition for comparison between product types, and reduce the cost of testing and benchmarking contaminant sorption efficacy significantly compared to kinetics/isothermal modelling.
  • the contaminants that may be used in the methods will reflect those that are typically present at remediation sites, and include inorganic contaminants such as metals, metalloids, halogens and nutrients (particularly, one or more of antimony, arsenic, boron, cadmium, chromium, cobalt, copper, cyanide, fluoride, lead, manganese, mercury, molybdenum, nickel, phosphate, selenium, uranium, and zinc) and organic contaminants including, for example, polycyclic aromatic hydrocarbons (PAHs), total petroleum hydrocarbons (TPH), "benzene, toluene, ethylbenzene and xylenes" (BTEX), benzo[a]pyrene (B(a)P), volatile organic compounds (VOCs), organic pesticides and herbicides, fertilisers, polychlorinated biphenyls (PCBs), per- and poly-fluorinated hydrocarbons (PFASs) such as perfluoro
  • the sorbent may be any sorbent that is typically used for the stabilisation of inorganic contaminants, organic contaminants, or the simultaneous stabilisation of inorganic and organic contaminants.
  • the sorbent may be an alum-based sorbent, a carbon-based sorbent, a mineral-based sorbent, a resin-based sorbent, or a combination thereof.
  • carbon-based sorbents are activated charcoal, and Biochar, which is a product of the slow pyrolysis of biomass.
  • An example of a mineralbased sorbent is Fluoro-Sorb®, which is composed of bentonite and long-chain quaternary ammonium salts.
  • An example of an alum-based sorbent is an alum sludge composition.
  • a suitable alum sludge composition is described in WO 2011/038459.
  • the sorbent may be an alum-based sorbent or a carbonbased sorbent, or a combination thereof.
  • a combination of an alum-based sorbent and a carbon-based sorbent is also described in WO 2011/038459 and is sold under the trade name RemBind®.
  • the methods comprise the first step (Step 1) of testing a first mixture comprising a solution and a contaminant (and, in one method, a matrix) to determine an initial contaminant concentration (“IC”).
  • IC is the initial concentration of the contaminant in the solution of the first mixture and is intended to reflect the concentration of the contaminant before any, or before any substantial, sorption of the contaminant to the sorbent (and, in one method, the matrix) has occurred.
  • the solution and contaminant will be combined and briefly mixed.
  • the testing can be conducted by any means known to be suitable to a person skilled in the art. For example, an aliquot of the mixture may be removed, processed appropriately, and analysed by, for example, Eiquid Chromatography-Mass Spectrometry (LC- MS) to determine the IC.
  • LC- MS Eiquid Chromatography-Mass Spectrometry
  • the solution of the first mixture may be an aqueous solution.
  • the aqueous solution may be water.
  • the water may be purified water.
  • the purified water may have been obtained through purification by, for example, distillation and/or filtration.
  • the purified water may be ultrapure water.
  • the contaminant may be added to the first mixture from a stock solution of the contaminant.
  • the concentration of the contaminant in the stock solution may be about 50 mg/E.
  • the contaminant may be added to the first mixture to achieve a contaminant concentration of about 1 mg/L in the second mixture.
  • the contaminant concentration will be as close to 1 mg/L as possible, but when a matrix is also used in the method, there may be some variation in this as there may be some contaminant already present in the matrix.
  • a dilution of the first mixture may be carried out if, for example, a particular volume of the second mixture is required of to carry out Step 3) of the methods.
  • the stock solution may be an alcohol solution.
  • the alcohol may be methanol or ethanol. Reagent grade alcohol solutions may be used. Testing the first mixture, as discussed above, will confirm the concentration of the contaminant in the first mixture i.e., the IC.
  • a matrix is also used, it will be understood by a person skilled in the art that the matrix that may be used will reflect those materials that are typically present at remediation sites. Matrices that have already been contaminated (for example, matrices obtained from sites requiring remediation) or matrices that have not yet been contaminated can be used in the methods. The methods may be applied to any matrix type, however, the methods are particularly suitable for application to matrices such as soils, mining tailings and by-products, sludge wastes (e.g. effluent treatment sludges), industrial wastes, tunnelling and excavation spoils, rock, asphalt, compost and biosolids, or mixtures thereof. Preferably, the matrix is soil. The methods may be used in land management (i.e., where soil is treated with sorbent and reused on the same site), and may also be applied to contaminated matrix that has been taken from a site, such as stockpiled material, transient soil, and in treatment facilities.
  • land management i.e., where soil
  • the weight ratio of solution to matrix may be about 1:20.
