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王玉功, 王华, 刘建军, 余志峰. 沙棘树干茎流液中总氮总磷联合消解的测定方法[J]. 岩矿测试, 2014, 33(5): 665-669.
引用本文: 王玉功, 王华, 刘建军, 余志峰. 沙棘树干茎流液中总氮总磷联合消解的测定方法[J]. 岩矿测试, 2014, 33(5): 665-669.
Yu-gong WANG, Hua WANG, Jian-jun LIU, Zhi-feng YU. Determination Method on Total Nitrogen and Total Phosphorus in Sea-buckthorn Stem Flow Liquid with Combined Digestion[J]. Rock and Mineral Analysis, 2014, 33(5): 665-669.
Citation: Yu-gong WANG, Hua WANG, Jian-jun LIU, Zhi-feng YU. Determination Method on Total Nitrogen and Total Phosphorus in Sea-buckthorn Stem Flow Liquid with Combined Digestion[J]. Rock and Mineral Analysis, 2014, 33(5): 665-669.

沙棘树干茎流液中总氮总磷联合消解的测定方法

Determination Method on Total Nitrogen and Total Phosphorus in Sea-buckthorn Stem Flow Liquid with Combined Digestion

  • 摘要: 对于总氮和总磷的测定,国家标准HJ 636—2012和GB 11893—89规定总氮用碱性过硫酸钾消解,紫外分光光度法测定,总磷用中性过硫酸钾消解,分光光度法测定,两种方法分别取样、消解,分析效率低。本文对国家标准方法进行改进,建立了在一份样品中用过硫酸钾作为氧化剂一次消解,分光光度法联合测定树干茎流液中总氮、总磷含量的方法。样品中的含氮化合物在碱性过硫酸钾溶液中,在高温下氧化分解转化为硝酸盐氮(NO3--N),其吸光度与总氮浓度成正比;含磷化合物在酸性过硫酸钾溶液中,在高温下氧化分解转化成正磷酸盐(PO43--P),其吸光度与正磷酸盐浓度成正比。经实际样品验证,方法精密度(RSD,n=5)为总氮 < 2%,总磷 < 4%,加标回收率为98.0%~104.2%(总氮)和94.0%~107.0%(总磷)。本方法将国家标准方法中配制两条标准系列、两次高压消解改进为配制一条标准系列、一次消解,可以节省50%的样品使用量,且提高了分析效率。由于有机质含量较高时,在本法条件下样品不易消解清亮,影响总氮、总磷的测定,该方法适用于有机质含量较低的树干茎流样品分析。

     

    Abstract: National Standards HJ 636-2012 and GB 11893-89 illustrated that total nitrogen (TN) is digested with alkaline potassium persulfate and then determined using ultraviolet spectrophotometry and that total phosphorus (TP) is digested with neutral potassium persulfate and then determined using spectrophotometry. However, the analysis efficiency is low due to individual sampling and digestion for TN and TP. Based on national standard methods, a modified and effective method to respectively determine the contents of TN and total TP in one sample from trunk stem flow liquid, which would be digested once using potassium persulfate as the oxidant combined with spectrophotometry is focused on, and reported here. The results indicated that nitrogenous compounds from the sample in the alkaline potassium persulfate solution would be oxidized and decomposed into the form of NO3--N, whose absorbance is proportional to the concentration of TN under high temperature. Phosphorous compounds from the sample in the acidic potassium persulfate solution were oxidized and decomposed into the form of PO43--P, whose absorbance was proportional to the concentration of TP under high temperature. The precision (RSD, n=5) of this method for determination of the actual samples is TN < 2% and TP < 4%. The standard addition recovery rates of TN and TP are 98.0%-104.2% and 94.0%-107.0%, respectively. Therefore, two standard series and high pressure digestion twice, which were needed in the national standard methods, were modified to only one standard series and high pressure digestion once saving 50% of the sample amount and enhancing the analytical efficiency. This modified determination was proved to be effective in the analysis of samples with low contents of organic matter from stem flow liquid, due to the difficulty of digestion and interference of determination of TN and TP in those samples with high contents of organic matters under the before mentioned conditions.

     

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