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On the Use of Hydrofluoric Acid Pretreatment of Soils for Phosphorus-31 Nuclear Magnetic Resonance Analyses

机译：用氢氟酸预处理土壤进行磷31核磁共振分析

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Solid-state 31P nuclear magnetic resonance (NMR) has the potential to be used for investigating soil P forms without the need for extractions or pretreatment. Solid-state spectra typically suffer from poor resolution and low observability, however, in part due to interferences by paramagnetic species present in soil. Hydrofluoric acid treatment is routinely used in 13C and 15N NMR analysis of soil organic matter to remove these paramagnetic species and improve NMR spectra. We evaluated the use of HF pretreatment to improve 31P NMR spectra of four pasture soils. Hydrofluoric acid treatment of soils for 24 h resulted in almost complete removal of inorganic P (>90%), but also resulted in the loss of organic P (up to 49%). Mass-balance calculations revealed that much of the organic P removed was hydrolyzed. In contrast, most model organic P compounds were found to be resistant to acid-mediated hydrolysis. Little (<4%) of the P contained in phytic acid, ß-D-glucose phosphate, or DNA was hydrolyzed by HF in 24 h, although 29% of P in adenosine triphosphate was hydrolyzed. The observability of P (Pobs) by solid-state 31P NMR increased on HF treatment, but was still generally poor. Attempts to analyze the HF extracts by solution 31P NMR were unsuccessful due to the presence of high concentrations of paramagnetics. Comparison of solution 31P NMR spectra of NaOH–EDTA extracts of the soils before and after HF treatment indicated that specific organic P compounds, in particular inositol phosphates, were removed by HF. In this regard, HF treatment may have a role in the separation or fractionation of different organic P forms.
机译：固态 31 P核磁共振（NMR）具有 的潜力，可用于研究土壤P形式，而无需进行 提取或预处理。固态光谱通常因分辨率低和可观察性差而受到损害，但是部分受到土壤中顺磁性物质的干扰。 氢氟酸在土壤中有机物的 13 C和 15 N NMR分析中通常使用这种方法去除这些顺磁性 物种和改善NMR光谱。我们评估了使用HF 预处理来改善四种牧场土壤的 31 P NMR谱图。 氢氟酸处理土壤24小时几乎导致 完全去除了无机P（> 90％），但也导致了 有机P的损失（高达49％）。质量平衡计算 表明大部分被去除的有机磷都被水解了。 相反，大多数模型有机磷化合物被发现 酸介导的水解。植酸，ß-D-磷酸葡萄糖， 或DNA中所含的 P很少（<4％）在24小时内被HF水解，尽管P的29％在三磷酸腺苷中被水解。 固态 31 P NMR对P（P obs ）的可观察性在HF处理时有所提高，但仍为 普遍较差。由于存在高浓度的顺磁性物质，未能通过溶液 31 P NMR分析HF提取物的尝试未能成功。 HF处理前后土壤中 NaOH-EDTA提取物的溶液 31 P NMR光谱比较表明，特定的有机P化合物，特别是HF清除了肌醇 磷酸盐。在这方面，HF处理 可能在不同的 有机P形式的分离或分馏中起作用。

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  • 来源
    《Soil Science Society of America Journal》 |2007年第4期|1111-1118|共8页
  • 作者

    Warwick J. Dougherty; Ronald J. Smernik; Else K. Bünemann; David J. Chittleborough;

  • 作者单位

    Soil and Land Systems, School of Earth and Environmental Sciences, Univ. of Adelaide, South Australia 5064, Australia;

    Soil and Land Systems, School of Earth and Environmental Sciences, Univ. of Adelaide, South Australia 5064, Australia;

    Soil and Land Systems, School of Earth and Environmental Sciences, Univ. of Adelaide, South Australia 5064, Australia;

    Soil and Land Systems, School of Earth and Environmental Sciences, Univ. of Adelaide, South Australia 5064, Australia;

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