Determination of Ammonium Nitrogen and Nitrate Nitrogen in Soil by Gas Phase Molecular Absorption Spectrometry
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摘要:
通过测定土壤中铵态氮和硝态氮的含量，能够为农业领域土壤精准施肥和土壤的环境保护提供重要参考。目前基于分光光度法的土壤中铵态氮和硝态氮的分析方法容易受到提取试液颜色、浑浊度、其他共存离子等干扰不能直接测定，必须进行脱色等前处理操作，费时耗力。因此，本文建立了一次性同时浸提，不经脱色处理，采用气相分子吸收光谱法测定农田土壤中铵态氮和硝态氮含量的方法。利用该方法测定农田土壤中铵态氮和硝态氮，避免了繁琐的显色反应过程，一个批次样品(50个)的分析流程仅需5h。在0.10~2.00mg/L (铵态氮)和0.20~4.00mg/L (硝态氮)浓度范围内，工作曲线线性良好；方法检出限分别为0.013mg/kg及0.002mg/kg；相对标准偏差(RSD) < 1%；加标回收率为96.3%~100.7%。较之基于传统分光光度法的国家标准方法，本方法在检出限、精密度和回收率等指标方面均有显著改善，能够满足农田土壤中铵态氮和硝态氮的批量精准分析需求。
Abstract:BACKGROUND Determination of ammonium nitrogen and nitrate nitrogen in soil makes great sense for indication of the nutrient status and environment evaluation of soil. The standard methods based on spectrophotometry are susceptible to interference from the color of the extraction test solution, turbidity, and other coexisting ions. Moreover, those methods are time-consuming due to the demand of decoloration.
OBJECTIVES To establish a convenient and high sensitivity method for the determination of ammonium nitrogen and nitrate nitrogen in soil, based on simultaneous extraction.
METHODS Ammonium nitrogen and nitrate nitrogen in soil were simultaneously extracted with KCl solution without decoloration, and determined by gas phase molecular absorption spectrometry.
RESULTS 50 samples were determined within 5h due to the avoidance of the color reaction process. The dynamic linear ranges of ammonium nitrogen and nitrate nitrogen were 0.10-2.00mg/L and 0.20-4.00mg/L, respectively. The detection limits were 0.013mg/kg and 0.002mg/kg, respectively. The recoveries ranged from 96.3% to 100.7%, and the relative standard deviation was below 1%.
CONCLUSIONS Compared with the national standard method based on traditional spectrophotometry, this method has significantly improved the detection limit, precision and recovery. The method can be widely used in the field of detection of ammonium nitrogen and nitrate nitrogen in farmland soil.
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表 1 铵态氮和硝态氮空白样品测定结果
Table 1. Analytical results of ammonium nitrogen and nitrate nitrogen in blank samples
测定次数
(n=7)铵态氮空白样品 硝态氮空白样品 吸光度 铵态氮测定值
(mg/kg)吸光度 硝态氮测定值
(mg/kg)1 0.0042 0.066 0.0046 0.070 2 0.0047 0.072 0.0047 0.071 3 0.0041 0.065 0.0047 0.071 4 0.0042 0.066 0.0045 0.069 5 0.0050 0.075 0.0046 0.070 6 0.0045 0.069 0.0047 0.071 7 0.0050 0.075 0.0047 0.071 
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表 2 土壤样品中铵态氮和硝态氮精密度测试结果
Table 2. Precision tests of the method for ammonium nitrogen and nitrate nitrogen in soil samples
检测
项目样品编号 7次平行测定值
(mg/kg)平均值
(mg/kg)RSD
(%)铵态氮 BYHT-1 0.881 0.881 0.876 0.881 0.886 0.881 0.882 0.881 0.32 BYHT-2 1.41 1.39 1.39 1.40 1.40 1.41 1.40 1.40 0.60 硝态氮 BYHT-1 4.43 4.44 4.43 4.43 4.43 4.44 4.44 4.43 0.06 BYHT-2 4.06 4.07 4.08 4.06 4.08 4.09 4.05 4.07 0.37
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表 3 土壤中铵态氮和硝态氮测定加标回收实验结果
Table 3. Spiked recovery tests of the method for ammonium nitrogen and nitrate nitrogen in soil samples
检测
项目样品编号 本底值
(mg/kg)加标量
(mg/kg)7次检测平均值
(mg/kg)回收量
(mg/kg)回收率
(%)铵态氮 BYHT-1 0.88 1.00 1.863±0.033 0.983 98.3 2.00 2.864±0.112 1.984 99.2 BYHT-2 1.40 2.00 3.325±0.105 1.925 96.3 4.00 5.397±0.230 3.997 99.9 硝态氮 BYHT-1 4.43 5.00 9.35±0.13 4.92 98.5 10.00 14.515±0.3210 10.07 100.7 BYHT-2 4.07 5.00 8.99±0.228 4.92 98.5 10.00 14.12+0.312 10.05 100.5
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