CAJ | 학술논문

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(H_2L)与Be~(2+)形成螯合物,该螯合物可用C18固相萃取柱富集,而Al~(3+)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Be~(2+)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%H_2L水溶液螯合Be~(2+),水相上柱,用2 mL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Al~(3+)的干扰,Be~(2+)的测定范围为0.05～16 μg/L,检出限为0.025 μg/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.
건립료고상췌취-석묵로원자흡수광보법측정려합금중피적방법.이용우담신산류시제7-(2′-신산기-5′-최산)분우담-8-간기규람-5-광산(H_2L)여Be~(2+)형성오합물,해오합물가용C18고상췌취주부집,이Al~(3+)칙불피보류.채용석묵로원자흡수광보법(GF-AAS)측정C18주세탈액중적Be~(2+)적오합물,종이실현려합금중피적분리검측.최가실험조건위:채용pH=3.0적5%H_2L수용액오합Be~(2+),수상상주,용2 mL체적비위50%적갑순/수용액작위세탈액.결과표명:경과C18주고상췌취가이거제Al~(3+)적간우,Be~(2+)적측정범위위0.05～16 μg/L,검출한위0.025 μg/L,가표회수솔위92%～108%.응용해법우려합금표양중피적측정,결과여인정치상부.
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(H_2L) and determination with graphite furnace-atomic absorption spectrometry. H_2L was chosen as the extraction agent to separate Al~(3+) and Be~(2+). 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% H_2L(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).