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Technical Reports

2022-2023 | 2021-2022 | 2019-2020 | 2018-2019

2022-2023 TAG Kick-Off Meeting Report

Work accomplished during this reporting period:

  • TAG members list finalized and attached

  • The project website updated with the current information and personnel

  • TAG Kick Meeting is now planned for November 11, 2022 (Please see the tentative flyer with this report).

2022-2023 First Quarterly Report

Work accomplished during this reporting period:

  • Recruitment and hiring of student workers for the project completed.

  • Students have completed the SFID requirements lab safety training before starting working on the project.

  • Planned and executed the TAG meeting on December 14, 2022, via the WebEx Virtual Meeting Platform

  • Re-located and re-installed the solar simulator in our new research lab at Florida Poly.

  • Performed baseline experiments of Methyl Orange degradation via solar-enhanced photocatalysis using TiO2 microencapsulated organic dye particles.

Video Recording of 2022-2023 TAG Kick-off Meeting

2022-2023 Second Quarterly Report

Work accomplished during this reporting period:

  • Synthesis of TiO2 encapsulated Thermochromic Materials

We have successfully synthesized the TiO2-encapsulated TCM dye particles using a microemulsion process. In this process, a systematic wet chemical approach is followed based on the procedure given in the experiment and results section of this quarterly report. The as-prepared TiO2@TCMs are characterized to understand the physico-chemical behavior such as thermal and microstructural properties.

 

  • Calibration of kinetic degradation of MO and Leachate samples via TiO2@TCM adsorption

A model contaminant such as Azo dye, Methyl Orange, and raw leachate adsorption mechanism was calibrated for the extended kinetic degradation. The concentration of MO varied as 40ppm, 100ppm, and 200ppm in DI water via the presence of TiO2@TCM catalyst. Extended kinetic degradation studies up to 20 hours were examined after dispersing the TiO2@TCM catalyst of less than 5mg.

 

  • Synthesis and characterization of TiO2@PW12 nanocomposites

A preliminary synthesis of novel TiO2@PW12 nanocomposites is prepared using a sol-gel process. This material has shown in the literature that has high photocatalytic activity towards PFAS treatment in short-chain and long-chain organic PFAS/PFOA compounds. The structural characterizations and spectrometric analyses are planned in the summer months.

2022-2023 Third Quarterly Report

  • UV-Vis, Fluoride ion, and COD characterizations on the Leachate, HFBA model liquids with and without solar simulated radiation and modified TiO2 catalysts.

  • XRD characterization studies of modified TiO2 photocatalysts, for example, PW12@TiO2 nanocomposites.

2021-2022 Final Report

ABSTRACT:

Poly- and perfluoroalkyl substances (PFAS) are persistent in the environment and they have been detected in harmful quantities in the food chain, watersheds, municipal drinking water, and as a component of landfill leachate. PFAS have been used for decades and although several have been banned, they continue to be found in thousands of current products that will eventually be landfilled. Throughout the US, many landfills treat leachate through municipal wastewater treatment plants (WWTP) and, therefore, the presence of any persistent chemical has the potential to end up in waterways and, ultimately, in the water supplied to municipal systems. This project is aimed at the characterization of the distribution of PFAS in landfill leachate with respect to environmental conditions as well as the further development and demonstration of a new solar photocatalytic approach to remediate these persistent species in landfill leachate. The project has successfully utilized a novel, sustainable, solar initiated photocatalytic process involving a combination of recyclable, co-catalysts. The studies have been carried out on PFAS with less than eight carbons as current methods are incapable of remediating these smaller PFAS and they are often the byproducts of the remediation of larger PFAS. We have established the optimum pH, cocatalysts’, and oxygen concentrations necessary to remediate the PFAS systems to non-toxic CO2 and fluoride ion (F-). Additionally, aside from these targeted fluorinated products, potential degradation byproducts not containing fluorine have been examined. Upon optimization of the process in model PFAS waste simulant systems, the developed approach has been utilized in real leachate samples collected on a quarterly basis from local landfills. Quantification of reaction products were evaluated using fluoride ion selective electrode measurements as well as solid phase extraction followed by liquid chromatographic separation with triple quadrupole mass spectrometric measurements to determine the pre- and post-treatment fluorinated species present, the overall efficiency of the PFAS remediation process, and the potential non-fluorinated byproducts that may be species of concern.

2021-2022 Third  Quarterly Report

Work accomplished during this reporting period:

  • Additional runs of solar photocatalytic treatment of small PFAS carboxylic acid, HFBA, utilizing fluoride ion selective electrode measurements.

  • Began synthesis of the first phosphotungstic acid immobilized TiO2 (TiO2@PW12) nanocomposite.

  • Characterization of raw leachate samples via Optical Emission Spectroscopy (OES) and chemical oxygen demand (COD) measurements.

  • Sample preparation and arranging analysis (solid phase extraction/UHPLC/MS) of raw and photo catalytically treated leachate samples collected from Polk County’s North Central Landfill.

2021-2022 Second  Quarterly Report

Work accomplished during this reporting period:

  • Extended hours of solar photocatalytic treatment of HFBA and the fluoride ion measurements (ppm concentration and electric voltage).

  • Literature survey of modified photocatalysts development for the HFBA remediation with plans to incorporate boron carbide.