  • the term “about” in the context of this weight ratio is intended to refer to a variation of +/- 5%.
  • Step 2 sorbent is added to the first mixture to produce a second mixture.
  • the weight ratio of solution to sorbent may be about 2500:1.
  • the weight ratio of solution to sorbent may be about 25:1. The term “about” in the context of these weight ratios is intended to refer to a variation of +/- 5%.
  • Step 3) of the methods comprises subjecting the second mixture to conditions sufficient to facilitate sorption of the contaminant to the sorbent (and, when present, the matrix), thereby producing a third mixture.
  • condition sufficient to facilitate sorption of the contaminant to the sorbent refers to any conditions that the first mixture may be subjected to that induce, or allow, the contaminant to adsorb onto or absorb into the sorbent in such a way that the contaminant is retained on or by the sorbent.
  • condition sufficient to facilitate sorption of the contaminant to the sorbent and/or the matrix refers to any conditions that the first mixture may be subjected to that induce, or allow, the contaminant to adsorb onto or absorb into the sorbent and/or matrix in such a way that the contaminant is retained on or by the sorbent and/or the matrix.
  • any potential effects that the matrix may have on the efficacy of the sorbent at sorbing the contaminant can be observed. In this way, the performance of a particular sorbent at sorbing a contaminant in a real setting e.g., in a remediation site, can be assessed.
  • the same matrix that is present at a site of interest may be used.
  • the conditions may be achieved by agitating the first mixture in any suitable way known to a person skilled in the art.
  • the mixture may be shaken, centrifuged, or stirred.
  • the first mixture may be shaken (e.g., tumbled) for about 24 hours at about 30 rpm.
  • An example of a suitable apparatus is an end-over-end shaker.
  • the agitation may be carried out at room temperature.
  • Step 4) of the methods comprises testing the third mixture to determine the concentration of the contaminant remaining in the solution (“SC”).
  • SC is the concentration of the contaminant remaining in the solution after the second mixture has been subjected to conditions that facilitate sorption of the contaminant to the sorbent (and, in the case where matrix is also present, to the matrix) and is therefore intended to reflect the amount of contaminant that has not been sorbed by the sorbent (and/or the matrix).
  • the testing can be conducted by any means known to be suitable to a person skilled in the art. For example, an aliquot of the mixture may be removed, processed appropriately, and analysed by, for example, Liquid Chromatography-Mass Spectrometry (LC-MS) to determine the SC.
  • LC-MS Liquid Chromatography-Mass Spectrometry
  • Step 5) of the methods comprises replacing the liquid in the third mixture with an aqueous solution devoid of the contaminant to give a fourth mixture.
  • the solution present in the third mixture may be removed by, for example, carefully decanting the solution from the mixture. Ideally, in this step, as little as possible of the remaining components of the mixture are removed along with the liquid. Therefore, it may be preferable to allow the mixture to settle for a period of time after Step 3) and before removing the liquid.
  • an aqueous solution is added to the remaining components, thereby forming a fourth mixture.
  • the aqueous solution should not contain any (or should contain only an undetectable amount) of the contaminant(s) that are being assessed using the methods.
  • the aqueous solution of Step 5 should be devoid of the contaminant.
  • the aqueous solution may be water.
  • the water may be pure water i.e., purified water.
  • the purified water may have been obtained through purification by, for example, distillation and/or filtration.
  • the water may be ultrapure water (also commonly known as high purity water or highly purified water).
  • Step 5 A person skilled in the art will understand that, rather than testing the third mixture after Step 3), the third mixture could be tested after the liquid has been removed from the second mixture (and replaced with an aqueous solution), as in Step 5). That is, the liquid that has been removed from the third mixture can be tested to determine the SC. Therefore, in the methods of the present invention, the order of Steps 4) and 5) can be reversed, such that Step 4) may be carried out after Step 5).
  • the amount of contaminant that desorbs from the sorbent (and/or the matrix) may be determined.
  • Step 6) comprises subjecting the fourth mixture to conditions sufficient to facilitate the desorption of the contaminant from the sorbent (and/or the matrix) into the aqueous solution, thereby forming a fifth mixture.
  • condition sufficient to facilitate desorption of the contaminant from the sorbent refers to any conditions that the fourth mixture may be subjected to that induce, or allow, the contaminant that has so far remained sorbed onto or into the sorbent to detach or desorb from the sorbent in such a way that the contaminant leeches from the sorbent into the aqueous solution.
  • condition sufficient to facilitate desorption of the contaminant from the sorbent and/or the matrix refers to any conditions that the fourth mixture may be subjected to that induce, or allow, the contaminant that has so far remained sorbed onto or into the sorbent and/or the matrix to detach or desorb from the sorbent and/or the matrix in such a way that the contaminant leeches from the sorbent and/or the matrix into the aqueous solution.
