对于含氮量较高的氮化钒铁而言,其熔点高达1450~1650℃,给测定碳和硫的含量带来难题。利用钒铁标准物质建立校准曲线,钒铁标准物质进行校准验证,设定分析时间为50 s,以0．4 g纯铁和1．4 g钨粒为助熔剂进行助熔,建立了高频燃烧红外吸收法测定氮化钒铁中碳和硫的分析方法。方法中碳和硫的检出限分别为0．0011%和0．0013%,方法测定下限分别为0．0035%和0．0042%。由于缺乏氮化钒铁标准物质,取一定量的钒铁标准物质,分别与氮化硅铁标准物质混合,参照FeV45 N10、FeV55 N11氮化钒铁的成分配比配制氮化钒铁合成样品1#和2#,按照实验方法进行测定,所得测定值和理论值基本一致。实验方法测定氮化钒铁样品中碳含量结果的相对标准偏差(RSD,n=8)在1．2%~3．0%之间,硫在2．2%~4．2%之间。
The melting point of ferrovanadium nitride with high content of nitrogen is relatively high, and it is up to 1 450-1 650 ℃. This brings problems to determination of carbon and sulfur. Ferrovanadium certified reference ma-terial was used to prepare and verified the calibration curve. 0. 4 g of pure iron and 1. 4 g of tungsten particle was used as flux. An analysis method of carbon and sulfur in ferrovanadium nitride was established by high frequency combustion infrared absorption with analytical time as 50 s. The detection limit of carbon and sulfur in this method was 0. 001 1% and 0. 001 3%, respectively, and the low limit of determination was 0. 003 5% and 0. 004 2%, re-spectively. Since there was no certified reference material of ferrovanadium nitride, appropriate ferrovanadium certi-fied reference material and ferrosilicon nitride certified reference material were mixed to prepare ferrovanadium ni-tride synthetic samples 1 # and 2 # according to the composition of FeV45 N10 and FeV55 N11 . The synthetic sam-ples were determined according to the experimental method, and the results were basically consistent with the theo-retical values. The proposed method was applied to the determination of carbon and sulfur content in ferrovanadium nitride sample. The relative standard deviation (RSD, n=8) was 1. 2%-3. 0% for carbon and 2. 2%-4. 2% for sulfur, respectively.
参考文献
| [1] | 柳轶男;姜立强;张书菊;刘志强.CS-800红外碳硫分析仪测定合金钢中的碳和硫[J].光谱实验室,2011(4):1958-1962. |
| [2] | 林光西;郭凤云.高频-红外碳硫仪测定硫铁矿中的碳[J].分析仪器,2008(3):62-64. |
| [3] | 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(6):90-91. |
| [4] | 钟华.纯化学物质校准-高频燃烧红外吸收法测定钛及钛合金中碳[J].冶金分析,2012(3):30-34. |
| [5] | 李正权.红外吸收光谱法测定金属中碳硫的影响因素[J].河北冶金,2011(04):3-6. |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%