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Nitrite Fixation by Humic Substances

Nitrogen-15 Nuclear Magnetic Resonance Evidence for Potential Intermediates in Chemodenitrification

K.A. Thorna and M.A. Mikitab

a U.S. Geological Survey, Box 25046 M.S. 408, Denver Federal Center, Denver, CO 80225 USA
b Dep. of Chemistry, California State University, Bakersfield, CA 93311 USA




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Fig. 1 Liquid-phase 15N nuclear magnetic resonance (NMR) chemical shifts of nitroso, oxime, and related compounds. Reference 63 (a), References 53 and 64 (b), References 65(c), Reference 35 (d), Reference 51 (e), determined in solid state (f)

 


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Fig. 2 Quantitative liquid phase 13C nuclear magnetic resonance spectra of fulvic acids (FA) and humic acids (HA) recorded in DMSO-d6. LB is line broadening in hertz

 


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Fig. 3 Solid-state CP–MAS 15N nuclear magnetic resonance (NMR) spectra of naturally abundant nitrogens in International Humic Substances Society Pahokee peat fulvic acid (FA), peat humic acid (HA), and peat. LB is line broadening in hertz

 


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Fig. 4 Liquid-phase ACOUSTIC 15N nuclear magnetic resonance (NMR) spectra (nuclear Overhauser enhancement retained) of Suwannee River fulvic acid (SRFA) (a) reacted with 15NH2OH, (b) reacted with Na15NO2 at pH 3, and (c) reacted with Na15NO2 at pH 6

 


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Fig. 5 Liquid phase ACOUSTIC 15N nuclear magnetic resonance (NMR) spectra (nuclear Overhauser enhancement retained) of soil fulvic acids (FA) reacted with Na15NO2. (a) Armadale, pH 3; (b) Laurentian, pH 3; (c) Laurentian, pH 6; (d) Laurentian, dilute, pH 4

 


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Fig. 6 Liquid-phase 15N nuclear magnetic resonance (NMR) spectra of International Humic Substance Society Pahokee peat humic acid (HA) reacted with Na15NO2. Recorded in DMSO-d6. (a) ACOUSTIC spectrum showing quantitative distribution of all nitrogens, (b) DEPT spectrum showing nitrogens directly bonded to protons, (c) DEPT spectrum, nitrogens bonded to one proton in positive phase, nitrogens bonded to two protons inverted

 


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Fig. 7 Solid-state CP/MAS 15N nuclear magnetic resonance (NMR) spectra of International Humic Substance Society Pahokee peat and peat humic acid (HA) reacted with Na15NO2. LB is line broadening in hertz

 


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Fig. 8 Liquid-phase DEPTGL 13C nuclear magnetic resonance (NMR) spectra, showing all protonated carbons, of unreacted and nitrosated International Humic Substance Society soil humic acid (HA). LB is line broadening in hertz

 


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Fig. 9 Liquid-phase ACOUSTIC 15N NMR spectra (NOE retained) of Suwannee River fulvic acid (SRFA) reacted with 15NH4OH and sequentially treated with 15NH4OH and Na14NO2. Nitrosation performed at pH 4.5

 





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