da Silva José Bento Borba, Borges Daniel Lázaro Gallindo, da Veiga Márcia Andréia Mesquita Silva, Curtius Adilson José, Welz Bernhard
Departamento de Química, Universidade Federal de Minas Gerais, Belo Horizonte, MG, Brazil.
Talanta. 2003 Jul 27;60(5):977-82. doi: 10.1016/S0039-9140(03)00182-6.
The feasibility of Ru as a permanent modifier for the determination of Cd in biological samples treated with tetramethylammonium hydroxide (TMAH) by ET AAS was investigated. The tube treatment with Ru was carried out only once and lasted for about 300 atomization cycles. The pyrolysis and atomization temperatures, 750 degrees C and 1300 degrees C, respectively, were chosen from the temperature curves. The sample dissolution procedure was very simple: a sample aliquot was mixed with a small volume of a 25% m/v TMAH solution, the volume was made up to 50 ml and the mixture was kept at 60 degrees C for 1 h. Six certified biological reference materials were analyzed and the obtained Cd concentrations are within the 95% confidence interval of the certified values, proving the accuracy of the proposed procedure for a variety of biological samples. The calibration curve, with correlation coefficient higher than 0.99, was established for a working range up to 10 microg l(-1). The precision was good as demonstrated by relative standard deviations below 3%, except for one sample. The limit of detection (3sigma) was 0.05 microg l(-1) and the characteristic mass was 1.30 pg, obtained in the presence of the Ru modifier.
研究了钌作为永久性改性剂,通过电热原子吸收光谱法(ET AAS)测定用氢氧化四甲铵(TMAH)处理的生物样品中镉的可行性。用钌进行的管处理仅进行一次,持续约300个原子化循环。从温度曲线中分别选择750℃和1300℃的热解温度和原子化温度。样品溶解过程非常简单:取一份样品与少量25%(m/v)的TMAH溶液混合,定容至50 ml,混合物在60℃下保持1 h。分析了六种有证生物参考物质,所得镉浓度在认证值的95%置信区间内,证明了该方法对各种生物样品的准确性。建立了相关系数高于0.99的校准曲线,工作范围高达10 μg l⁻¹。除一个样品外,相对标准偏差低于3%表明精密度良好。在钌改性剂存在下,检测限(3σ)为0.05 μg l⁻¹,特征质量为1.30 pg。