电感耦合等离子体发射光谱法同时测定土壤样品中的硼、磷、钠、钾的方法研究

Study on Simultaneous Determination of Boron, Phosphorus, Sodium and Potassium in Soil Samples by Inductively Coupled Plasma Optical Emission Spectrometry

  • 摘要: 土壤样品中的硼元素在酸溶体系中易挥发,采用碱熔法则无法同时测定钾、钠,并且大量的盐类也不利于检测. 而在盐酸-氢氟酸-硝酸三酸体系中,通过加入甘露醇可以保护硼在密闭消解条件下不易挥发损失. 以电感耦合等离子体发射光谱法(ICP-OES)为测试手段,使用耐氢氟酸进样系统,可以有效避免待测元素受到污染,通过预加内标的方法来纠正体积偏差后,可以实现对土壤样品中硼、磷、钠、钾元素的同时测定. 试验结果表明,在没有加稳定剂时,硼在消解过程中会因挥发而损失严重,但在有稳定剂的存在下,即使在160 ℃以上,硼也没有检测到挥发损失,证明采用甘露醇作为稳定剂是可行的. 通过有证土壤和水系沉积物标准样品的测试验证,对于硼质量分数高于10 mg/kg的土壤样品,其测试结果与认定值相对偏差小于10%,具有很好的灵敏度且操作简单,易用于大批量的检测任务.

     

    Abstract: The boron in soil samples is volatile in the acid soluble system, and potassium and sodium cannot be determined simultaneously by the alkali fusion method, the interference of salts also hinders detection. In the HCl-HF-HNO3 tri-acid system, the addition of mannitol can protect boron from volatilization loss under sealed digestion conditions. Using inductively coupled plasma emission spectrometry (ICP-OES) as the testing method, and employing a hydrofluoric acid-resistant sampling system, contamination of the elements to be tested was effectively prevented. By pre-adding an internal standard to correct volume deviations, the simultaneous determination of boron, phosphorus, sodium and potassium in soil samples can be achieved. The experimental results indicated that in the absence of a stabilizer, boron suffers severely loss due to volatilization during digestion. However, in the presence of a stabilizer, no measurable volatilization loss of boron was observed even above 160 ℃, proving that the use of mannitol as a stabilizer was feasible. By testing and verifying with certified soil and aquatic sediment standard samples, the relative deviation of test results from the recommended values was less than 10% for soil samples with boron content higher than 10 mg/kg. The method has a good sensitivity, simple operation, and can be suitable for large-scale testing tasks.

     

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