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When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
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The 1D NMR spectrum of large and complex molecules like natural products has complicated splitting patterns and overlapping signals, which can be easily interpreted using 2-dimensional (2D) NMR. Unlike 1D NMR, 2D NMR has two frequency axes that provide the coupling information between the nucleus A and nucleus B in a molecule. The process from which 2D spectra are obtained has four steps.
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The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
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A conventional Raman spectrophotometer includes a laser source, a sample holding system, a wavelength selector, and a detector.
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A 1H Background-Free 3D Printing Digital Light Processing Resin for Applications in NMR Spectroscopy.

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A novel "NMR invisible" perfluorinated resin enables 3D printing of Nuclear Magnetic Resonance (NMR) components. This advancement supports new biological and environmental applications, including challenging marine research.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Spectroscopy

Background:

  • Nuclear Magnetic Resonance (NMR) spectroscopy is a vital analytical tool.
  • Current limitations in 3D printing NMR hardware stem from the lack of 1H NMR background-free resins.
  • Existing NMR accessories are often costly and limit complex sample analysis.

Purpose of the Study:

  • To develop a novel photobleached perfluorinated resin for 3D printing of 1H NMR invisible components.
  • To demonstrate the utility of this resin for creating both standard and novel NMR accessories.
  • To expand the application scope of NMR, particularly in biological and environmental research.

Main Methods:

  • Development of a photobleached perfluorinated resin.
  • 3D printing of NMR components, including magnetic susceptibility plugs, coaxial inserts, multicompartment holders, and salt-tolerant inserts.
  • Characterization of the resin using 1H NMR and solvent exposure tests.
  • Testing of accessories with challenging samples, including high-salt marine conditions and the organism Tigriopus californicus.

Main Results:

  • The developed resin exhibits no 1H NMR spectral background and is compatible with common NMR solvents.
  • 3D printed commercial accessories (plugs, inserts) were successfully fabricated.
  • Novel accessories, such as multicompartment holders and salt-tolerant inserts, were demonstrated.
  • Salt-tolerant inserts maintained cryoprobe performance in 5 M salt, unlike standard NMR tubes which showed significant signal-to-noise ratio loss.

Conclusions:

  • The "NMR invisible" perfluorinated resin offers an economical, accessible, and versatile method for fabricating NMR components.
  • This technology enables rapid prototyping and the development of novel accessories.
  • The resin significantly expands the potential applications of NMR spectroscopy in diverse fields, including marine research.