原子荧光光谱法测定合金钢中锑

Determination of Antimony in Alloy Steel by Atomic Fluorescence Spectrometry

采用氢化物原子荧光光谱法测定合金钢中痕量锑，用抗坏血酸一硫脲体系去除消解液中铁、镍、铜等元素对氢化物生成的影响，硫脲使锑元素还原为3价离子，在酸性条件下，溶液中3价锑离子与硼氢化钾进行反应，生成锑氢化物气体，锑化氢气体引入原子荧光光谱仪，从而测定出锑的浓度。在实验条件下，锑的最低检出限为0．02μg/g，加标回收率为94．0％-104．0％。本方法操作简便。灵敏度、准确度都有很大的提高，结果可靠，能够满足合金钢中痕量锑的测定要求。

Trace antimony in steel was determined by hydride generation atomic fluorescence spectrometry, uses ascorbic acid-thiourea system to remove the effect of iron, nickel, copper and other elements in digestion solution on the hydride generation. Thiourea makes antimony reduce to trivalent ions. In acidic conditions, the trivalent antimony ion in the solution reacts with potassium borohydride, generating antimony hydride gas. Stibine gas is then introduced into the atomic fluorescence spectrome- ter, in order to determine the concentration of antimony. Under the experimental circumstances, the minimum detection limit of the antimony is 0.02μg/g and the recovery of standard addition is 94%- 104%. The method is simple, sensitive and accuracy is greatly improved, and the result is reliable, which can meet the requirements of the determination of trace antimony in alloy steel.