联合消解测定海水底泥中全氮、全磷含量.docVIP

联合消解测定海水底泥中全氮、全磷含量摘 要：通过硫酸-过氧化氢联合消解，分别使用自动定氮仪和紫外分光光度计测定海水底泥中全氮、全磷的含量，建立了一种海水底泥中全氮、全磷的测定方法。并对硫酸和过氧化氢的用量进行了研究。结果表明，硫酸用量对结果无明显影响，而过氧化氢有显著影响，加入8 mL硫酸和1 mL过氧化氢较为适宜。同时进行了方法学试验，其中全氮及全磷的重复性（RSD）分别为2.54%~5.06%和4.87 %~8.99 %；回收率分别为95.7 %~98.4 %和96.3 %~100.5 %。该方法重复性好，准确度高，简便快捷，适合于大批量样品测定 关键词：海水底泥；消解；测定；全氮；全磷 中图分类号：X522 文献标识码：A DOI编码：10.3969/j.issn.1006－6500.2011.06.013 Determination of Total Nitrogen and Total Phosphorus of Marine Sediment by Sulfuric Acid - Hydrogen Peroxide Digest LIU Ye-tong,CHEN Qiu-sheng,ZHANG Qiang, MENG Zhao-fang (Central Laboratory of Tianjin Academy of Agricultural Sciences,Tianjin 300381，China) Ａｂｓｔｒａｃｔ: A method of measuring total nitrogen and total phosphorus of marine sediment was established through digesting by sulfuric acid - hydrogen peroxide and determined by automatic nitrogen analyzer and UV spectrophotometer, respectively.The influence of the amount of sulfuric acid and hydrogen peroxide was analyzed. The results indicated that the amount of sulfuric acid had no effect on measuring, but hydrogen peroxide had effect significantly. The optional conditions were as follows: 8 mL of sulfuric acid and 1 mL of hydrogen peroxide. The RSD of total nitrogen and total phosphorus were 2.54%~5.06% and 4.87%~8.99%, respectively. The recoveries of total nitrogen and total phosphorus were 95.7% ~ 98.4% and 96.3%~100.5%, respectively. Key words: marine sediment;digestion;measure;total nitrogen; total phosphorus 随着世界经济高速发展，人类制造的大量污染物排放到海水中并逐渐在底泥中富集，使底泥受到不同程度的污染[1]。其中氮和磷是水生生态系统的重要要素，过量输入会导致水体富营养化，引发赤潮，而近岸水体中的营养物质有很大一部分来源于沉积物与上覆水之间的物质交换，沉积物―水界面间的营养元素交换和扩散对上覆水体水质（富营养化）具有重要的影响[2-5]。底泥中有机物分解出的营养物质在海岸动力因素（波浪、潮流）作用下也会季节性地扩散到上层水体中，使水体发生富营养化。研究底泥中氮和磷的含量，对海水富营养化和赤潮的研究具有重要意义[6-8]。目前，中国尚没有颁布测定海水底泥全氮、全磷含量方法的国家标准，国内外针对污泥全氮、全磷测定方法的研究，主要借用土壤、水质中总氮、总磷的测定方法[9-10]。由于污泥与土壤的形成机理、条件及组分构成等各不相同，在测定污泥全氮、全磷时完全按照土壤、水质测定方法不恰当。本研究结合有机肥的行业标准设计了海水底泥中全氮、全磷的测定方法[11]，并进行了方法验证，为今后的研究工作奠定基础 1 材料和方法 1.1 仪器及试剂 仪器：自动定氮仪、紫外分光光度计 试剂：硫酸（分析纯）、30%过氧化氢（分析纯）、2%硼酸吸收液、定氮