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以线扫描进行激光剥蚀进样,采用激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)定量分析不锈钢中主、次和痕量元素.考察了激光剥蚀池载气及流量、激光脉冲频率、激光剥蚀孔径、激光输出能量密度对分析性能的影响,对激光剥蚀参数进行了优化.以基体57 Fe为内标,校正了元素分馏和灵敏度漂移;以湿法分析用不锈钢屑状标准物质通过环氧树脂等固化剂镶嵌成集合式标准物质作为校准样品,建立了校准曲线.结果表明,除P和Pb校准曲线的线性相关系数分别为0.978 2和0.967 9外,其他各待测元素均达到0.99以上;各元素的检出限为0.02~39.71 μg/g.将方法应用于不锈钢标准样品分析,测定值与认定值吻合,除样品BSCA 316-4中Al和Pb外,其它各元素测定值的相对标准偏差(RSD,n=5)在10%以内,而Pb元素的含量本身较低,因此其RSD为10.3%也满足要求.

参考文献

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