| 基于液相31P核磁共振分析的沉积物样品制备方法研究 |
| 摘要点击 2927 全文点击 2077 投稿时间：2010-08-14 修订日期：2010-10-15 |
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| 中文关键词 有机磷 沉积物 31P核磁共振 样品制备 方法 |
| 英文关键词 organic phosphorus sediment phosphorus-31 nuclear magnetic resonance spectroscopy (31P-NMR) sample preparation method |
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| 中文摘要 |
| 液相31P核磁共振（phosphorus-31 nuclear magnetic resonance,31P-NMR）是近年来用于分析沉积物有机磷组成的新技术.本研究围绕31P-NMR分析沉积物样品的制备过程（包括样品前处理方法、提取时间、提取剂比例、样品浓缩等）进行探讨.结果表明，采用风干的沉积物样品进行提取，磷的提取效率明显提高.提取过程中，沉积物磷的释放主要在前8 h，为提高磷的提取效率，可将提取时间延长至12 ～16 h.提取比例［m(沉积物)∶V(提取剂）］1∶8与1∶20相比，在浓缩倍数相同的情况下，前者获得的31P-NMR信号峰多于后者，因此提取比例倾向于使用1∶8.提取液样品在28℃下旋转蒸发浓缩，并经低温离心后，磷无显著损失. |
| 英文摘要 |
| Solution phosphorus-31 nuclear magnetic resonance spectroscopy (31P-NMR) is a novel technology in characterization of organic phosphorus (P) composition in sediments. This study was aim to refine sample preparation procedures for 31P-NMR, including determination of sample pretreatment, extraction time, sample to extractant ratio and concentration method. The results showed that recovery of P with air dried sample treatment was higher than that for the fresh samples. Most of the P was extracted within the first 8 hours, and the time could extend to 12 to 16 hours in order to improve the recovery of P. Using the extraction ratio ［m(sediment)∶V(extractant)］ of 1∶8 received more spectral signals compared to 1∶20 when both the extracts were concentrated at the same time. No evident loss of P was found when the extract was concentrated at 28℃ followed by centrifugation under low temperature. |
