碱性过硫酸盐消解-紫外二阶导数光谱法测定地热水中总溶解氮

Determination of Total Dissolved Nitrogen in Geothermal Water by Ultraviolet Second Derivative Spectrometry with Alkaline Persulfate Digestion

  • 摘要: 地热水的过度开发利用导致地热水中总溶解氮含量过高,造成水质恶化,同时伴随地热水中总溶解氮中不同形态氮的相互转化,对人类健康和经济发展造成严重影响。因此,地热水中总溶解氮的测定,对研究总溶解氮的生物地球化学循环和地热水的合理开发利用具有重要意义。针对地热水具有化学成分复杂多变、干扰组分多的特点,本文建立了碱性过硫酸盐消解-紫外二阶导数光谱法测定地热水中总溶解氮的方法,其中总溶解氮以硝酸根-氮的形式定量测定,其二阶导数光谱图可消除大部分干扰因素。通过研究硝酸根-氮紫外二阶导数光谱图,确定波长266.6nm对应的二阶导数值为特征吸光度。通过单因素水平实验和双因素方差分析实验优化消解反应中的消解参数,表明在一定条件范围内,稀释步骤是影响总溶解氮测定最重要的因素,推荐选择消解温度为120℃,消解时间为20min,碱性过硫酸钾溶液体积为5.0mL;选择样品体积为10.0mL,稀释步骤安排在样品消解前。共存离子干扰实验表明,高含量溴离子对总溶解氮的测定有正干扰。在0.20~5.0mg/L线性范围内,建立硝酸根(以氮计)标准溶液校准曲线,其决定系数R2=0.9996。本方法加标回收率在94.0%~103.5%之间,相对偏差在0.83%~3.36%之间,准确度和可靠性高,干扰因素可控,需要样品量小,仪器成本低,可满足地热水中总溶解氮的快速、简单、准确批量检测需求。

     

    Abstract: The method for the determination of total dissolved nitrogen in geothermal water by alkaline persulfate digestion-ultraviolet second derivative spectrometry was developed. The total dissolved nitrogen was quantitatively determined in the form of nitrate-nitrogen. The second derivative value corresponding to wavelength 266.6nm was determined as the characteristic absorbance. The parameters in digestion reaction were optimized by single-factor level experiments and a two-factor ANOVA experiment. The digestion temperature, digestion time and solution volume of alkaline potassium persulfate were recommended to be 120℃, 20min and 5.0mL, respectively. The sample volume was 10.0mL and the dilution time was before sample digestion. High content of bromide ions had a positive interference on the determination of total dissolved nitrogen. In the linear range of 0.20-5.0mg/L, the calibration curve of nitrate-nitrogen was established with its coefficient of determination R2=0.9996. The actual samples were determined with the recovery rate (94.0%-103.5%) and the relative deviation (0.83%-3.36%). Compared with the industry standard method, the experimental results were satisfactory. This method has high accuracy and reliability, controllable interference factors, small sample amount, low instrument cost, and can meet the rapid, simple and accurate batch detection of total dissolved nitrogen in geothermal water. The BRIEF REPORT is available for this paper at http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202411210239.

     

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