Grantee Research Project Results
Final Report: Rapid, Field-Deployable Water Sampling Device to Facilitate On-Site Total PFAS Measurement
EPA Contract Number: 68HERC23C0014Title: Rapid, Field-Deployable Water Sampling Device to Facilitate On-Site Total PFAS Measurement
Investigators: MacMillan, Hunter
Small Business: Forever Analytical Services, Inc.
EPA Contact: Richards, April
Phase: I
Project Period: December 12, 2022 through June 11, 2023
Project Amount: $99,983
RFA: Small Business Innovation Research (SBIR) Phase I (2023) RFA Text | Recipients Lists
Research Category: SBIR - Homeland Security , SBIR - Air and Climate , SBIR - Sustainability , SBIR - Water
Description:
The state-of-the-art quantification method of PFAS in aqueous samples is liquid chromatography tandem mass spectrometry (LC-MS/MS) with method 537.1 and 533. When combined with various SPE techniques, these methods yield part-per-trillion (ppt) limits of detection (LOD) along with the ability to speciate PFAS that are in the ever-expanding library of standards. However, because of the nature of preparing multiple PFAS standards and the chromatographic separation steps required to identify individual PFAS of interest when using this method, LC-MS/MS methods are inherently slow and expensive. In addition, LC-MS/MS techniques require a library of known compounds to which to compare, which means that this technique is blind to thousands of types of PFAS, some of which may be precursor PFAS that subsequently degrade into regulated chemicals.
Summary/Accomplishments (Outputs/Outcomes):
Because of these issues, recent attention has been directed towards the development of total fluorine analytical methods. These methods offer the ability to quantify the total fluorine content of a water sample, meaning all PFAS present can be considered. In addition, total fluorine methods are typically much faster and cheaper than LC-MS/MS methods. Furthermore, because water samples tested using traditional LC-MS/MS methods are often blank with respect to PFAS, a total organic fluorine method could be used to screen water samples for the presence of PFAS, avoiding unnecessary LC-MS/MS testing. Numerous total fluorine techniques exist, including nuclear magnetic resonance (NMR) spectroscopy and combustion ion chromatography (CIC); however, they either do not have sufficiently low LODs to be useful for most water samples of interest, or are too slow to be practical or suffer from inherent challenges such as varying PFAS combustion efficiencies and the need for inorganic/organic fluorine calibration before measurement.
These attributes make PIGE this an ideal screening tool in the field to delineate the extent of the contamination at AFFF-impacted sites for example. If there is no organo-fluorine detectable, there is no PFAS contamination. If there is significant organo-fluorine measured, then the eluent from that sample can be shipped to any ELAP-accredited LC-MS/MS laboratory, and analyzed to identify which specific PFAS are present. PIGE would also be used to monitor remediation efforts of water treatment systems by simply measuring the total fluorine content quickly and inexpensively each day/week/month and doing a full LC-MS/MS characterization quarterly or annually rather than doing a full LC-MS/MS characterization each time. Rapid field quantification is the motivation to develop this method. Thus, PIGE emerges as a leading technique that could be applied to hundreds of samples per day per instrument, if the technique could be brought to the field. We believe this technology can be a “game-changer” in the way PFAS contamination of ground and surface water is assessed, and complements the well-established LC-MS/MS methods currently in use.
Conclusions:
To date the FAS SPE/PIGE method has been extensively validated in the laboratory under controlled conditions. In this proposal, FAS extended the application of this technique to the field by deploying a field-deployable SPE device to be used in conjunctions with SERDP-funded (ER- 1142) field-deployable particle accelerator previously developed by Starfire Industries under the DARPA ICONS program (Jurczyk 2019 IPAC Conferences) adapted to directly detect total organic fluorine via PIGE by the University of Notre Dame under the limited SERDP project (Peaslee 2021 Final Report ER19-C2-1142).
SBIR Phase II:
Scaling Up a Field-Deployable Water Sampling Device to Rapidly Screen Adsorbable Organic Fluorine in situThe perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Conclusions drawn by the principal investigators have not been reviewed by the Agency.