Analytical Chemistry Division, Chemistry Department, Lomonosov Moscow State University, Vorob'evy Gory, GSP-2, house 1, structure 3, 119992 Moscow, Russia.
Talanta. 2003 Nov 4;61(3):315-29. doi: 10.1016/S0039-9140(03)00271-6.
A simple method for the elements preconcentration on thin-layer paraffin-treated cellulose filters was proposed. It was found that pyrrolydinedithiocarbamates of As(III), Bi, Cd, Co, Cu, Fe(III), Ni, Pb, Se(IV), V(V) and Zn obtained after mixing of sample (3-5 ml min(-1)) and reagent (0.7-1.0 ml min(-1)) streams were quantitatively recovered from 100 ml sample. The sample acidity was adjusted to pH 4.8-5.2 for preconcentration of Cd, Co, Cu, Fe(III), Ni, Pb, V(V) and Zn, and to 2 M HCl for preconcentration of As, Bi and Se. The optimum reagent concentration was found to be 0.1%. The elements were determined on the filters by X-ray fluorescence spectrometry. The detection limits achieved were 0.1-4.0 mug of element on the filter. Relative standard deviation (R.S.D.) was not higher than 0.08 while determining 5-50 mug of elements on filter. Accuracy and precision of the technique proposed were evaluated by the analysis of spiked natural samples.
提出了一种在薄层石蜡处理纤维素滤纸上预富集元素的简单方法。研究发现，将样品（3-5ml/min）和试剂（0.7-1.0ml/min）混合后，形成的 As(III)、Bi、Cd、Co、Cu、Fe(III)、Ni、Pb、Se(IV)、V(V)和 Zn 的吡咯二硫代氨基甲酸盐可以从 100ml 样品中定量回收。为了预富集 Cd、Co、Cu、Fe(III)、Ni、Pb、V(V)和 Zn，将样品酸度调节至 pH 4.8-5.2，而为了预富集 As、Bi 和 Se，则需要调节至 2M HCl。发现最佳试剂浓度为 0.1%。通过 X 射线荧光光谱法在滤纸上测定这些元素。在滤纸上测定元素的检出限为 0.1-4.0μg。当在滤纸上测定 5-50μg 的元素时，相对标准偏差（R.S.D.）不高于 0.08。通过对加标天然样品的分析，评估了所提出技术的准确性和精密度。