  • the conditions may be achieved by agitating the fourth mixture in any suitable way known to a person skilled in the art.
  • the mixture may be shaken, centrifuged, or stirred.
  • the fourth mixture may be shaken (e.g., tumbled) for about 24 hours at about 30 rpm.
  • An example of a suitable apparatus is an end-over-end shaker.
  • the agitation may be carried out at room temperature.
  • Step 7) comprises testing the fifth mixture, formed by agitating the fourth mixture, to determine the concentration of the contaminant in the aqueous solution (“DC”).
  • the DC is the concentration of the contaminant in the solution after the fourth mixture has been subjected to conditions that facilitate desorption of the contaminant from the sorbent (and, in the case where matrix is also present, from the matrix) and is therefore intended to reflect the amount of contaminant that was sorbed by the sorbent (and/or the matrix) in Step 3).
  • the testing can be conducted by any means known to be suitable to a person skilled in the art. For example, an aliquot of the mixture may be removed, processed appropriately, and analysed by, for example, Liquid Chromatography-Mass Spectrometry (LC-MS) to determine the DC.
  • LC-MS Liquid Chromatography-Mass Spectrometry
  • the Percentage Sorbed measures the proportion of contaminant mass removed from the solution by the sorbent (and/or the matrix, in the method where a matrix is present in Step 1). This value can range from 1% to 100%.
  • a high PS i.e., >90 %) means that the sorbent has performed well at removing the contaminant under the standardized testing conditions.
  • the Percentage Desorbed (PD) measures the proportion of the contaminant that has been remobilized into the aqueous solution devoid of the contaminant, based on the IC.
  • a low PD e.g., of about 1 to about 5%
  • a low PD means that contaminant sorption to the sorbent (and/or the matrix) is not easily reversible.
  • the Performance Quotient is a measure of the irreversible sorption/desorption of the contaminant and is heavily weighted towards desorption. A higher PQ is desirable, however, if a small amount of the contaminant is remobilized during the desorption testing (i.e., Step 6)) this will greatly decrease the PQ. Therefore, the PQ needs to be considered in the context of the PS and PD.
  • the Net Removal (NR) is the total percentage mass of the contaminant that has been removed from the first mixture irreversibly under the standardized conditions. As with PS, higher numbers show better performance of the sorbent, with values ranging from 0% to 100%.
  • the SSQM score is based on the PQ and the NR, with both weighted evenly. Higher performing sorbents will exhibit a higher SSQM score. An SSQM score closer to 1 indicates that the sorbent has low efficacy at sorbing the contaminant thereto, and an SSQM score closer to 100 indicates that the sorbent has high efficacy at sorbing the contaminant thereto.
  • the MSQM score is much like the SSQM score, except that it presents the outcomes for the method including a matrix, where a control (containing no sorbent) is used to estimate the total contaminant sorbed by the matrix, and the difference between SSQM and MSQM (once corrected for the control) is the impact of the matrix on sorption/desorption of the contaminant to the sorbent.
  • a reference to “a” component e.g., a contaminant, a sorbent, or a matrix
  • a reference to “a” component does not mean that the methods of the present invention are limited to the use of only one contaminant, one sorbent or one matrix, for example.
  • the methods of the present invention only require that at least one contaminant, at least one sorbent and/or at least one matrix be present.
  • Steps i and ii a solution to solid weight ratio of 25:1 is used, with a total sorbent value of approximately 1% weight by weight.
  • Steps iii, iv and v a solution to solid (matrix, or matrix plus sorbent) weight ratio of 1:20 is used with a 1% sorbent weight by weight value (i.e., the ratio of sorbent to solid has been standardized, such that the mass of sorbent is 1% of the matrix, even when a matrix is not used).
  • a PFAS spiking stock solution containing all PFAS to be tested by SSQM is prepared at 50 mg/L in methanol (50 mg/L for each tested PFAS species in the combined stock).
  • ii. 25 - 250 g of sorbent based on final test solution volume of 50 - 500 mL is weighed out into a PP or HDPE test vessel.
  • iii. For MSQM only 2.5 - 25 g of matrix sample is weighed into test the vessel.
  • iv. 24 - 240 mL of ultrapure water is added to the test vessel.
  • a 1 - 10 mL aliquot of spiking solution is added to test vessel.
  • test vessel The final 24 - 240 mL of ultrapure water is added to test vessel to make the final volume (50 - 500 mL) at a final concentration of 1 mg/L PFAS for each tested species in the test solution. A solution to solid ratio of 1:20 is used for final volume.
