Peter M Costa,Katrina Steiner,Daniel H Lysak,Jacob Pellizzari,William W Wolff,Katelyn Downey,Kiera Ronda,Vincent Moxley-Paquette,Owen Vander Meulen,Caroline Terry,W Wesley Dowd,Daniel Schmidig,Peter De Castro,Stephan Graf,Simon Gloor,Falko Busse,Venita Busse,Agnes Haber,Wolfgang Bermel,Rajeev Kumar,Martine Monette,Myrna Simpson,Andre Simpson
{"title":"A 1H Background-Free 3D Printing Digital Light Processing Resin for Applications in NMR Spectroscopy.","authors":"Peter M Costa,Katrina Steiner,Daniel H Lysak,Jacob Pellizzari,William W Wolff,Katelyn Downey,Kiera Ronda,Vincent Moxley-Paquette,Owen Vander Meulen,Caroline Terry,W Wesley Dowd,Daniel Schmidig,Peter De Castro,Stephan Graf,Simon Gloor,Falko Busse,Venita Busse,Agnes Haber,Wolfgang Bermel,Rajeev Kumar,Martine Monette,Myrna Simpson,Andre Simpson","doi":"10.1021/acs.analchem.5c03472","DOIUrl":null,"url":null,"abstract":"Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful analytical technique with a wide range of applications. To support the analysis of diverse and complex samples, various NMR tools and accessories have been created. Three-dimensional (3D) printing is an underutilized production method for NMR hardware, mainly due to the lack of 1H NMR background-free resins. Here, a photobleached perfluorinated resin was developed for 3D printing of 1H NMR invisible components. 1H NMR showed the resin produced no spectral background while solvent exposure tests demonstrated compatibility with all common NMR solvents. To demonstrate NMR applications of the resin, first commercially available accessories were 3D printed, including magnetic susceptibility plugs and coaxial inserts. Finally, novel accessories that open up new biological and environmental applications were demonstrated. This included a multicompartment holder that, when combined with NMR slice selection techniques, allows the simultaneous study of various samples. Furthermore, salt-tolerant inserts were developed that allowed for NMR to be collected even under the most challenging marine conditions, thus expanding NMR's potential for oceanic research. The effectiveness of the salt-tolerant inserts was demonstrated with the marine organism, Tigriopus californicus. Even in 5 M salt, the full performance of a cryoprobe could be retained using the inserts, whereas using a standard NMR tube, radiofrequency performance was beyond the power handling limits of the probe and 3-fold loss in SNR was seen. In summary, the development and use of \"NMR invisible\" perfluorinated resins presents an economical, accessible, rapid, and versatile approach for building NMR components allowing new applications and prototyping.","PeriodicalId":27,"journal":{"name":"Analytical Chemistry","volume":"65 1","pages":""},"PeriodicalIF":6.7000,"publicationDate":"2025-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Analytical Chemistry","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1021/acs.analchem.5c03472","RegionNum":1,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0
Abstract
Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful analytical technique with a wide range of applications. To support the analysis of diverse and complex samples, various NMR tools and accessories have been created. Three-dimensional (3D) printing is an underutilized production method for NMR hardware, mainly due to the lack of 1H NMR background-free resins. Here, a photobleached perfluorinated resin was developed for 3D printing of 1H NMR invisible components. 1H NMR showed the resin produced no spectral background while solvent exposure tests demonstrated compatibility with all common NMR solvents. To demonstrate NMR applications of the resin, first commercially available accessories were 3D printed, including magnetic susceptibility plugs and coaxial inserts. Finally, novel accessories that open up new biological and environmental applications were demonstrated. This included a multicompartment holder that, when combined with NMR slice selection techniques, allows the simultaneous study of various samples. Furthermore, salt-tolerant inserts were developed that allowed for NMR to be collected even under the most challenging marine conditions, thus expanding NMR's potential for oceanic research. The effectiveness of the salt-tolerant inserts was demonstrated with the marine organism, Tigriopus californicus. Even in 5 M salt, the full performance of a cryoprobe could be retained using the inserts, whereas using a standard NMR tube, radiofrequency performance was beyond the power handling limits of the probe and 3-fold loss in SNR was seen. In summary, the development and use of "NMR invisible" perfluorinated resins presents an economical, accessible, rapid, and versatile approach for building NMR components allowing new applications and prototyping.
期刊介绍:
Analytical Chemistry, a peer-reviewed research journal, focuses on disseminating new and original knowledge across all branches of analytical chemistry. Fundamental articles may explore general principles of chemical measurement science and need not directly address existing or potential analytical methodology. They can be entirely theoretical or report experimental results. Contributions may cover various phases of analytical operations, including sampling, bioanalysis, electrochemistry, mass spectrometry, microscale and nanoscale systems, environmental analysis, separations, spectroscopy, chemical reactions and selectivity, instrumentation, imaging, surface analysis, and data processing. Papers discussing known analytical methods should present a significant, original application of the method, a notable improvement, or results on an important analyte.