Abstract：Nitrogen content was one of the important technical indicators for the quality of vanadium-nitrogen alloy. At present, the content of nitrogen was usually determined by wet method in China. The analysis results were reliable, but the efficiency was low. Therefore, it was necessary to establish a rapid method for the determination of nitrogen content in vanadium-nitrogen alloy. The determination of nitrogen in vanadium-nitrogen alloy by Dumas combustion was explored in experiments. The particle size, sample mass, combustion time and flux dosage were optimized. The following conditions were selected: the particle size was not larger than 0.074mm; the sample mass was in range of 0.0400-0.0600g; the combustion time was 270s; 0.1g of pure nickel and 0.1g of pure tungsten were used as flux. The results showed that under the optimized experimental conditions, the mass fraction of nitrogen showed a linear relationship with the corresponding peak area when its content was in range of 13.14%-16.64% (mass fraction). The linear correlation coefficient (r) of the calibration curve was 0.9996. The content of nitrogen in certified reference materials of vanadium-nitrogen alloy was determined according to the experimental method. The relative error between the measured value and the standard value was 0.21%-0.38%. The proposed method was applied to the determination of nitrogen (13.55%-15.56%) in actural samples. The relative standard deviation (RSD, n=10) of the determination results was 0.42%-0.50%.
刘秋生,黄绍明,易伟湘,等.V2O5烧成钒氮合金工艺设备研究[J].工业加热,2008,37(2):19-20.LIU Qiu-sheng,HUANG Shao-ming,YI Wei-xiang,et al.Research on V2O5 sintering equipment of vanadium nitrogen alloy[J].Industrial Heating,2008,37(2):19-20.
[2]
王爱军,张祖辉,常相征,等.钒氮合金中氮的测定[J].冶金分析,2004,24(1):80-81.WANG Ai-jun,ZHANG Zu-hui,CHANG Xiang-zheng,et al.Determination of nitrogen in vanadium nitrogen alloy[J].Metallurgical Analysis,2004,24(1):80-81.
[3]
袁冬雪,李健强.蒸馏-中和滴定法测定氮化锰铁中氮含量的方法研究[J].铁合金,2017,48(3):42-45.YUAN Dong-xue,LI Jian-qiang.Method study on determination of nitrogen content in nitided FeMn by distillation neutralization titration method[J].Ferro-alloys,2017,48(3):42-45.
[4]
薛明浩,王俊秀,张小燕,等.水蒸气蒸馏-酸碱滴定法测定氮钒合金中氮[J].山东冶金,2013(2):45-46.XUE Ming-hao,WANG Jun-xiu,ZHANG Xiao-yan,et al.Determination of nitrogen in nitrogen vanadium alloy by steam distillation acid base titration[J].Shandong Metallurgy,2013(2):45-46.
[5]
郑福丽,谭德水,马征,等.自动定氮仪碱解蒸馏电位滴定法测定土壤中水解性氮含量[J].山东化工,2019,48(9):120-121.ZHENG Fu-li,TAN De-shui,MA Zheng,et al.Determination of hydrolytic nitrogen content in soil by potentiometric titration with alkaline distillation of automatic nitrogen determinator[J].Shandong Chemical Industry,2019,48(9):120-121.
[6]
洪流,索卫国,李福龙,等.杜马斯燃烧法测定烟草中总氮的含量[J].理化检验:化学分册,2018,54(10):1207-1209.HONG Liu,SUO Wei-guo,LI Fu-long,et al.Determination of total nitrogen in tobacco by Dumas combustion method[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(10):1207-1209.
[7]
周冰群,王鑫海,侯峰.杜马斯燃烧法与连续流动法测定再造烟叶中总氮量的比较[J].理化检验:化学分册,2018,54(7):757-760.ZHOU bing-qun,WANG Xin-hai,HOU Feng.Comparison of the determination of total nitrogen in reconstituted tobacco leaves by Dumas combustion method and continuous flow method[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(7):757-760.
[8]
陈秀明,张子皓,李双,等.杜马斯燃烧定氮法在食品检测中的应用[J].理化检验:化学分册,2015,51(11):1617-1618.CHEN Xiu-ming,ZHANG Zi-hao,LI Shuang,et al.The application of Dumas combustion nitrogen determination method in food detection[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2015,51(11):1617-1618.
[9]
汪红,魏亮亮,李通,等.杜马斯燃烧法快速测定粮油中粗蛋白质含量研究[J].粮油食品科技,2018,26(2):49-53.WANG Hong,WEI Liang-liang,LI Tong,et al.Study on rapid determination of crude protein in grain and oil by Dumas combustion method[J].Science and Technology of Cereals,Oils and Foods,2018,26(2):49-53.
[10]
张长均,王蓬,张之果.影响高频红外碳硫仪分析结果稳定性因素的探讨[J].冶金分析,2006,26(6):90-91.ZHANG Chang-jun,WANG Peng,ZHANG Zhi-guo.Discussion on the factors affecting the stability of high frequency infrared carbon sulfur analyzer[J].Metallurgical Analysis,2006,26(6):90-91.
[11]
徐本平,李晖.钒氮合金中的高含量氮的测定[J].冶金分析,2004,24(z1):358-360.XU Ben-ping,LI Hui.Determination of high nitrogen content in vanadium nitrogen alloy[J].Metallurgical Analysis,2004,24(z1):358-360.
