Novel, Sorbent Mediated Pre-Concentration and Direct Analysis of PFAS Substances
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Bays, Nathan Robert↗
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Novel Methods for Direct Analysis of PFAS on Adsorbents
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Bays, Nathan Robert↗
Comprehensive review of combustion ion chromatography for the analysis of total, adsorbable, and extractable organic fluorine
Poly‐ and perfluoroalkyl substances (PFAS) are a class of persistent organic pollutants whose high stability and appreciable water solubility have led to near‐global contamination. PFAS are bioaccumulative toxins that have been linked to a myriad of disorders and have been detected nearly universally in human blood. Liquid chromatography‐tandem mass spectrometry is the most frequent method used for quantitation, though this typically only measures a few dozen of the >14 000 known PFAS and has been shown to account for a small portion of the total organic fluorine present. Sum parameter methods such as total, extractable, and adsorbable organic fluorine have emerged as alternative measurements for PFAS determination. Combustion ion chromatography has become the preferred method for organofluorine measurement where the sorbent or extract containing PFAS is combusted and the emitted hydrofluoric acid (HF) is a measure of the cumulative organofluorine present. Herein we critically review the types of organofluorine measurement, their separation from the sample matrix, and key parameters of the analytical instrument that affect sensitivity, reproducibility, and recovery with regards to PFAS analysis.
Chemistry↗
Exploring Approaches for Accelerated Mass Spectrometric Detection of Fluorochemicals from Aqueous Solutions Using Indirect, Adsorbent-Facilitated Desorption Ionization
There is a growing need for rapid, low-cost analytical tools to screen water supplies for persistent contaminants. Due to their ubiquitous presence in the environment and their detrimental effects on human health, there is a public interest in widespread testing for perfluoroalkyl substances (PFAS). However, the most common methods for PFAS analysis can be time-intensive, requiring a preconcentration step followed by liquid chromatography–mass spectrometry (LC–MS), and are cost-prohibitive for most members of the public. To address these challenges, this study explores a novel method for rapid analysis of aqueous analytes by concentrating analytes on solid adsorbents and detecting them using mass spectrometric analysis via desorption ionization directly from the adsorbent surface. We demonstrate this general approach of indirect solution analysis (ISA) with desorption electrospray ionization (ISA-DESI) and laser desorption ionization (ISA-LDI). Various adsorbent materials were screened, including commercial mesoporous carbons, alumina, and metal–organic frameworks (MOFs). Using ISA-DESI, we consistently detect concentrations as low as 5–100 parts per trillion (ppt) for perfluorooctanoic acid (PFOA) and 10–100 ppt for perfluoroundecanoic acid (PFUnDA). This approach enables rapid detection in under 5 min, making it suitable for applications requiring trace detection with fast response times. We further demonstrate the use of ISA-DESI on a range of environmentally relevant contaminants. Advantages of this indirect solution analysis approach include simplified sample preparation, accelerated analysis, and low cost with readily available materials, making it a promising tool to accelerate mass spectrometric PFAS detection for identifying contaminated sites, performing laboratory studies, and monitoring industrial waste streams.
Bays, Nathan Robert [Sandia National Laboratories ↗
Sewage Treatment Plant #1 Area, SWMU 117 Per- and Polyfluoroalkyl Substances (PFAS) Site Assessment Progress Report
This Per- and Polyfluoroalkyl Substances (PFAS) Site Assessment (SA) Progress Report (SAPR) discusses the investigation activities and findings for the Sewage Treatment Plant #1 (STP1) Area located at Kennedy Space Center (KSC), Florida (Figure 1-1). This site has been designated Solid Waste Management Unit (SWMU) 117 under KSC’s Resource Conservation and Recovery Act (RCRA) Corrective Action Program, as the sewage treatment plant and associated areas were identified as a potential source of PFAS to the environment. This PFAS SAPR was prepared by Tetra Tech, Inc., for the National Aeronautics and Space Administration (NASA) under Indefinite Delivery Indefinite Quantity Contract 80KSC019D0011-80KSC019F0070. This is the first progress report to document on-going SA activities; supplemental progress reports will be provided as additional data is collected. PFAS SA activities were conducted between April 2020 and March 2022 to collect additional data to supplement the existing datasets to better understand the extent of PFAS impacts to the environment in the STP1 Area. The SA for the STP1 Area covers an approximately 130-acre investigation area with multiple structures and buildings. The focus of the SA is the STP1 Complex