Cross polarization-single pulse/magic angle spinning (CPSP/MAS): A robust technique for routine soil analysis by solid-state NMR

作者: Denis Courtier-Murias , Hashim Farooq , James G. Longstaffe , Brian P. Kelleher , Kris M. Hart

DOI: 10.1016/J.GEODERMA.2014.03.006

关键词:

摘要: Soils are amongst the largest organic carbon reservoirs on earth containing approximately three times contained in all living systems and roughly double amount present atmosphere. Soil matter is central to agriculture, cycling, contaminant sequestration, but due its extreme heterogeneity it challenging study with most modern analytical approaches. As such 13C NMR spectroscopy has emerged as an indispensable technique for characterization of soil solid-state. Single pulse (SP) approaches theoretically provide highest level quantitation matter, however, relative insensitivity, sample analysis can take a prohibitively long time. Consequently, routine studies more sensitive approach cross-polarization under magic angle spinning conditions (CP/MAS) commonly utilized. In particular, CP extremely useful when low content samples compared normally used reveal nature, transformations fate soils. Here, performance novel scheme, which so far not yet been applied soils samples, investigated. The ramp-CPSP scheme adds SP block ramp-CP taking advantage both techniques without extending experimental This method shows enhancements higher than 100% key regions spectra also provides profiles that closer quantitative widely scheme. addition, critical these presented. Even worst case scenario, element little additional signal, result still reflects conventional experiment. be implemented fashion drawback. results shown here suggest replacing sequence solid-state since save considerable time representative spectrum general.

参考文章(44)
Hashim Farooq, Denis Courtier-Murias, Ronald Soong, Hussain Masoom, Werner Maas, Michael Fey, Rajeev Kumar, Martine Monette, Henry Stronks, Myrna J. Simpson, André J. Simpson, Rapid parameter optimization of low signal-to-noise samples in NMR spectroscopy using rapid CPMG pulsing during acquisition: application to recycle delays Magnetic Resonance in Chemistry. ,vol. 51, pp. 129- 135 ,(2013) , 10.1002/MRC.3923
C T De Rosa, H R Pohl, M Williams, A A Ademoyero, C H Chou, D E Jones, Public health implications of environmental exposures. Environmental Health Perspectives. ,vol. 106, pp. 369- 378 ,(1998) , 10.1289/EHP.98106S1369
Hussain Masoom, Denis Courtier-Murias, Hashim Farooq, Ronald Soong, Myrna J. Simpson, Werner Maas, Rajeev Kumar, Martine Monette, Henry Stronks, André J. Simpson, Rapid estimation of nuclear magnetic resonance experiment time in low-concentration environmental samples. Environmental Toxicology and Chemistry. ,vol. 32, pp. 129- 136 ,(2013) , 10.1002/ETC.2028
Diyun Chen, Baoshan Xing, Wenbiao Xie, Sorption of phenanthrene, naphthalene and o-xylene by soil organic matter fractions Geoderma. ,vol. 139, pp. 329- 335 ,(2007) , 10.1016/J.GEODERMA.2007.02.011
Ingrid Kögel-Knabner, Analytical approaches for characterizing soil organic matter Organic Geochemistry. ,vol. 31, pp. 609- 625 ,(2000) , 10.1016/S0146-6380(00)00042-5
Klaus Lorenz, Rattan Lal, Juan J. Jiménez, Characterization of soil organic matter and black carbon in dry tropical forests of Costa Rica Geoderma. ,vol. 158, pp. 315- 321 ,(2010) , 10.1016/J.GEODERMA.2010.05.011
J. M. Oades, J. A. Baldock, M. A. Wilson, A. M. Vassallo, A. G. Waters, X. Peng, Aspects of the chemical structure of soil organic materials as revealed by solid-state 13C NMR spectroscopy Biogeochemistry. ,vol. 16, pp. 1- 42 ,(1992) , 10.1007/BF00024251
Wei-Guo Hu, Jingdong Mao, Baoshan Xing, Klaus Schmidt-Rohr, Poly(methylene) Crystallites in Humic Substances Detected by Nuclear Magnetic Resonance Environmental Science & Technology. ,vol. 34, pp. 530- 534 ,(2000) , 10.1021/ES990506L