  • Leachate sample collections from Polk County’s North Central Landfill and re-establishing the technical advisory (TAG) for the project.

  • Sample preparation and shipping of raw leachate samples collected from the North Central Landfill to Stony Brooke University.

2021-2022 First  Quarterly Report

Work accomplished during this reporting period:

  • Interviewing & Recruiting students to work on this new project from September 2021.

  • Planned and executed the TAG meeting on November 17, 2021, via the WebEx Virtual Meeting Platform

  • Calibration and standardization experiments regarding fluoride ion testing and analysis of TiO2 photocatalytic oxidation of heptafluorobutyric acid (HFBA).

Video Recording of 2022-2023 TAG Kick-off Meeting

2019-2020 Final Report

Technical work accomplished during the project period:

  • Successfully executed the Kick-off and Closing TAG meetings and presented our research results.

  • The closing TAG meeting was held on Friday, 26, 2021 at 4 PM

  • Preparation of PFAS molecularly imprinted polymer (MIP) using titanium (IV) isopropoxide, sol-gel reaction.

  • Studies using a new, efficient photosensitizer system, Poly-X, to examine the potential of this mixture for remediating organics such as active pharmaceutical ingredients (API).

  • Examined the remediation capability of several chemically modified Poly-X compounds to degrade complex organics.

  • Investigation of PFAS model compound, heptafluorobutyric acid, remediation in water using standard TiO2 photocatalysis and Poly-X photosensitizer systems.

  • Studied remediation of per- and poly- fluoroalkane systems (PFAS)  using unmodified and chemically modified Poly-X compounds with TiO2.

  • Studied PFAS remediation in landfill leachate using standard TiO2 photocatalysis and Poly-X photosensitizer systems.

  • Examination of PFAS remediation utilizing TiO2 and the Synergistic Chemical Oxidative and Photocatalytic Enhancer System (SCOPES) previously developed as part of the Hinkley Center for Solid and Hazardous Waste Management Grant Number GR-1900004 using waste simulants (PFAS and organics) and landfill leachate (PFAS).

  • Initiation of a critical collaboration for the success of this project with PFAS mass spectrometry expert, Professor Carrie McDonough, Civil Engineering Department, Stony Brook University, Stony Brook, NY.

2018-2019 Final Report

Technical work accomplished during the project period:

  • The Hinkley Center-Florida Poly project kick-off meeting was successfully held on the 8th of November at the campus and also conducted via WebEx online services. TAG members, Collaborators, Stakeholders, and Hinkley Center Project Coordinators and Project participants (faculty, staff, and students) have joined the kick-off meeting via WebEx and in-person at the venue (Annexure 4 – Flyer and other documents related to the kick-off TAG meeting).

  • The final TAG list is prepared based on the availability, willingness, and support confirmation from all the proposed TAG members (Annexure 5 – Finalized TAG list with full info).

  • A website is constructed with all the project-relevant info and a link is created at the Florida Poly’s PI page. Updates will be done periodically on the website to reflect the project activities, milestones, deliverables, etc (Annexure 6 – Webpages of the project).

  • Model contaminant Methyl Orange (MO) standardization in terms of dilution calibration was done using the standard operating procedure of dilution series experiment and graph plotting using Beer’s law.

  • The concentration optimization of MO was carried out systematically using our 250 ml (with 300W light bulbs) and 500 ml (with 600W light bulbs) batch reactors fabricated in our FL Poly laboratory.

  • Irradiance measurements of the custom-built batch reactor, continuous flow reactor, and the solar simulated reactor for wastewater remediation were performed using Ocean Optics Spectrometer. https://floridapoly.edu/news/leading-scientific-company-holds-workshop-students-faculty/

  • Leachate samples collection from the Hillsborough County (Lithia) Landfill site was executed on February 8th, 2019. A new collaboration has been established between FL Poly and the Hillsborough County Landfill for the periodical collection of leachate samples for characterization and remediation purposes using our proposed SCOPES.

  • Training was provided on the Hach Spectrophotometer for the COD analysis, to all the Hinkley research project students by Dr. Scott Wallen, project co-investigator.

  • The new FL Poly-Hinkley project website was designed on Wix.com and the web link is given in the project website section above.

  • Photocatalytic reactors and the UV-Vis light radiations under black light and solar-simulated light are underway for the future development of the project for leachate remediation studies.

  • Reduction of total organic nitrogen COD analysis.

  • Photocatalysis - using TiO2 activated by the UV-Vis light for the remediation of landfill leachate.

  • Chemical oxidation – addition of persulfate and peroxide to enhance and achieve better remediation results.

  • Materials’ development – use of dopants to increase visible light photocatalysis (bandgap shifting) to make magnetic catalyst (for separation).

  • Removal of persulfate from the leachate to reduce its interference in the COD analysis.

  • Identified spectral interference in COD measurements of SCOPES-treated systems.

  • Materials’ development – use of dopants to increase visible light photocatalysis (bandgap shifting) to make magnetic catalyst (for separation).

  • SCOPES photocatalysis - using TiO2 activated with chemical oxidants and UV-Vis light for the remediation of landfill leachate.

  • Discovery of a new class of abundant compounds that act as a co-photosensitizer with titanium dioxide for unprecedented remediation of model contaminant, methyl orange.

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