研究了以纳米Fe2O4为固相吸附剂对痕量无机砷形态的吸附与分离富集,建立了无需洗脱分离的悬浮进样一氢化物发生一原子荧光法测定砷形态的方法。选择的反应体系为0.64g/LFe,O。悬浮液-1.O%(m/V)NaBH。溶液.5.0%(V/V)HCl(pH8),进样5.0mL时,得到本方法的检出限为13.5ng/L;As0田D浓度在0.05~3.5μg/L范围内呈良好的线性关系;测定0.5μg/LAs0(Ⅲ)的精密度RSD=3.4%。用国家标准物质GBWl0010(大米)验证了本方法测定砷的准确性,测定结果(0.101+0.010μg/g)与标准值(0.102+0.008μg/g)吻合。采用本方法测定了近海海水和雪水样品中的无机砷形态,并进行了加标回收实验。对As㈣和As(v)的加标回收率在95%-110%之间,结果令人满意。
Fe3 04 nano-particles as adsorbent were investigated for the adsorption preconcentration of arsenic species, and a slurry sampling procedure was developed by coupling with hydride generation-atomic fluorescence spectrometry for arsenic determination and inorganic arsenic speciation. In this process, the elution procedure was eliminated which simplifies the entire operation. Under optimal conditions, e.g. , pH 8, 0.64 g/L Fe304 slurry, 1.0% (m/V) NaBH4, 5.0% (V/V) HC1, 5.0 mL sample solution, a detection limit of 13.5 ng/L was achieved for arsenic within a linear range of O. 05-3.5 μg/L, along with a precision of 3.4% RSD at 0.5 μg/L As(I). The procedure was validated by analyzing arsenic in a certified reference material GBW 10010 (rice), a fair agreement between the obtained value and the certified value was achieved. The speciation of inorganic arsenic in coastal sea water and snow water samples was also performed.