and associated structures, including the former Polishing Pond, former Sludge Disposal8 Area, and former Spray Field. The STP1 Complex is located in the KSC Industrial Area, at the southwest corner of 4th Street SE and C Avenue SE. The STP1 Complex is located approximately ¼-mile south and downgradient of the Fire Station #1 site (SWMU 116), which is also currently undergoing a PFAS SA because of potential releases of PFAS-containing aqueous film-forming foam (AFFF). During the SA, a total of seven soil, 131 groundwater direct push technology (DPT), 24 groundwater monitoring well, and 11 surface water samples were collected between April 2020 and March 2022. Monitoring well samples were analyzed for 18 PFAS compounds, with all other samples analyzed for 28 PFAS compounds. The SA sample results were used along with historical results to evaluate the extent of PFAS impacts to the environment in the STP1 Area. Data generated to date and prior results were screened against the United States Environmental Protection Agency (USEPA) May 2022 Tap Water Regional Screening Levels (RSL) for groundwater and residential RSLs for soil (hazard quotient of 0.1). Surface water results were screened against the State of Florida Human Health Surface Water Screening Levels (SWSLs). Results from the SA showed exceedances of the applicable screening criteria for groundwater and surface water. Considering the current and historical dataset, PFOS is the prevalent PFAS compound. Based on these results, additional groundwater DPT and surface water sampling should be considered for PFAS analysis, focused on evaluating surface water bodies in the southeast portion of the Industrial Area, which discharge into the Banana River. Additionally, installation of monitoring wells should be considered to evaluate the interaction between the groundwater and surface water at the site. Collection of additional samples for TOC analysis should also be considered from representative groundwater (saturated soils) and surface water locations to further evaluate potential correlations between PFAS and TOC to provide a more comprehensive dataset to assist in fate and transport analyses.
Sewage Treatment Plant↗
Fire Station #2, Former Sewage Treatment Plant #17, and Towway Area-SWMU 114 PFAS Site Assessment Progress Report Kennedy Space Center, Florida
This PFAS Site Assessment Progress Report (SAPR) presents the findings of the 2022 PFAS investigation conducted from November 2021 through August 2022 at Solid Waste Management Unit (SWMU) 114 located within Kennedy Space Center (KSC), Florida. SWMU 114 includes area around Fire Station #2, Former Sewage Treatment Plant #17, the southern portion of the Shuttle Landing Facility Runway, Remote Launch Vehicle Hangar, and the Towway area. Fire Station #2 was constructed in 2008 and is currently active, housing fire station personnel and equipment, including aqueous film forming foam (AFFF). Releases of AFFF has occurred at SWMU 114. Previous environmental assessments have been performed at SWMU 114, including soil, groundwater, and surface water sampling for volatile organic compounds, polycyclic aromatic hydrocarbons, total petroleum hydrocarbons, and metals. No active remediation has been performed at the SWMU 114. PFAS site assessment field activities were conducted at SWMU 114 from November 2021 through August 2022. During the 2021-2022 Site Assessment, 124 direct-push samples were collected from 27 locations, 17 surface water samples were collected from 15 locations, 41 groundwater samples were collected from 37 newly installed monitoring wells, five concrete samples were collected from four locations, and one asphalt sample was collected. Additionally, two soil borings were advanced to 60 feet for lithologic descriptions, ten staff gauges were installed, and one round of water level measurements were collected from monitoring wells and staff gauges for groundwater flow determination. All groundwater and surface water samples were analyzed for 25 PFAS analytes by USEPA Method 537M. Concrete, and asphalt samples were analyzed by synthetic precipitation leaching procedure (SPLP) PFAS analysis by USEPA Modified Method 537M. Groundwater results were compared to the most recent Regional Screening Levels (RSLs) published by USEPA for residential tap water (USEPA, 2022a) to determine the extent of PFAS contamination at SWMU 114 for six PFAS analytes (PFOA, PFNA, PFBS, PFHxS, PFOS, and GenX). Surface water results were compared to the FDEP surface water screening levels (SW SLs) (FDEP, 2020) for PFOA and PFOS. The PFAS investigation concluded that groundwater exceeding RSLs extends east and south to Banana Creek and west to approximately the center of the SLF runway. The extent of PFAS is approximated to the north, to an area between Sharkey Road and Astronaut Road, where samples below the RSLs do not fully bound SWMU 114. At least two distinct PFAS source areas are located near Fire Station #2 and along Towway, at S114-MW0007S, within SWMU 114. Groundwater head measurements indicate that flow at SWMU 114 is generally similar