摘要
建立了氢化物发生-原子荧光光谱法测定钢铁中微量锡的新方法。对实验仪器的参数和锡的氢化物发生条件进行了优化，采用主量元素匹配法，对钢铁中常见共存元素的干扰情况进行了探讨，并研究了不同掩蔽剂对各种干扰元素的掩蔽效果。结果表明：酒石酸对基体元素Fe和共存元素V，Cr，Si，Mn有很好的掩蔽作用；EDTA能够消除大量W和Mo的影响；Cu的干扰必须通过硫脲和EDTA的联合作用消除。在选定的实验条件下测定，锡量在0～80ng／mL范围内线性关系良好，方法的检出限是0．1084ng／mL，对20ng／mL的锡标准溶液进行11次重复测验，相对标准偏差为1．82％。通过测试标准钢样进行方法验证，测定结果与认定值相符，用于普通钢样分析，加标回收率在94％～108％。
A new method for determination of trace tin in the steel by hydride generation atomic fluorescence spectrometry （HG-AFS） was investigated. The conditions of instrument and hydride generation were optimized. The major element matching method was used to study the interferences of familiar coexisting elements in steel. Besides, the effect of different masking reagents was discussed. The results indicated that tartaric acid had better masking effect on the interferences of the substrate element Fe and coexisting elements V, Cr, Si, Mn. The EDTA could eliminate the influences of large amounts of W and Mo, and the interference from Cu could be masked by the thiourea and EDTA. Under optimal experimental conditions, a good linearity was achieved for tin concentration range between 0 and 80 ng/mL. The detection limit of tin is 0. 108 4 ng/mL and the relative standard deviation for 20 ng/mL tin is 1.82 % （n=11）. The method has been applied to the determination of trace tin in the standard reference steel sample and the result was in agreement with the certified value. The recoveries of general steel are ranged from 94% to 108 %.
出处
《冶金分析》
EI
CAS
CSCD
北大核心
2008年第6期45-48,共4页
Metallurgical Analysis
关键词
氢化物发生-原子荧光光谱法
钢铁
锡
hydride generation atomic fluorescence spectrometry
steel
tin
