火花源原子发射光谱法测定FeCuNbSiB 合金中铜铌硅硼

探讨了火花源原子发射光谱法测定FeCuNbSiB合金中铜、铌、硅和硼的分析条件。在高纯氩气(φ≥99.999%)流量为180 L/h和氩气冲洗时间为4 s,预燃(HEPS)时间为6 s,积分时间为8 s(硅)、8 s(铌)、3 s(硼)和3 s(铜)的最佳分析条件下,用自制的标准样品绘制了铜、铌、硅和硼的校准曲线。在校正了共存元素干扰影响后,拟合校准曲线。其中,用B 345.1 nm/Fe 360.7 nm 分析线对绘制高含量硼的校准曲线,硼的分析范围为0.94%～3.37%;用Nb 319.5 nm/Fe 297.1 nm分析线对绘制铌的校准曲线,使仪器软件中已建立的钢中铌的校准曲线得到了延伸,铌的分析范围扩展为0.002 0%～7.16%;用Si 390.6 nm/Fe 281.3 nm分析线对和Cu 212.3 nm/Fe 216.2 nm 分析线对分别绘制了硅和铜的校准曲线,使仪器软件中已建立的钢中硅和铜的校准曲线得到了充实,硅的分析范围为0.010 0%～19.40%,铜的分析范围为0.001 3%～3.95%。用此方法测定了FeCuNbSiB合金分析样品中铜、铌、硅和硼含量,其测定结果的相对标准偏差(n=8)小于1.0%,所得的分析结果与用重量法和电感耦合等离子体原子发射光谱法(ICP-AES)的测定值一致,并且实现了分析样品的一次激发可同时测定FeCuNbSiB合金分析样品中铜、铌、硅和硼以及其他合金元素。

Determination of copper,niobium, silicon and boron in FeCuNbSiB alloy by spark source atomic emission spectrometry

The analytical conditions of copper, niobium, silicon and boron in FeCuNbSiB alloy by spark source atomic emission spectrometry were discussed. The optimal analytical conditions were as follows: the flow rate of high-purity argon (φ≥99.999%) was 180 L/h, the flush time of argon was 4 s, the pre-combustion (HEPS) time was 6 s, the integral time for silicon, niobium, boron and copper was 8 s, 8 s, 3 s and 3 s, respectively. The calibration curves of copper, niobium, silicon and boron were prepared using the self-made standard samples. The calibration curves were fitted after correcting the interference of coexisting elements. The analytical lines of B 345.1 nm/Fe 360.7 nm were used to prepare the calibration curve of high-content boron, and the analytical range of boron was 0.94%-3.37%. The analytical lines of Nb 319.5 nm/Fe 297.1 nm were used to prepare the calibration curve of niobium, extending the calibration curve of niobium in steel which had been established in instrumental software. The analytical range of niobium was extended to 0.002 0%-7.16%. The analytical lines of Si 390.6 nm/Fe 281.3 nm and Cu 212.3 nm/Fe 216.2 nm were used to prepare the calibration curve of silicon and copper, respectively. The calibration curves of silicon and copper in steel which had been established in instrumental software were improved. The analytical range of silicon and copper was 0.010 0%-19.40% and 0.001 3%-3.95%, respectively. The proposed method was applied to the determination of copper, niobium, silicon and boron in FeCuNbSiB alloy sample, and the relative standard deviations (RSD, n=8) of determination results were less than 1.0%. The found results were consistent with those obtained by gravimetric method and inductively coupled plasma atomic emission spectrometry (ICP-AES). The copper, niobium, silicon, boron and other alloying elements in FeCuNbSiB alloy sample could be simultaneously determined after excitation once of analytical samples.