Application of 13C ramp CPMAS NMR with phase-adjusted spinning sidebands (PASS) for the quantitative estimation of carbon functional groups in natural organic matter

详细信息    查看全文

• 作者：Kosuke Ikeya ; Akira Watanabe
• 关键词：Solid ; state 13C NMR ; Phase ; adjusted side band suppressing (PASS) ; Cross polarization/magic angle spinning (CPMAS) ; Direct polarization (DPMAS) ; Carbon functional groups ; Humic substances
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2016
• 出版时间：January 2016
• 年：2016
• 卷：408
• 期：2
• 页码：651-655
• 全文大小：413 KB
• 参考文献：1.Cook RL (2004) Coupling NMR to NOM. Anal Bioanal Chem 378:1484–1503CrossRef
  2.Smernik RJ, Olk DC, Mahieu N (2004) Quantitative solid-state 13C NMR spectroscopy of organic matter fractions in lowland rice soils. Eur J Soil Sci 55:367–379CrossRef
  3.Mao JD, Chen N, Cao X (2011) Characterization of humic substances by advanced solid state NMR spectroscopy: demonstration of a systematic approach. Org Geochem 42:891–902CrossRef
  4.Cook RL, Langford C, Yamdagni R, Preston CM (1996) A modified cross-polarization magic angle spinning 13C NMR procedure for the study of humic materials. Anal Chem 68:3979–3986CrossRef
  5.Berns AE, Conte P (2011) Effect of ramp size and sample spinning speed on CPMAS 13C NMR spectra of soil organic matter. Org Geochem 42:926–935CrossRef
  6.Mets G, Wu X, Smith SO (1994) Ramped-amplitude cross polarization in magic-angle-spinning NMR. J Magn Reson 110:219–227CrossRef
  7.Johnson RL, Schmidt-Rohr K (2014) Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization. J Magn Reson 239:44–49CrossRef
  8.Dixon WT (1982) Spinning-sideband-free and spinning-sideband-only NMR spectra in spinning samples. J Chem Phys 77:1800–1809CrossRef
  9.Antzutkin ON (1999) Sideband manipulation in magic-angle-spinning nuclear magnetic resonance. Prog Nucl Mag Res Sp 35:203–266CrossRef
  10.Antzutkin ON, Shekar SC, Levitt MH (1995) 2-dimensional side-band separation in magic-angle-spinning NMR. J Magn Reson 115:7–19CrossRef
  11.Kuwatsuka S, Watanabe A, Itoh K, Arai S (1992) Comparison of two methods of preparation of humic and fulvic acids, IHSS method and NAGOYA method. Soil Sci Plant Nutr 38:23–30CrossRef
  12.Watanabe A, Itoh K, Arai S, Kuwatsuka S (1994) Comparison of the composition of humic and fulvic acids prepared by the IHSS method and NAGOYA method. Soil Sci Plant Nutr 40:601–608CrossRef
  13.Watanabe A, Maie N, Hepburn A, McPhail D, Abe T, Ikeya K, Ishida Y, Ohtani H (2004) Chemical characterization of Japanese Humic Substances Society standard soil humic and fulvic acids by spectroscopic and degradative analyses. Humic Sub Res 1:18–28
  14.Mao JD, Hu WG, Schmidt-Rohr K, Davies G, Ghabbour EA, Xing B (2000) Quantitative characterization of humic substances by solid-state carbon-13 nuclear magnetic resonance. Soil Sci Soc Am J 64:873–884CrossRef
  15.Monteil-Rivera F, Brouwer EB, Masset S, Deslandes Y, Dumonceau J (2000) Combination of X-ray photoelectron and solid-state 13C nuclear magnetic resonance spectroscopy in the structural characterisation of humic acids. Anal Chim Acta 424:243–255CrossRef
  
• 作者单位：Kosuke Ikeya (1) (2)
  Akira Watanabe (1)
  
  1. Graduate School of Bioagricultural Sciences, Nagoya University, Chikusa, Nagoya, 464-8601, Japan
  2. Graduate School of Environmental Studies, Nagoya University, Chikusa, Nagoya, 464-8601, Japan
  
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Food Science
  Inorganic Chemistry
  Physical Chemistry
  Monitoring, Environmental Analysis and Environmental Ecotoxicology
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1618-2650

文摘

The composition of carbon (C) functional groups in natural organic matter (NOM), such as dissolved organic matter, soil organic matter, and humic substances, is frequently estimated using solid-state 13C NMR techniques. A problem associated with quantitative analysis using general cross polarization/magic angle spinning (CPMAS) spectra is the appearance of spinning side bands (SSBs) split from the original center peaks of sp 2 hybridized C species (i.e., aromatic and carbonyl C). Ramp CP/phase-adjusted side band suppressing (PASS) is a pulse sequence that integrates SSBs separately and quantitatively recovers them into their inherent center peaks. In the present study, the applicability of ramp CP/PASS to NOM analysis was compared with direct polarization (DPMAS), another quantitative method but one that requires a long operation time, and/or a ramp CP/total suppression side band (ramp CP/TOSS) technique, a popular but non-quantitative method for deleting SSBs. The test materials were six soil humic acid samples with various known degrees of aromaticity and two fulvic acids. There were no significant differences in the relative abundance of alkyl C, O-alkyl C, and aromatic C between the ramp CP/PASS and DPMAS methods, while the signal intensities corresponding to aromatic C in the ramp CP/TOSS spectra were consistently less than the values obtained in the ramp CP/PASS spectra. These results indicate that ramp CP/PASS can be used to accurately estimate the C composition of NOM samples. Keywords Solid-state 13C NMR Phase-adjusted side band suppressing (PASS) Cross polarization/magic angle spinning (CPMAS) Direct polarization (DPMAS) Carbon functional groups Humic substances