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  1. Project S1Assessment of pharmaceutical residue levels in industrial waste waters and their removal using photocatalysisResearcher: Ann-Marie DeeganPrincipal Investigator’s: Anne Morrissey, Kieran Nolan and John TobinDublin City UniversityCollaborator: Professor Michael Oelgemoeller Industrial Mentor: Clodagh Ettarh, Astellas

  2. Project Summary • Development of techniques for the determination of low levels of pharmaceuticals in industrial wastewater • Development of methods for the removal of pharmaceuticals using photocatalysis • Start date: October 2007 • End date: September 2010

  3. Project Objectives • Develop a SPE-LC-MS/MS detection method for the monitoring of the active pharmaceutical ingredients (APIs) • Monitor pharmaceutical residues in influent and effluent samples • Degrade APIs using photocatalysis

  4. Potential benefits for industry • Techniques for the API determination • Monitoring of APIs in waste streams • Sustainable removal of APIs • Enable compliance with future legislation and terms of licensing • Identify product loss

  5. Routes of entry to the environment

  6. Routes of entry to the environment

  7. Analytes • Active Ingredient A: Famotidine • H2 receptor anatagonist, inhibits stomach acid production • Active ingredient B: Tamsulosin hydrochloride • Blocks alpha receptors, treatment of benign prostatic hyperplasia • Active Ingredient C: Solifenacin succinate • Muscarinic antagonist, used in the treatment of overactive bladder

  8. Detection of APIs in aqueous samples [SPE, SPME, LLE]

  9. Influent Method Limits

  10. Effluent Method Limits

  11. Sampling points

  12. Concentration (mgL-1)

  13. Concentration (mgL-1)

  14. Concentration (mgL-1)

  15. 3rd Nov 2009 - 2nd March 2010 Summary

  16. Removal Techniques • TiO2 photocatalysis • Photo-Fenton oxidation

  17. TiO2 Photocatalysis • generation of electron-hole pairs h+-e– • formation of highly reactive HO• radicals

  18. Immersion Well Experiment Active Ingredient A Figure: Degradation of active ingredient A and degradation products monitored over 300 min

  19. Immersion Well Experiment Active Ingredient A Figure: Degradation of active ingredient A and degradation products monitored over 300 min Figure: Initial monitoring of degradation products using HPLC identification of breakdown products will be conducted using mass spectrometry

  20. Enviolet Reactor Experiment UV Degradation of active ingredient A monitored from 190 nm to 350 nm over 300 min

  21. Enviolet Reactor Experiment UV Degradation of active ingredient A monitored from 190 nm to 350 nm over 300 min Degradation of active ingredient A and degradation products monitored over 300 min

  22. Dark Fenton OH· OH· Photo-Fenton oxidation Photo-Fenton at pH 3 H2O Fe3+ H2O2 Fe2+

  23. Dark Fenton OH· OH· Photo-Fenton oxidation Photo-Fenton at pH 3 H2O Fe3+ H2O2 Fe2+

  24. Dark Fenton OH· OH· Photo-Fenton oxidation Photo-Fenton at pH 3 H2O Fe3+ H2O2 Fe2+

  25. Summary and future work • SPE-LC-MS/MS method developed and validated • 6 month sampling programme complete • TiO2 photocatalysis and Fentons oxidation both show high removal efficiency • Continuation of Fenton experiments

  26. Any Questions?