脉冲加热-红外吸收热导法同时测定钢铁材料中氧和氢

针对钢铁材料中氧和氢的同时测定, 提出了一种新型的气路结构和检测原理, 解决了传统技术中转化效率及后续吸收脱除问题, 并通过研究分析功率、助熔剂等对氧和氢释放的影响, 确定了分析功率2 250 W、加入锡片作助熔剂的最佳分析条件。选用合适的钢中氧和氢标准样品, 建立了方法的校准曲线, 实现了钢铁材料中氧和氢的脉冲加热-红外吸收热导法测定。利用对空白的标准偏差计算得氧和氢的检出限分别为0.000 051%、0.000 024%, 氧和氢的分析范围分别为0.000 05%~0.1%、0.000 03%~0.05%。实验方法避免了中间处理阶段对测定结果的准确性与稳定性的影响, 用于实际样品的测定结果与对照值一致, 完全满足钢铁材料氧和氢快速、准确的分析要求。

Simultaneous determination of oxygen and hydrogen in steel materials by pulse heating-infrared absorption and thermal conductivity method

A novel gas circuit structure and detection principle was proposed to solve the problems including both conversion efficiency of conventional technique and subsequent absorption removal in simultaneous determination of oxygen and hydrogen in steel materials. Through studying the effect of analysis power and flux on the release of oxygen and hydrogen, it was determined the optimal analytical power was 2 250 W and the optimal flux was stannum piece. Appropriate standard samples of oxygen and hydrogen in steel were selected for establishing calibration curve, then the determination of oxygen and hydrogen in iron and steel materials by pulse heating-infrared absorption and thermal conductivity method was realized.The detection limit of oxygen and hydrogen calculated with blank standard deviation was 0.000 051% and 0.000 024%, respectively. The analytical range of oxygen and hydrogen was 0.000 05%-0.1% and 0.000 03%-0.05%. The proposed method could avoid the effect of intermediate processing phase on determination accuracy and stability. The determination results of practical samples were consistent with the reference values, completely satisfying the requirements of fast and accurate determination of oxygen and hydrogen in iron and steel materials.