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首页> 外文期刊>Analytica chimica acta >Determination of total phosphorus and nitrogen in turbid waters by oxidation with alkaline potassium peroxodisulfate and low pressure microwave digestion, autoclave heating or the use of closed vessels in a hot water bath: comparison with kjeldahl di
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Determination of total phosphorus and nitrogen in turbid waters by oxidation with alkaline potassium peroxodisulfate and low pressure microwave digestion, autoclave heating or the use of closed vessels in a hot water bath: comparison with kjeldahl di

机译：用碱性过二硫酸钾氧化和低压微波消解，高压釜加热或在热水浴中使用密闭容器测定混浊水中的总磷和氮：与凯氏定氮法比较

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摘要

The evaluation of the use of alkaline peroxodisulfate digestion with low pressure microwave, autoclave or hot water bath heating for the determination of total phosphorus and nitrogen in turbid lake and river waters is described. The efficiency of these digestion procedures were compared to a Kjeldahl digestion procedure with sulphuric acid -potassium sulfate and copper sulfate. The final solution before digestion was 0.045 M in potassium peroxodisulfate and 0.04 M in sodium hydroxide. Procedures were evaluated by the analysis of suspensions of two reference materials, National Institute of Environmental Science, Japan, no. 3 Chlorella and no. 2 pond sediment and natural turbid waters. Best recoveries of phosphorus and nitrogen by microwave heating were obtained when solutions were digested at 95 deg C for 40 min. Quantitative recoveries of phosphorus from Chlorella suspensions up to 1000 mg/l were obtained by all three heating procedures, but incomplete recoveries of nitrogen occurred above 20 mg N/l in the digested sample. Good recoveries of phosphorus and nitrogen from suspended sediment suspensions were obtained only from solutions containing < 150 mg/l of phosphorus from phosphorus compounds containing C-O-P and C-P bonds added to distilled water were quantitative (94-113%) except for polyphosphates (microwave, 34 +- 8; autoclave, 114 +- 6; water bath, 96 +-4) and aluminium phosphate (8-23%). Recoveries of nitrogen compounds containing C-N bonds added to distilled water were quantitative (94-96%). The analysis of a range of natural turbid water samples by alkaline peroxodisulfate and microwave, autoclave and water bath heating gave similar total phosphorus and nitrogen results. All procedures using alkaline peroxodisulfate underestimate phosphorus concentrations at high suspended sediment concentrations (> 150 mg/l) and are only suitable for the analysis of very turbid samples when the turbidity is due to organic matter (algal cells, plant detritus). Underestimation of nitrogen occurs when samples contain more than 20 mg N/l.
机译：描述了在低压微波，高压釜或热水浴加热下使用碱性过二硫酸盐消化法测定混浊的湖泊和河水中总磷和氮的评估。将这些消化过程的效率与使用硫酸-硫酸钾和硫酸铜的凯氏消化过程进行了比较。消化前的最终溶液是在过二硫酸钾中的0.045 M和在氢氧化钠中的0.04M。通过分析两种参考物质（日本国立环境科学研究所，日本，No.4，No.1）的悬浮液来评估程序。 3小球藻，没有。 2池塘沉积物和天然浑浊水域。当溶液在95摄氏度下消化40分钟时，通过微波加热可获得最佳的磷和氮回收率。通过所有三种加热程序，可从小球藻悬浮液中定量回收高达1000 mg / l的磷，但在消化的样品中，高于20 mg N / l时氮的回收率不完全。从悬浮沉淀物悬浮液中磷和氮的良好回收率仅是通过定量添加到蒸馏水中的，含有COP和CP键的磷化合物中含磷<150 mg / l的溶液定量得到的（94-113％），除了多磷酸盐（微波，34 +-8;高压釜114 +-6;水浴96 + -4）和磷酸铝（8-23％）。添加到蒸馏水中的含C-N键的氮化合物的回收率是定量的（94-96％）。用碱性过二硫酸盐和微波，高压釜和水浴加热对一系列天然浑浊水样进行分析，得出总磷和氮的结果相近。所有使用碱性过二硫酸盐的方法都低估了高悬浮沉淀物浓度（> 150 mg / l）中的磷浓度，并且仅适用于当浊度是由于有机物（藻类细胞，植物碎屑）引起的非常浑浊的样品时进行的分析。当样品中的氮含量超过20 mg / l时，会低估氮含量。

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