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在用高效液相色谱测定金(Ⅰ)氰化物的方法中,样品在线预富集在C_18柱上进行,用离子相互作用色谱解吸,采用的流动相为含有5mM的四丁基铵离子,乙腈与水之比为32:68,然后在214nm波长下用紫外吸收法进行测定。样品预富集是将样品通过上述流动相处理过的C_18的前置柱,从前置柱的离子吸附容量和校正曲线的线性范围的角度讨论了离子相互作用剂的选择。在最佳条件下,观察到样品达到3mL时,氰亚金酸盐能定量地吸附在柱上,其检测限为0.43ppb金。当金的含量在10ppb时,方法的精密度为0.9％相对标准偏差。所拟的色谱条件适合于在高浓度的游离氰离子存在下,同时测定超痕量的Au(Ⅰ),Pd(Ⅱ)和Pt(Ⅱ)的氰络合物。
In the method for the determination of gold (I) cyanide by high performance liquid chromatography, samples were preconcentrated on a C 18 column and desorbed by ion-exchange chromatography using a mobile phase containing tetrabutylammonium ion (5 mM), acetonitrile Water ratio of 32:68, and then measured by UV absorption at 214 nm. Sample pre-enrichment is the pre-column of C_18 treated with the above mobile phase. The choice of ionic interaction agent is discussed in terms of the ion adsorption capacity of the pre-column and the linear range of the calibration curve. Under optimal conditions, when the sample reached 3 mL, the adsorption of cyanate on the column was quantified with a detection limit of 0.43 ppb gold. When the gold content is 10 ppb, the precision of the method is 0.9% relative standard deviation. The proposed chromatographic conditions are suitable for simultaneous determination of ultra-trace amount of cyanide complexes of Au (Ⅰ), Pd (Ⅱ) and Pt (Ⅱ) in the presence of high concentration of free cyanide ions.