高级检索

    电感耦合等离子体原子发射光谱法测定锆合金中5种元素的含量

    Determination of 5 Elements in Zirconium Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry

    • 摘要: 提出了电感耦合等离子体原子发射光谱法测定锆合金中锡、铌、铁、铬、镍含量的方法。取样品0.1 g,加入5 mL水、5 mL硝酸和0.5 mL氢氟酸,于100 ℃加热5 min,用水定容至25 mL。设置仪器射频功率为1 300 W,雾化气流量为0.80 L·min-1,进样量为2.0 mL·min-1,测定5种元素在Sn 242.949 nm、Nb 309.418 nm、Fe 259.941 nm、Ni 221.648 nm、Cr 267.716 nm等分析谱线处的响应强度,基质匹配法定量。结果表明:锡、铌的质量浓度在150 μg·mL-1以内,铁、铬、镍的质量浓度在15 μg·mL-1以内分别与对应的响应强度呈线性关系;锡检出限(3s)为16 μg·g-1,其他元素检出限(3s)均低于3.0 μg·g-1;各元素方法重复性的相对标准偏差(n=10)均小于2.0%,加标回收率为99.0%~109%;采用锆合金标准物质SRM360b进行验证,测定值均在认定值的不确定度范围内。

       

      Abstract: A method for the determination of Sn, Nb, Fe, Cr and Ni in zirconium alloy by inductively coupled plasma atomic emission spectrometry was proposed. The sample (0.1 g) was taken, and 5 mL of water, 5 mL of nitric acid and 0.5 mL of hydrofluoric acid were added. After heating at 100 ℃ for 5 min, the volume of the mixed solution was made up to 25 mL with water. The response intensities of 5 elements at Sn 242.949 nm, Nb 309.418 nm, Fe 259.941 nm, Ni 221.648 nm and Cr 267.716 nm were determined with the radio frequency power of 1 300 W, the atomizing gas flow rate of 0.80 L·min-1, and the sample injection amount of 2.0 mL·min-1, and the matrix matching method was used for quantification. It was shown that linear relationships between mass concentration and response intensity were kept within 150 μg·mL-1 for Sn and Nb, and 15 μg·mL-1 for Fe, Cr and Ni, and the detection limit (3s) of Sn was 16 μg·g-1, and the detection limits (3s) of other elements were lower than 3.0 μg·g-1. RSD (n=10) for the method reproducibility of each element was less than 2.0%, and the spiked recoveries were in the range of 99.0%-109%. Zirconium alloy standard substance SRM360b was used for verification, and the determined values were within the uncertainty ranges of the confirmed values.

       

    /

    返回文章
    返回