基于液相^(31)P核磁共振分析的沉积物样品制备方法研究  

Refining Sample Preparation Procedures for Solution ^(31)P-NMR Analysis of Organic P in Sediment

作　　者：白秀玲[1,2] 周云凯[3] 李斌[2] 丁士明[2] 

机构地区：[1]河南大学资源与环境研究所,开封475004 [2]中国科学院南京地理与湖泊研究所湖泊与环境国家重点实验室,南京210008 [3]河南大学环境与规划学院,开封475004

出　　处：《环境科学》2011年第7期1980-1985,共6页Environmental Science

基　　金：国家自然科学基金项目(40871220;41001319);中国科学院南京地理与湖泊研究所前沿领域项目(CXNIGLAS200811)

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.Solution phosphorus-31 nuclear magnetic resonance spectroscopy （31↑P-NMR） is a novel technology in characterization of organic phosphorus （P） composition in sediments. This study was aim to refine sample preparation procedures for 31↑P-NMR, including determination of sample pretreatment, extraction time, sample to extraetant 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.

关 键 词：有机磷 沉积物 31↑P核磁共振 样品制备 方法 

分 类 号：X132[环境科学与工程—环境科学]