以太湖沉积物为研究对象,采用钼酸铵比色方法与液相31P-核磁共振技术(31P-NMR),研究不同浓度NaOH及NaOH与EDTA不同配比(NaOH-EDTA)对沉积物有机磷的提取及31P-NMR组成分析的影响.结果表明:不同浓度NaOH或不同配比的NaOH-EDTA,其提取沉积物总磷和有机磷量均随溶液pH值的增加而增加;在强碱和EDTA螯合沉积物金属离子的双重作用下,NaOH-EDTA提取效率明显高于NaOH,但EDTA螯合作用也使溶液中金属离子含量明显增加,在一定程度上会干扰核磁共振波谱,使得部分峰出现重叠,但局部重叠可采取一定的措施予以消除.在综合考虑EDTA螯合作用及溶液pH值对沉积物有机磷提取影响的基础上,0.25mol·L-1NaOH-50 mmol·L-1EDTA是沉积物有机磷提取剂的最佳选择.
Procedures for chemical extraction of organic phosphorus(OP) from sediments of Taihu Lake were optimized using solution 31P nuclear magnetic resonance spectroscopy(31P-NMR).The results showed that the extraction efficiencies for total phosphorus and OP increased with pH when NaOH and EDTA were used as solutes.The extraction efficiency of NaOH-EDTA was significantly higher than that of NaOH alone.The mixture of 0.25 mol · L-1 NaOH and 50 mmol · L-1 EDTA was the best extractant for OP extraction,as evidenced by the 31P-NMR spectrum.The release of sediment-bound OP in chemical extraction could be attributed to the double effects of OH-competition under strong alkaline conditions and EDTA chelation for metal ions.It should be noticed that the chelation of metal ions with EDTA simultaneously increased the extraction of magnetic ions(such as Fe3+ and Mn2+) from sediment,which may result in interferences,such as peak overlap on the 31P-NMR spectrum.