开氏法测定煤中氮含量的消解条件改进研究OA
Study on the improvement of digestion conditions for determining nitrogen content in coal by Kjeldahl method
为探索采用硫酸钾和硫酸铜作为催化剂替代现行国家标准中开氏法测定煤中氮含量的催化剂进行样品消解,以催化剂用量、浓硫酸用量、消解温度和消解时间为试验变量,通过单因素变量试验和正交试验,对不同变质程度的 6 个煤炭样品进行试验研究,探究样品的最优消解条件.单因素变量试验结果表明,最佳催化剂用量为5g、最佳浓硫酸用量为6 mL~10 mL、最佳消解温度为420℃,最佳消解时间为120 min~240 min.正交试验结果表明,各因素对煤样消解影响大小顺序为消解温度>浓硫酸用量>催化剂用量>消解时间,消解温度和浓硫酸用量对测定结果有显著影响,催化剂用量及消解时间对测定结果影响不明显.综合单因素试验结果和正交试验结果,称取0.2g 煤样,加入 5g 硫酸钾和硫酸铜作为催化剂和 8mL 浓硫酸,在 420℃消解120 min时,样品消解效果最佳,各样品所测氮含量结果准确.
To explore the use of potassium sulfate and copper sulfate as catalysts to replace the current national stand⁃ard's Kjeldahl method for coal nitrogen determination,this study conducted sample digestion experiments with cata⁃lyst dosage,concentrated sulfuric acid dosage,digestion temperature,and digestion time as variables.Through sin⁃gle⁃factor experiments and orthogonal experiments,six coal samples with varying degrees of metamorphism were tested to determine optimal digestion conditions.The single⁃factor experiment results showed that the optimal catalyst dosage was 5 g,the optimal concentrated sulfuric acid dosage was 6 mL~10 mL,the optimal digestion temperature was 420℃,and the optimal digestion time was 120 min~240 min.The orthogonal experiment results indicated that the influ⁃ence order of factors on coal sample digestion was:digestion temperature>concentrated sulfuric acid dosage>catalyst dosage>digestion time.Both digestion temperature and concentrated sulfuric acid dosage significantly affected the measurement results,while catalyst dosage and digestion time showed minimal impact.Combining the single⁃factor and orthogonal experiment results,when 0.2 g coal sample was weighed and 5 g potassium sulfate and copper sulfate(as catalysts)along with 8 mL concentrated sulfuric acid were added,digestion at 420℃for 120 minutes achieved the best digestion efficiency,yielding accurate nitrogen content measurements for all samples.
富坤
煤炭科学技术研究院有限公司,北京 100013||国家煤炭质量检验检测中心,北京 100013
化学化工
煤氮开氏定氮催化剂正交试验最优消解条件
coalnitrogenKjeldahl determinationcatalystorthogonal testoptimal digestion conditions
《煤质技术》 2026 (2)
86-92,7
煤炭科学技术研究院有限公司科技发展基金支持项目(2024JC-13)
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