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Princeton University

1. Fortmeyer, Ivy Camille. Characterization of the fluid and solid components of cyanogel systems during the gelation process .

Degree: PhD, 2016, Princeton University

The work in this thesis concerns the sol-gel transformation in cyanogel systems comprised of d8 square planar chlorometalates (M=Pd(II), Pt(II)) and d6 octahedral hexacyanometalates (M=Fe(II), Co(III), Ru(II)). The body of this thesis is split into two chapters. The first chapter examines the physical changes in the solvent phase of the sol-gel network, and the second focuses on the polymer backbone of the gel. Studies on the water component of cyanogel systems during the gelation process were carried out with a variety of in situ spectroscopic techniques. The use of high resolution-magic angle spinning nuclear magnetic resonance (HR-MAS NMR) to identify and characterize different water environments was explored, but was ultimately found to disrupt gelation. Standard solution-phase 1H NMR proved sufficient for calculation and qualitative modeling of spin-spin and spin-lattice relaxations, providing distinct spectral markers of the gelation point and subsequent aging process. Vibrational spectroscopy was used to explore the hydrogen bonding environment of the water during gelation. The kinetics of polymerization of the cyanogel backbone was explored using both in situ and ex situ techniques. Data collected by 13C NMR and 195Pt NMR primarily demonstrated first order kinetics, implying a dissociative substitution mechanism at the chlorometalate center. Rate constants for gelation in the presence of various added monopotassium and nitrate salts were calculated. Added chloride was found to significantly slow gelation and was further explored using NMR and vibrational spectroscopy. A mechanism was proposed for the polymerization taking into account the dissociative substitution and the bridging geometries implied by 13C NMR. Advisors/Committee Members: Bocarsly, Andrew B (advisor).

Subjects/Keywords: coordination polymer; cyanogel; gelation; NMR spectroscopy; spectroscopy

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6th Edition):

Fortmeyer, I. C. (2016). Characterization of the fluid and solid components of cyanogel systems during the gelation process . (Doctoral Dissertation). Princeton University. Retrieved from http://arks.princeton.edu/ark:/88435/dsp01np193c65d

Chicago Manual of Style (16th Edition):

Fortmeyer, Ivy Camille. “Characterization of the fluid and solid components of cyanogel systems during the gelation process .” 2016. Doctoral Dissertation, Princeton University. Accessed November 21, 2019. http://arks.princeton.edu/ark:/88435/dsp01np193c65d.

MLA Handbook (7th Edition):

Fortmeyer, Ivy Camille. “Characterization of the fluid and solid components of cyanogel systems during the gelation process .” 2016. Web. 21 Nov 2019.

Vancouver:

Fortmeyer IC. Characterization of the fluid and solid components of cyanogel systems during the gelation process . [Internet] [Doctoral dissertation]. Princeton University; 2016. [cited 2019 Nov 21]. Available from: http://arks.princeton.edu/ark:/88435/dsp01np193c65d.

Council of Science Editors:

Fortmeyer IC. Characterization of the fluid and solid components of cyanogel systems during the gelation process . [Doctoral Dissertation]. Princeton University; 2016. Available from: http://arks.princeton.edu/ark:/88435/dsp01np193c65d

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