氯化铵浸提-电感耦合等离子体发射光谱法测定土壤交换性和易还原性锰

Determination of Exchangeable and Reducible Manganese in Soil by ICP-OES with Ammonium Chloride Extraction

  • 摘要: 锰是植物必需且重要的矿物元素。土壤中有效态锰的含量对植物生长具有重要意义。交换性锰(ExMn)和易还原性锰(RMn)是土壤中有效态锰中最主要的两种形式,建立准确快速检测土壤中交换性锰和易还原性锰的方法,对于土壤锰的有效性评价具有重要意义。本文利用氯化铵浸提土壤交换性锰,氯化铵-对苯二酚和抗坏血酸(1∶2,m/m)浸提易还原性锰,在浸提过程中利用氯化铵代替乙酸铵,既可以抑制石灰性土壤中碳酸盐结合态锰的析出,又可以有效地浸提土壤中交换性锰和易还原性锰,利用超声提取代替振荡提取,将浸提时间由30min缩短为5min。通过电感耦合等离子体发射光谱法(ICP-OES)直接测定溶液中的交换性锰含量,差减法获得易还原性锰含量。在检测过程中,通过仪器条件优化,选择谱线为257.61nm,获得方法检出限为0.13mg/kg。采用本方法检测交换性锰,测定结果的相对标准偏差(RSD)为0.4%~3.3%,而火焰原子吸收光谱法(FAAS) RSD为2.1%~6.9%,比色法RSD为3.6%~9.8%;检测易还原性锰时,本方法RSD为0.7%~3.6%,FAAS法RSD为0.9%~5.3%,比色法RSD为1.1%~9.2%,表明采用本文建立的ICP-OES法可以同时测定土壤样品中的交换性锰和易还原性锰,具有较高的精密度。

     

    Abstract: Manganese is an essential and important mineral element for plants. The content of available manganese in soil is very beneficial to plant growth. Exchangeable manganese (ExMn) and reducible manganese (RMn) are the two most important forms of available manganese in soil. Establishing an accurate and rapid method for detecting ExMn and RMn in soil is of great significance for the evaluation of manganese availability in soil. In this paper, ammonium chloride was used to extract ExMn from soil, and ammonium chloride-hydroquinone and ascorbic acid (1:2, m:m) were used to extract RMn. Ammonium chloride was used instead of ammonium acetate in the extraction process, which not only inhibited the precipitation of carbonate-bound manganese in calcareous soil but also effectively extracted ExMn and RMn from soil. Ultrasonic extraction was used instead of shaking extraction, reducing the extraction time from 30 minutes to 5 minutes. The content of ExMn in the solution was directly determined by inductively coupled plasma-optical emission spectrometry (ICP-OES), and the content of RMn was obtained by the difference method. During the detection process, the instrument conditions were optimized, and the spectral line of 257.61nm was selected, with a detection limit of 0.13mg/kg. By using this method (ICP-OES) to detect ExMn, the relative standard deviation (RSD) of the determination results was 0.4%-3.3%, while the RSD of the AAS method was 2.1%-6.9% and that of the colorimetric method was 3.6%-9.8%. When detecting RMn, the RSD of this method was 0.7%-3.6%, that of the AAS method was 0.9%-5.3%, and that of the colorimetric method was 1.1%-9.2%. It indicates that the ICP-OES method established in this paper can simultaneously determine ExMn and RMn in soil samples, and has high precision.

     

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