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Mineralization of captured perfluorooctanoic acid and perfluorooctane sulfonic acid at zero net cost using flash Joule heating

Nature Water volume 3, pages 486–496 (2025)Cite this article

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Abstract

Per- and polyfluorinated alkyl substances (PFAS), including perfluorooctanoic acid (PFOA) and perfluorooctane sulfonic acid (PFOS), are persistent environmental contaminants that have infiltrated freshwater systems. Granular activated carbon (GAC) is widely used for PFAS removal but becomes secondary waste (PFAS-GAC). Current treatment methods are energy intensive and release hazardous fluorocarbons. This study demonstrates electrothermal mineralization of PFOA and PFOS-GAC via flash Joule heating, a scalable and efficient process. Heating PFAS-GAC with sodium or calcium salts converts PFAS into inert fluoride salts with >90% fluorine conversion and >99% PFOA and PFOS removal. Simultaneously, the spent carbon is upcycled into flash graphene, offsetting treatment costs by US$60–100 per kg. This solvent- and catalyst-free method substantially reduces energy use, greenhouse gas emissions and secondary waste. A techno-economic assessment highlights its scalability and environmental benefits, offering a rapid (~1 s), cost-effective solution for PFAS remediation and upcycling of waste carbon into high-value products.

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Fig. 1: Scheme, current and temperature of the FJH study.
Fig. 2: Quantification and analysis of the mineralization process.
Fig. 3: Simulations of PFOA reacting with NaOH at high temperatures.
Fig. 4: Comparative LCA and TEA of FJH as compared to other PFAS-GAC remediation methods.

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Data availability

Supplementary datasets for Monte Carlo LCA and TEA calculations are available via Zenodo at https://doi.org/10.5281/zenodo.14852070 (ref. 60).

Code availability

Custom Python scripts were used to analyse Raman spectral mapping data by comparing peak intensity ratios and peak height. These scripts are available via Github at https://github.com/jlb48249/FJH_ML.

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Acknowledgements

The funding of the research is provided by Air Force Office of Scientific Research (FA9550-22-1-0526, J.M.T.), US Army Corps of Engineers, ERDC (W912HZ-21-2-0050, J.M.T., B.I.Y., Y.Z., S.G.Z., C.G.), the National Science Foundation Graduate Research Fellowship Program (J.L.B.), the Stauffer–Rothwell Scholarship from Rice University (K.M.W.) and Rice Academy Fellowship (Y.C.). Computer resources were provided through the US Department of Energy award (BES-ERCAP0027822, B.I.Y.). C.-H.C. and Y.H. acknowledge Welch Foundation (C-2065), and American Chemical Society Petroleum Research Fund (67236-DNI10). Permission to publish was granted by Director, Geotechnical and Structures Laboratory, ERDC. We acknowledge and thank A. Kimble and J. Puhnaty from ERDC, who contributed to the preparation of the PFOA-GAC used in this work. B. Chen aided in the XPS analysis. We acknowledge C. Kittrell for his advice and support in the early stages on this project. The characterization equipment used in this project is partly from the Shared Equipment Authority and the Electron Microscopy Core at Rice University.

Author information

Authors and Affiliations

  1. Department of Materials Science and Nanoengineering, Rice University, Houston, TX, USA

    Phelecia Scotland, Chi Hun Choi, Yimo Han, Michael S. Wong, Boris I. Yakobson, Yufeng Zhao & James M. Tour

  2. Department of Chemistry, Rice University, Houston, TX, USA

    Phelecia Scotland, Kevin M. Wyss, Yi Cheng, Lucas Eddy, Jacob L. Beckham, Justin Sharp, Chi Hun Choi, Tengda Si, Bing Deng, Michael S. Wong, Boris I. Yakobson & James M. Tour

  3. Smalley-Curl Institute, Rice University, Houston, TX, USA

    Lucas Eddy & James M. Tour

  4. Department of Applied Physics, Rice University, Houston, TX, USA

    Lucas Eddy

  5. Department of Chemical and Biomolecular Engineering, Rice University, Houston, TX, USA

    Youngkun Chung, Bo Wang, Juan A. Donoso & Michael S. Wong

  6. Nanosystems Engineering Research Center for Nanotechnology-Enabled Water Treatment, Houston, TX, USA

    Youngkun Chung, Bo Wang & Juan A. Donoso

  7. Rice Water Technologies, Entrepreneurship and Research (WaTER) Institute, Houston, TX, USA

    Youngkun Chung

  8. Rice Sustainability Institute, Houston, TX, USA

    Youngkun Chung

  9. Department of Civil and Environmental Engineering, Rice University, Houston, TX, USA

    Yu-Yi Shen, Mason Tomson & Michael S. Wong

  10. US Army Engineer Research and Development Center, Vicksburg, MS, USA

    Sarah Grace Zetterholm & Christopher Griggs

  11. Corban University, Salem, OR, USA

    Yufeng Zhao

  12. NanoCarbon Center and Rice Advanced Materials Institute, Rice University, Houston, TX, USA

    James M. Tour

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  1. Phelecia Scotland
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Contributions

