机构地区: 宁波大学材料科学与化学工程学院宁波市新型功能材料及其制备科学国家重点实验室培育基地
出 处: 《分析科学学报》 2010年第2期183-186,共4页
摘 要: 建立了固相萃取-石墨炉原子吸收光谱法测定铝合金中铍的方法。利用偶氮砷酸类试剂7-(2′-胂酸基-5′-羧酸)苯偶氮-8-羟基喹啉-5-磺酸(H2L)与Be2+形成螯合物,该螯合物可用C18固相萃取柱富集,而Al3+则不被保留。采用石墨炉原子吸收光谱法(GF-AAS)测定C18柱洗脱液中的Be2+的螯合物,从而实现铝合金中铍的分离检测。最佳实验条件为:采用pH=3.0的5%H2L水溶液螯合Be2+,水相上柱,用2mL体积比为50%的甲醇/水溶液作为洗脱液。结果表明:经过C18柱固相萃取可以去除Al3+的干扰,Be2+的测定范围为0.05~16μg/L,检出限为0.025μg/L,加标回收率为92%~108%。应用该法于铝合金标样中铍的测定,结果与认定值相符。 A new method for the determination of beryllium in aluminum alloy sample was established by pre-extraction with 7-(2'-Arsenazo acid-5'-carboxylic acid) phenylazo-8-hydroxyl-quinoline-5-sulfonic acid(H2L) and determination with graphite furnace-atomic absorption spectrometry. H2L was chosen as the extraction agent to separate Al3+ and Be2+. C18-solid phase extraction was employed for the separation and enrichment of beryllium in alloy samples. The optimum experimental conditions were as following,5.0% H2L(pH=3.0),flow rate of 1.5 mL/min. elution with 2.0 mL 50% (V/V) methanol/water solution. The linear range of the method was 0.05~16 μg/L,the recovery was between 92%~108% and the detection limit was 0.025 μg/L. The method has been applied to the determination of beryllium in certified reference material and the results obtained were in good agreement with certified values,giving the RSD of 2.3%(n=5).