氯化钯作基体改进剂石墨炉原子吸收光谱法测定土壤中的铍
Determination of Beryllium in Soils by Graphite Furnace Atomic Absorption Spectrometry with Palladium Chloride as a Matrix Modifier
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摘要: 铍是一种对人体有害的金属元素,土壤中铍的测定目前尚无国家标准方法。本文采用盐酸-硝酸-氢氟酸体系微波消解、石墨炉原子吸收光谱法测定土壤样品中的铍,实验了钯、硝酸铝、硝酸镁、钙盐的增敏效果。结果表明,以氯化钯为基体改进剂,灰化温度和原子化温度分别提高到1100 ℃和2650 ℃,原子化峰形尖锐,背景吸收很小,提高了测定灵敏度;其他三种基体改进剂虽然也能提高测定灵敏度,但背景吸收较大。采用优化的实验条件,Fe、Mg、K、Na、Ca、Ti、Cu、Ba、Mn、Zn、Pb、Sr等共存元素对测定不产生干扰。铍的浓度在0~4.00 μg/L范围内线性良好,方法检出限为0.01 μg/g,精密度(RSD,n=6)为3.5%~6.7%,实际土壤样品的加标回收率为84.0%~113.0%,土壤国家标准物质的测定值在标准值的误差范围内。本法与萃取光度法、电感耦合等离子体发射光谱/质谱法相比,操作简便,分析成本较低。Abstract: Beryllium is a harmful metal element and there is no national standard method for its determination in soils. A method system was established for the determination of Beryllium in soils by Graphite Furnace Atomic Absorption Spectrometry (GFAAS) with hydrochloric acid-nitric acid-hydrofluoric as microwave digestion. The sensitizing effects of palladium, aluminum nitrate, magnesium nitrate and calcium salt were investigated. The results showed that atomic shape was sharp, background absorption was small and sensitivity was improved with palladium chloride as the matrix modifier when the ashing temperature and atomization temperature were increased to 1100℃ and 2650℃, respectively. The other 3 modifiers improved sensitivity but background absorptions were larger. The conditions of experiment were optimized and the coexisting elements Fe, Mg, K, Na, Ca, Ti, Cu, Ba, Mn, Zn, Pb and Sr had no interference. The results showed that good linearity ranged from 0 μg/L to 4.00 μg/L, detection limit was 0.01 μg/g (sampling quality was 0.2000 g and constant volume was 50 mL), RSD of standard samples were from 3.5% to 6.7%, and spiked recoveries of the actual soil sample were from 84.0% to 113.0%. The result of national standard material was in the range of certified values. Compared with extraction spectrophotometric method, Inductively Coupled Plasma-Atomic Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry, this method is simple and inexpensive.
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