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功能化树脂的合成及其在在线系统中的应用,用于火焰原子吸收光谱法测定食品中的铜预富集。

Synthesis and application of a functionalized resin in on-line system for copper preconcentration and determination in foods by flame atomic absorption spectrometry.

机构信息

Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, BA 45200-000, Brazil.

出版信息

Talanta. 2003 Dec 4;61(5):675-82. doi: 10.1016/S0039-9140(03)00328-X.

Abstract

An on-line system for preconcentration and determination of copper at mug l(-1) level by flame atomic absorption spectrometry (FAAS) is proposed. Amberlite XAD-2 functionalized with 3,4-dihydroxybenzoic acid packed in a minicolumn was used as sorbent. Copper(II) ions were sorbed in the minicolumn, from which it could be eluted by hydrochloric acid solution directly to the nebulizer-burner system of the FAAS. Eluent solution was carried by water at a flow rate of 5.00 ml min(-1). Signals were measured as peak height by using an instrument software. Achieved sampling rate was 27 samples per hour. Analytical parameters were evaluated and the results demonstrated that copper can be determined, with acetate buffer to adjust the sample pH at 6.0, preconcentration time of 120 s and a sample flow rate of 6.50 ml min(-1). The desorption was carried out with 30 mul of a 1.0 mol l(-1) hydrochloric acid solution. An enrichment factor of 33 in 13.00 ml of sample (120 s preconcentration time) was achieved by using the time-based technique. The detection limit (DL) (3 s) was 0.27 mug l(-1) and the precision (assessed as the relative standard deviation) reached values of 5.7-1.1% in copper solutions of 5.00 to 50.00 mug l(-1) concentration, respectively. The accuracy of procedure was confirmed by copper determination in certified reference materials. Recoveries of spike additions (1.0 or 2.0 mug g(-1)) to food samples were quantitative (90.0-110.0%). These results proved also that the procedure is not affected by matrix interference and can be applied satisfactorily for copper determination in rice flour and starch samples.

摘要

提出了一种在线预富集火焰原子吸收光谱法测定痕量铜的新方法。采用 3,4-二羟基苯甲酸功能化的 Amberlite XAD-2 作为吸附剂,将其填充在 minicolumn 中。铜(II)离子被吸附在 minicolumn 中,然后可以用盐酸溶液直接洗脱到 FAAS 的雾化器-燃烧器系统中。洗脱液以 5.00ml/min 的流速输送。通过仪器软件测量峰高作为信号。实现的采样率为每小时 27 个样品。评估了分析参数,结果表明,在 pH 值为 6.0 的醋酸盐缓冲液中,可以在 120s 的预浓缩时间和 6.50ml/min 的样品流速下测定铜。用 30μl 1.0mol/L 盐酸溶液进行洗脱。采用基于时间的技术,在 13.00ml 样品(120s 预浓缩时间)中实现了 33 倍的富集因子。(3s)的检测限为 0.27μg/L,在 5.00-50.00μg/L 浓度范围内,铜溶液的精密度(以相对标准偏差表示)分别达到 5.7-1.1%。通过对食品中铜的测定,验证了该程序的准确性。对食品样品进行(1.0 或 2.0μg/g)的加标回收率均为定量(90.0-110.0%)。这些结果还表明,该方法不受基质干扰的影响,可以满意地应用于米粉和淀粉样品中铜的测定。

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