Steps to achieving high-resolution NMR spectroscopy on solutions at GPa pressure

Clicks: 4
ID: 305789
2017
Free PDF
Article Quality & Performance Metrics
Overall Quality
Not rated
Combines reader engagement with the AI quality analysis. This article has not been analysed, so there is no overall score — reader engagement is measured and shown alongside.
AI Quality Assessment
Not analyzed
Readership in this journal
Emerging

Ranked #830 of 8,486 articles by views in american journal of science

Most read Least read

Bar heights use a square-root scale. Only the 120 most-read articles are drawn; the journal has 8,486 in total.

Mint this article as an NFT
Not yet minted

Create a permanent, verifiable on-chain record of this article on the Scimatic Network. The NFT is held in your Journament account, and you can withdraw it to your own wallet at any time.

5 SUSD one-off · no wallet required
Sign in to mint
Abstract
Recent theoretical advances and molecular-dynamic estimates of the dielectric constant of water have extended the HKF model for aqueous solution chemistry up to 6.0 gigapascals (GPa), which are conditions well beyond the capabilities of conventional NMR spectroscopy (Pan and others, 2013; Sverjensky and others, 2014, see also Wasserman and others, 1995). These developments provide strong motivation to design a simple NMR probe that allows experiments on solutions, at high resolution, to pressures of a few GPa (Pautler and others, 2014; Ochoa and others, 2015, 2016). Here we describe the performance of a compact NMR probe that can reach several GPa pressures. The probe is made by placing a solenoid microcoil inside of a standard piston-cylinder device used in solid-state physics. High pressures are achieved in the sample by applying force to a coaxial piston. Early designs of the probe, although useful, were limited in sample size to ∼10 to 15 μL. Here we describe modifications that allow greatly improved resolution and sensitivity, including ^1^H-^1^H NMR correlation spectroscopy, on solutions at 2.8 GPa pressure. Sample sizes can be expanded if, instead of a standard NMR spectrometer that is built around a superconducting magnet, one employs a magnetic-resonance imaging (MRI) system that is built around a permanent magnet. The MRI systems can apply larger magnetic field gradients than conventional spectrometers, and thus have more robust shimming capability, which is needed because of the juxtaposition of different alloys in the pressure cell. More importantly, these systems can have magnetic fields that are oriented perpendicular to the magnet bore, which allows rotation of the coil within the axis of the pressure cell to increase sample volumes and pressure. Sensitivity is improved by replacing the traditional, but reduced-volume, *closed* sample container mounted in the center of the NMR detection coil with an *open* NMR coil that dangles freely in solution, thus making the sample solution itself the pressure-transmission fluid. The efficacy of these modifications are demonstrated by measuring ^1^H NMR spectra for ethyl alcohol and ethyl alcohol/methyl alcohol mixtures at pressures up to 2.8 GPa. Further developments are discussed that will allow geochemists to acquire aqueous solution NMR spectra at higher 3 to 4 GPa pressures.
Reference Key
openalex_W2755805307 Use this key to autocite in the manuscript while using SciMatic Manuscript Manager or Thesis Manager
Authors Matthew P. Augustine, Gerardo Ochoa, William H. Casey
Journal american journal of science
Year 2017
DOI
10.2475/07.2017.03
URL
https://doi.org/10.2475/07.2017.03
Keywords Keywords not found

Citations

No citations found. To add a citation, contact the admin at info@scimatic.org

Comments

No comments yet. Be the first to comment on this article.