Carneiro M C, Campos R C, Curtius A J
Departamento de Química, Pontifícia Universidade Católica do Rio de Janeiro, 22453-900, Rio de Janeiro, RJ, Brazil.
Talanta. 1993 Dec;40(12):1815-22. doi: 10.1016/0039-9140(93)80101-v.
A microdigestion procedure performed directly in the autosampler cup is proposed. Small quartz filter pieces loaded with the particulate material are transferred to the cup. The sample is digested by a mixture of nitric, sulfuric and hydrofluoric acid (1:1:1) under sonication. After the addition of a boric acid solution the elements are determined by graphite furnace atomic absorption spectrometry using the autosampler to deliver the slurry into the furnace. A mixture of palladium and magnesium nitrates was used as a modifier for Sb. Spiking studies showed recoveries close to 100% using aqueous analytical curves for Ni and Sb. For V, an analytical curve in the blank slurry, obtained by submitting an unloaded filter to the same procedure, was used. The method was applied to two standard reference materials, Coal Fly Ash (NIST 1633a) and Urban Particulate (NIST 1648) and the concentrations showed good agreement with the certified or recommended values using aqueous analytical solutions.
本文提出了一种直接在自动进样器杯中进行的微量消解方法。将装载有颗粒物质的小石英滤片转移至杯中。样品在超声作用下用硝酸、硫酸和氢氟酸（1:1:1）的混合液进行消解。加入硼酸溶液后，使用自动进样器将浆液输送至石墨炉中，通过石墨炉原子吸收光谱法测定元素。钯和硝酸镁的混合物用作锑的基体改进剂。加标研究表明，使用镍和锑的水溶液分析曲线时回收率接近100%。对于钒，使用通过将未装载滤片进行相同程序获得的空白浆液中的分析曲线。该方法应用于两种标准参考物质，煤飞灰（NIST 1633a）和城市颗粒物（NIST 1648），使用水溶液分析溶液时，测定浓度与认证值或推荐值显示出良好的一致性。
