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首页> 外文期刊>Journal of Environmental Quality >Caution Needed in Pretreatment of Sediments for Refining Phosphorus-31 Nuclear Magnetic Resonance Analysis: Results from a Comprehensive Assessment of Pretreatment with Ethylenediaminetetraacetic Acid
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Caution Needed in Pretreatment of Sediments for Refining Phosphorus-31 Nuclear Magnetic Resonance Analysis: Results from a Comprehensive Assessment of Pretreatment with Ethylenediaminetetraacetic Acid

机译：沉积物的预处理需要提纯磷31核磁共振分析的注意事项：乙二胺四乙酸预处理的综合评估结果

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摘要

Pretreatment with chemicals such as ethylenediaminetetraacetic acid (EDTA) is often used to improve the analysis of sediment P with solution P-31 nuclear magnetic resonance spectroscopy (P-31-NMR), but there is a lack of a comprehensive assessment of the methodology. In this study, the effects of EDTA pretreatment on sediment P extracted using a mixture of 0.25 mol L-1 NaOH and 50 mmol L-1 EDTA (NaOH-EDTA) were examined with 45 different sediments. The results showed that EDTA pre-extraction decreased the amount of P extracted by NaOH-EDTA when the concentration ratio of sediment Ca to the sum of sediment Fe and Al [Ca/(Fe+Al), on a wt/vol basis] was lower than 0.4. An increase in total extracted P. coupled with substantial increases in total extracted paramagnetic ions such as Fe and Mn, was observed for another group of sediments with Ca/(Fe+Al) > 0.5, possibly due to the matrix effect. Analysis of 16 representative sediments with P-31-NMR showed that orthophosphate diesters were substantially removed by EDTA pre-extraction for sediments with Ca/(Fe+Al) between 0.4 and 0.7, reflecting a high risk posed by this pretreatment. Phosphorus diversity and concentration of individual P compounds were markedly improved for sediments with Ca/(Fe+Al) > 0.7, suggesting that EDTA pretreatment was particularly useful for P-31-NMR analysis of calcareous sediments. The present study showed that sediment properties played an important role in determining pretreatment effects. Caution is advised when applying pretreatment methods to different sediments.
机译：通常使用诸如乙二胺四乙酸（EDTA）之类的化学品进行预处理，以改进溶液P-31核磁共振波谱（P-31-NMR）对沉积物P的分析，但缺乏对该方法的综合评估。在这项研究中，研究了EDTA预处理对使用0.25 mol L-1 NaOH和50 mmol L-1 EDTA（NaOH-EDTA）混合物提取的沉积物P的影响，并分析了45种不同的沉积物。结果表明，当沉积物Ca与沉积物Fe和Al之和的浓度比[Ca /（Fe + Al），以wt / vol为基准]为ED2时，EDTA预萃取减少了NaOH-EDTA提取的P量。低于0.4。对于另一组Ca /（Fe + Al）> 0.5的沉积物，观察到总提取P.的增加以及总提取顺磁性离子（如Fe和Mn）的大量增加，这可能是由于基质效应所致。用P-31-NMR分析16种代表性沉积物表明，对于Ca /（Fe + Al）在0.4和0.7之间的沉积物，EDTA预萃取可将正磷酸二酯基本除去。这反映了这种预处理带来的高风险。 Ca /（Fe + Al）> 0.7的沉积物的磷多样性和单个P化合物的浓度显着提高，这表明EDTA预处理对于钙质沉积物的P-31-NMR分析特别有用。本研究表明，沉积物的性质在决定预处理效果方面起着重要作用。当对不同的沉积物采用预处理方法时，建议小心。

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