摘要 采用高频燃烧红外吸收法,比较了标准方法GB/T 4333.10—1990(以下简称GB)和JIS G 1312-2∶2011(以下简称JIS)中的两种助熔剂条件对硅铁样品中碳的测定结果。试验现象和结果表明:GB方法测定时,熔液飞溅现象较JIS方法严重,导致其测定结果的精密度较JIS方法差。鉴于满足JIS方法中所用铁粉助熔剂的分析成本较高,实验对现有GB方法的助熔剂条件进行了改进,措施是在硅铁样品中混入三氧化钨粉,再加入铁、锡、钨助熔剂,然后采用高频燃烧红外吸收法对其中碳进行测定。试验结果表明三氧化钨粉能有效提高硅铁样品在铁、锡、钨条件下燃烧的稳定性。改进后的测定条件为:称取0.20g样品与0.5g三氧化钨粉在坩埚中混合,再加入0.6g纯铁屑、0.4g锡粒和1.5g钨粒。将实验方法应用于硅铁实际样品中0.006%~0.080%(质量分数)碳的测定,相对标准偏差(RSD,n=8)在0.8%~5.0%之间。在硅铁样品中加入碳标准溶液进行碳的加标回收试验,回收率为91%~120%。
Abstract：The effect of two flux conditions in GB/T 4333.10-1990 (GB method) and JIS G 1312-2: 2011 (JIS method) on the determination results of carbon in ferrosilicon sample was investigated by high frequency combustion infrared absorption method. The experimental phenomenon and results showed that the melt splashing phenomenon of GB method was worse than that of JIS method, leading to lower precision of determination results. However, the analytical cost of iron powder flux in JIS method was relatively high. The flux condition in existing GB method was improved: after mixing tungsten trioxide powder into ferrosilicon sample, the flux of iron, tin, and tungsten was added. Then the content of carbon was determined by high frequency combustion infrared absorption method. The experimental results indicated that the tungsten trioxide powder could effectively enhance the combustion stability of ferrosilicon sample in presence of iron, tin and tungsten. The improved determination conditions were listed as follows: 0.20g of sample was mixed with 0.5g of tungsten trioxide powder in crucible; then 0.6g of pure iron crumb, 0.4g of tin particle and 1.5g of tungsten particle were added. The content of carbon with mass fraction in range of 0.006%-0.080% in actual ferrosilicon sample was determined according to the proposed method. The relative standard deviations (RSD, n=8) were between 0.8% and 5.0%. The standard solution of carbon was added into ferrosilicon sample for recovery test. The recoveries were between 91% and 120%.
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