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摘要: 【研究目的】本文通过开展优化消解程序、蒸馏时间等实验条件和方法准确度等方面的研究，建立了一种全自动凯氏定氮仪测定岩石中全氮含量的分析方法。【研究方法】该方法在消解过程中加入硫酸，样品中的含氮有机物转变为无机氮硫酸铵，在由硫酸钾与五水硫酸铜制成的催化片作用下加速反应进行，与氢氧化钠作用释放出氨气，收集于硼酸溶液中用标准盐酸溶液进行全氮的滴定。【研究结果】结果显示，方法检出限为23.90 μg/g，用国家一级标准物质GBW07729进行验证，本方法的相对标准偏差RSD（n=4）为1.07%，实验的回收率在95.40%～103.8%之间。【结论】本方法利用全自动凯式定氮法测定岩石中全氮含量，操作简单、准确，完全能够满足地质行业的测试要求。关 键 词：岩石；全氮；全自动凯式定氮仪Abstract: This paper is the result of titration of total nitrogen content in rocks.[Objective] This article established an analytical method for determining total nitrogen content in rocks using a fully automatic Kjeldahl nitrogen analyzer by conducting research on optimizing digestion procedures, distillation time and other experimental conditions, as well as accuracy of methods. [Methods] This method added sulfuric acid during the digestion process, and the nitrogen-containing organic matter in the sample was transformed into inorganic ammonium nitrosulfate.Under the action of a catalytic plate that made of potassium sulfate and pentahydrate copper sulfate, the reaction was accelerated, and ammonia gas was released by reacting with sodium hydroxide which was collected in a boric acid solution and titrated with standard hydrochloric acid solution for total nitrogen. [Results] The results showed that the detection limit of the method was 23.90 μg/g and the method was validated using the national first-class standard material GBW 07729, with a relative standard deviation (RSD) of 1.07% (n=4), and the recovery rate of the experiment was between 95.40% and 103.8%. [Conclusions] This method used a fully automatic Kjeldahl nitrogen analyzer to determine the total nitrogen content in rocks which is simple and accurate, and could fully meet the testing requirements of the geological industry.
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Key words:
- rock /
- total nitrogen /
- automatic Kjeldahl nitrogen analyzer /
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