流动注射氢化物发生原子吸收光谱法测定蒸馏酒中的铅

Determination of Lead in Distilled Liquor With FI-HG-AAS

目的研究流动注射氢化物发生原子吸收光谱法测定铅的最佳条件。方法将酒中铅以铁氰化钾氧化、硼氢化钾还原生成铅化氢,用原子分光光度计检测。结果本实验选择载气流量为150mL/min,硼氢化钾浓度为1.5%,介质0.3%NaOH,氧化时间为25℃,20min(夏季氧化时间可缩短为10min),0.5%盐酸溶液作为样品和标准溶液的稀释介质调节酸度。本法检出限为0.20μg/L,相对标准偏差3.0%～6.1%,回收率范围96.2%～103.8%,平均回收率为100.1%。结论本方法简便、重现性好、准确度高、灵敏度好,能满足国家标准的要求。

Objective To study the best conditions for determining lead with FI-HG-AAS （flow injection-hydride generation-atomic absorption spectrometry）. Methods After liquor lead is oxided with potassium ferrocyanide and deoxidized with potassium borohydride into lead of hydrogen, then detected by atomic spectrophotometer. Results This experiment was done under the flow rate of carrier gas： 150mL / min, KBH4 concentration of 1.5 %, medium 0. 3 % NaOH, oxidation time for the 25 ℃, 20 min （ the time could be shortened to 10 min in summer） , 0. 5 % hydrochloric acid as samples and the standard solution acidity of diluting medium. The method of detection limit： 0. 20 μg/L, the relative standard deviation ： 3.0% to 6. 1%, percent recovery： 103.8 % to 96.2 %, and the average recovery ： 100. 1%. Conclusion The method is simple, reproducible, high accuracy, sensitivity, and satisfied with national standards.