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Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies. / Hodgetts, Rebecca Y.; Kiryutin, Alexey S.; Nichols, Peter et al.

In: ACS Energy Letters, Vol. 5, No. 3, 13.03.2020, p. 736-741.

Research output: Contribution to journal › Article › peer-review

Harvard

Hodgetts, RY, Kiryutin, AS, Nichols, P, Du, HL, Bakker, JM, MacFarlane, DR & Simonov, AN 2020, 'Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies', ACS Energy Letters, vol. 5, no. 3, pp. 736-741. https://doi.org/10.1021/acsenergylett.9b02812

APA

Hodgetts, R. Y., Kiryutin, A. S., Nichols, P., Du, H. L., Bakker, J. M., MacFarlane, D. R., & Simonov, A. N. (2020). Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies. ACS Energy Letters, 5(3), 736-741. https://doi.org/10.1021/acsenergylett.9b02812

Vancouver

Hodgetts RY, Kiryutin AS, Nichols P, Du HL, Bakker JM, MacFarlane DR et al. Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies. ACS Energy Letters. 2020 Mar 13;5(3):736-741. doi: 10.1021/acsenergylett.9b02812

Author

Hodgetts, Rebecca Y. ; Kiryutin, Alexey S. ; Nichols, Peter et al. / Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies. In: ACS Energy Letters. 2020 ; Vol. 5, No. 3. pp. 736-741.

BibTeX

@article{7b7e764ca50e4b0d8eece3cd0d821063,
title = "Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies",
abstract = "As research on sustainable ammonia synthesis via electrochemical and photochemical N2 reduction progresses to include a wider variety of aqueous and aprotic electrolytes, 1H NMR spectroscopy is increasingly adopted as a means for ammonium quantification. However, this method is highly sensitive to experimental parameters, as demonstrated herein using a highly versatile and robust NMR pulse program. We demonstrate the sensitivity of the measurement to the final pH of the analyzed solution and identify a [H+] concentration range enabling robust quantification. We compare direct quantification versus calibration approaches to show that the former is highly sensitive to spin relaxation effects and identify the latter as the most reliable approach. This method, when optimized, enables direct, rapid quantification of both 14NH4 + and 15NH4 + within 12-22 min. The limit of detection of 5-10 μM, depending on the solvent, which meets the needs of current electrochemical and photochemical N2 reduction research.",
keywords = "NITROGEN REDUCTION, BERTHELOT REACTION, SALICYLATE, CATALYSTS, ELECTROREDUCTION, TEMPERATURE, CHEMISTRY, PRESSURE, SODIUM, N-15",
author = "Hodgetts, {Rebecca Y.} and Kiryutin, {Alexey S.} and Peter Nichols and Du, {Hoang Long} and Bakker, {Jacinta M.} and MacFarlane, {Douglas R.} and Simonov, {Alexandr N.}",
note = "Publisher Copyright: {\textcopyright} 2020 American Chemical Society.",
year = "2020",
month = mar,
day = "13",
doi = "10.1021/acsenergylett.9b02812",
language = "English",
volume = "5",
pages = "736--741",
journal = "ACS Energy Letters",
issn = "2380-8195",
publisher = "ACS Publication",
number = "3",

}

RIS

TY - JOUR

T1 - Refining Universal Procedures for Ammonium Quantification via Rapid 1H NMR Analysis for Dinitrogen Reduction Studies

AU - Hodgetts, Rebecca Y.

AU - Kiryutin, Alexey S.

AU - Nichols, Peter

AU - Du, Hoang Long

AU - Bakker, Jacinta M.

AU - MacFarlane, Douglas R.

AU - Simonov, Alexandr N.

N1 - Publisher Copyright: © 2020 American Chemical Society.

PY - 2020/3/13

Y1 - 2020/3/13

N2 - As research on sustainable ammonia synthesis via electrochemical and photochemical N2 reduction progresses to include a wider variety of aqueous and aprotic electrolytes, 1H NMR spectroscopy is increasingly adopted as a means for ammonium quantification. However, this method is highly sensitive to experimental parameters, as demonstrated herein using a highly versatile and robust NMR pulse program. We demonstrate the sensitivity of the measurement to the final pH of the analyzed solution and identify a [H+] concentration range enabling robust quantification. We compare direct quantification versus calibration approaches to show that the former is highly sensitive to spin relaxation effects and identify the latter as the most reliable approach. This method, when optimized, enables direct, rapid quantification of both 14NH4 + and 15NH4 + within 12-22 min. The limit of detection of 5-10 μM, depending on the solvent, which meets the needs of current electrochemical and photochemical N2 reduction research.

AB - As research on sustainable ammonia synthesis via electrochemical and photochemical N2 reduction progresses to include a wider variety of aqueous and aprotic electrolytes, 1H NMR spectroscopy is increasingly adopted as a means for ammonium quantification. However, this method is highly sensitive to experimental parameters, as demonstrated herein using a highly versatile and robust NMR pulse program. We demonstrate the sensitivity of the measurement to the final pH of the analyzed solution and identify a [H+] concentration range enabling robust quantification. We compare direct quantification versus calibration approaches to show that the former is highly sensitive to spin relaxation effects and identify the latter as the most reliable approach. This method, when optimized, enables direct, rapid quantification of both 14NH4 + and 15NH4 + within 12-22 min. The limit of detection of 5-10 μM, depending on the solvent, which meets the needs of current electrochemical and photochemical N2 reduction research.

KW - NITROGEN REDUCTION

KW - BERTHELOT REACTION

KW - SALICYLATE

KW - CATALYSTS

KW - ELECTROREDUCTION

KW - TEMPERATURE

KW - CHEMISTRY

KW - PRESSURE

KW - SODIUM

KW - N-15

UR - http://www.scopus.com/inward/record.url?scp=85082394087&partnerID=8YFLogxK

U2 - 10.1021/acsenergylett.9b02812

DO - 10.1021/acsenergylett.9b02812

M3 - Article

AN - SCOPUS:85082394087

VL - 5

SP - 736

EP - 741

JO - ACS Energy Letters

JF - ACS Energy Letters

SN - 2380-8195

IS - 3

ER -

ID: 23892590