  • Test vessels are weighed and recorded.
  • Test vessels with sorbent, matrix (if MSQM), and PFAS solution are tumbled at 30 rotations per minute for 24 hours.
  • Glass fibre filters are pre-dried and weighed before end of tumbling period.
  • Test solutions are left to settle for 30 minutes and a 5 mL aliquot is removed, centrifuged, diluted with methanol to 50:50 (MeOJLFLO), filtered using syringe filters, and prepared for analysis by LC-MS/MS.
  • Test solution is decanted from test vessels through dried glass fibre filters with care taken to avoid sorbent loss from solution. Glass fibre filters are then dried for 4 hours at 100 °C and weighed to determine sorbent mass loss.
  • xii The test vessel still containing sorbent, matrix, and some final test solution is weighed and recorded.
  • xiii For desorption, 50 - 500 mL of ultrapure water is added to these test vessels and weighed.
  • Test vessels with sorbent, matrix (if MSQM), and PFAS test solution are tumbled at 30 rotations per minute for 24 hours.
  • Test solutions are left to settle for 30 minutes and a 5 mL aliquot is removed, centrifuged, diluted with methanol to 50:50 (MeOJLFLO), filtered using syringe filters, and prepared for analysis by LC-MS/MS.
  • MeOJLFLO methanol to 50:50
  • Calculation of percentage sorbed, percentage desorbed, performance quotient, net removal percentage, and SSQM/MSQM score are completed as per the following Tables.
  • S 1 to S7 are experimental carbonaceous sorbents derived from waste organics under different pyrolysis conditions (sold as Green Man Biochar and produced by pyrolyzing the trunk and limbs of invasive trees in an oxygen-limited environment, followed by quenching with water to develop pore microstructure) ;
  • PAC is a high-performance lignite-derived activated carbon that has undergone an acid and/or steam activation process (also sold as ActiCarb);
  • MM is a mixed mineral product (an alum and carbon blend). The higher the SSQM score, the more effective the sorbent is at binding the contaminant.

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Abstract

La présente divulgation concerne la remédiation de matériaux contaminés. Dans une forme particulière, la présente invention concerne un procédé qui prend en charge des processus de remédiation impliquant l'utilisation de sorbants. Le procédé permet de déterminer l'efficacité de sorption de contaminants pour divers types de sorbant sur divers matériaux, tels que ceux généralement trouvés au niveau de sites industriels, notamment des sols, des résidus miniers et des sous-produits, des déchets de boues, des déchets industriels, des déblais de creusement de tunnels et d'excavation, de la roche et de l'asphalte (ou des mélanges de ceux-ci).
PCT/AU2023/050738 2023-08-07 2023-08-07 Procédé standardisé de mesure de l'efficacité de sorption d'un sorbant Pending WO2025030201A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080248155A1 (en) * 2005-05-10 2008-10-09 Sud-Chemie Ag Use of Stevensite For Mycotoxin Adsorption
US20120219683A1 (en) * 2009-08-27 2012-08-30 Sud-Chemie Ag Toxin adsorbent
US20210145025A1 (en) * 2017-07-20 2021-05-20 Tolsa, S.A. Mycotoxin-Adsorbent Compound and Use Thereof

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Publication number Priority date Publication date Assignee Title
US20080248155A1 (en) * 2005-05-10 2008-10-09 Sud-Chemie Ag Use of Stevensite For Mycotoxin Adsorption
US20120219683A1 (en) * 2009-08-27 2012-08-30 Sud-Chemie Ag Toxin adsorbent
US20210145025A1 (en) * 2017-07-20 2021-05-20 Tolsa, S.A. Mycotoxin-Adsorbent Compound and Use Thereof

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VOUDRIAS E, FYTIANOS K, BOZANI E: "Sorption-Desorption Isotherms of Dyes from Aqueous Solutions and Wastewaters with Different Sorbent Materials", GLOBAL NEST: THE INT. J., vol. 4, no. 1, 1 January 2002 (2002-01-01), pages 75 - 83, XP093280195 *
XIE SHUANG, WEN ZHANG, ZHAN HONGBIN, JIN MENGGUI: "An Experimental Study on the Adsorption and Desorption of Cu(II) in Silty Clay", GEOFLUIDS, BLACKWELL PUBLISHING LTD., OXFORD, GB, vol. 2018, 14 August 2018 (2018-08-14), GB , pages 1 - 12, XP093280197, ISSN: 1468-8115, DOI: 10.1155/2018/3610921 *

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