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胡婧, 刘卫国. 离子交换色层法测定低浓度铵态氮水样的氮同位素研究[J]. 岩矿测试, 2013, 32(3): 495-501.
引用本文: 胡婧, 刘卫国. 离子交换色层法测定低浓度铵态氮水样的氮同位素研究[J]. 岩矿测试, 2013, 32(3): 495-501.
Jing HU, Wei-guo LIU. Determination of Nitrogen Isotope of Water Samples with Low Ammonium Nitrogen by Ion Exchange Method[J]. Rock and Mineral Analysis, 2013, 32(3): 495-501.
Citation: Jing HU, Wei-guo LIU. Determination of Nitrogen Isotope of Water Samples with Low Ammonium Nitrogen by Ion Exchange Method[J]. Rock and Mineral Analysis, 2013, 32(3): 495-501.

离子交换色层法测定低浓度铵态氮水样的氮同位素研究

Determination of Nitrogen Isotope of Water Samples with Low Ammonium Nitrogen by Ion Exchange Method

  • 摘要: 采用氯化铵、氯化钾为原料的离子交换色层法结合扩散法处理低浓度铵态氮水样,测定其铵态氮同位素时,减小全流程空白、避免同位素分馏、获取准确的铵态氮同位素值是需解决的关键问题。本文建立一套尽可能密闭的离子交换系统,避免了在大气环境下低浓度铵态氮水样在离子交换色层预处理过程中的污染;采用蠕动泵过柱的方法,调节蠕动泵的转速控制氯化铵溶液的过柱速率为1.2 L/h,洗脱速率为0.2 L/h,缩短了样品处理时间,减少了空气对铵态氮样品的污染,样品中的NH4+可完全被阳离子交换树脂吸附,铵态氮回收率为93.5%~102.8%,且不会引起氮同位素分馏;将优级纯氯化钾试剂置于450℃马弗炉中灼烧24 h,降低了氯化钾试剂引入的铵态氮污染。建立的方法使全流程的铵态氮空白浓度低于检出限0.02 mg/L,解决了在大气环境下采用离子交换色层法处理低浓度铵态氮水样的污染问题,加速了样品前处理的过程,提高了样品处理效率。

     

    Abstract: When the δ15N-NH4+ in water samples is pretreated by using the ion exchange and diffusion method with NH4Cl and KCl, the key problem is how to reduce the blank, avoid isotopic fractionation and yield accurate isotope results. In this study, a closed ion exchange system was set up to prevent the small amount of NH4+ contamination to the water samples. Furthermore, the sample and elution flow rates of 1.2 L/h and 0.2 L/h respectively were achieved by adjusting the speed of a peristaltic pump. Thus, both the experiment time and the contamination were reduced. In addition, all of the NH4+ in the sample is absorbed on the ion exchange resin and the N recoveries were from 93.5% to 102.8%. Therefore, the whole process will not cause isotopic fractionation. The blank introduced by KCl was reduced by being heated at 450℃ for 24 h. As a result, the blank ion exchange was reduced to below the detection limit of 0.02 mg/L by using the closed ion exchange system. The problem of contamination for water sample pretreatment in air was solved. The process was accelerated and efficiency was improved

     

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