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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Cu2+,Co2+,Ni2+,Mn2+,Zn2+,Cr3+,Cd2+,Ag+,Mo3+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5.0 g/LL-半胱氨酸为预还原剂与样品以70 r/min等速进样40 s,于沸水浴中停留60 s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/L As(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。
An analytical method for the determination of trace arsenic in steel samples by flow injection ion exchange on-line separation-hydride generation atomic fluorescence spectrometry was proposed. The flow path and operating procedure of ion exchange for flow injection on-line are designed and the chemical conditions and flow path parameters are optimized. The use of 732 strong acid cation exchange resin to eliminate the Cu2 +, Co2 +, Ni2 +, Mn2 +, Zn2 +, Cr3 +, Cd2 +, Ag +, Mo3 + and other metal ions interference, but also to a large number of matrix elements Fe and the measured elemental arsenic separation. 5.0 g / LL-cysteine was used as prereducing agent and the sample was injected at a constant velocity of 70 r / min for 40 s, and the reaction was stopped in a boiling water bath for 60 s before being tested. Hydride generation atomic fluorescence spectrometry Determination of Trace Arsenic in. The linear range of arsenic was 0.6 ~ 120μg / L, the limit of detection was 0.3μg / L, and the RSD of 11th consecutive determination of 20μg / L As (Ⅴ) standard solution was 3.04%. The method is applied to the analysis of steel standard samples, and the results are consistent with the certified values.