Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand

Seipp, Charles A.; Williams, Neil J.; Custelcean, Radu

doi:10.3791/54411

Title: Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand

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Abstract

One simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, 1,4-benzene-bis(iminoguanidinium) (BBIG), is demonstrated. The ligand is synthesized as the chloride salt (BBIG-Cl) by in situ imine condensation of terephthalaldehyde with aminoguanidinium chloride in water, followed by crystallization as the sulfate salt (BBIG-SO4). Alternatively, BBIG-Cl is synthesized ex situ in larger scale from ethanol. Furthermore, the sulfate separation ability of the BBIG ligand is demonstrated by selective and quantitative crystallization of sulfate from seawater. These ligands can then be recycled by neutralization of BBIG-SO4 with aqueous NaOH and crystallization of the neutral bis-iminoguanidine, which can be converted back into BBIG-Cl with aqueous HCl and reused in another separation cycle. Finally, 35S-labeled sulfate and β liquid scintillation counting are employed for monitoring the sulfate concentration in solution. Overall, this protocol will instruct the user in the necessary skills to synthesize a ligand, employ it in the selective crystallization of sulfate from aqueous solutions, and quantify the separation efficiency.

Authors:

Seipp, Charles A. ^[1]; Williams, Neil J. ^[2]; Custelcean, Radu ^[3]

Univ. of Texas, Austin, TX (United States). Dept. of Chemistry
Univ. of Tennessee, Knoxville, TN (United States). Dept. of Chemistry
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Division

Publication Date:: Fri Jan 01 00:00:00 EST 2016

Research Org.:: Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1325430

Grant/Contract Number:: AC05-00OR22725

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Visualized Experiments

Additional Journal Information:: Journal Volume: 115; Journal Issue: 115; Journal ID: ISSN 1940-087X

Publisher:: MyJoVE Corp.

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; crystallization; separations; guanidinium; self-assembly; sulfate; water

Citation Formats


                    Seipp, Charles A., Williams, Neil J., and Custelcean, Radu. Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand.  United States: N. p., 2016. 
Web.  doi:10.3791/54411.

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                    Seipp, Charles A., Williams, Neil J., & Custelcean, Radu. Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand.  United States.  https://doi.org/10.3791/54411

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                    Seipp, Charles A., Williams, Neil J., and Custelcean, Radu. Fri .  
"Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand".  United States.  https://doi.org/10.3791/54411.  https://www.osti.gov/servlets/purl/1325430.

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@article{osti_1325430,

  title        = {Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand},

  author       = {Seipp, Charles A. and Williams, Neil J. and Custelcean, Radu},

  abstractNote = {One simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, 1,4-benzene-bis(iminoguanidinium) (BBIG), is demonstrated. The ligand is synthesized as the chloride salt (BBIG-Cl) by in situ imine condensation of terephthalaldehyde with aminoguanidinium chloride in water, followed by crystallization as the sulfate salt (BBIG-SO4). Alternatively, BBIG-Cl is synthesized ex situ in larger scale from ethanol. Furthermore, the sulfate separation ability of the BBIG ligand is demonstrated by selective and quantitative crystallization of sulfate from seawater. These ligands can then be recycled by neutralization of BBIG-SO4 with aqueous NaOH and crystallization of the neutral bis-iminoguanidine, which can be converted back into BBIG-Cl with aqueous HCl and reused in another separation cycle. Finally, 35S-labeled sulfate and β liquid scintillation counting are employed for monitoring the sulfate concentration in solution. Overall, this protocol will instruct the user in the necessary skills to synthesize a ligand, employ it in the selective crystallization of sulfate from aqueous solutions, and quantify the separation efficiency.},

  doi          = {10.3791/54411},

  journal      = {Journal of Visualized Experiments},

  number       = 115,

  volume       = 115,

  place        = {United States},

  year         = {Fri Jan 01 00:00:00 EST 2016},

  month        = {Fri Jan 01 00:00:00 EST 2016}

}

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