across the shallow and intermediate water tables. A northeast to southwest trending groundwater divide is located near the middle of Towway where groundwater southeast of the divide flows to the south and groundwater northwest of the divide flows to the west. The groundwater divide generally separates the two areas of higher PFAS concentrations. Surface water samples indicated concentrations of PFOS above the SW SLs in surface water bodies across the site. Further assessment and sampling are required to better understand the interaction between groundwater and surface water at SWMU 114. Concrete and asphalt samples collected confirm that a significant release of AFFF occurred near the stormwater pond northwest of Fire Station #2. Additional concrete samples surrounding Fire Station #2 and at the northwest and southeast edges of the SLF tarmac indicate elevated PFOS concentrations. These results indicate that discharges of AFFF in these locations have infiltrated into asphalt and concrete and may act as a continuing source of PFAS to groundwater and surface water after rain events. Additional direct-push samples are required to delineate PFAS at SWMU 114. Samples may need to extend beyond the Former SLF Rescue Building and Morpheous Test Site to delineate PFAS in groundwater. Monitoring wells should be sampled and gauged quarterly to determine if seasonal impacts are observable, especially in shallow wells near surface water features. Furthermore, surface water samples should be collected from additional ditches to further define the extent of surface water impacts at SWMU 114 and extending along the SLF runway. Staff gauges should be gauged quarterly with groundwater gauging to determine surface water flow and interaction with groundwater. The PFAS sampling results and path forward for SWMU 114 were presented to the KSC Remediation Team in October 2022. Once the PFAS SAPR is approved, it will be submitted to the Florida Department of Environmental Protection.
Howard Franklin Fowler↗
Model-based economic analysis under uncertainty for PFAS treatment by granular activated carbon and ion exchange technologies
Recent drinking water regulations have imposed the need for per- and polyfluoroalkyl substances (PFAS) remediation. In response, treatment facilities may be required to retrofit existing treatment schemes to treat PFAS below maximum contaminant levels (MCLs). Adsorption technologies such as granular activated carbon (GAC) and ion exchange (IX) have been demonstrated to be effective; however, there are limited techno-economic metrics available which provide guidance on technology selection and design for diverse PFAS-containing source water conditions. Process systems engineering (PSE) tools which can traditionally perform these analyses are hindered by the data availability, model validity, and understanding of treatment phenomena for emerging contaminants. This work employs published data regressions, statistical models, process models, techno-economic analyses, and other process systems tools in a model-based uncertainty framework to consider the limitations of emerging contaminant research. Through this analysis framework, economic results are provided as probabilistic distributions based on the uncertainty of the models and diverse conditions that treatment facilities experience.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
A modified QuEChERS sample processing method for the determination of per- and polyfluoroalkyl substances (PFAS) in environmental biological matrices
Not Available
59 BASIC BIOLOGICAL SCIENCES↗
Emerging Per- and Polyfluoroalkyl Substances in Tap Water from the American Healthy Homes Survey II
Humans experience widespread exposure to anthropogenic per- and polyfluoroalkyl substances (PFAS) through various media, which can lead to a wide range of negative health impacts. Tap water is an important source of exposure in communities with any degree of contamination but routine or large-scale PFAS monitoring often depends on targeted analytical methods limited to measuring specific PFAS. We analyzed 680 tap water samples from the American Healthy Homes Survey II for PFAS using non-targeted analysis (NTA) to expand the range of detectable PFAS. Based on detection frequency and relative abundance, about half of the identified PFAS were found only by NTA. We identified (with varying degrees of confidence) 75 distinct PFAS, including 57 exclusively detected by NTA. The identified PFAS are members of seven structural subclasses differentiated by their head groups and degree of fluorination. Clustering analysis categorized the PFAS into four coabundance groups dominated by specific PFAS subclasses. One group uniquely identified by NTA contains zwitterionic PFAS and other PFAS transformation products which are likely associated with aqueous firefighting foam contaminants in a small number of spatially correlated samples. These results help further characterize the scope of exposure to emerging PFAS experienced by the U.S. population via tap water and augment nationwide targeted-PFAS monitoring programs.
