An organogel library for solution NMR analysis of nanoparticle suspensions in non-aqueous samples

Sedinkin, Sergey L.; An, Yeongseo; Naik, Pranjali; Slowing, Igor I.; Venditti, Vincenzo

doi:10.1016/j.jmr.2020.106874

Cited by 3 publications

(8 citation statements)

References 29 publications

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“…To this end, we determined how the 13 C transverse relaxation rates (Δ R 2 ) of the substrate signals change when the catalyst is added to the solution. The value of Δ R 2 is proportional to the fraction of molecules that bind the catalyst surface and lose magnetization because of the slower molecular tumbling of adsorbed species. ,, Although we observed a large increase in transverse relaxation rate (average Δ R 2 7.0 ± 0.3 s –1 ) when setting 4-Cl-PhOH in the presence of the catalyst, no significant changes (Δ R 2 ∼ 0 s –1 ) were observed when the catalyst was added to solutions of Cl-Ph or 4-Cl-PhOMe (Figure S10). These results indicate that while 4-Cl-PhOH interacts strongly with the catalyst, the non-hydroxylated haloaromatics have a weaker affinity for Pd/CeO 2 .…”

Section: Resultsmentioning

confidence: 77%

“…The value of ΔR 2 is proportional to the fraction of molecules that bind the catalyst surface and lose magnetization because of the slower molecular tumbling of adsorbed species. 9,10,28 Although we observed a large increase in transverse relaxation rate (average ΔR 2 7.0 ± 0.3 s −1 ) when setting 4-Cl-PhOH in the presence of the catalyst, no significant changes (ΔR 2 ∼ 0 s −1 ) were observed when the catalyst was added to solutions of Cl-Ph or 4-Cl-PhOMe (Figure S10). These results indicate that while 4- Cl-PhOH interacts strongly with the catalyst, the nonhydroxylated haloaromatics have a weaker affinity for Pd/ CeO 2 .…”

Section: ■ Results and Discussionmentioning

confidence: 84%

“…Pd/CeO2 was degassed at 100 °C under vacuum for 24 h. The pre-dried catalyst was then introduced into NMR tubes containing 4-Cl-PhOH solution (1 mL, 100 mM, benzene-d6) or only benzene-d6 as a control. 13 C transverse relaxation rate (R2) measurement were acquired on gel-stabilized NMR samples 27 prepared by following previously described procedures 28 . Briefly, the appropriate amount of the nanoparticle and 12-Hydroxyoctadecanamide gelator was weighed directly into an NMR tube followed by the addition of 10 mM substrate solution in cyclohexane-d12 to produce 0.5 wt % nanoparticle and 0.5 wt % gelator sample.…”

Section: Hydrodehalogenation Reactions (Hdh)mentioning

confidence: 99%

“…13 C transverse relaxation rate (R 2 ) measurements were acquired on gel-stabilized NMR samples 27 prepared by following previously described procedures. 28 Briefly, the appropriate amount of the nanoparticle and the 12hydroxyoctadecanamide gelator was weighed directly into an NMR tube followed by the addition of 10 mM substrate solution in cyclohexane-d 12 to produce a 0.5 wt % nanoparticle and a 0.5 wt % gelator sample. The capped NMR tube was placed into a sonic bath (Branson 1800) and heated to a temperature of ∼70 °C.…”

Section: ■ Introductionmentioning

confidence: 99%

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Non-Innocent Role of the Ceria Support in Pd-Catalyzed Halophenol Hydrodehalogenation

Naik

Sedinkin

et al. 2021

ACS Catal.

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The hydrodehalogenation (HDH) of halophenols is efficiently catalyzed by palladium supported on high surface ceria (Pd/CeO2) under mild conditions (35 °C, 1 atm H2). A combination of NMR, DRIFTS, Raman spectroscopy and XPS studies as well as HDH kinetics of substituted halobenzenes suggest the reaction proceeds mainly via a sequence of dissociative adsorption of phenolic hydroxyl onto the support, oxidative addition of Pd into the C-halogen bond and reductive elimination to give phenol and hydrogen halide. The dissociative adsorption of -OH group onto oxygen vacancies of the ceria support results in an electron-rich intermediate that facilitates the turnover-limiting reductive elimination step. In contrast, the direct pathway catalyzed by Pd without dissociative adsorption of the reactants on the support takes place at a slower rate. The mechanistic insights gained in this study were used to modify reaction conditions for enabling HDH of recalcitrant halides such as fluorides and iodides.

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Section: Resultsmentioning

confidence: 77%

Section: ■ Results and Discussionmentioning

confidence: 84%

Section: Hydrodehalogenation Reactions (Hdh)mentioning

confidence: 99%

Section: ■ Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Non-Innocent Role of the Ceria Support in Pd-Catalyzed Halophenol Hydrodehalogenation

Naik

Sedinkin

et al. 2021

ACS Catal.

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“…A library of small molecule gelators that satisfy these requirements was recently developed to stabilize NP suspensions in a number of NMR-friendly aqueous 155 and organic solvents. 156 …”

Section: Solution Nmr Methods For Characterizing Sorption Equilibriamentioning

confidence: 99%

Solution NMR methods for structural and thermodynamic investigation of nanoparticle adsorption equilibria

Sedinkin

Venditti

2022

Nanoscale Adv.

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Binding Between Antibiotics and Polystyrene Nanoparticles Examined by NMR

et al. 2022

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Elucidating the interactions between plastic nanoparticles and small molecules is important to understanding these interactions as they occur in polluted waterways. For example, plastic that breaks down into micro-and nanoscale particles will interact with small molecule pollutants that are also present in contaminated waters. Other components of natural water, such as dissolved organic matter, will also influence these interactions. Here we use a collection of complementary NMR techniques to examine the binding between polystyrene nanoparticles and three common antibiotics, belonging to a class of molecules that are expected to be common in polluted water. Through examination of proton NMR signal intensity, relaxation times, saturation-transfer difference (STD) NMR, and competition STD-NMR, we find that the antibiotics have binding strengths in the order amoxicillin < metronidazole ≪ levofloxacin. Levofloxacin is able to compete for binding sites, preventing the other two antibiotics from binding. The presence of tannic acid disrupts the binding between levofloxacin and the polystyrene nanoparticles, but does not influence the binding between metronidazole and these nanoparticles.

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An organogel library for solution NMR analysis of nanoparticle suspensions in non-aqueous samples

Cited by 3 publications

References 29 publications

Non-Innocent Role of the Ceria Support in Pd-Catalyzed Halophenol Hydrodehalogenation

Non-Innocent Role of the Ceria Support in Pd-Catalyzed Halophenol Hydrodehalogenation

Solution NMR methods for structural and thermodynamic investigation of nanoparticle adsorption equilibria

Binding Between Antibiotics and Polystyrene Nanoparticles Examined by NMR

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