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Extractions:

  • In order to run analysis on the samples, the water must be absorbed (by MgSO4) and the contaminant must be transferred to tetrahydrofuran (THF)
  • 0.5 mL of sample, 1 mL of THF, and 0.5 g of MgSO4 are added to a vial
  • Remaining liquid is removed from the vial and moved to another vial containing 0.2 g of MgSO4
  • Wait for 10 minutes to ensure complete adsorption of water
  • The remaining liquid is removed using glass syringes into vials ready for gas chromatography mass spectrometry (GCMS) analysis

Development of a Biobased Carbon Adsorbent for Treating Emerging Contaminants in Recycled Water on the International Space Station

Savanna Vacek, Madeline Carroll, Gabson Baguma

Mentor: Dr. Erica Marti

Department of Civil and Environmental Engineering, University of Nevada - Las Vegas

This material is based upon work supported by the National Aeronautics and Space Administration under Cooperative Agreement No. 80NSSC20M0043.

I would also like to thank Dr. Erica Marti, Dr. Eakalak Khan, Gabson Baguma, and Madeline Carroll for their help and contributions.

Introduction

Research Objectives

Prior Work

Results

Discussion/Conclusion

Acknowledgements

  • The International Space Station (ISS) operates as a closed system
  • Water is recycled from humidity and urine and held in a wastewater tank; part of the Water Processing Assembly (WPA)
  • Potable treated water is used indirectly in the Sabatier Reactor
  • The Sabatier Reactor is a key component in the Environmental Control and Life Support System (ECLSS)
  • Three main functions of ECLSS: water recovery, air revitalization, and oxygen generation
  • Sabatier Reactor recently failed due to contamination of DMSO2, dimethyl sulfone, and DMSD, dimethylsilanediol
  • DMSO2 and DMSD are emerging contaminants that are not removed by the media used in the WPA due to their low affinity
  • DMSO2 and DMSD are introduced into the water system through personal hygiene products such as lotion, conditioner, and wipes, which all contain volatile methyl siloxanes (VMS)
  • VMS are decomposed into DMSO2 or DMSD and are found in urine

Objectives:

  • Synthesize at least 3 biobased ionic liquids
  • Analyze and quantify how much DMSO2 is removed by the ionic liquids through liquid-liquid extractions
  • Coat GAC with the most effective biobased ionic liquids
  • Analyze and quantify how much DMSO2 is removed with uncoated GAC and ionic liquid coated GAC through batch adsorption testing

  • The following ionic liquids were synthesized: a liquid result is successful, but any recrystallization is an unsuccessful result

Batch Adsorption Testing:

  • 0 hours started with 756 ppb of DMSO2
  • Over 24-96 hours, concentration stayed relatively the same around 515 ppb DMSO2
  • 24 hours can be determined as the equilibrium time with only a 32% removal
  • Demonstrates a need for ionic liquid coated GAC since uncoated GAC is not sufficient in removing DMSO2 from water

Extractions:

  • Water was successfully absorbed by MgSO4, contaminant was transferred to THF phase for GCMS analysis

FTIR Characterization:

  • Peaks show that all ionic liquid trials contained both a HBD and HBA
  • X-axis location of peaks is consistent with ionic liquid formation across all thymol and decanoic acid liquids
  • X-axis location of peaks is not consistent with ionic liquid formation across all thymol and dodecanoic acid liquids

Future Work

  • Analysis by GCMS will be completed to determine the DMSO2 adsorption by liquid-liquid extractions
  • The best two ionic liquids, determined by analysis, will be coated onto biochar
  • The two ionic liquid coated GACs will go through batch adsorption tests - equilibrium, isotherm, and kinetic testing
  • The results of the adsorption experiments will be analyzed to determine the removal of DMSO2
  • If removal was successful, the ionic liquid coated biochar would be a good recommendation to fix the Sabatier Reactor

DMSD

DMSO2

International Space Station Water Processing Assembly - Graphic Credit: Dr. Khan’s Lab

Equilibrium Batch Adsorption Testing with Uncoated GAC:

  • 100 mg of coconut granular activated carbon ranging in sizes from 400-595 microns is added to a 45 mL vial containing 800 ppb DMSO2
  • Solution is shaken until reaching equilibrium
  • Equilibrium time is determined by taking samples over time - 24, 48, 72, and 96 hours
  • Samples are filtered to separate GAC from water
  • Samples are analyzed by gas chromatography mass spectrometry (GCMS) to measure the concentration of DMSO2

References

Thymol and Decanoic Acid:

  • Absorbance intensities differ at 2800 and 2900 peak (C-H stretching)
  • Similar absorbance intensities at 1735 peak (C=O stretching)
  • Small differences in intensity overall, 2:1 ratio more intense

Thymol and Dodecanoic Acid:

  • Much higher absorbance for all compared to other ionic liquids
  • 2:1 ratio shows the highest absorbance for every peak
  • All synthesized ionic liquids were not successful

Thymol and Undecylenic Acid:

  • Higher absorbance at 2800 and 2900 peak for 1:1 ratio (C-H stretching)
  • 2:1 ratio shows very low to almost negative intensity, and was an unsuccessful ionic liquid
  • Absorbance intensity is higher in 1:1 ratio than 2:1 ratio

Please view the PDF for references via QR code

  • Ambersorb 4652, a styrenic polymer adsorbent that is not biobased or sustainable, is the current media used in the multifiltration beds in WPA on the ISS
  • Costly and unsustainable, Ambersorb 4652 is challenged to remove DMSD and DMSO2 from recycled water
  • Granular activated carbon (GAC) works similarly to a styrenic polymer adsorbent and can be made from biobased materials
  • Ionic liquids are liquid molten salts at temperatures < 100 ℃ that are typically composed of large and unsymmetrical organic cations and organic or inorganic ions
  • Composed of a hydrogen bond acceptor (HBA) and a hydrogen bond donor (HBD)
  • Remarkable solvation ability for a broad range of natural and synthetic materials and compounds

Methodology

  • The following ionic liquids were synthesized:

Granular Activated Carbon (GAC)

Synthesized Ionic Liquids

Extraction Vials

Batch Adsorption Testing

Synthesized Ionic Liquid Results

Uncoated GAC Equilibrium Batch Adsorption Test Results

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