P.S. conceived the idea to use sodium as a mineralizing agent for PFOA, PFOS and PTFE, conducted IC, LCMS, CIC, NMR, XRD, XPS, TEA and paper writing under the guidance of J.M.T. K.M.W performed GC-MS, Raman spectroscopy and contributed to the experimental design ideas and LCA. Y. Cheng aided with experimental design and experiments, L.E. contributed to initial experiment testing. J.L.B. contributed to Raman analysis and paper writing. J.S. contributed to the LCA and TEA. C.H.C. performed TEM characterization. T.S. contributed to NMR analysis. Y. Chung and B.W. contributed to IC and LCMS. Y.-Y.S. and J.A.D. contributed to IC. B.D. contributed to experimental design ideas and part of the reaction schematics. Y.Z. contributed to DFT and computational data. Y.H. supervised C.H.C. in performing TEM characterization. B.I.Y. supervised Y.Z. in performing computational experiments. M.S.W. supervised Y.C. B.W. and J.A.D. M.T. supervised Y.-Y.S. S.G.Z. and C.G. contributed PFAS-adsorbed GAC samples. J.M.T. supervised P.S. for all the process, guided P.S. in paper writing and oversaw the entire project.

Corresponding authors

Correspondence to Yufeng Zhao or James M. Tour.

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Competing interests

Intellectual property (IP) has been filed by Rice University on the FJH strategy for PFAS destruction, which is being licensed to companies in which J.M.T. is a shareholder, but not an officer, director or employee. Conflicts of interest are mitigated by disclosure to and compliance with the Office of Sponsored Programs and Research Compliance at Rice University. The other authors declare no competing interests.

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Nature Water thanks Feng Xiao and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Extended data

Extended Data Fig. 1 Quantification of inorganic and organic F.

a) Ion chromatography results of 0.1 g of GAC/PFOA and GAC/PFOA/x1.2Na after FJH, (n = 3 for all samples). b) Inductive Couple Plasma-Mass spectrometry (ICP-MS) of the filtrate of i) neat GAC (n = 1), ii) GAC/130 V (n = 3), and iii) GAC/PFOA/130 V (n = 3). c) LCMS quantification of the remaining organic F derived from PFOA. d) LCMS results of the GAC/PFOA and GAC/PFOA/NaOH when FJH at 130 V for 1.00 s. The data in 1a, 1b ii-iii, and 1 d are presented as the mean ± s.d. of the LCMS results from 3 parallel experiments (n = 3).

Source data

Extended Data Fig. 2 Gas chromatograph mass spectrometry (GC-MS) analysis of reaction byproducts.

a) A picture of the gas capture setup to collect gases evolved by flash Joule heating. A perforated brass electrode allows for the capture of gases evolved during the reaction. The captured gases are then analyzed using GC-MS to probe possible perfluorocarbon production during the PFOA degradation process. The instrumental scan resolution was set to end at 300 m/z, so higher mass fragments were not observed. b) Mass spectrum of peak #1, the perfluoro pentene peak. c) Mass spectrum of peak #2, the perfluoro hexene peak. d) Mass spectrum of peak #3, the perfluoro heptene peak, the decarboxylated parent PFOA peak.

Source data

Extended Data Fig. 3 Characterization of the reactants and FJH reaction products.

a) Statistic Raman spectrum of PFOA-GAC starting material and optimized GAC-derived flash graphene (FG) product that was FJH at 150 V and 1.00 s. The solid line and colored shadows represent the average value and standard deviation of 100 sampling points, respectively. b) Reaction mass yield with respect to reaction voltage at two different pulse times. The data are presented as the mean ± s.d. of the reaction mass yield from 3 parallel experiments (n = 3). c) XRD spectra of the raw materials and FJH products before and after rinsing (Powder Diffraction File 00-041-1487, Graphite-2H and 01-080-8615, NaF). d) XPS survey spectra of the raw material and FJH products before and after rinsing. e) BET surface area analysis isotherms of the raw starting material GAC and the FJH reaction products. f) TEM analysis of the produced graphene. The inset shows an FFT of the highlighted area, the scale bar is the same as the TEM image.

