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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。
A New Method for the Determination of Trace Antimony in Iron and Steel by Hydride Generation Atomic Fluorescence Spectrometry. The effects of common elements such as Cu, V, Cr, Mn, Mo, Si, W, Ni and Ti on the determination of antimony in steel were tested. The effects of atomizer height, carrier gas velocity, shielding gas velocity, carrier acid and potassium borohydride concentration on the determination were investigated, and the determination conditions were optimized. The results show that the mixed solution of potassium iodide and ascorbic acid can not only act as a pre-reductant of Sb5 +, but also mask the interferences of Fe, Cu, V, Cr, Mn, Mo, Si, W and Ti under the selected experimental conditions. The interference of coexisting element Ni requires EDTA-thiourea for joint masking. The linear range of the method was 0-120 ng / mL (correlation coefficient r = 0.9990) with a detection limit of 0.24 ng / mL and a relative standard deviation of 5.1% (n = 10). With the method of national standard steel samples were analyzed, the measured results are consistent with the standard value.