首页|优化次溴酸盐-叠氮化钠化学法测定海水中铵态氮同位素

优化次溴酸盐-叠氮化钠化学法测定海水中铵态氮同位素

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利用次溴酸盐将海水样品中的NH4+氧化为NO2-并与叠氮化钠反应转化为N2O,测试其氮同位素组成,探讨转化过程中试剂添加量、NH4+浓度、溶解有机氮(DON)含量及高浓度样品稀释对测试结果的影响,确定最佳实验条件,同时绘制不同丰度铵态氮同位素标样校准曲线。结果表明,在最佳反应条件下,NH4+浓度范围在 5~50 μmol/L之间,其NH4+-N2O转化率均在 92%以上,且水样中DON含量对NH4+-N2O转化率和δ15Nair值准确度无显著影响。4种丰度铵态氮同位素标样校准曲线斜率为 0。465,相关系数R2 为 0。999,相关性良好。铵态氮同位素标样δ15Nair值标准偏差为 0。35‰(n=5),测量值与参考值的差值为 0。26‰,精密度与准确度符合环境样品测试要求。5个海水样品铵态氮δ15Nair值范围为 11。46‰~22。31‰,标准偏差在0。20‰~0。62‰(n=5)之间。
The Optimization of Hypobromite Oxidation Combined with Sodium Azide Chemical Methods and Determination of the Nitrogen Isotopic Composition of Dissolved Ammonium in Seawater
Ammonium is a key dissolved inorganic nitrogen(DIN)in the biogeochemical cycle of nitrogen in the ocean.Depending on the environment,the 15N natural abundance(δ15Nair)of NH4+can provide insights into N sources and mechanisms of N transformations in terrestrial ecosystems.A variety of methods have been developed for δ15Nair determination for NH4+during the past several decades,such as the steam distillation method,ammonia diffusion method,ion exchange method and chemical conversion method.The former three methods are not unsuitable for low NH4+concentration in seawater samples.In this study,a pretreatment method was developed for determination of nitrogen isotopic composition in ammonium based on the chemical method by hypobromite oxidation combined with sodium azide.To determine the reagent blank source and the effection on the yield rate and the value of δ15Nair,the appropriate reagent additions,NH4+concentration were analyzed.There is no interference from any of the nitrogen-containing compounds tested.Higher concentration samples are readily diluted to lower concentration or taken a small volume.When the NH4+concentration ranged from 5 to 50 μmol/L,the yield rate of ammonium converting to N2O was greater than 92%.And the calibration curves of ammonium isotopic standards with different abundances showed a good linearity The slope was 0.465 which was close to the theoretical values of 0.5.The standard deviation of δ15Nair measurements was 0.35‰(n=5),and the difference between the measured value and the reference value was 0.26‰.This method was used to determination of the nitrogen isotopic composition of dissolved ammonium in seawater,and δ15Nair(NH4+)value were between 11.46‰to 22.31‰.The standard deviation were between 0.20‰to 0.62‰(n=5).This method meet the requirements of ammonium nitrogen isotope analysis in seawater.

chemical methodhypobromatenitrogen isotopeammonium nitrogenN2O

杨海丽

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自然资源部第三海洋研究所分析测试中心,厦门 361005

中国地质调查局舟山海洋地质灾害野外科学观测研究站,青岛 266237

化学法 次溴酸盐 氮同位素 铵态氮 氧化亚氮

中国地调局舟山海洋地质灾害野外科学观测研究站开放基金国家自然科学基金国家自然科学基金

ZSORS-22-104197605042176057

2024

同位素
中国核学会同位素分会

同位素

CSTPCD
影响因子:0.405
ISSN:1000-7512
年,卷(期):2024.37(3)