氢化物发生-原子荧光光谱法分析钢铁中痕量锑  

DETERMINATION OF TRACE STIBIUM CONTENT IN STEEL BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY

作　　者：杨惠玲 杜天军 唐静[2] 韩华云[3] 张西林[3] 

机构地区：[1]河南省有色金属地质勘查总院,郑州450002 [2]河南省文物考古研究所,郑州450000 [3]郑州大学分析测试中心,郑州450052

出　　处：《化学分析计量》2009年第3期61-64,共4页Chemical Analysis And Meterage

摘　　要：建立氢化物发生-原子荧光光谱法分析钢铁中痕量锑的新方法。试验了钢铁中常见元素Cu、V、Cr、Mn、Mo、Si、W、Ni和Ti等对锑元素测定的影响。考察了原子化器高度、载气流速、屏蔽气流速、载流酸和硼氢化钾浓度等因素对测定的影响,优化了测定条件。结果表明,在选定的实验条件下,碘化钾-抗坏血酸混合溶液不仅能作为Sb5＋的预还原剂,并且还能有效掩蔽Fe、Cu、V、Cr、Mn、Mo、Si、W和Ti的干扰,而共存元素Ni的干扰需要EDTA-硫脲进行联合掩蔽。方法的线性范围为0-120 ng/mL（相关系数r=0.9990）,检出限为0.24 ng/mL,测定结果的相对标准偏差为5.1%（n=10）。用该法对国家标准钢样进行分析,测定结果与标准值相符合。The determination of stibium in steel by hydride generation-atomic fluorescence spectrometry（HG-AFS） was developed.Interference effect of coexistent elements in steel such as Cu,V,Cr,Mn,Mo,Si,W,Ni and Ti on the determination of stibium was investigated.The influence of instrument parameters such as atomizer height,carrier gas rate,shield gas rate and concentration of HCl and KBH4 on the determination of stibium were studied and the conditions were optimized.The results showed that Kalium iodide and ascorbic acid were not only the best beforehand reducer for Sb^5＋ , but also the occultation reagent for Fe, Cu,V, Cr, Mn, Mo,Si, W and Ti. Interference of Ni was eliminated by using EDTA - Thiourea. Under the optimized conditions, the linear range of stibium was 0 - 120 ng/mL, and the detection limit was 0.24 ng/mL. The relative standard deviation of determination result was 5.1% （n = 10）. Standard samples were determined by the method and the detection results were cosistent with the standard values.

关 键 词：氢化物发生-原子荧光光谱法 钢铁 锑 

分 类 号：O657.71[理学—分析化学] X832[理学—化学]