摘要

在0.050 0 g样品中滴加10滴200 g·L-1氢氧化钠溶液,于150℃加热15 s,待剧烈反应停止后,再加入200 g·L-1氢氧化钠溶液6 mL,于200℃加热40 min。取下烧杯,加入30%(质量分数)过氧化氢溶液2 mL。继续于200℃加热20 min,以分解溶液中过量的过氧化氢。冷却,加入50%(体积分数)硝酸溶液20 mL,盐酸2 mL,于200℃加热至溶液变清亮,冷却,用水稀释至100 mL,供电感耦合等离子体原子发射光谱仪测定其中铁、铜、镁、锌、镍、铬、锆、锡、钛、锶、镓、铍、铅、镉、硅、锰、钒等17种元素含量,设置射频功率为1 300 W,观测高度为12 mm,雾化气流量为0.65 L·min-1。通过优选谱线消除基体干扰中的光谱干扰,基体匹配法和同步背景校正法消除基体干扰中的物理干扰。按照上述方法处理10种标准样品,其中17种元素的质量分数均在一定范围内与其对应的谱线强度呈线性关系,检出限(3s)为0.000 3%~0.027 2%。方法分别用于实际样品以及标准样品的分析,实际样品测定值的相对标准偏差(n=11,RSD)为0.23%~3.1%,标准样品测定值的相对误差为-0.22%~5.0%,RSD(n=11)为0.17%~4.5%。

  • 单位
    太原重工股份有限公司
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