63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗
Sampling and Analysis Plan for LSL2 Underground Storage Tank Evaluation of PFAS in Soil: Protection of Groundwater
This SAP gathers all pertinent information relevant to the sampling and analysis of soil at the removal site for a former 10,000-gallon UST and reference sites in the vicinity of the excavation site. Data Quality Objectives establishes the process and steps for the acquisition of data. Data Flow Diagram establishes the decisions and next steps. Quality Assurance Project Plan establishes the quality requirements for data collection, including planning, implementation, and assessment of sampling, field measurements, and laboratory analysis. The work is being completed for DOE-SC Pacific Northwest Site Office.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Predictive Integrated Stratigraphic Modeling (PRISM®) Work Plan Center Wide Per- and Polyfluoroalkyl Substances (PFAS) Potential Release Location (PRL) 237 Kennedy Space Center, Florida
This document presents a description of various site investigation activities that will be used to improve the conceptual site model (CSM) at the Kennedy Space Center (KSC) to develop a better understanding of the fate and transport of per- and polyfluoroalkyl substances (PFAS) in groundwater and surface water. The activities proposed herein include three primary tasks: a sequence stratigraphic analysis, groundwater and surface water gauging and sampling, and a stormwater pollutant modeling analysis.
PFAS↗
Components Refurbishment and Chemical Analysis Facility, SWMU #041 - Per- and Polyfluoroalkyl Substances Site Assessment Report Kennedy Space Center, Florida
This PFAS Site Assessment (SA) Report presents the activities and results associated with PFAS investigations at the Components Refurbishment and Chemical Analysis (CRCA) facility located at Kennedy Space Center (KSC), Florida. In 2022, CRCA was identified as an Area of Potential Concern because the facility stores several potential PFAS-containing chemicals. A groundwater sample collected from an onsite monitoring well detected PFOA and PFOS at concentrations greater than State of Florida provisional Groundwater Cleanup Target Levels (pGCTLs). PFAS SA activities were conducted between March 2022 and February 2024. During this timeframe, a total of 16 direct-push technology (DPT) locations and 82 discrete samples were collected from these locations, along with 90 monitoring well samples. The analytical data screening process focused on State of Florida pGCTLs and United States Environmental Protection Agency (USEPA) Regional Screening Level (RSLs) from November 2023 to evaluate the data. Analytical results identified PFOS, PFOA, and PFBA at concentrations exceeding their respective RSLs at each depth interval (shallow, intermediate, and deep). PFOS and PFOA had the largest footprint of RSL exceedances in each depth interval, but pGCTL exceedances were only observed at limited locations in the shallow and intermediate intervals. PFBA had the highest detections of any PFAS compound, with concentrations exceeding 180,000 nanograms per liter (ng/L), which is 100-times the RSL of 1,800 ng/L in the shallow and intermediate intervals and 10-times the RSL in the deep interval. The maximum PFBA detection was 841,000 ng/L at shallow monitoring well, MW0006. The PFAS SA also included samples collected from the onsite hydraulic containment system (HCS) which was installed to control and treat the onsite chlorinated volatile organic compound (CVOC) plume. Influent and effluent aqueous samples were collected monthly from the system. PFAS concentrations were relatively the same for both influent and effluent samples, indicating that while the HCS has been effective for CVOC treatment, it does not provide any additional treatment for PFAS compounds. Since the HCS has achieved its objectives, the system was shut down in December 2024. PFAS data gaps still exist, to include surface water and soil, which were not sampled during this SA. Soil sampling near the Chemical Process Area is recommended. Surface water and soil sampling at select stormwater outfalls is also recommended. Additionally, further groundwater sampling is recommended (DPT and monitoring well) in all depth intervals to delineate the extent of PFAS impacts at CRCA.
K Alex Murphy↗
PFAS remediation: Evaluating the infrared spectra of complex gaseous mixtures to determine the efficacy of thermal decomposition of PFAS
Due to their widespread production and known environmental contamination, the need for the detection and remediation of per- and polyfluoroalkyl substances (PFAS) has grown quickly. While destructive thermal treatment of PFAS at low temperatures (e.g., 200 to 500oC) is of interest due to lower energy and infrastructure requirements, the range of possible degradation products remains underexplored. To better understand the low temperature decomposition of PFAS species, we have coupled gas-phase infrared spectroscopy with a multivariate curve resolution (MCR) analysis and a database of high-resolution PFAS infrared reference spectra to detect and quantify a complex mixture resulting from potassium perfluorooctanesulfonate (PFOS-K) decomposition. Nine prevalent decomposition products (namely smaller perfluorocarbon species) are identified and quantified.
54 ENVIRONMENTAL SCIENCES↗
Evaluating Process Costs and Performance Metrics of Granular Activated Carbon for the Removal of PFAS Under Model Uncertainty
The data is contained within an oral presentation with graphical results of PFAS process simulation pertaining to an ongoing WaterTAP analysis.
