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ACS Publications. Most Trusted. Most Cited. Most Read
Exploration of Materials for Three-Dimensional NMR Microcoil Production via CNC Micromilling and Laser Etching
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    Exploration of Materials for Three-Dimensional NMR Microcoil Production via CNC Micromilling and Laser Etching
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    • Vincent Moxley-Paquette
      Vincent Moxley-Paquette
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Jacob Pellizzari
      Jacob Pellizzari
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Daniel Lane
      Daniel Lane
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
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    • Katrina Steiner
      Katrina Steiner
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Peter M. Costa
      Peter M. Costa
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • William W. Wolff
      William W. Wolff
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Daniel H. Lysak
      Daniel H. Lysak
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Rajshree Ghosh Biswas
      Rajshree Ghosh Biswas
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Katelyn Downey
      Katelyn Downey
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
    • Kiera Ronda
      Kiera Ronda
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
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    • Ronald Soong
      Ronald Soong
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
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    • Dmitri Zverev
      Dmitri Zverev
      NSCNC Manufacturing LTD, 19358 96 Ave, Unit 150, Surrey, British Colombia V4N 4C1, Canada
    • Peter De Castro
      Peter De Castro
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
    • Thomas Frei
      Thomas Frei
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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    • Danijela Al Adwan-Stojilkovic
      Danijela Al Adwan-Stojilkovic
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Stephan Graf
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Simon Gloor
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Daniel Schmidig
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Rainer Kuemmerle
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Till Kuehn
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Falko Busse
      Bruker BioSpin AG, Industriestrasse 26, 8117 Fällanden, Switzerland
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      Nathan Haberer
      Aidlab, 651 N., Broad St., Suite 201, Middletown, Delaware 19709, United States
    • Jakub Domaszewicz
      Jakub Domaszewicz
      Aidlab, 651 N., Broad St., Suite 201, Middletown, Delaware 19709, United States
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      Ryan Scatena
      Thermal Conductive Bonding Inc., 6210 88th Street, Sacramento, California 95828, United States
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      Andressa Lacerda
      Synex Medical, 2 Bloor Street E, Suite 310, Toronto, ON M4W 1A8, Canada
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      Ben Nashman
      Synex Medical, 2 Bloor Street E, Suite 310, Toronto, ON M4W 1A8, Canada
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      Jens Anders
      University of Stuttgart, Pfaffenwaldring 47, 70569 Stuttgart, Germany
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      Marcel Utz
      School of Chemistry, University of Southampton, Southampton SO17 1BJ, U.K.
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    • André J. Simpson*
      André J. Simpson
      Environmental NMR Center, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4, Canada
      *Email: [email protected]
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    Analytical Chemistry

    Cite this: Anal. Chem. 2024, 96, 33, 13588–13597
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.analchem.4c02373
    Published August 8, 2024
    Copyright © 2024 American Chemical Society

    Abstract

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    The excellent versatility of 5-axis computer numerical control (CNC) micromilling has led to its application for prototyping NMR microcoils tailored to mass-limited samples (reducing development time and cost). However, vibrations during 5-axis milling can hinder the creation of complex 3D volume microcoils (i.e., solenoids and saddle coils). To address these limitations, a high-resolution NSCNC ELARA 4-axis milling machine was developed with the extra precision required for making complex 3D volume microcoils. Upon investigating the performance of resonators made with various copper-coated dielectrics, resonators with poly(methyl methacrylate) (PMMA) provided the best SNR/line shape. Thus, complex 1.7 mm microcoil designs were machined from Cu-coated PMMA. A milled 6.4 mm solenoid also provided 6.6× the total carbon signal for a 13C-labeled broccoli seed compared to a commercial inverse 5 mm NMR probe (demonstrating potential for larger coil designs). However, the manufacture of coils <1.7 mm with copper-coated PMMA rods was challenging as ∼0.5 mm of remaining PMMA was needed to retain their structural integrity. To manufacture smaller microcoils, both a solenoid and saddle coil (both with 1 mm O.D., 0.1 mm thick walls) were etched from Cu-coated glass capillaries using a UV picosecond laser that was mounted onto an NSCNC 5-axis MiRA7L. Both resonators showed excellent signal and identified a wide range of metabolites in a 13C-labeled algae extract, while the solenoid was further tested on two copepod egg sacs (∼4 μg of total sample). In summary, the flexibility to prototype complex microcoils in-house allows laboratories to tailor microcoils to specific mass-limited samples while avoiding the costs of cleanrooms.

    Copyright © 2024 American Chemical Society

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.analchem.4c02373.

    • Detailed experimental methods, design schematics for the various microcoils, and additional spectra comparing the performance between various resonators (PDF)

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    Analytical Chemistry

    Cite this: Anal. Chem. 2024, 96, 33, 13588–13597
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.analchem.4c02373
    Published August 8, 2024
    Copyright © 2024 American Chemical Society

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