摘要
提出了流动注射离子交换在线分离～氢化物发生原子荧光光谱法测定钢铁样品中痕量砷的分析方法。设计了流动注射在线离子交换的流路和操作程序，优化了各项化学条件和流路参数。采用732强酸性阳离子交换树脂消除了Cu^2＋，Co^2＋，Ni^2＋，Mn^2＋，Zn^2＋，Cr^2＋，Cd^2＋，A^＋，Mo^3＋等金属离子的干扰，也使大量基体元素Fe与被测元素砷分离。选用5．0g／L L-半胱氨酸为预还原剂与样品以70r／min等速进样40S，于沸水浴中停留60S后进行检测，实现了氢化物发生原子荧光光谱法对钢铁中痕量砷的在线测定。砷的线性范围为0．6～120μg／L，方法的检出限为0．3μg／L，对20μg／LAs（V）标准溶液连续测定11次的RSD为3．04％。方法应用于钢铁标准样品分析，结果与认定值相吻合。
A technique for the determination of trace arsenic in steel by on-line ion-exchange flow injection （FI） system combined with hydride generation atomic fluorescence spectrometry was developed . A manifold for the FI was designed. The parameters and chemical conditions of the FI manifold were optimized. The 732 strong acid cation exchange resin could be used to eliminate the interferences of Cu2＋ ,Co2＋ , Ni2＋ , Mn2＋ , Zn2＋ , Cr3＋ , Cd2＋ , Ag＋ , Mo3＋ and iron matrix. 5.0 g/L L-cysteine solution was selected as a pre-reducing agent and was mixed mixing on-line with the sample. Sampling continues for 40 s at the speed of 70 r/min, and then the sample was measured by atomic fluorescence spectrometry after staying in boiling water for 60 s. The detection limit and the linear range for As （V） are 0.3 μg/L and 0.6--120 μg/L, respectively. The RSD（n=11） was 3.04% for measurement of 20 μg/L As（V） standard solution. The method has been used to the determination of As（V） in steel certified reference materials and the results are in a good agreement with the certified values.
出处
《冶金分析》
CAS
CSCD
北大核心
2008年第6期11-14,共4页
Metallurgical Analysis
基金
科技部专项基金(2006FY120306-11)
关键词
流动注射
离子交换
氢化物发生
原子荧光光谱法
砷
钢铁
flow injection
ion-exchange
hydride generation
atomic fluorescence spectrometry
arsenic
iron and steel