Source data

Extended Data Fig. 4 Characterization of GAC/PFOS/Na before and after FJH.

a) LCMS results for GAC/PFOS/Na FJH at 130 V for 2.00 s. The PFOS removal efficiency is 99.97%. The data are presented as the mean ± s.d. of the LCMS results from 3 parallel experiments (n = 3). b) XRD spectra of the raw materials and FJH products. The blue trace represents a sample containing a slightly higher loading of PFOS so that we can observe the NaF peaks in the XRD spectra. c) 19F NMR spectra of the raw material and FJH products before and after rinsing, d) XPS elemental spectra of the raw material and FJH products.

Source data

Extended Data Fig. 5 Analysis of PFOA-GAC mixed with Ca(OH)2 (0.5 calcium ions for every fluoride atom) and FJH at 110-150 V for 0.50 s.

a-b) Ion chromatography analysis of the samples, post-FJH. 94% of elemental F present in the starting material is recovered as mineralized fluoride when FJH at 150 V (n = 1). One set of reactions was conducted as a proof of concept to limit the exposure of the sensitive analytical equipment to dilute H2SO4. c) Thermodynamics analysis using the HSC chemistry package shows that the mineralizing agent reacts readily with all fluorocarbons. This suggests that the addition of Ca(OH)2 drives the mineralization process. d) The average Raman spectra of the 110 V and 130 V flash at 59 mF. The spectra were collected from 100 sampling points of the powdered product. The average D/G and 2D/G intensity ratios of the 110 V flash are 0.34 and 0.68, respectively. The graphene yield is 96%. The average D/G and 2D/G intensity ratios of the 130 V flashes are 0.25 and 0.72, respectively. The graphene yield is 98%. High-quality FG was produced. e) Bulk crystal structure analysis by XRD of the Ca(OH)2, PFOA-GAC mixed with Ca(OH)2, and the product after FJH at 130 V. The green circles highlight the CaF2 phase. f) TEM image containing an FFT inset of the highlighted area shows turbostratic stacking of the domains and strong graphitic character with minimal amorphous character.

Source data

Extended Data Fig. 6 Analysis of PFOA-Resin mixed with 2 molar eq of sodium per mole F in PFOA using NaOH, and FJH at 80 V for 1.00 s.

a) XPS shows the high F content in the original PFOA-Resin. b) Fourier-transform infrared spectroscopy (FTIR) of the anion exchange resin with adsorbed PFOA. The C-F stretching vibration can be observed at 1204 and 1148 cm-1. c) Thermal gravimetric analysis-differential scanning calorimetry (TGA-DSC) shows the various stages of weight loss of the resin. The first stage includes PFOA degradation followed by depolymerization of the resin then blackening. d) Reaction vessel after FJH. The sample shatters due to rapid gas formation and expansion. 80 V is the maximum voltage where the solid remains in the inner chamber and can be analyzed. e) XRD analysis of the post-reaction powder shows the presence of NaF. f) Ion chromatography results of the reactions. 66.7% of the PFOA is mineralized into inorganic NaF. The apparatus is a constraint of these samples as the glass tube shatters at high voltages. The data are presented as the mean ± s.d. of the IC results from 3 parallel experiments (n = 3).

Source data

Extended Data Fig. 7 Molecular model depictions of the simulations, and the chemical equations derived from those simulations.

Reaction Pathway 1 derived from Density Functional Theory (DFT) simulations.

Extended Data Fig. 8 DFT simulations.

a) Reaction Pathway 2 derived from DFT simulations. b) Energy calculations for the reaction steps of reaction pathways 1 and 2. The total energy goes down steadily step by step, which indicates that the above three rules of thumb are valid for energetics analysis. The reaction is driven by the reduction of F by Na. Because of the high electronegativity of F atoms, the F-C covalent bonds are highly frustrated, and the frustration can be released by replacing F with OH or removal of F through forming C = C double bonds.

Source data

Extended Data Fig. 9 Reaction pathways for production of NaF and Na2SiF6.

Proposed reaction pathway for the degradation of PFOA in the presence of NaOH via FJH into inorganic fluorine salts.

Extended Data Fig. 10 Scaled up reaction to mineralize gram scale PFOA-GAC.

This demonstrates our scale up technology in the lab to treat 3 g of PFOA on waste GAC. The starting PFOA concentration was 6.3 mg g-1 GAC. No short chain PFOA remained and the removal efficiency for PFOA was >99.9%. The balance shows that 2.6 g of graphene formed with small amounts of metal fluoride salts.

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Supplementary Notes and Sections 1–10, Figs. 1–32, Tables 1–10 and Refs. 1–45.

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Scotland, P., Wyss, K.M., Cheng, Y. et al. Mineralization of captured perfluorooctanoic acid and perfluorooctane sulfonic acid at zero net cost using flash Joule heating. Nat Water 3, 486–496 (2025). https://doi.org/10.1038/s44221-025-00404-z

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