Barber, Hunter↗
Atomically Precise Hexanuclear Ce(IV) Clusters as Functional Fluorescent Nanosensors for Rapid One-Step Detection of PFAS
Here, the presence of poly- and perfluoroalkyl substances (PFAS) in the environment is associated with adverse health effects but measuring PFAS is challenging due to the associated high cost and technical complexities of the analysis. Here, the reactivity of atomically precise metal-oxo clusters is reported and the foundation for their use is provided as fluorescent nanosensors for PFAS detection. The material comprises crystalline, water soluble, hexanuclear cerium-oxo clusters [Ce 6 (µ 3 -O) 4 (µ 3 -OH) 4 ] 12+ decorated with glycine molecules (Ce-Gly) characterized by fluorescence emission at 353 nm. The Ce-Gly fluorescence is found sensitive to long chain carboxylated PFAS of CF 3 –(CF 2 ) n –, where n ≥ 6, such as perfluorooctanoic, perfluorononanoic and perfluorodecanoic acids. This unique reactivity leads to a change in the emission spectra in a concentration dependent manner, enabling PFAS detection through ligand exchange and aggregation-induced emission (AIE) enhancement. No significant cross-reactivity from potentially co-existing species, including sulfonated PFAS, octanoic and dodecanoic acids, humic acid, and inorganic ions is observed. With an optimal concentration of 3.3 µg mL -1 Ce-Gly, the method demonstrated detection limits of 0.24 ppb for PFOA and 0.4 ppb for PFNA. These findings highlight the potential of fluorescence-based detection strategies utilizing nanoscale probes such as Ce-Gly as fluorescent probes and nanosensors for PFAS.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Assessment of Fluoropolymer Production and Use With Analysis of Alternative Replacement Materials
This report focuses on fluoropolymers, which are a subgroup of the much larger class of fluorinated chemicals known as per- and polyfluoroalkyl substances (PFAS). Clearly distinguishing fluoropolymers is important to understanding their distinctive chemical properties, associated risks and benefits, and roles in commerce. In this report, the factors that are considered in a lifecycle assessment (LCA) of fluoropolymers will be discussed. These include the manufacturing of fluoropolymers, their use in industry, and available replacement technologies. Emphasis is placed on fluoropolymer plastics because of their extensive use in the commerce sectors considered here, specifically aerospace, automotive, battery, building construction, chemical processing, electronics, infrastructure, semiconductor, solar panel, and wind energy industries.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Molecular detection of per- and polyfluoroalkyl substances in water using time-of-flight secondary ion mass spectrometry
Detection of per- and polyfluoroalkyl substances (PFASs) is crucial in environmental mitigation and remediation of these persistent pollutants. We demonstrate that time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a viable technique to analyze and identify these substances at parts per trillion (ppt) level in real field samples without complicated sample preparation due to its superior surface sensitivity. Several representative PFAS compounds, such as perfluorooctanesulfonic acid (PFOS), perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), perfluoheptanoic acid (PFHpA), and perfluorononanoic acid (PFNA), and real-world groundwater samples collected from monitoring wells installed around at a municipal wastewater treatment plant located in Southern California were analyzed in this work. ToF-SIMS spectral comparison depicts sensitive identification of pseudo-molecular ions, characteristic of reference PFASs. Additionally, principal component analysis (PCA) shows clear discrimination among real samples and reference compounds. Our results show that characteristic molecular ion and fragments peaks can be used to identify PFASs. Furthermore, SIMS two-dimensional (2D) images directly exhibit the distribution of perfluorocarboxylic acid (PFCA) and PFOS in simulated mixtures and real wastewater samples. Such findings indicate that ToF-SIMS is useable to determine PFAS compounds in complex environmental water samples. In conclusion, ToF-SIMS provides simple sample preparation and high sensitivity in mass spectral imaging, offering an alternative solution for environmental forensic analysis of PFASs in wastewater in the future.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Electron Beam Irradiation for Water Treatment of Per- and Polyfluoroalkyl Substances (PFAS)
Per- and polyfluoroalkyl substances (PFAS) are widely used but are now considered a water contamination risk. Fermi National Accelerator Laboratory’s IARC group has demonstrated that passing water through electron beam radiation can destroy PFAS. This project aims to develop a process to scale the system for bulk water treatment. The key is efficient radiation usage, ensuring that all water receives only the minimum dose. Software was developed for this purpose, consisting of a computational fluid dynamics model (CFD) in COMSOL, which calculates particle trajectories through the radiation area. A MATLAB script integrates the radiation dose of these particles, and statistical analysis is performed to evaluate the radiation utilization efficiency. These models are validated with a flow test where colored dye is injected and optically tracked. Radiation dose is measured by testing under an e-beam to measure the degradation of a PFAS analog.
Mueller, Scott [Northern Illinois U.]↗